Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-52-735-5271' _publ_contact_author_fax '+81-52-735-5488' _publ_contact_author_email 'inai@mse.nitech.ac.jp' loop_ _publ_author_name 'Yoshihito Inai, Tatsuo Oshikawa, Mitsuji Yamashita, Tadamichi Hirabayashi, and Yuji Kurokawa' data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Yoshihito Inai' 'Tatsuo Oshikawa' 'Mitsuji Yamashita' 'Tadamichi Hirabayashi' 'Yuji Kurokawa' _publ_contact_author_name 'Dr Yoshihito Inai' _publ_contact_author_address ; Dr Yoshihito Inai Department of Environmental Technology and Urban Planning Graduate School of Engineering Nagoya Institute of Technology Gokiso-cho Showa-ku Nagoya 466-8555 JAPAN ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-52-735-5271' _publ_contact_author_fax '+81-52-735-5488' _publ_contact_author_email 'inai@mse.nitech.ac.jp' _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation.(1995).teXsan. Single Crystal Structure Analysis Software.Version 1.7. MSC,3200 Research Forest Drive,The Woodlands,TX 77381,USA. ; data_(peptide 1: Boc-(Aib-\d^Z^Phe)~2~-Aib-OMe) _database_code_CSD 157037 #--------------------------------------------------------------------------- #-- _audit_creation_date 'Fri Oct 14 15:34:38 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 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ' Synthesis by Inai, et al.' _chemical_name_common ' Boc-(Aib-\d^Z^Phe)~2~-Aib-OMe ' _chemical_formula_weight 723.86 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H53 N5 O9 ' _chemical_formula_moiety 'C38 H53 N5 O9 ' _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _cell_length_a 10.812(2) _cell_length_b 19.228(4) _cell_length_c 19.324(3) _cell_angle_alpha 90 _cell_angle_beta 101.98(1) _cell_angle_gamma 90 _cell_volume 3929(1) _cell_formula_units_Z 4 _cell_measurement_temperature 223.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 25.4 _cell_measurement_theta_max 29.6 #--------------------------------------------------------------------------- #-- _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 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1552.00 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 223.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\ a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_%- 4.15 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 1 2 -1 2 2 0 2 _diffrn_reflns_number 6321 _reflns_number_total 5964 _reflns_number_observed 3124 _reflns_observed_criterion '>2.0sigma(I)' _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.068 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 59.62 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05781 _diffrn_orient_matrix_UB_12 0.00653 _diffrn_orient_matrix_UB_13 0.04714 _diffrn_orient_matrix_UB_21 -0.01761 _diffrn_orient_matrix_UB_22 -0.04872 _diffrn_orient_matrix_UB_23 0.01329 _diffrn_orient_matrix_UB_31 0.07271 _diffrn_orient_matrix_UB_32 -0.01699 _diffrn_orient_matrix_UB_33 -0.01999 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 152 0.018 0.009 ;International Tables for Crystallography (1992,Vol.C,Tables 4.2.6.8 and 6.1.1.4) ; H 0 212 0.000 0.000 ;International Tables for Crystallography (1992,Vol.C,Table 6.1.1.4) ; N 0 20 0.031 0.018 ;International Tables for Crystallography (1992,Vol.C,Tables 4.2.6.8 and 6.1.1.4) ; O 0 36 0.049 0.032 ;International Tables for Crystallography (1992,Vol.C,Tables 4.2.6.8 and 6.1.1.4) ; #--------------------------------------------------------------------------- #-- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags O(1) 1.0493(3) 0.2700(2) 0.2292(2) 0.0529(8) Uani d . 1.00 . O(2) 1.2281(3) 0.3026(2) 0.3994(2) 0.0610(9) Uani d . 1.00 . O(3) 1.2639(3) 0.1182(2) 0.2212(2) 0.0617(9) Uani d . 1.00 . O(4) 1.3025(3) 0.2094(2) -0.0155(2) 0.0622(9) Uani d . 1.00 . O(5) 1.1644(3) 0.3077(2) 0.5048(2) 0.0634(9) Uani d . 1.00 . O(8) 1.4745(3) 0.2434(2) 0.1614(2) 0.072(1) Uani d . 1.00 . O(9) 0.9084(4) 0.1676(2) 0.4390(2) 0.080(1) Uani d . 1.00 . O(10) 1.3190(6) 0.0450(3) -0.0693(2) 0.123(2) Uani d . 1.00 . O(11) 1.1337(6) 0.0734(3) -0.0486(2) 0.111(2) Uani d . 1.00 . N(1) 1.0434(4) 0.1930(2) 0.3182(2) 0.0465(9) Uani d . 1.00 . N(2) 1.2925(4) 0.2114(2) 0.2953(2) 0.0494(10) Uani d . 1.00 . N(3) 1.0200(4) 0.3080(2) 0.4051(2) 0.0507(10) Uani d . 1.00 . N(4) 1.2681(4) 0.2623(2) 0.1576(2) 0.0497(10) Uani d . 1.00 . N(5) 1.2607(4) 0.1425(2) 0.0740(2) 0.054(1) Uani d . 1.00 . C(1) 1.2266(4) 0.1557(3) 0.2659(2) 0.050(1) Uani d . 1.00 . C(2) 1.1455(5) 0.3060(2) 0.4339(2) 0.049(1) Uani d . 1.00 . C(3) 1.2413(5) 0.2674(2) 0.0823(2) 0.049(1) Uani d . 1.00 . C(4) 1.0264(4) 0.2580(2) 0.2877(2) 0.045(1) Uani d . 1.00 . C(6) 0.9598(5) 0.0358(2) 0.3001(2) 0.051(1) Uani d . 1.00 . C(7) 1.0691(5) 0.0714(3) 0.2823(3) 0.052(1) Uani d . 1.00 . C(8) 1.2728(5) 0.2039(2) 0.0437(2) 0.053(1) Uani d . 1.00 . C(9) 1.4085(4) 0.2348(3) 0.2731(2) 0.056(1) Uani d . 1.00 . C(10) 1.1658(5) 0.3944(2) 0.0685(3) 0.053(1) Uani d . 1.00 . C(11) 1.1942(5) 0.3239(3) 0.0450(3) 0.054(1) Uani d . 1.00 . C(12) 0.8281(5) 0.3026(3) 0.3147(3) 0.058(1) Uani d . 1.00 . C(13) 0.8435(5) 0.0665(3) 0.3033(3) 0.063(1) Uani d . 1.00 . C(14) 1.3868(5) 0.2455(3) 0.1931(3) 0.053(1) Uani d . 1.00 . C(16) 1.0016(7) 0.3869(3) 0.3032(3) 0.064(1) Uani d . 1.00 . C(17) 0.9742(5) -0.0371(3) 0.3133(3) 0.063(1) Uani d . 1.00 . C(18) 1.2917(5) 0.2984(3) 0.5503(3) 0.063(1) Uani d . 1.00 . C(19) 1.3055(6) 0.0764(3) 0.0491(3) 0.062(1) Uani d . 1.00 . C(20) 1.1370(5) 0.4108(3) 0.1336(3) 0.060(1) Uani d . 1.00 . C(21) 1.1179(6) 0.4792(3) 0.1512(3) 0.070(2) Uani d . 1.00 . C(22) 0.7471(6) 0.0274(4) 0.3206(3) 0.074(2) Uani d . 1.00 . C(23) 1.1252(6) 0.5330(3) 0.1048(4) 0.074(2) Uani d . 1.00 . C(24) 1.1711(6) 0.4485(3) 0.0208(3) 0.068(1) Uani d . 1.00 . C(25) 0.8752(6) -0.0757(3) 0.3308(3) 0.071(2) Uani d . 1.00 . C(26) 1.3810(7) 0.3553(4) 0.5359(4) 0.084(2) Uani d . 1.00 . C(27) 1.5176(6) 0.1826(4) 0.2967(4) 0.076(2) Uani d . 1.00 . C(28) 0.7618(7) -0.0433(4) 0.3351(3) 0.078(2) Uani d . 1.00 . C(29) 1.4431(7) 0.3070(4) 0.3074(4) 0.075(2) Uani d . 1.00 . C(30) 1.1513(6) 0.5172(3) 0.0392(4) 0.079(2) Uani d . 1.00 . C(31) 1.253(1) 0.0164(4) 0.0878(4) 0.086(2) Uani d . 1.00 . C(32) 1.4499(7) 0.0751(4) 0.0656(4) 0.089(2) Uani d . 1.00 . C(33) 1.2546(9) 0.0668(3) -0.0288(3) 0.091(2) Uani d . 1.00 . C(34) 0.9811(7) 0.1349(4) 0.4992(4) 0.092(2) Uani d . 1.00 . C(35) 1.2633(9) 0.3057(8) 0.6236(4) 0.111(3) Uani d . 1.00 . C(36) 1.3389(7) 0.2251(4) 0.5404(5) 0.095(2) Uani d . 1.00 . C(37) 1.114(1) 0.0387(6) -0.1273(5) 0.29(1) Uani d . 1.00 . C(38) 1.061(1) 0.0842(6) 0.4786(5) 0.171(5) Uani d . 1.00 . C(40) 0.9721(4) 0.3152(2) 0.3292(2) 0.047(1) Uani d . 1.00 . C(41) 1.1039(4) 0.1386(2) 0.2876(2) 0.047(1) Uani d . 1.00 . H(1) 1.112(5) 0.579(3) 0.119(3) 0.0781(2) Uiso calc . 1.00 . H(2) 1.09(1) 0.0745(9) -0.1625(5) 0.2685 Uiso calc . 1.00 . H(5) 1.491(6) 0.029(3) 0.059(3) 0.0904(2) Uiso calc . 1.00 . H(6) 1.495(7) 0.116(4) 0.044(4) 0.1339(4) Uiso calc . 1.00 . H(7) 1.482(6) 0.075(3) 0.122(4) 0.1115(3) Uiso calc . 1.00 . H(8) 0.888(5) -0.126(3) 0.342(3) 0.0755(2) Uiso calc . 1.00 . H(13) 1.404(6) 0.343(3) 0.488(4) 0.0912(2) Uiso calc . 1.00 . H(14) 1.326(7) 0.405(4) 0.543(4) 0.1194(3) Uiso calc . 1.00 . H(15) 1.183(6) 0.435(3) -0.029(3) 0.0991(3) Uiso calc . 1.00 . H(16) 1.151(6) 0.551(3) 0.006(3) 0.0872(2) Uiso calc . 1.00 . H(17) 1.100(6) 0.494(3) 0.199(3) 0.0908(2) Uiso calc . 1.00 . H(18) 1.122(6) 0.373(3) 0.169(3) 0.1008(3) Uiso calc . 1.00 . H(19) 1.177(4) 0.317(2) -0.009(3) 0.0526(2) Uiso calc . 1.00 . H(20) 1.292(6) -0.027(4) 0.073(3) 0.0942(3) Uiso calc . 1.00 . H(21) 1.176(5) 0.021(3) 0.076(3) 0.0537(3) Uiso calc . 1.00 . H(22) 1.294(6) 0.024(3) 0.140(4) 0.0891(2) Uiso calc . 1.00 . H(23) 1.249(4) 0.139(2) 0.121(3) 0.0517(2) Uiso calc . 1.00 . H(24) 1.205(5) 0.265(2) 0.183(3) 0.0573(2) Uiso calc . 1.00 . H(25) 1.513(6) 0.326(3) 0.286(3) 0.0805(2) Uiso calc . 1.00 . H(26) 1.465(6) 0.300(3) 0.363(4) 0.1105(3) Uiso calc . 1.00 . H(27) 1.369(6) 0.346(3) 0.292(3) 0.0929(3) Uiso calc . 1.00 . H(28) 1.254(5) 0.238(3) 0.333(3) 0.0722(2) Uiso calc . 1.00 . H(29) 1.549(6) 0.181(4) 0.351(4) 0.1126(3) Uiso calc . 1.00 . H(30) 1.486(5) 0.130(3) 0.274(3) 0.0844(2) Uiso calc . 1.00 . H(31) 1.586(6) 0.196(3) 0.275(3) 0.0973(3) Uiso calc . 1.00 . H(32) 1.015(6) 0.188(3) 0.364(3) 0.1063(3) Uiso calc . 1.00 . H(33) 1.130(5) 0.036(3) 0.260(3) 0.0781(2) Uiso calc . 1.00 . H(34) 0.826(5) 0.118(3) 0.291(3) 0.0894(2) Uiso calc . 1.00 . H(35) 0.665(5) 0.053(3) 0.328(3) 0.0726(2) Uiso calc . 1.00 . H(36) 0.702(6) -0.071(3) 0.351(3) 0.0826(2) Uiso calc . 1.00 . H(37) 1.067(6) -0.063(3) 0.302(3) 0.1007(2) Uiso calc . 1.00 . H(38) 0.922(7) 0.115(4) 0.540(4) 0.1221(3) Uiso calc . 1.00 . H(40) 1.092(7) 0.392(3) 0.307(3) 0.0928(3) Uiso calc . 1.00 . H(41) 0.963(5) 0.391(2) 0.251(3) 0.0607(2) Uiso calc . 1.00 . H(42) 0.962(5) 0.421(3) 0.328(3) 0.0626(2) Uiso calc . 1.00 . H(43) 0.794(5) 0.306(3) 0.261(3) 0.0807(2) Uiso calc . 1.00 . H(44) 0.799(5) 0.256(3) 0.336(3) 0.0885(2) Uiso calc . 1.00 . H(45) 0.793(5) 0.336(3) 0.343(3) 0.0693(2) Uiso calc . 1.00 . H(46) 0.972(5) 0.311(3) 0.439(3) 0.0743(2) Uiso calc . 1.00 . H(47) 1.462(8) 0.353(4) 0.571(4) 0.1262(3) Uiso calc . 1.00 . H(48) 1.236(8) 0.348(4) 0.631(4) 0.1168(5) Uiso calc . 1.00 . H(49) 1.333(6) 0.302(3) 0.656(4) 0.0836(2) Uiso calc . 1.00 . H(50) 1.19(1) 0.279(5) 0.631(5) 0.1601(5) Uiso calc . 1.00 . H(51) 1.428(8) 0.206(4) 0.582(4) 0.1447(4) Uiso calc . 1.00 . H(53) 1.366(6) 0.226(3) 0.497(3) 0.0805(3) Uiso calc . 1.00 . H(54) 1.190(3) 0.015(5) -0.132(2) 0.2685 Uiso calc . 1.00 . H(56) 1.110(5) 0.105(1) 0.448(3) 0.1875 Uiso calc . 1.00 . H(57) 1.03(1) 0.172(6) 0.545(6) 0.2142(6) Uiso calc . 1.00 . H(58) 1.046(6) 0.006(4) -0.133(2) 0.2685 Uiso calc . 1.00 . H(59) 1.011(1) 0.047(2) 0.455(3) 0.1875 Uiso calc . 1.00 . H(60) 1.118(4) 0.066(3) 0.5199(6) 0.1875 Uiso calc . 1.00 . 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) 0.065(2) 0.043(2) 0.003(2) 0.014(1) 0.005(1) O(2) 0.051(2) 0.080(2) 0.054(2) -0.005(2) 0.016(2) -0.008(2) O(3) 0.071(2) 0.060(2) 0.062(2) 0.006(2) 0.032(2) 0.002(2) O(4) 0.081(2) 0.060(2) 0.054(2) 0.011(2) 0.033(2) 0.002(2) O(5) 0.049(2) 0.094(3) 0.044(2) 0.005(2) 0.003(1) -0.001(2) O(8) 0.055(2) 0.097(3) 0.070(2) 0.004(2) 0.030(2) 0.005(2) O(9) 0.107(3) 0.075(3) 0.062(2) 0.001(2) 0.028(2) 0.006(2) O(10) 0.207(6) 0.103(4) 0.060(3) 0.079(4) 0.030(3) -0.001(2) O(11) 0.109(4) 0.152(5) 0.074(3) -0.043(4) 0.021(3) -0.008(3) N(1) 0.049(2) 0.048(2) 0.045(2) 0.000(2) 0.015(2) -0.001(2) N(2) 0.045(2) 0.058(2) 0.046(2) -0.007(2) 0.013(2) 0.001(2) N(3) 0.043(2) 0.068(3) 0.040(2) 0.002(2) 0.007(2) -0.005(2) N(4) 0.057(3) 0.056(2) 0.041(2) 0.006(2) 0.020(2) 0.002(2) N(5) 0.072(3) 0.043(2) 0.051(2) 0.006(2) 0.025(2) 0.000(2) C(1) 0.049(3) 0.059(3) 0.043(3) 0.007(2) 0.015(2) 0.007(2) C(2) 0.052(3) 0.054(3) 0.041(3) 0.001(2) 0.009(2) -0.002(2) C(3) 0.054(3) 0.046(3) 0.052(3) 0.008(2) 0.023(2) -0.002(2) C(4) 0.039(3) 0.053(3) 0.043(3) -0.001(2) 0.007(2) -0.001(2) C(6) 0.056(3) 0.051(3) 0.047(3) -0.007(2) 0.009(2) -0.001(2) C(7) 0.053(3) 0.052(3) 0.055(3) -0.004(2) 0.018(2) -0.001(2) C(8) 0.058(3) 0.053(3) 0.051(3) 0.010(2) 0.022(2) 0.004(2) C(9) 0.047(3) 0.071(3) 0.051(3) -0.005(2) 0.014(2) 0.003(2) C(10) 0.058(3) 0.047(3) 0.056(3) 0.006(2) 0.017(2) 0.000(2) C(11) 0.064(3) 0.053(3) 0.048(3) 0.006(2) 0.020(2) 0.002(2) C(12) 0.043(3) 0.077(4) 0.053(3) 0.005(3) 0.006(2) -0.006(3) C(13) 0.053(3) 0.059(4) 0.075(4) -0.002(3) 0.012(3) 0.003(3) C(14) 0.048(3) 0.060(3) 0.053(3) 0.003(2) 0.016(2) 0.004(2) C(16) 0.072(4) 0.056(3) 0.066(4) 0.003(3) 0.019(3) 0.001(3) C(17) 0.068(4) 0.053(3) 0.067(3) -0.015(3) 0.013(3) -0.005(2) C(18) 0.043(3) 0.082(4) 0.057(3) 0.002(3) -0.004(2) 0.001(3) C(19) 0.090(4) 0.046(3) 0.054(3) 0.005(3) 0.027(3) -0.004(2) C(20) 0.071(4) 0.047(3) 0.068(3) 0.008(3) 0.024(3) -0.005(3) C(21) 0.079(4) 0.060(4) 0.074(4) 0.005(3) 0.019(3) -0.009(3) C(22) 0.056(4) 0.086(5) 0.077(4) -0.015(3) 0.012(3) -0.002(3) C(23) 0.074(4) 0.052(4) 0.093(5) 0.003(3) 0.011(3) -0.015(3) C(24) 0.082(4) 0.056(3) 0.067(4) 0.010(3) 0.018(3) 0.011(3) C(25) 0.085(5) 0.059(4) 0.068(4) -0.017(3) 0.010(3) 0.001(3) C(26) 0.074(4) 0.098(5) 0.072(4) -0.018(4) -0.002(4) -0.005(4) C(27) 0.053(4) 0.098(5) 0.078(4) 0.015(3) 0.013(3) 0.024(4) C(28) 0.085(5) 0.082(5) 0.065(4) -0.033(4) 0.012(3) 0.003(3) C(29) 0.071(4) 0.088(4) 0.070(4) -0.028(4) 0.028(3) -0.014(3) C(30) 0.095(5) 0.053(4) 0.089(5) 0.009(3) 0.023(4) 0.014(3) C(31) 0.134(8) 0.058(4) 0.069(5) 0.001(5) 0.029(5) 0.003(3) C(32) 0.082(5) 0.089(5) 0.099(6) 0.040(4) 0.027(4) 0.007(4) C(33) 0.156(7) 0.058(4) 0.064(4) -0.016(4) 0.033(5) 0.002(3) C(34) 0.087(5) 0.113(5) 0.078(4) 0.026(4) 0.023(4) 0.006(4) C(35) 0.070(5) 0.20(1) 0.051(4) 0.010(7) -0.006(4) 0.005(5) C(36) 0.087(5) 0.081(5) 0.111(6) 0.026(4) 0.003(5) 0.009(4) C(37) 0.49(3) 0.19(1) 0.105(7) -0.20(1) -0.15(1) 0.072(7) C(38) 0.20(1) 0.22(1) 0.095(6) 0.090(9) 0.023(6) 0.008(6) C(40) 0.040(3) 0.059(3) 0.040(2) 0.000(2) 0.005(2) 0.002(2) C(41) 0.047(3) 0.053(3) 0.045(2) 0.000(2) 0.018(2) -0.001(2) #--------------------------------------------------------------------------- #-- _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ ' _refine_ls_number_reflns 3124 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_obs 0.0731 _refine_ls_wR_factor_all 0.2317 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 1.335 _refine_ls_restrained_S_all 1.335 _refine_ls_goodness_of_fit_obs ? _refine_ls_shift/esd_max 0.0870 _refine_ls_shift/esd_mean 0.0060 _refine_diff_density_min -0.48 _refine_diff_density_max 0.56 _refine_diff_density_rms 0.07 #--------------------------------------------------------------------------- #-- _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(4) 1.228(6) 1_555 1_555 yes O(2) C(2) 1.222(6) 1_555 1_555 yes O(3) C(1) 1.255(6) 1_555 1_555 yes O(4) C(8) 1.254(6) 1_555 1_555 yes O(5) C(2) 1.343(5) 1_555 1_555 yes O(5) C(18) 1.483(5) 1_555 1_555 yes O(8) C(14) 1.233(7) 1_555 1_555 yes O(9) C(34) 1.410(8) 1_555 1_555 yes O(10) C(33) 1.22(1) 1_555 1_555 yes O(11) C(33) 1.29(1) 1_555 1_555 yes O(11) C(37) 1.63(1) 1_555 1_555 yes N(1) C(4) 1.377(6) 1_555 1_555 yes N(1) C(41) 1.426(6) 1_555 1_555 yes N(1) H(32) 1.00(6) 1_555 1_555 no N(2) C(1) 1.345(6) 1_555 1_555 yes N(2) C(9) 1.477(7) 1_555 1_555 yes N(2) H(28) 1.04(6) 1_555 1_555 no N(3) C(2) 1.357(6) 1_555 1_555 yes N(3) C(40) 1.459(6) 1_555 1_555 yes N(3) H(46) 0.92(6) 1_555 1_555 no N(4) C(3) 1.426(6) 1_555 1_555 yes N(4) C(14) 1.363(6) 1_555 1_555 yes N(4) H(24) 0.92(6) 1_555 1_555 no N(5) C(8) 1.337(6) 1_555 1_555 yes N(5) C(19) 1.476(7) 1_555 1_555 yes N(5) H(23) 0.95(6) 1_555 1_555 no C(1) C(41) 1.509(7) 1_555 1_555 yes C(3) C(8) 1.506(7) 1_555 1_555 yes C(3) C(11) 1.345(7) 1_555 1_555 yes C(4) C(40) 1.547(7) 1_555 1_555 yes C(6) C(7) 1.468(7) 1_555 1_555 yes C(6) C(13) 1.402(8) 1_555 1_555 yes C(6) C(17) 1.426(7) 1_555 1_555 yes C(7) C(41) 1.343(7) 1_555 1_555 yes C(7) H(33) 1.10(6) 1_555 1_555 no C(9) C(14) 1.528(7) 1_555 1_555 yes C(9) C(27) 1.544(8) 1_555 1_555 yes C(9) C(29) 1.550(9) 1_555 1_555 yes C(10) C(11) 1.481(7) 1_555 1_555 yes C(10) C(20) 1.393(8) 1_555 1_555 yes C(10) C(24) 1.398(8) 1_555 1_555 yes C(11) H(19) 1.03(6) 1_555 1_555 no C(12) C(40) 1.543(7) 1_555 1_555 yes C(12) H(43) 1.03(6) 1_555 1_555 no C(12) H(44) 1.06(6) 1_555 1_555 no C(12) H(45) 0.97(6) 1_555 1_555 no C(13) C(22) 1.381(9) 1_555 1_555 yes C(13) H(34) 1.03(6) 1_555 1_555 no C(16) C(40) 1.523(8) 1_555 1_555 yes C(16) H(40) 0.97(8) 1_555 1_555 no C(16) H(41) 1.01(6) 1_555 1_555 no C(16) H(42) 0.96(6) 1_555 1_555 no C(17) C(25) 1.401(9) 1_555 1_555 yes C(17) H(37) 1.18(6) 1_555 1_555 no C(18) C(26) 1.522(10) 1_555 1_555 yes C(18) C(35) 1.517(10) 1_555 1_555 yes C(18) C(36) 1.525(9) 1_555 1_555 yes C(19) C(31) 1.54(1) 1_555 1_555 yes C(19) C(32) 1.528(9) 1_555 1_555 yes C(19) C(33) 1.504(8) 1_555 1_555 yes C(20) C(21) 1.384(8) 1_555 1_555 yes C(20) H(18) 1.03(6) 1_555 1_555 no C(21) C(23) 1.383(9) 1_555 1_555 yes C(21) H(17) 1.02(6) 1_555 1_555 no C(22) C(28) 1.390(10) 1_555 1_555 yes C(22) H(35) 1.05(6) 1_555 1_555 no C(23) C(30) 1.39(1) 1_555 1_555 yes C(23) H(1) 0.95(6) 1_555 1_555 no C(24) C(30) 1.396(9) 1_555 1_555 yes C(24) H(15) 1.03(6) 1_555 1_555 no C(25) C(28) 1.39(1) 1_555 1_555 yes C(25) H(8) 0.99(6) 1_555 1_555 no C(26) H(13) 1.03(7) 1_555 1_555 no C(26) H(14) 1.15(8) 1_555 1_555 no C(26) H(47) 0.99(8) 1_555 1_555 no C(27) H(29) 1.03(8) 1_555 1_555 no C(27) H(30) 1.13(6) 1_555 1_555 no C(27) H(31) 1.13(6) 1_555 1_555 no C(28) H(36) 0.94(6) 1_555 1_555 no C(29) H(25) 1.00(6) 1_555 1_555 no C(29) H(26) 1.06(8) 1_555 1_555 no C(29) H(27) 1.09(6) 1_555 1_555 no C(30) H(16) 0.91(6) 1_555 1_555 no C(31) H(20) 1.00(7) 1_555 1_555 no C(31) H(21) 0.82(6) 1_555 1_555 no C(31) H(22) 1.02(8) 1_555 1_555 no C(32) H(5) 1.01(6) 1_555 1_555 no C(32) H(6) 1.06(8) 1_555 1_555 no C(32) H(7) 1.07(8) 1_555 1_555 no C(34) C(38) 1.42(1) 1_555 1_555 yes C(34) H(38) 1.18(8) 1_555 1_555 no C(34) H(57) 1.17(11) 1_555 1_555 no C(35) H(48) 0.89(8) 1_555 1_555 no C(35) H(49) 0.88(7) 1_555 1_555 no C(35) H(50) 0.98(11) 1_555 1_555 no C(36) H(51) 1.18(8) 1_555 1_555 no C(36) H(53) 0.94(6) 1_555 1_555 no C(37) H(2) 0.96(2) 1_555 1_555 no C(37) H(54) 0.96(6) 1_555 1_555 no C(37) H(58) 0.96(7) 1_555 1_555 no C(38) H(56) 0.96(5) 1_555 1_555 no C(38) H(59) 0.95(4) 1_555 1_555 no C(38) H(60) 0.97(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(2) O(5) C(18) 121.9(4) 1_555 1_555 1_555 yes C(33) O(11) C(37) 99.5(7) 1_555 1_555 1_555 yes C(4) N(1) C(41) 121.4(4) 1_555 1_555 1_555 yes C(4) N(1) H(32) 115(3) 1_555 1_555 1_555 no C(41) N(1) H(32) 123(3) 1_555 1_555 1_555 no C(1) N(2) C(9) 121.9(4) 1_555 1_555 1_555 yes C(1) N(2) H(28) 115(2) 1_555 1_555 1_555 no C(9) N(2) H(28) 122(2) 1_555 1_555 1_555 no C(2) N(3) C(40) 122.0(4) 1_555 1_555 1_555 yes C(2) N(3) H(46) 112(3) 1_555 1_555 1_555 no C(40) N(3) H(46) 125(3) 1_555 1_555 1_555 no C(3) N(4) C(14) 120.1(4) 1_555 1_555 1_555 yes C(3) N(4) H(24) 121(2) 1_555 1_555 1_555 no C(14) N(4) H(24) 117(2) 1_555 1_555 1_555 no C(8) N(5) C(19) 123.3(4) 1_555 1_555 1_555 yes C(8) N(5) H(23) 122(2) 1_555 1_555 1_555 no C(19) N(5) H(23) 111(2) 1_555 1_555 1_555 no O(3) C(1) N(2) 122.0(5) 1_555 1_555 1_555 yes O(3) C(1) C(41) 119.5(4) 1_555 1_555 1_555 yes N(2) C(1) C(41) 118.5(4) 1_555 1_555 1_555 yes O(2) C(2) O(5) 125.8(4) 1_555 1_555 1_555 yes O(2) C(2) N(3) 124.1(4) 1_555 1_555 1_555 yes O(5) C(2) N(3) 110.1(4) 1_555 1_555 1_555 yes N(4) C(3) C(8) 115.5(4) 1_555 1_555 1_555 yes N(4) C(3) C(11) 125.2(4) 1_555 1_555 1_555 yes C(8) C(3) C(11) 119.3(4) 1_555 1_555 1_555 yes O(1) C(4) N(1) 121.9(4) 1_555 1_555 1_555 yes O(1) C(4) C(40) 120.9(4) 1_555 1_555 1_555 yes N(1) C(4) C(40) 117.1(4) 1_555 1_555 1_555 yes C(7) C(6) C(13) 126.0(4) 1_555 1_555 1_555 yes C(7) C(6) C(17) 115.9(5) 1_555 1_555 1_555 yes C(13) C(6) C(17) 118.1(5) 1_555 1_555 1_555 yes C(6) C(7) C(41) 131.1(5) 1_555 1_555 1_555 yes C(6) C(7) H(33) 112(2) 1_555 1_555 1_555 no C(41) C(7) H(33) 116(2) 1_555 1_555 1_555 no O(4) C(8) N(5) 122.8(4) 1_555 1_555 1_555 yes O(4) C(8) C(3) 120.7(4) 1_555 1_555 1_555 yes N(5) C(8) C(3) 116.4(4) 1_555 1_555 1_555 yes N(2) C(9) C(14) 111.9(4) 1_555 1_555 1_555 yes N(2) C(9) C(27) 111.0(4) 1_555 1_555 1_555 yes N(2) C(9) C(29) 107.0(4) 1_555 1_555 1_555 yes C(14) C(9) C(27) 109.5(5) 1_555 1_555 1_555 yes C(14) C(9) C(29) 106.6(4) 1_555 1_555 1_555 yes C(27) C(9) C(29) 110.7(4) 1_555 1_555 1_555 yes C(11) C(10) C(20) 125.6(5) 1_555 1_555 1_555 yes C(11) C(10) C(24) 116.0(5) 1_555 1_555 1_555 yes C(20) C(10) C(24) 118.3(5) 1_555 1_555 1_555 yes C(3) C(11) C(10) 130.9(5) 1_555 1_555 1_555 yes C(3) C(11) H(19) 114(2) 1_555 1_555 1_555 no C(10) C(11) H(19) 114(2) 1_555 1_555 1_555 no C(40) C(12) H(43) 108(3) 1_555 1_555 1_555 no C(40) C(12) H(44) 115(3) 1_555 1_555 1_555 no C(40) C(12) H(45) 107(3) 1_555 1_555 1_555 no H(43) C(12) H(44) 111(4) 1_555 1_555 1_555 no H(43) C(12) H(45) 114(4) 1_555 1_555 1_555 no H(44) C(12) H(45) 99(4) 1_555 1_555 1_555 no C(6) C(13) C(22) 120.7(5) 1_555 1_555 1_555 yes C(6) C(13) H(34) 121(3) 1_555 1_555 1_555 no C(22) C(13) H(34) 118(3) 1_555 1_555 1_555 no O(8) C(14) N(4) 119.8(4) 1_555 1_555 1_555 yes O(8) C(14) C(9) 121.8(4) 1_555 1_555 1_555 yes N(4) C(14) C(9) 118.2(4) 1_555 1_555 1_555 yes C(40) C(16) H(40) 109(3) 1_555 1_555 1_555 no C(40) C(16) H(41) 108(2) 1_555 1_555 1_555 no C(40) C(16) H(42) 107(3) 1_555 1_555 1_555 no H(40) C(16) H(41) 105(4) 1_555 1_555 1_555 no H(40) C(16) H(42) 116(4) 1_555 1_555 1_555 no H(41) C(16) H(42) 109(4) 1_555 1_555 1_555 no C(6) C(17) C(25) 120.3(5) 1_555 1_555 1_555 yes C(6) C(17) H(37) 116(3) 1_555 1_555 1_555 no C(25) C(17) H(37) 122(3) 1_555 1_555 1_555 no O(5) C(18) C(26) 110.5(4) 1_555 1_555 1_555 yes O(5) C(18) C(35) 101.6(5) 1_555 1_555 1_555 yes O(5) C(18) C(36) 109.3(4) 1_555 1_555 1_555 yes C(26) C(18) C(35) 111.3(7) 1_555 1_555 1_555 yes C(26) C(18) C(36) 113.6(6) 1_555 1_555 1_555 yes C(35) C(18) C(36) 109.9(8) 1_555 1_555 1_555 yes N(5) C(19) C(31) 107.9(5) 1_555 1_555 1_555 yes N(5) C(19) C(32) 109.7(5) 1_555 1_555 1_555 yes N(5) C(19) C(33) 110.8(4) 1_555 1_555 1_555 yes C(31) C(19) C(32) 110.5(6) 1_555 1_555 1_555 yes C(31) C(19) C(33) 107.3(5) 1_555 1_555 1_555 yes C(32) C(19) C(33) 110.6(6) 1_555 1_555 1_555 yes C(10) C(20) C(21) 120.6(5) 1_555 1_555 1_555 yes C(10) C(20) H(18) 122(3) 1_555 1_555 1_555 no C(21) C(20) H(18) 117(3) 1_555 1_555 1_555 no C(20) C(21) C(23) 121.4(6) 1_555 1_555 1_555 yes C(20) C(21) H(17) 123(3) 1_555 1_555 1_555 no C(23) C(21) H(17) 114(3) 1_555 1_555 1_555 no C(13) C(22) C(28) 121.4(6) 1_555 1_555 1_555 yes C(13) C(22) H(35) 119(3) 1_555 1_555 1_555 no C(28) C(22) H(35) 119(3) 1_555 1_555 1_555 no C(21) C(23) C(30) 118.5(6) 1_555 1_555 1_555 yes C(21) C(23) H(1) 118(3) 1_555 1_555 1_555 no C(30) C(23) H(1) 123(3) 1_555 1_555 1_555 no C(10) C(24) C(30) 120.4(6) 1_555 1_555 1_555 yes C(10) C(24) H(15) 117(3) 1_555 1_555 1_555 no C(30) C(24) H(15) 121(3) 1_555 1_555 1_555 no C(17) C(25) C(28) 120.2(6) 1_555 1_555 1_555 yes C(17) C(25) H(8) 119(3) 1_555 1_555 1_555 no C(28) C(25) H(8) 120(3) 1_555 1_555 1_555 no C(18) C(26) H(13) 105(3) 1_555 1_555 1_555 no C(18) C(26) H(14) 101(3) 1_555 1_555 1_555 no C(18) C(26) H(47) 109(4) 1_555 1_555 1_555 no H(13) C(26) H(14) 122(4) 1_555 1_555 1_555 no H(13) C(26) H(47) 105(5) 1_555 1_555 1_555 no H(14) C(26) H(47) 111(5) 1_555 1_555 1_555 no C(9) C(27) H(29) 112(3) 1_555 1_555 1_555 no C(9) C(27) H(30) 108(2) 1_555 1_555 1_555 no C(9) C(27) H(31) 108(3) 1_555 1_555 1_555 no H(29) C(27) H(30) 112(4) 1_555 1_555 1_555 no H(29) C(27) H(31) 109(5) 1_555 1_555 1_555 no H(30) C(27) H(31) 105(4) 1_555 1_555 1_555 no C(22) C(28) C(25) 119.4(7) 1_555 1_555 1_555 yes C(22) C(28) H(36) 124(3) 1_555 1_555 1_555 no C(25) C(28) H(36) 116(3) 1_555 1_555 1_555 no C(9) C(29) H(25) 106(3) 1_555 1_555 1_555 no C(9) C(29) H(26) 107(3) 1_555 1_555 1_555 no C(9) C(29) H(27) 113(3) 1_555 1_555 1_555 no H(25) C(29) H(26) 115(4) 1_555 1_555 1_555 no H(25) C(29) H(27) 102(4) 1_555 1_555 1_555 no H(26) C(29) H(27) 111(4) 1_555 1_555 1_555 no C(23) C(30) C(24) 120.8(6) 1_555 1_555 1_555 yes C(23) C(30) H(16) 120(4) 1_555 1_555 1_555 no C(24) C(30) H(16) 118(4) 1_555 1_555 1_555 no C(19) C(31) H(20) 105(3) 1_555 1_555 1_555 no C(19) C(31) H(21) 103(4) 1_555 1_555 1_555 no C(19) C(31) H(22) 103(3) 1_555 1_555 1_555 no H(20) C(31) H(21) 118(5) 1_555 1_555 1_555 no H(20) C(31) H(22) 106(4) 1_555 1_555 1_555 no H(21) C(31) H(22) 117(5) 1_555 1_555 1_555 no C(19) C(32) H(5) 116(3) 1_555 1_555 1_555 no C(19) C(32) H(6) 116(4) 1_555 1_555 1_555 no C(19) C(32) H(7) 108(3) 1_555 1_555 1_555 no H(5) C(32) H(6) 110(5) 1_555 1_555 1_555 no H(5) C(32) H(7) 93(4) 1_555 1_555 1_555 no H(6) C(32) H(7) 108(5) 1_555 1_555 1_555 no O(10) C(33) O(11) 121.3(6) 1_555 1_555 1_555 yes O(10) C(33) C(19) 123.0(8) 1_555 1_555 1_555 yes O(11) C(33) C(19) 115.0(7) 1_555 1_555 1_555 yes O(9) C(34) C(38) 110.2(6) 1_555 1_555 1_555 yes O(9) C(34) H(38) 114(3) 1_555 1_555 1_555 no O(9) C(34) H(57) 116(5) 1_555 1_555 1_555 no C(38) C(34) H(38) 114(3) 1_555 1_555 1_555 no C(38) C(34) H(57) 116(5) 1_555 1_555 1_555 no H(38) C(34) H(57) 84(7) 1_555 1_555 1_555 no C(18) C(35) H(48) 111(5) 1_555 1_555 1_555 no C(18) C(35) H(49) 110(4) 1_555 1_555 1_555 no C(18) C(35) H(50) 114(5) 1_555 1_555 1_555 no H(48) C(35) H(49) 102(6) 1_555 1_555 1_555 no H(48) C(35) H(50) 99(8) 1_555 1_555 1_555 no H(49) C(35) H(50) 115(7) 1_555 1_555 1_555 no C(18) C(36) H(51) 116(3) 1_555 1_555 1_555 no C(18) C(36) H(53) 105(3) 1_555 1_555 1_555 no H(51) C(36) H(53) 103(5) 1_555 1_555 1_555 no O(11) C(37) H(2) 109(1) 1_555 1_555 1_555 no O(11) C(37) H(54) 109(2) 1_555 1_555 1_555 no O(11) C(37) H(58) 109(3) 1_555 1_555 1_555 no H(2) C(37) H(54) 109(7) 1_555 1_555 1_555 no H(2) C(37) H(58) 109(6) 1_555 1_555 1_555 no H(54) C(37) H(58) 109(6) 1_555 1_555 1_555 no C(34) C(38) H(56) 109(2) 1_555 1_555 1_555 no C(34) C(38) H(59) 109(1) 1_555 1_555 1_555 no C(34) C(38) H(60) 109(2) 1_555 1_555 1_555 no H(56) C(38) H(59) 109(4) 1_555 1_555 1_555 no H(56) C(38) H(60) 109(4) 1_555 1_555 1_555 no H(59) C(38) H(60) 109(4) 1_555 1_555 1_555 no N(3) C(40) C(4) 111.1(4) 1_555 1_555 1_555 yes N(3) C(40) C(12) 107.5(4) 1_555 1_555 1_555 yes N(3) C(40) C(16) 111.3(4) 1_555 1_555 1_555 yes C(4) C(40) C(12) 105.8(4) 1_555 1_555 1_555 yes C(4) C(40) C(16) 110.2(4) 1_555 1_555 1_555 yes C(12) C(40) C(16) 110.8(4) 1_555 1_555 1_555 yes N(1) C(41) C(1) 117.4(4) 1_555 1_555 1_555 yes N(1) C(41) C(7) 126.4(4) 1_555 1_555 1_555 yes C(1) C(41) C(7) 115.9(4) 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(4) O(9) 2.845(5) 1_555 4_554 ? O(4) N(3) 3.081(6) 1_555 4_554 ? O(4) C(12) 3.357(7) 1_555 4_554 ? O(4) C(34) 3.542(9) 1_555 4_554 ? O(8) C(35) 3.48(1) 1_555 4_554 ? O(9) C(11) 3.401(7) 1_555 4_455 ? O(10) C(32) 3.392(10) 1_555 3_855 ? C(1) C(23) 3.566(8) 1_555 2_745 ? C(6) C(37) 3.57(1) 1_555 3_755 ? C(11) C(34) 3.490(10) 1_555 4_554 ? C(17) C(37) 3.522(10) 1_555 3_755 ? C(24) C(30) 3.501(9) 1_555 3_765 ? C(25) C(34) 3.519(9) 1_555 3_756 ? C(29) C(37) 3.58(1) 1_555 4_555 ? C(30) C(30) 3.37(1) 1_555 3_765 ? C(30) C(38) 3.45(1) 1_555 2_755 ? #--------------------------------------------------------------------------- #===END data_(peptide 2: Boc-L-Pro-(Aib-\d^Z^Phe)~2~-Aib-OMe) _database_code_CSD 157038 #--------------------------------------------------------------------------- #-- _audit_creation_date 'Wed Apr 27 08:41:31 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 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _chemical_compound_source ' Synthesis by Inai, et al. ' _chemical_name_common ' Boc-L-Pro-(Aib-\d^Z^Phe)~2~-Aib-OMe' _chemical_formula_weight 774.91 _chemical_formula_analytical ? _chemical_formula_sum 'C41 H54 N6 O9 ' _chemical_formula_moiety 'C41 H54 N6 O9 ' _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- #-- _cell_length_a 19.099(3) _cell_length_b 19.789(2) _cell_length_c 11.980(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4527.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 26.8 _cell_measurement_theta_max 29.9 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1656.00 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.17 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -4 -1 -3 0 -2 -3 -1 -2 _diffrn_reflns_number 3798 _reflns_number_total 3797 _reflns_number_observed 2114 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.338 _diffrn_reflns_av_sigmaI/netI 0.076 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 60.08 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01695 _diffrn_orient_matrix_UB_12 -0.01418 _diffrn_orient_matrix_UB_13 -0.07543 _diffrn_orient_matrix_UB_21 -0.02522 _diffrn_orient_matrix_UB_22 -0.04401 _diffrn_orient_matrix_UB_23 0.00817 _diffrn_orient_matrix_UB_31 -0.04264 _diffrn_orient_matrix_UB_32 0.02039 _diffrn_orient_matrix_UB_33 -0.03481 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 164 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H 0 216 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N 0 24 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O 0 36 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #--------------------------------------------------------------------------- #-- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags O(1) 1.1613(5) -0.0561(5) 0.9078(7) 0.053(2) Uani d . 1.00 . O(2) 1.0493(5) 0.1043(4) 0.6252(8) 0.053(2) Uani d . 1.00 . O(3) 1.0055(5) -0.0660(5) 0.7313(8) 0.057(2) Uani d . 1.00 . O(4) 1.2662(5) -0.1153(5) 0.6788(9) 0.066(3) Uani d . 1.00 . O(9) 1.0301(6) 0.1712(5) 0.8546(9) 0.070(3) Uani d . 1.00 . O(10) 1.1131(6) 0.2573(5) 0.844(1) 0.080(3) Uani d . 1.00 . O(11) 1.2041(6) -0.2934(5) 0.7510(9) 0.072(3) Uani d . 1.00 . O(33) 1.1692(6) -0.3257(5) 0.990(1) 0.086(4) Uani d . 1.00 . O(34) 1.2858(5) -0.3308(5) 0.984(1) 0.077(3) Uani d . 1.00 . N(3) 1.1476(5) -0.1237(5) 0.6828(9) 0.042(3) Uani d . 1.00 . N(5) 1.0397(6) 0.2410(5) 0.7049(9) 0.053(3) Uani d . 1.00 . N(6) 0.9342(5) 0.0983(6) 0.6692(9) 0.051(3) Uani d . 1.00 . N(7) 1.0040(6) 0.0316(6) 0.8365(9) 0.049(3) Uani d . 1.00 . N(8) 1.1383(5) 0.0090(5) 0.7568(9) 0.047(3) Uani d . 1.00 . N(9) 1.1872(6) -0.2023(6) 0.8621(9) 0.050(3) Uani d . 1.00 . C(1) 1.1239(7) -0.0148(7) 0.859(1) 0.046(3) Uani d . 1.00 . C(3) 1.1467(7) -0.1967(7) 0.672(1) 0.050(3) Uani d . 1.00 . C(4) 0.9843(8) 0.2090(7) 0.641(1) 0.051(4) Uani d . 1.00 . C(5) 0.9921(7) 0.1319(7) 0.645(1) 0.044(3) Uani d . 1.00 . C(6) 1.1198(7) -0.2293(7) 0.586(1) 0.053(4) Uani d . 1.00 . C(7) 1.0563(7) 0.0088(6) 0.909(1) 0.043(3) Uani d . 1.00 . C(10) 0.9942(8) 0.2377(7) 0.524(1) 0.058(4) Uani d . 1.00 . C(11) 1.0563(9) 0.0161(7) 1.021(1) 0.066(4) Uani d . 1.00 . C(13) 1.2094(8) -0.0892(7) 0.690(1) 0.050(3) Uani d . 1.00 . C(14) 1.2371(7) -0.2257(7) 0.950(1) 0.062(4) Uani d . 1.00 . C(17) 1.0710(8) 0.2986(8) 0.647(1) 0.065(4) Uani d . 1.00 . C(18) 1.2695(7) 0.0177(8) 0.746(1) 0.062(4) Uani d . 1.00 . C(19) 1.0597(9) 0.2192(8) 0.807(1) 0.062(4) Uani d . 1.00 . C(20) 1.0923(7) -0.2029(8) 0.482(1) 0.058(4) Uani d . 1.00 . C(21) 1.215(1) -0.1906(8) 1.059(1) 0.077(5) Uani d . 1.00 . C(24) 1.0201(8) 0.3085(7) 0.547(1) 0.067(4) Uani d . 1.00 . C(27) 0.9421(10) -0.0063(8) 0.551(1) 0.076(5) Uani d . 1.00 . C(35) 0.9851(7) -0.0058(7) 0.749(1) 0.054(4) Uani d . 1.00 . C(36) 1.3098(8) -0.2097(10) 0.910(2) 0.084(6) Uani d . 1.00 . C(38) 1.2247(8) -0.3003(7) 0.973(1) 0.058(4) Uani d . 1.00 . C(39) 1.1829(7) -0.2355(7) 0.765(1) 0.052(3) Uani d . 1.00 . C(40) 0.967(2) 0.086(1) 1.271(2) 0.12(1) Uani d . 1.00 . C(41) 0.929(1) 0.0424(9) 1.061(2) 0.082(5) Uani d . 1.00 . C(42) 1.186(1) 0.166(1) 0.910(2) 0.088(6) Uani d . 1.00 . C(43) 1.2027(7) -0.0125(7) 0.693(1) 0.048(3) Uani d . 1.00 . C(45) 0.9294(7) 0.0241(7) 0.667(1) 0.061(4) Uani d . 1.00 . C(46) 1.018(1) 0.0628(9) 1.196(1) 0.087(6) Uani d . 1.00 . C(47) 1.1925(9) 0.0143(7) 0.573(1) 0.062(4) Uani d . 1.00 . C(48) 0.8573(8) 0.004(1) 0.716(2) 0.102(7) Uani d . 1.00 . C(49) 1.054(2) -0.1162(10) 0.353(2) 0.135(10) Uani d . 1.00 . C(50) 0.879(2) 0.067(1) 1.137(2) 0.118(8) Uani d . 1.00 . C(51) 1.073(1) -0.1383(9) 0.456(2) 0.107(8) Uani d . 1.00 . C(52) 1.078(1) -0.248(1) 0.397(2) 0.107(8) Uani d . 1.00 . C(53) 1.157(1) 0.2363(8) 0.939(1) 0.079(5) Uani d . 1.00 . C(54) 1.283(1) -0.4055(9) 1.021(2) 0.109(8) Uani d . 1.00 . C(56) 1.109(1) 0.230(1) 1.045(2) 0.107(7) Uani d . 1.00 . C(57) 1.061(2) -0.228(1) 0.296(2) 0.13(1) Uani d . 1.00 . C(58) 1.207(1) 0.289(1) 0.947(2) 0.120(9) Uani d . 1.00 . C(59) 0.896(2) 0.086(1) 1.237(3) 0.13(1) Uani d . 1.00 . C(60) 1.048(1) -0.164(1) 0.272(1) 0.102(7) Uani d . 1.00 . C(337) 1.0007(9) 0.0423(8) 1.093(1) 0.064(4) Uani d . 1.00 . H(1) 1.2596 -0.4106 1.0901 0.216(2) Uiso calc . 1.00 S H(2) 1.2574 -0.4314 0.9653 0.1209(9) Uiso calc . 1.00 S H(3) 1.3288 -0.4239 1.0258 0.0956(5) Uiso calc . 1.00 S H(4) 1.2445 -0.2034 1.1188 0.0363(4) Uiso calc . 1.00 S H(5) 1.2216 -0.1408 1.0500 0.0521(4) Uiso calc . 1.00 S H(6) 1.1681 -0.1976 1.0760 0.178(2) Uiso calc . 1.00 S H(7) 1.3441 -0.2227 0.9670 0.0360(3) Uiso calc . 1.00 S H(8) 1.3213 -0.2319 0.8436 0.179(2) Uiso calc . 1.00 S H(9) 1.3162 -0.1614 0.8997 0.1031(8) Uiso calc . 1.00 S H(10) 1.0446 -0.0671 0.3402 0.0792(6) Uiso calc . 1.00 S H(11) 1.0689 -0.1066 0.5206 0.158(1) Uiso calc . 1.00 S H(12) 1.0841 -0.2964 0.4094 0.0599(4) Uiso calc . 1.00 S H(13) 1.0579 -0.2612 0.2377 0.1114(6) Uiso calc . 1.00 S H(14) 1.0337 -0.1530 0.1975 0.1268(9) Uiso calc . 1.00 S H(15) 1.2747 -0.0006 0.8210 0.0364(4) Uiso calc . 1.00 S H(16) 1.3097 0.0038 0.7043 0.0945(7) Uiso calc . 1.00 S H(17) 1.2673 0.0646 0.7502 0.159(1) Uiso calc . 1.00 S H(18) 1.1892 0.0624 0.5757 0.0392(4) Uiso calc . 1.00 S H(19) 1.2343 0.0030 0.5313 0.0882(7) Uiso calc . 1.00 S H(20) 1.1538 -0.0051 0.5417 0.771(3) Uiso calc . 1.00 S H(21) 0.9817 0.1011 1.3447 0.1517(10) Uiso calc . 1.00 S H(22) 0.9149 0.0251 0.9883 0.1000(9) Uiso calc . 1.00 S H(23) 1.0656 0.0596 1.2183 0.194(2) Uiso calc . 1.00 S H(24) 0.8305 0.0660 1.1143 0.339(3) Uiso calc . 1.00 S H(25) 0.8600 0.1002 1.2903 0.0806(7) Uiso calc . 1.00 S H(26) 0.9384 -0.0551 0.5526 0.0258(3) Uiso calc . 1.00 S H(27) 0.9079 0.0102 0.4999 0.0357(3) Uiso calc . 1.00 S H(28) 0.9873 0.0053 0.5254 0.0859(8) Uiso calc . 1.00 S H(29) 0.8538 0.0238 0.7884 0.404(3) Uiso calc . 1.00 S H(30) 0.8222 0.0267 0.6692 0.168(1) Uiso calc . 1.00 S H(31) 0.8501 -0.0412 0.7161 1.16(1) Uiso calc . 1.00 S H(32) 0.9405 0.2210 0.6693 0.607(4) Uiso calc . 1.00 S H(33) 1.0278 0.2119 0.4816 0.0000(3) Uiso calc . 1.00 S H(34) 0.9507 0.2364 0.4830 0.133(1) Uiso calc . 1.00 S H(35) 1.0727 0.3383 0.6959 0.0361(4) Uiso calc . 1.00 S H(36) 1.1178 0.2901 0.6234 0.0812(6) Uiso calc . 1.00 S H(37) 1.0423 0.3287 0.4839 0.133(1) Uiso calc . 1.00 S H(38) 0.9810 0.3383 0.5672 0.0434(4) Uiso calc . 1.00 S H(39) 1.1496 0.1346 0.9001 0.0446(5) Uiso calc . 1.00 S H(40) 1.2146 0.1688 0.8466 0.1241(10) Uiso calc . 1.00 S H(41) 1.2147 0.1509 0.9727 0.0499(4) Uiso calc . 1.00 S H(42) 1.0871 0.2701 1.0618 0.471(3) Uiso calc . 1.00 S H(43) 1.0719 0.1953 1.0318 0.0834(8) Uiso calc . 1.00 S H(44) 1.1350 0.2133 1.1079 0.0701(6) Uiso calc . 1.00 S H(45) 1.2417 0.2806 1.0056 0.0930(5) Uiso calc . 1.00 S H(46) 1.2357 0.2924 0.8779 0.0247(3) Uiso calc . 1.00 S H(47) 1.1873 0.3316 0.9593 0.225(2) Uiso calc . 1.00 S 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) 0.061(6) 0.055(5) 0.042(5) 0.013(5) -0.007(5) 0.000(5) O(2) 0.051(5) 0.049(5) 0.059(6) -0.006(5) -0.007(5) 0.010(5) O(3) 0.062(5) 0.047(6) 0.061(6) 0.001(5) -0.014(5) 0.003(5) O(4) 0.055(6) 0.065(6) 0.080(7) 0.023(5) 0.005(6) -0.007(6) O(9) 0.098(8) 0.056(6) 0.056(6) -0.001(6) -0.009(6) 0.008(6) O(10) 0.104(8) 0.054(6) 0.082(8) 0.001(6) -0.035(7) 0.000(6) O(11) 0.101(8) 0.045(6) 0.069(7) 0.026(6) -0.010(7) -0.010(5) O(33) 0.080(7) 0.052(6) 0.13(1) -0.018(6) -0.034(8) 0.034(7) O(34) 0.066(6) 0.055(6) 0.109(9) 0.004(5) -0.033(7) 0.019(6) N(3) 0.051(6) 0.030(5) 0.046(6) -0.007(5) -0.006(5) 0.000(5) N(5) 0.058(7) 0.048(6) 0.052(7) 0.004(6) -0.020(6) 0.007(6) N(6) 0.041(6) 0.049(6) 0.062(7) -0.003(5) -0.005(6) 0.014(6) N(7) 0.059(7) 0.053(7) 0.035(6) 0.002(6) 0.006(6) 0.004(5) N(8) 0.051(6) 0.042(6) 0.048(6) -0.001(5) 0.010(6) 0.004(5) N(9) 0.061(7) 0.044(6) 0.046(6) 0.003(5) -0.011(6) 0.001(6) C(1) 0.061(8) 0.044(7) 0.034(7) -0.010(7) 0.002(7) 0.003(7) C(3) 0.049(7) 0.045(7) 0.055(8) 0.016(6) 0.000(7) 0.002(7) C(4) 0.059(9) 0.047(8) 0.047(8) 0.016(7) -0.003(8) 0.014(7) C(5) 0.038(7) 0.051(7) 0.043(7) 0.011(6) 0.011(6) 0.007(6) C(6) 0.055(8) 0.047(8) 0.059(9) 0.002(7) -0.005(8) -0.019(8) C(7) 0.053(8) 0.039(7) 0.035(7) 0.003(6) -0.005(6) 0.008(6) C(10) 0.059(9) 0.069(9) 0.046(8) -0.001(8) 0.008(8) 0.000(8) C(11) 0.10(1) 0.051(8) 0.046(9) 0.012(9) 0.020(9) 0.002(7) C(13) 0.073(10) 0.041(7) 0.035(7) 0.002(8) 0.007(8) 0.006(6) C(14) 0.061(9) 0.052(8) 0.07(1) -0.012(7) -0.028(8) 0.016(8) C(17) 0.07(1) 0.064(9) 0.058(9) -0.010(8) 0.002(9) 0.003(8) C(18) 0.049(9) 0.07(1) 0.07(1) -0.004(7) 0.012(8) 0.003(9) C(19) 0.069(10) 0.052(9) 0.07(1) 0.013(8) -0.017(9) -0.007(8) C(20) 0.061(8) 0.073(10) 0.041(8) 0.001(8) -0.003(7) -0.012(8) C(21) 0.11(2) 0.06(1) 0.06(1) 0.007(9) -0.04(1) -0.011(8) C(24) 0.08(1) 0.051(9) 0.07(1) -0.003(8) -0.013(9) 0.005(8) C(27) 0.10(1) 0.065(10) 0.07(1) -0.019(10) -0.03(1) 0.008(8) C(35) 0.049(8) 0.055(9) 0.059(9) -0.008(7) 0.005(8) 0.017(8) C(36) 0.057(10) 0.08(1) 0.11(2) -0.022(9) -0.046(10) 0.06(1) C(38) 0.064(9) 0.038(7) 0.07(1) -0.003(8) -0.027(9) 0.016(8) C(39) 0.064(9) 0.050(8) 0.042(8) -0.007(7) -0.004(7) -0.005(7) C(40) 0.24(3) 0.09(1) 0.04(1) 0.01(2) 0.02(2) 0.01(1) C(41) 0.10(1) 0.07(1) 0.08(1) 0.007(10) 0.04(1) 0.008(10) C(42) 0.08(1) 0.11(2) 0.08(1) 0.01(1) -0.01(1) 0.00(1) C(43) 0.056(8) 0.045(7) 0.044(7) -0.001(7) 0.003(7) -0.003(6) C(45) 0.048(8) 0.056(9) 0.08(1) -0.013(7) -0.024(8) 0.021(8) C(46) 0.14(2) 0.08(1) 0.043(10) 0.02(1) 0.03(1) 0.004(9) C(47) 0.08(1) 0.050(8) 0.052(9) 0.016(8) 0.036(9) 0.013(7) C(48) 0.049(9) 0.12(2) 0.14(2) -0.01(1) 0.00(1) 0.05(2) C(49) 0.23(3) 0.07(1) 0.11(2) 0.02(2) -0.09(2) -0.01(1) C(50) 0.16(2) 0.08(1) 0.12(2) 0.01(1) 0.08(2) 0.01(1) C(51) 0.18(2) 0.06(1) 0.08(1) 0.01(1) -0.08(1) -0.026(10) C(52) 0.17(2) 0.08(1) 0.06(1) 0.04(1) -0.05(1) -0.03(1) C(53) 0.11(1) 0.056(9) 0.07(1) 0.022(10) -0.05(1) -0.025(9) C(54) 0.12(2) 0.05(1) 0.15(2) -0.01(1) -0.07(2) 0.04(1) C(56) 0.15(2) 0.11(2) 0.07(1) 0.02(2) -0.04(1) -0.02(1) C(57) 0.26(3) 0.07(1) 0.07(1) 0.01(2) -0.06(2) -0.01(1) C(58) 0.16(2) 0.08(2) 0.12(2) -0.03(2) -0.07(2) 0.02(1) C(59) 0.21(3) 0.09(2) 0.09(2) 0.02(2) 0.09(2) 0.02(2) C(60) 0.12(2) 0.15(2) 0.032(9) -0.02(2) -0.02(1) 0.01(1) C(337) 0.09(1) 0.053(9) 0.051(9) 0.025(9) 0.033(9) 0.010(7) #--------------------------------------------------------------------------- #-- _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0(1) _refine_ls_number_reflns 2114 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1934 _refine_ls_R_factor_obs 0.1177 _refine_ls_wR_factor_all 0.3287 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 1.973 _refine_ls_restrained_S_all 1.973 _refine_ls_goodness_of_fit_obs ? _refine_ls_shift/esd_max 1.5430 _refine_ls_shift/esd_mean 0.1370 _refine_diff_density_min -0.36 _refine_diff_density_max 1.96 _refine_diff_density_rms 0.13 #--------------------------------------------------------------------------- #-- _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(1) 1.24(2) 1_555 1_555 yes O(2) C(5) 1.24(2) 1_555 1_555 yes O(3) C(35) 1.27(2) 1_555 1_555 yes O(4) C(13) 1.21(2) 1_555 1_555 yes O(9) C(19) 1.24(2) 1_555 1_555 yes O(10) C(19) 1.35(2) 1_555 1_555 yes O(10) C(53) 1.46(2) 1_555 1_555 yes O(11) C(39) 1.23(2) 1_555 1_555 yes O(33) C(38) 1.19(2) 1_555 1_555 yes O(34) C(38) 1.32(2) 1_555 1_555 yes O(34) C(54) 1.55(2) 1_555 1_555 yes N(3) C(3) 1.45(2) 1_555 1_555 yes N(3) C(13) 1.37(2) 1_555 1_555 yes N(5) C(4) 1.45(2) 1_555 1_555 yes N(5) C(17) 1.46(2) 1_555 1_555 yes N(5) C(19) 1.35(2) 1_555 1_555 yes N(6) C(5) 1.32(2) 1_555 1_555 yes N(6) C(45) 1.47(2) 1_555 1_555 yes N(7) C(7) 1.40(2) 1_555 1_555 yes N(7) C(35) 1.33(2) 1_555 1_555 yes N(8) C(1) 1.34(2) 1_555 1_555 yes N(8) C(43) 1.51(2) 1_555 1_555 yes N(9) C(14) 1.49(2) 1_555 1_555 yes N(9) C(39) 1.34(2) 1_555 1_555 yes C(1) C(7) 1.50(2) 1_555 1_555 yes C(3) C(6) 1.32(2) 1_555 1_555 yes C(3) C(39) 1.52(2) 1_555 1_555 yes C(4) C(5) 1.53(2) 1_555 1_555 yes C(4) C(10) 1.52(2) 1_555 1_555 yes C(4) H(32) 0.934 1_555 1_555 no C(6) C(20) 1.44(2) 1_555 1_555 yes C(7) C(11) 1.35(2) 1_555 1_555 yes C(10) C(24) 1.51(2) 1_555 1_555 yes C(10) H(33) 0.963 1_555 1_555 no C(10) H(34) 0.964 1_555 1_555 no C(11) C(337) 1.46(2) 1_555 1_555 yes C(13) C(43) 1.52(2) 1_555 1_555 yes C(14) C(21) 1.54(2) 1_555 1_555 yes C(14) C(36) 1.50(2) 1_555 1_555 yes C(14) C(38) 1.52(2) 1_555 1_555 yes C(17) C(24) 1.56(2) 1_555 1_555 yes C(17) H(35) 0.977 1_555 1_555 no C(17) H(36) 0.955 1_555 1_555 no C(18) C(43) 1.54(2) 1_555 1_555 yes C(18) H(15) 0.976 1_555 1_555 no C(18) H(16) 0.955 1_555 1_555 no C(18) H(17) 0.932 1_555 1_555 no C(20) C(51) 1.37(2) 1_555 1_555 yes C(20) C(52) 1.39(2) 1_555 1_555 yes C(21) H(4) 0.945 1_555 1_555 no C(21) H(5) 0.999 1_555 1_555 no C(21) H(6) 0.930 1_555 1_555 no C(24) H(37) 0.954 1_555 1_555 no C(24) H(38) 0.983 1_555 1_555 no C(27) C(45) 1.54(2) 1_555 1_555 yes C(27) H(26) 0.969 1_555 1_555 no C(27) H(27) 0.952 1_555 1_555 no C(27) H(28) 0.944 1_555 1_555 no C(35) C(45) 1.56(2) 1_555 1_555 yes C(36) H(7) 0.977 1_555 1_555 no C(36) H(8) 0.940 1_555 1_555 no C(36) H(9) 0.972 1_555 1_555 no C(40) C(46) 1.40(4) 1_555 1_555 yes C(40) C(59) 1.41(5) 1_555 1_555 yes C(40) H(21) 0.976 1_555 1_555 no C(41) C(50) 1.41(4) 1_555 1_555 yes C(41) C(337) 1.42(3) 1_555 1_555 yes C(41) H(22) 0.980 1_555 1_555 no C(42) C(53) 1.53(3) 1_555 1_555 yes C(42) H(39) 0.944 1_555 1_555 no C(42) H(40) 0.934 1_555 1_555 no C(42) H(41) 0.979 1_555 1_555 no C(43) C(47) 1.55(2) 1_555 1_555 yes C(45) C(48) 1.55(2) 1_555 1_555 yes C(46) C(337) 1.34(2) 1_555 1_555 yes C(46) H(23) 0.956 1_555 1_555 no C(47) H(18) 0.953 1_555 1_555 no C(47) H(19) 0.970 1_555 1_555 no C(47) H(20) 0.914 1_555 1_555 no C(48) H(29) 0.954 1_555 1_555 no C(48) H(30) 0.986 1_555 1_555 no C(48) H(31) 0.901 1_555 1_555 no C(49) C(51) 1.36(3) 1_555 1_555 yes C(49) C(60) 1.36(3) 1_555 1_555 yes C(49) H(10) 0.999 1_555 1_555 no C(50) C(59) 1.30(4) 1_555 1_555 yes C(50) H(24) 0.961 1_555 1_555 no C(51) H(11) 1.002 1_555 1_555 no C(52) C(57) 1.32(3) 1_555 1_555 yes C(52) H(12) 0.968 1_555 1_555 no C(53) C(56) 1.58(3) 1_555 1_555 yes C(53) C(58) 1.42(3) 1_555 1_555 yes C(54) H(1) 0.938 1_555 1_555 no C(54) H(2) 0.975 1_555 1_555 no C(54) H(3) 0.953 1_555 1_555 no C(56) H(42) 0.923 1_555 1_555 no C(56) H(43) 0.997 1_555 1_555 no C(56) H(44) 0.956 1_555 1_555 no C(57) C(60) 1.32(3) 1_555 1_555 yes C(57) H(13) 0.965 1_555 1_555 no C(58) H(45) 0.986 1_555 1_555 no C(58) H(46) 0.997 1_555 1_555 no C(58) H(47) 0.926 1_555 1_555 no C(59) H(25) 0.982 1_555 1_555 no C(60) H(14) 0.957 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(19) O(10) C(53) 122(1) 1_555 1_555 1_555 yes C(38) O(34) C(54) 115(1) 1_555 1_555 1_555 yes C(3) N(3) C(13) 120(1) 1_555 1_555 1_555 yes C(4) N(5) C(17) 112(1) 1_555 1_555 1_555 yes C(4) N(5) C(19) 122(1) 1_555 1_555 1_555 yes C(17) N(5) C(19) 124(1) 1_555 1_555 1_555 yes C(5) N(6) C(45) 123(1) 1_555 1_555 1_555 yes C(7) N(7) C(35) 120(1) 1_555 1_555 1_555 yes C(1) N(8) C(43) 121(1) 1_555 1_555 1_555 yes C(14) N(9) C(39) 119(1) 1_555 1_555 1_555 yes O(1) C(1) N(8) 123(1) 1_555 1_555 1_555 yes O(1) C(1) C(7) 120(1) 1_555 1_555 1_555 yes N(8) C(1) C(7) 115(1) 1_555 1_555 1_555 yes N(3) C(3) C(6) 123(1) 1_555 1_555 1_555 yes N(3) C(3) C(39) 115(1) 1_555 1_555 1_555 yes C(6) C(3) C(39) 120(1) 1_555 1_555 1_555 yes N(5) C(4) C(5) 110(1) 1_555 1_555 1_555 yes N(5) C(4) C(10) 103(1) 1_555 1_555 1_555 yes N(5) C(4) H(32) 110(1) 1_555 1_555 1_555 no C(5) C(4) C(10) 112(1) 1_555 1_555 1_555 yes C(5) C(4) H(32) 109(1) 1_555 1_555 1_555 no C(10) C(4) H(32) 110(1) 1_555 1_555 1_555 no O(2) C(5) N(6) 123(1) 1_555 1_555 1_555 yes O(2) C(5) C(4) 121(1) 1_555 1_555 1_555 yes N(6) C(5) C(4) 115(1) 1_555 1_555 1_555 yes C(3) C(6) C(20) 129(1) 1_555 1_555 1_555 yes N(7) C(7) C(1) 117(1) 1_555 1_555 1_555 yes N(7) C(7) C(11) 125(1) 1_555 1_555 1_555 yes C(1) C(7) C(11) 115(1) 1_555 1_555 1_555 yes C(4) C(10) C(24) 102(1) 1_555 1_555 1_555 yes C(4) C(10) H(33) 111(1) 1_555 1_555 1_555 no C(4) C(10) H(34) 110(1) 1_555 1_555 1_555 no C(24) C(10) H(33) 111(1) 1_555 1_555 1_555 no C(24) C(10) H(34) 113(1) 1_555 1_555 1_555 no H(33) C(10) H(34) 107(1) 1_555 1_555 1_555 no C(7) C(11) C(337) 128(1) 1_555 1_555 1_555 yes O(4) C(13) N(3) 123(1) 1_555 1_555 1_555 yes O(4) C(13) C(43) 120(1) 1_555 1_555 1_555 yes N(3) C(13) C(43) 115(1) 1_555 1_555 1_555 yes N(9) C(14) C(21) 106(1) 1_555 1_555 1_555 yes N(9) C(14) C(36) 107(1) 1_555 1_555 1_555 yes N(9) C(14) C(38) 109(1) 1_555 1_555 1_555 yes C(21) C(14) C(36) 115(1) 1_555 1_555 1_555 yes C(21) C(14) C(38) 103(1) 1_555 1_555 1_555 yes C(36) C(14) C(38) 114(1) 1_555 1_555 1_555 yes N(5) C(17) C(24) 101(1) 1_555 1_555 1_555 yes N(5) C(17) H(35) 111(1) 1_555 1_555 1_555 no N(5) C(17) H(36) 112(1) 1_555 1_555 1_555 no C(24) C(17) H(35) 112(1) 1_555 1_555 1_555 no C(24) C(17) H(36) 111(1) 1_555 1_555 1_555 no H(35) C(17) H(36) 106(1) 1_555 1_555 1_555 no C(43) C(18) H(15) 108(1) 1_555 1_555 1_555 no C(43) C(18) H(16) 109(1) 1_555 1_555 1_555 no C(43) C(18) H(17) 111(1) 1_555 1_555 1_555 no H(15) C(18) H(16) 106(1) 1_555 1_555 1_555 no H(15) C(18) H(17) 108(1) 1_555 1_555 1_555 no H(16) C(18) H(17) 110(1) 1_555 1_555 1_555 no O(9) C(19) O(10) 128(1) 1_555 1_555 1_555 yes O(9) C(19) N(5) 122(1) 1_555 1_555 1_555 yes O(10) C(19) N(5) 109(1) 1_555 1_555 1_555 yes C(6) C(20) C(51) 129(1) 1_555 1_555 1_555 yes C(6) C(20) C(52) 117(1) 1_555 1_555 1_555 yes C(51) C(20) C(52) 112(1) 1_555 1_555 1_555 yes C(14) C(21) H(4) 111(1) 1_555 1_555 1_555 no C(14) C(21) H(5) 108(1) 1_555 1_555 1_555 no C(14) C(21) H(6) 112(1) 1_555 1_555 1_555 no H(4) C(21) H(5) 105(1) 1_555 1_555 1_555 no H(4) C(21) H(6) 111(1) 1_555 1_555 1_555 no H(5) C(21) H(6) 107(1) 1_555 1_555 1_555 no C(10) C(24) C(17) 103(1) 1_555 1_555 1_555 yes C(10) C(24) H(37) 112(1) 1_555 1_555 1_555 no C(10) C(24) H(38) 110(1) 1_555 1_555 1_555 no C(17) C(24) H(37) 112(1) 1_555 1_555 1_555 no C(17) C(24) H(38) 111(1) 1_555 1_555 1_555 no H(37) C(24) H(38) 106(1) 1_555 1_555 1_555 no C(45) C(27) H(26) 111(1) 1_555 1_555 1_555 no C(45) C(27) H(27) 109(1) 1_555 1_555 1_555 no C(45) C(27) H(28) 110(1) 1_555 1_555 1_555 no H(26) C(27) H(27) 107(1) 1_555 1_555 1_555 no H(26) C(27) H(28) 108(1) 1_555 1_555 1_555 no H(27) C(27) H(28) 109(1) 1_555 1_555 1_555 no O(3) C(35) N(7) 124(1) 1_555 1_555 1_555 yes O(3) C(35) C(45) 117(1) 1_555 1_555 1_555 yes N(7) C(35) C(45) 117(1) 1_555 1_555 1_555 yes C(14) C(36) H(7) 110(1) 1_555 1_555 1_555 no C(14) C(36) H(8) 112(1) 1_555 1_555 1_555 no C(14) C(36) H(9) 111(1) 1_555 1_555 1_555 no H(7) C(36) H(8) 108(1) 1_555 1_555 1_555 no H(7) C(36) H(9) 105(1) 1_555 1_555 1_555 no H(8) C(36) H(9) 108(2) 1_555 1_555 1_555 no O(33) C(38) O(34) 125(1) 1_555 1_555 1_555 yes O(33) C(38) C(14) 125(1) 1_555 1_555 1_555 yes O(34) C(38) C(14) 108(1) 1_555 1_555 1_555 yes O(11) C(39) N(9) 124(1) 1_555 1_555 1_555 yes O(11) C(39) C(3) 121(1) 1_555 1_555 1_555 yes N(9) C(39) C(3) 114(1) 1_555 1_555 1_555 yes C(46) C(40) C(59) 118(2) 1_555 1_555 1_555 yes C(46) C(40) H(21) 118(3) 1_555 1_555 1_555 no C(59) C(40) H(21) 122(3) 1_555 1_555 1_555 no C(50) C(41) C(337) 119(1) 1_555 1_555 1_555 yes C(50) C(41) H(22) 120(2) 1_555 1_555 1_555 no C(337) C(41) H(22) 120(1) 1_555 1_555 1_555 no C(53) C(42) H(39) 111(1) 1_555 1_555 1_555 no C(53) C(42) H(40) 110(1) 1_555 1_555 1_555 no C(53) C(42) H(41) 108(1) 1_555 1_555 1_555 no H(39) C(42) H(40) 111(2) 1_555 1_555 1_555 no H(39) C(42) H(41) 107(2) 1_555 1_555 1_555 no H(40) C(42) H(41) 108(1) 1_555 1_555 1_555 no N(8) C(43) C(13) 111(1) 1_555 1_555 1_555 yes N(8) C(43) C(18) 111(1) 1_555 1_555 1_555 yes N(8) C(43) C(47) 105(1) 1_555 1_555 1_555 yes C(13) C(43) C(18) 109(1) 1_555 1_555 1_555 yes C(13) C(43) C(47) 108(1) 1_555 1_555 1_555 yes C(18) C(43) C(47) 110(1) 1_555 1_555 1_555 yes N(6) C(45) C(27) 113(1) 1_555 1_555 1_555 yes N(6) C(45) C(35) 108(1) 1_555 1_555 1_555 yes N(6) C(45) C(48) 107(1) 1_555 1_555 1_555 yes C(27) C(45) C(35) 108(1) 1_555 1_555 1_555 yes C(27) C(45) C(48) 112(1) 1_555 1_555 1_555 yes C(35) C(45) C(48) 105(1) 1_555 1_555 1_555 yes C(40) C(46) C(337) 121(2) 1_555 1_555 1_555 yes C(40) C(46) H(23) 120(1) 1_555 1_555 1_555 no C(337) C(46) H(23) 117(1) 1_555 1_555 1_555 no C(43) C(47) H(18) 108(1) 1_555 1_555 1_555 no C(43) C(47) H(19) 107(1) 1_555 1_555 1_555 no C(43) C(47) H(20) 109(1) 1_555 1_555 1_555 no H(18) C(47) H(19) 107(1) 1_555 1_555 1_555 no H(18) C(47) H(20) 112(1) 1_555 1_555 1_555 no H(19) C(47) H(20) 110(1) 1_555 1_555 1_555 no C(45) C(48) H(29) 107(1) 1_555 1_555 1_555 no C(45) C(48) H(30) 105(2) 1_555 1_555 1_555 no C(45) C(48) H(31) 113(1) 1_555 1_555 1_555 no H(29) C(48) H(30) 106(2) 1_555 1_555 1_555 no H(29) C(48) H(31) 113(2) 1_555 1_555 1_555 no H(30) C(48) H(31) 110(2) 1_555 1_555 1_555 no C(51) C(49) C(60) 116(1) 1_555 1_555 1_555 yes C(51) C(49) H(10) 120(2) 1_555 1_555 1_555 no C(60) C(49) H(10) 123(2) 1_555 1_555 1_555 no C(41) C(50) C(59) 121(2) 1_555 1_555 1_555 yes C(41) C(50) H(24) 118(2) 1_555 1_555 1_555 no C(59) C(50) H(24) 120(3) 1_555 1_555 1_555 no C(20) C(51) C(49) 125(1) 1_555 1_555 1_555 yes C(20) C(51) H(11) 115(1) 1_555 1_555 1_555 no C(49) C(51) H(11) 118(1) 1_555 1_555 1_555 no C(20) C(52) C(57) 121(1) 1_555 1_555 1_555 yes C(20) C(52) H(12) 120(1) 1_555 1_555 1_555 no C(57) C(52) H(12) 118(1) 1_555 1_555 1_555 no O(10) C(53) C(42) 106(1) 1_555 1_555 1_555 yes O(10) C(53) C(56) 108(1) 1_555 1_555 1_555 yes O(10) C(53) C(58) 103(1) 1_555 1_555 1_555 yes C(42) C(53) C(56) 108(1) 1_555 1_555 1_555 yes C(42) C(53) C(58) 116(1) 1_555 1_555 1_555 yes C(56) C(53) C(58) 112(1) 1_555 1_555 1_555 yes O(34) C(54) H(1) 111(1) 1_555 1_555 1_555 no O(34) C(54) H(2) 108(2) 1_555 1_555 1_555 no O(34) C(54) H(3) 110(1) 1_555 1_555 1_555 no H(1) C(54) H(2) 108(2) 1_555 1_555 1_555 no H(1) C(54) H(3) 110(2) 1_555 1_555 1_555 no H(2) C(54) H(3) 107(2) 1_555 1_555 1_555 no C(53) C(56) H(42) 111(2) 1_555 1_555 1_555 no C(53) C(56) H(43) 109(1) 1_555 1_555 1_555 no C(53) C(56) H(44) 111(2) 1_555 1_555 1_555 no H(42) C(56) H(43) 107(2) 1_555 1_555 1_555 no H(42) C(56) H(44) 111(2) 1_555 1_555 1_555 no H(43) C(56) H(44) 105(2) 1_555 1_555 1_555 no C(52) C(57) C(60) 122(1) 1_555 1_555 1_555 yes C(52) C(57) H(13) 117(2) 1_555 1_555 1_555 no C(60) C(57) H(13) 119(2) 1_555 1_555 1_555 no C(53) C(58) H(45) 112(2) 1_555 1_555 1_555 no C(53) C(58) H(46) 110(2) 1_555 1_555 1_555 no C(53) C(58) H(47) 114(2) 1_555 1_555 1_555 no H(45) C(58) H(46) 102(2) 1_555 1_555 1_555 no H(45) C(58) H(47) 108(2) 1_555 1_555 1_555 no H(46) C(58) H(47) 107(2) 1_555 1_555 1_555 no C(40) C(59) C(50) 120(3) 1_555 1_555 1_555 yes C(40) C(59) H(25) 119(2) 1_555 1_555 1_555 no C(50) C(59) H(25) 120(3) 1_555 1_555 1_555 no C(49) C(60) C(57) 119(1) 1_555 1_555 1_555 yes C(49) C(60) H(14) 122(2) 1_555 1_555 1_555 no C(57) C(60) H(14) 118(2) 1_555 1_555 1_555 no C(11) C(337) C(41) 122(1) 1_555 1_555 1_555 yes C(11) C(337) C(46) 118(1) 1_555 1_555 1_555 yes C(41) C(337) C(46) 118(1) 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) C(47) 3.52(2) 1_555 2_755 ? O(3) C(17) 3.38(2) 1_555 4_746 ? O(4) C(42) 3.50(2) 1_555 2_754 ? O(9) C(6) 3.55(2) 1_555 4_756 ? O(11) N(6) 3.53(2) 1_555 4_746 ? O(33) N(6) 3.13(2) 1_555 4_746 ? O(33) C(10) 3.37(2) 1_555 4_746 ? O(33) C(4) 3.39(2) 1_555 4_746 ? O(33) C(5) 3.58(2) 1_555 4_746 ? O(34) C(17) 3.42(2) 1_555 2_755 ? C(4) C(39) 3.56(2) 1_555 4_756 ?