############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section C. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section C, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method 'SHELXL-2016/6' _journal_date_recd_electronic 2019-01-25 _journal_date_accepted 2019-03-28 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2019 _journal_volume 75 _journal_issue 5 _journal_page_first 508 _journal_page_last 513 _journal_paper_category FA _journal_paper_doi 10.1107/S2053229619004248 _journal_coeditor_code CU3138 _publ_contact_author_name 'Zhang, Jinfang' _publ_contact_author_address ; China-Australia Joint Research Center for Functional Molecular Materials School of Chemical and Material Engineering Jiangnan University Wuxi 214122 People's Republic of China ; _publ_contact_author_email zjf260@jiangnan.edu.cn _publ_section_title ; A 4'-(4-carboxyphenyl)-3,2':6',3''-terpyridine-based luminescent cadmium(II) coordination polymer for the detection of 2,4,6-trinitrophenol ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Xu, Bin' . ; China-Australia Joint Research Center for Functional Molecular Materials School of Chemical and Material Engineering Jiangnan University Wuxi 214122 People's Republic of China ; 'Luo, Fuming' . ; China-Australia Joint Research Center for Functional Molecular Materials School of Chemical and Material Engineering Jiangnan University Wuxi 214122 People's Republic of China ; 'Tang, Guodong' . ; Jiangsu Key Laboratory for Chemistry of Low-Dimensional Materials Huaiyin Normal University Huaian 223300 People's Republic of China ; 'Zhang, Jinfang' . ; China-Australia Joint Research Center for Functional Molecular Materials School of Chemical and Material Engineering Jiangnan University Wuxi 214122 People's Republic of China ; _publ_section_synopsis ; The three-dimensional coordination polymer poly[bis[\m-4-(3,2':6',3''-terpyridin-4'-yl)benzoato]cadmium(II)] displays strong luminescence and good thermal stability indicating that it can potentially be used as a luminescence sensor. The compound also shows a highly selective and sensitive response to 2,4,6-trinitrophenol through the luminescence quenching effect. ; _database_code_depnum_ccdc_archive 'CCDC 1906400' _chemical_name_systematic ; Poly[bis[\m~3~-4-(3,2':6',3''-terpyridin-4'-yl)benzoato]cadmium(II)] ; _chemical_name_common '[Cd(cptpy)~2~]~n~' _chemical_formula_moiety 'C44 H28 N6 O4 Cd' _chemical_formula_sum 'C44 H28 Cd N6 O4' _chemical_formula_iupac '[Cd (C22 H14 N3 O2)2]' _chemical_formula_weight 817.12 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0100(2) _cell_length_b 9.5930(4) _cell_length_c 17.3488(8) _cell_angle_alpha 91.192(2) _cell_angle_beta 96.049(2) _cell_angle_gamma 92.858(2) _cell_volume 827.84(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 8991 _cell_measurement_theta_min 3.1372 _cell_measurement_theta_max 26.3891 _cell_measurement_temperature 150(2) _exptl_crystal_description PILL _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 414 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2012) ; _exptl_absorpt_correction_T_min 0.6598 _exptl_absorpt_correction_T_max 0.7454 _diffrn_ambient_temperature 150(2) _diffrn_source ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5557 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_unetI/netI 0.0394 _diffrn_reflns_theta_min 3.137 _diffrn_reflns_theta_max 26.392 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _refine_special_details ? _reflns_number_total 3379 _reflns_number_gt 3329 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.0596 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_number_reflns 3379 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.2706P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.556 _refine_diff_density_min -0.806 _refine_ls_extinction_method none _refine_ls_extinction_coef . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_cell_refinement ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; APEX2 (Bruker, 2012) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015) ; _computing_molecular_graphics ; SHELXL2016 (Sheldrick, 2015) ; _computing_publication_material ; publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.500000 0.000000 1.000000 0.01297(7) Uani d 1 . . C C1 1.0308(3) 0.21232(17) 0.96914(9) 0.0136(3) Uani d 1 . . O O2 1.2054(2) 0.17352(14) 1.02003(7) 0.0209(3) Uani d 1 . . N N2 2.3320(3) 0.98504(15) 0.86811(8) 0.0153(3) Uani d 1 . . C C2 1.1168(3) 0.32288(17) 0.91458(10) 0.0132(3) Uani d 1 . . N N3 1.6941(3) 0.79443(16) 0.66123(8) 0.0163(3) Uani d 1 . . C C7 1.3176(4) 0.51630(19) 0.81297(10) 0.0174(3) Uani d 1 . . C C8 1.4414(3) 0.61444(19) 0.76015(10) 0.0173(3) Uani d 1 . . C C9 1.6566(3) 0.70589(19) 0.78812(10) 0.0170(3) Uani d 1 . . H H9 1.718309 0.709015 0.840630 0.020 Uiso calc 1 . . C C10 1.7787(3) 0.79231(18) 0.73735(10) 0.0148(3) Uani d 1 . . C C11 1.4822(3) 0.70966(19) 0.63446(10) 0.0168(3) Uani d 1 . . C C12 1.3528(3) 0.61729(19) 0.68101(10) 0.0192(4) Uani d 1 . . H H12 1.209557 0.558388 0.659790 0.023 Uiso calc 1 . . C C13 2.0141(3) 0.88879(17) 0.76415(10) 0.0129(3) Uani d 1 . . C C14 2.1191(3) 0.90117(18) 0.84179(10) 0.0154(3) Uani d 1 . . H H14 2.035985 0.847856 0.877505 0.018 Uiso calc 1 . . C C15 2.1398(4) 0.9695(2) 0.71168(10) 0.0242(4) Uani d 1 . . H H15 2.064183 0.977275 0.660752 0.029 Uiso d 1 C . C C3A 0.9619(7) 0.3645(4) 0.8521(2) 0.0158(8) Uani d 0.499(3) A 1 H H3A 0.782249 0.333101 0.843929 0.019 Uiso calc 0.499(3) A 1 C C4A 1.0682(8) 0.4544(4) 0.7994(2) 0.0160(8) Uani d 0.499(3) A 1 H H4A 0.963827 0.472302 0.753466 0.019 Uiso calc 0.499(3) A 1 C C5A 1.3856(7) 0.3762(4) 0.93061(19) 0.0153(8) Uani d 0.499(3) A 1 H H5A 1.491225 0.349445 0.974614 0.018 Uiso calc 0.499(3) A 1 C C6A 1.4893(7) 0.4686(4) 0.8798(2) 0.0162(8) Uani d 0.499(3) A 1 H H6A 1.668591 0.500606 0.888215 0.019 Uiso calc 0.499(3) A 1 C C3B 1.0847(7) 0.2982(4) 0.8326(2) 0.0142(7) Uani d 0.501(3) A 2 H H3B 0.997962 0.215743 0.811842 0.017 Uiso calc 0.501(3) A 2 C C4B 1.1833(8) 0.3975(4) 0.78363(19) 0.0150(7) Uani d 0.501(3) A 2 H H4B 1.156407 0.381948 0.730220 0.018 Uiso calc 0.501(3) A 2 C C5B 1.2208(6) 0.4520(4) 0.94186(19) 0.0139(7) Uani d 0.501(3) A 2 H H5B 1.230328 0.472651 0.994723 0.017 Uiso calc 0.501(3) A 2 C C6B 1.3123(6) 0.5528(3) 0.89306(19) 0.0138(7) Uani d 0.501(3) A 2 H H6B 1.368693 0.641934 0.912107 0.017 Uiso calc 0.501(3) A 2 N N1A 1.1884(7) 0.6239(4) 0.42824(19) 0.0272(8) Uani d 0.500(3) B 1 C C18A 1.3875(3) 0.72172(19) 0.55086(10) 0.0176(3) Uani d 0.500(3) B 1 C C19A 1.2790(8) 0.6140(4) 0.5036(2) 0.0232(8) Uani d 0.500(3) B 1 H H19A 1.266320 0.526348 0.525207 0.028 Uiso calc 0.500(3) B 1 C C20A 1.4116(7) 0.8560(4) 0.5169(2) 0.0219(8) Uani d 0.500(3) B 1 H H20A 1.488323 0.933101 0.546027 0.026 Uiso calc 0.500(3) B 1 C C21A 1.3171(8) 0.8679(4) 0.4393(2) 0.0250(9) Uani d 0.500(3) B 1 H H21A 1.317850 0.954052 0.415694 0.030 Uiso calc 0.500(3) B 1 C C22A 1.2189(5) 0.7436(3) 0.39717(11) 0.0326(5) Uani d 0.500(3) B 1 H H22A 1.174002 0.749258 0.343968 0.039 Uiso calc 0.500(3) B 1 N N1B 1.4920(7) 0.7617(4) 0.42099(19) 0.0300(8) Uani d 0.500(3) B 2 C C18B 1.3875(3) 0.72172(19) 0.55086(10) 0.0176(3) Uani d 0.500(3) B 2 C C19B 1.5638(7) 0.7522(4) 0.4972(2) 0.0217(8) Uani d 0.500(3) B 2 H H19B 1.744861 0.767223 0.515047 0.026 Uiso calc 0.500(3) B 2 C C20B 1.1147(8) 0.6932(5) 0.5237(2) 0.0252(9) Uani d 0.500(3) B 2 H H20B 0.989380 0.669399 0.557744 0.030 Uiso calc 0.500(3) B 2 C C21B 1.0381(8) 0.7015(5) 0.4448(2) 0.0317(10) Uani d 0.500(3) B 2 H H21B 0.861629 0.677839 0.424875 0.038 Uiso calc 0.500(3) B 2 C C22B 1.2189(5) 0.7436(3) 0.39717(11) 0.0326(5) Uani d 0.500(3) B 2 H H22B 1.158523 0.761499 0.345963 0.039 Uiso calc 0.500(3) B 2 C C16A 2.3879(12) 1.0403(6) 0.7390(4) 0.0169(9) Uani d 0.538(6) C 1 H H16A 2.492199 1.082883 0.703969 0.020 Uiso calc 0.538(6) C 1 C C17A 2.4762(14) 1.0464(7) 0.8175(5) 0.0151(10) Uani d 0.538(6) C 1 H H17A 2.638292 1.094169 0.834805 0.018 Uiso calc 0.538(6) C 1 C C16B 2.3185(14) 1.0787(7) 0.7379(5) 0.0169(9) Uani d 0.462(6) C 2 H H16B 2.371949 1.147443 0.704885 0.020 Uiso calc 0.462(6) C 2 C C17B 2.4140(16) 1.0810(9) 0.8156(6) 0.0151(10) Uani d 0.462(6) C 2 H H17B 2.541193 1.151142 0.833782 0.018 Uiso calc 0.462(6) C 2 O O1A 0.8147(16) 0.1497(8) 0.9547(5) 0.0170(9) Uani d 0.483(9) D 1 O O1B 0.7699(15) 0.1864(7) 0.9647(4) 0.0170(9) Uani d 0.517(9) D 2 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 Cd1 0.01142(9) 0.01436(10) 0.01246(10) -0.00200(6) -0.00156(6) 0.00505(6) C1 0.0174(8) 0.0099(8) 0.0126(7) -0.0019(6) -0.0004(6) -0.0001(6) O2 0.0210(6) 0.0304(7) 0.0123(6) 0.0094(5) 0.0011(5) 0.0071(5) N2 0.0163(7) 0.0148(7) 0.0143(7) -0.0039(5) 0.0013(5) -0.0019(6) C2 0.0118(7) 0.0131(8) 0.0143(8) -0.0002(6) 0.0005(6) 0.0017(6) N3 0.0159(7) 0.0192(7) 0.0127(7) -0.0037(6) -0.0017(5) 0.0044(6) C7 0.0203(8) 0.0178(9) 0.0125(8) -0.0070(7) -0.0017(6) 0.0026(7) C8 0.0184(8) 0.0189(9) 0.0133(8) -0.0057(7) -0.0019(6) 0.0024(7) C9 0.0175(8) 0.0194(9) 0.0127(8) -0.0040(7) -0.0034(6) 0.0038(7) C10 0.0135(7) 0.0163(8) 0.0134(8) -0.0012(6) -0.0036(6) 0.0023(6) C11 0.0162(8) 0.0212(9) 0.0118(8) -0.0030(6) -0.0022(6) 0.0014(7) C12 0.0176(8) 0.0243(9) 0.0136(8) -0.0088(7) -0.0034(6) 0.0021(7) C13 0.0129(7) 0.0115(8) 0.0137(8) -0.0005(6) 0.0002(6) 0.0005(6) C14 0.0142(7) 0.0161(8) 0.0148(8) -0.0036(6) -0.0016(6) 0.0037(6) C15 0.0310(10) 0.0283(10) 0.0118(8) -0.0139(8) 0.0017(7) -0.0011(7) C3A 0.0121(15) 0.0139(17) 0.0205(17) -0.0034(14) -0.0014(13) 0.0019(14) C4A 0.0169(17) 0.0177(18) 0.0124(16) 0.0005(15) -0.0045(14) 0.0048(14) C5A 0.0171(16) 0.0151(17) 0.0128(15) -0.0002(13) -0.0018(12) 0.0020(13) C6A 0.0124(15) 0.0183(17) 0.0174(16) -0.0006(12) -0.0011(12) 0.0033(14) C3B 0.0142(15) 0.0108(16) 0.0160(16) -0.0047(13) -0.0030(13) 0.0001(13) C4B 0.0163(16) 0.0188(18) 0.0092(15) -0.0011(15) -0.0012(13) 0.0013(14) C5B 0.0141(15) 0.0161(17) 0.0109(15) -0.0019(12) -0.0009(12) 0.0023(13) C6B 0.0149(15) 0.0107(15) 0.0143(16) -0.0037(12) -0.0030(12) 0.0011(13) N1A 0.0313(18) 0.033(2) 0.0146(15) -0.0125(15) -0.0065(13) 0.0009(14) C18A 0.0181(8) 0.0221(9) 0.0116(8) -0.0024(7) -0.0022(6) 0.0030(7) C19A 0.0249(18) 0.025(2) 0.0172(17) -0.0096(15) -0.0035(14) 0.0055(15) C20A 0.0247(18) 0.0242(19) 0.0155(17) -0.0031(14) -0.0022(14) 0.0017(14) C21A 0.031(2) 0.026(2) 0.0162(18) -0.0017(15) -0.0042(15) 0.0078(15) C22A 0.0393(11) 0.0435(13) 0.0124(9) -0.0080(10) -0.0066(8) 0.0068(9) N1B 0.0369(19) 0.038(2) 0.0136(15) -0.0095(15) 0.0014(14) 0.0066(14) C18B 0.0181(8) 0.0221(9) 0.0116(8) -0.0024(7) -0.0022(6) 0.0030(7) C19B 0.0225(17) 0.024(2) 0.0169(17) -0.0061(14) -0.0014(14) 0.0049(15) C20B 0.0204(18) 0.040(2) 0.0145(17) -0.0027(16) -0.0013(14) 0.0012(16) C21B 0.0249(19) 0.048(3) 0.0193(19) -0.0013(19) -0.0092(16) 0.0009(18) C22B 0.0393(11) 0.0435(13) 0.0124(9) -0.0080(10) -0.0066(8) 0.0068(9) C16A 0.020(3) 0.015(3) 0.0161(10) -0.0036(15) 0.0043(18) 0.0019(19) C17A 0.011(3) 0.017(3) 0.0169(10) -0.0023(17) 0.001(2) -0.002(2) C16B 0.020(3) 0.015(3) 0.0161(10) -0.0036(15) 0.0043(18) 0.0019(19) C17B 0.011(3) 0.017(3) 0.0169(10) -0.0023(17) 0.001(2) -0.002(2) O1A 0.013(2) 0.017(3) 0.0204(19) -0.0044(16) -0.0011(13) 0.0058(19) O1B 0.013(2) 0.017(3) 0.0204(19) -0.0044(16) -0.0011(13) 0.0058(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 O1A . 2.292(9) ? Cd1 O1A 2_657 2.292(9) ? Cd1 O1B 2_657 2.320(8) ? Cd1 O1B . 2.320(8) ? Cd1 O2 1_455 2.3236(12) ? Cd1 O2 2_757 2.3236(12) ? Cd1 N2 1_345 2.3522(14) ? Cd1 N2 2_867 2.3522(14) ? C1 O1A . 1.211(9) ? C1 O2 . 1.252(2) ? C1 O1B . 1.312(8) ? C1 C2 . 1.513(2) ? N2 C17A . 1.324(8) ? N2 C14 . 1.338(2) ? N2 C17B . 1.386(10) ? C2 C3A . 1.344(4) ? C2 C5B . 1.374(4) ? C2 C5A . 1.414(4) ? C2 C3B . 1.427(4) ? N3 C11 . 1.341(2) ? N3 C10 . 1.345(2) ? C7 C4A . 1.352(4) ? C7 C4B . 1.356(4) ? C7 C6B . 1.429(4) ? C7 C6A . 1.465(4) ? C7 C8 . 1.486(2) ? C8 C9 . 1.395(2) ? C8 C12 . 1.399(2) ? C9 C10 . 1.389(2) ? C9 H9 . 0.9300 ? C10 C13 . 1.490(2) ? C11 C12 . 1.393(2) ? C11 C18B . 1.486(2) ? C11 C18A . 1.486(2) ? C12 H12 . 0.9300 ? C13 C15 . 1.388(2) ? C13 C14 . 1.394(2) ? C14 H14 . 0.9300 ? C15 C16B . 1.381(8) ? C15 C16A . 1.417(7) ? C15 H15 . 0.9300 ? C3A C4A . 1.398(5) ? C3A H3A . 0.9300 ? C4A H4A . 0.9300 ? C5A C6A . 1.384(5) ? C5A H5A . 0.9300 ? C6A H6A . 0.9300 ? C3B C4B . 1.396(5) ? C3B H3B . 0.9300 ? C4B H4B . 0.9300 ? C5B C6B . 1.390(4) ? C5B H5B . 0.9300 ? C6B H6B . 0.9300 ? N1A C22A . 1.288(4) ? N1A C19A . 1.345(5) ? C18A C19A . 1.360(4) ? C18A C20A . 1.433(4) ? C19A H19A . 0.9300 ? C20A C21A . 1.388(5) ? C20A H20A . 0.9300 ? C21A C22A . 1.424(5) ? C21A H21A . 0.9300 ? C22A H22A . 0.9300 ? N1B C19B . 1.340(5) ? N1B C22B . 1.388(4) ? C18B C19B . 1.375(4) ? C18B C20B . 1.410(4) ? C19B H19B . 0.9300 ? C20B C21B . 1.387(5) ? C20B H20B . 0.9300 ? C21B C22B . 1.342(5) ? C21B H21B . 0.9300 ? C22B H22B . 0.9300 ? C16A C17A . 1.387(10) ? C16A H16A . 0.9300 ? C17A H17A . 0.9300 ? C16B C17B . 1.381(13) ? C16B H16B . 0.9300 ? C17B H17B . 0.9300 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1A Cd1 O1A . 2_657 180.0 ? O1A Cd1 O1B . 2_657 168.40(16) ? O1A Cd1 O1B 2_657 2_657 11.60(16) ? O1B Cd1 O1B 2_657 . 180.0(4) ? O1A Cd1 O2 . 1_455 94.29(16) ? O1A Cd1 O2 2_657 1_455 85.71(17) ? O1A Cd1 O2 . 2_757 85.71(16) ? O1A Cd1 O2 2_657 2_757 94.29(17) ? O2 Cd1 O2 1_455 2_757 180.0 ? O1A Cd1 N2 . 1_345 82.4(2) ? O1A Cd1 N2 2_657 1_345 97.6(2) ? O2 Cd1 N2 1_455 1_345 89.77(5) ? O2 Cd1 N2 2_757 1_345 90.23(5) ? O1A Cd1 N2 . 2_867 97.6(2) ? O1A Cd1 N2 2_657 2_867 82.4(2) ? O2 Cd1 N2 1_455 2_867 90.23(5) ? O2 Cd1 N2 2_757 2_867 89.77(5) ? N2 Cd1 N2 1_345 2_867 180.0 ? O1A C1 O2 . . 122.1(4) ? O2 C1 O1B . . 127.5(4) ? O1A C1 C2 . . 119.3(4) ? O2 C1 C2 . . 117.40(15) ? O1B C1 C2 . . 114.0(3) ? C1 O2 Cd1 . 1_655 124.00(11) ? C17A N2 C14 . . 118.9(4) ? C14 N2 C17B . . 115.1(4) ? C17A N2 Cd1 . 1_765 118.1(4) ? C14 N2 Cd1 . 1_765 122.24(11) ? C3A C2 C5A . . 120.5(2) ? C5B C2 C3B . . 117.6(2) ? C3A C2 C1 . . 124.4(2) ? C5B C2 C1 . . 121.30(19) ? C5A C2 C1 . . 114.96(19) ? C3B C2 C1 . . 121.05(19) ? C11 N3 C10 . . 117.76(14) ? C4B C7 C6B . . 119.2(2) ? C4A C7 C6A . . 116.8(2) ? C4A C7 C8 . . 125.0(2) ? C4B C7 C8 . . 119.8(2) ? C6B C7 C8 . . 120.70(19) ? C6A C7 C8 . . 117.67(19) ? C9 C8 C12 . . 117.45(15) ? C9 C8 C7 . . 120.49(15) ? C12 C8 C7 . . 122.04(16) ? C10 C9 C8 . . 119.85(16) ? C10 C9 H9 . . 120.1 ? C8 C9 H9 . . 120.1 ? N3 C10 C9 . . 122.61(16) ? N3 C10 C13 . . 115.61(15) ? C9 C10 C13 . . 121.77(15) ? N3 C11 C12 . . 123.25(16) ? N3 C11 C18B . . 115.60(15) ? C12 C11 C18B . . 121.14(16) ? N3 C11 C18A . . 115.60(15) ? C12 C11 C18A . . 121.14(16) ? C11 C12 C8 . . 119.03(16) ? C11 C12 H12 . . 120.5 ? C8 C12 H12 . . 120.5 ? C15 C13 C14 . . 117.22(16) ? C15 C13 C10 . . 120.64(15) ? C14 C13 C10 . . 122.14(15) ? N2 C14 C13 . . 124.04(15) ? N2 C14 H14 . . 118.0 ? C13 C14 H14 . . 118.0 ? C16B C15 C13 . . 120.1(4) ? C13 C15 C16A . . 117.3(3) ? C16B C15 H15 . . 114.2 ? C13 C15 H15 . . 121.4 ? C16A C15 H15 . . 121.3 ? C2 C3A C4A . . 120.6(3) ? C2 C3A H3A . . 119.7 ? C4A C3A H3A . . 119.7 ? C7 C4A C3A . . 122.2(3) ? C7 C4A H4A . . 118.9 ? C3A C4A H4A . . 118.9 ? C6A C5A C2 . . 119.0(3) ? C6A C5A H5A . . 120.5 ? C2 C5A H5A . . 120.5 ? C5A C6A C7 . . 120.2(3) ? C5A C6A H6A . . 119.9 ? C7 C6A H6A . . 119.9 ? C4B C3B C2 . . 120.1(3) ? C4B C3B H3B . . 119.9 ? C2 C3B H3B . . 119.9 ? C7 C4B C3B . . 120.8(3) ? C7 C4B H4B . . 119.6 ? C3B C4B H4B . . 119.6 ? C2 C5B C6B . . 122.2(3) ? C2 C5B H5B . . 118.9 ? C6B C5B H5B . . 118.9 ? C5B C6B C7 . . 118.5(3) ? C5B C6B H6B . . 120.7 ? C7 C6B H6B . . 120.7 ? C22A N1A C19A . . 117.4(3) ? C19A C18A C20A . . 117.1(3) ? C19A C18A C11 . . 124.8(2) ? C20A C18A C11 . . 118.2(2) ? N1A C19A C18A . . 125.4(3) ? N1A C19A H19A . . 117.3 ? C18A C19A H19A . . 117.3 ? C21A C20A C18A . . 118.1(3) ? C21A C20A H20A . . 120.9 ? C18A C20A H20A . . 120.9 ? C20A C21A C22A . . 117.7(3) ? C20A C21A H21A . . 121.2 ? C22A C21A H21A . . 121.2 ? N1A C22A C21A . . 124.0(3) ? N1A C22A H22A . . 118.0 ? C21A C22A H22A . . 118.0 ? C19B N1B C22B . . 116.0(3) ? C19B C18B C20B . . 118.0(2) ? C19B C18B C11 . . 121.4(2) ? C20B C18B C11 . . 120.5(2) ? N1B C19B C18B . . 124.3(3) ? N1B C19B H19B . . 117.8 ? C18B C19B H19B . . 117.8 ? C21B C20B C18B . . 118.2(3) ? C21B C20B H20B . . 120.9 ? C18B C20B H20B . . 120.9 ? C22B C21B C20B . . 120.0(3) ? C22B C21B H21B . . 120.0 ? C20B C21B H21B . . 120.0 ? C21B C22B N1B . . 122.9(3) ? C21B C22B H22B . . 118.6 ? N1B C22B H22B . . 118.6 ? C17A C16A C15 . . 120.5(5) ? C17A C16A H16A . . 119.8 ? C15 C16A H16A . . 119.8 ? N2 C17A C16A . . 120.6(6) ? N2 C17A H17A . . 119.7 ? C16A C17A H17A . . 119.7 ? C15 C16B C17B . . 116.8(7) ? C15 C16B H16B . . 121.6 ? C17B C16B H16B . . 121.6 ? C16B C17B N2 . . 124.1(8) ? C16B C17B H17B . . 118.0 ? N2 C17B H17B . . 118.0 ? C1 O1A Cd1 . . 145.8(6) ? C1 O1B Cd1 . . 133.7(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C21B H21B N1B 1_455 0.93 2.05 2.814(6) 138.3 C14 H14 O2 2_867 0.93 2.26 3.111(2) 151.8 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_T_min 0.870 _shelx_estimated_absorpt_T_max 0.932 _shelx_hkl_file ; -1 0 0 3928.66 152.83 1 0 0 3968.08 152.67 -2 0 0 554.59 22.78 2 0 0 557.57 22.45 -3 0 0 814.07 33.53 3 0 0 821.67 32.95 -4 0 0 673.31 29.28 4 0 0 699.35 28.44 -5 0 0 387.50 18.69 5 0 0 378.56 17.30 -6 0 0 638.56 29.27 6 0 0 613.37 27.18 6 -1 0 394.34 17.69 -6 1 0 347.52 19.82 5 -1 0 292.42 14.15 -5 1 0 319.98 16.18 4 -1 0 919.04 36.67 -4 1 0 887.30 37.78 3 -1 0 1723.50 66.63 -3 1 0 1664.45 67.40 2 -1 0 1717.46 70.58 -2 1 0 1896.70 71.10 1 -1 0 1150.95 45.01 -1 1 0 1160.31 45.33 -1 -1 0 1199.84 46.25 1 1 0 1210.73 46.33 1 1 0 1128.17 46.24 -2 -1 0 1284.58 51.48 2 1 0 1328.32 51.42 -3 -1 0 727.54 30.00 3 1 0 730.89 29.70 -4 -1 0 284.16 14.38 4 1 0 311.67 13.85 -5 -1 0 232.87 13.08 5 1 0 245.46 12.32 -6 -1 0 307.58 20.42 6 1 0 326.31 16.06 6 -2 0 502.67 22.41 -6 2 0 511.70 25.44 5 -2 0 419.13 18.05 -5 2 0 393.50 19.98 4 -2 0 208.96 9.82 -4 2 0 190.82 11.36 3 -2 0 755.33 30.46 -3 2 0 760.71 31.63 -2 2 0 152.31 7.81 1 -2 0 1896.27 68.56 -1 2 0 1618.14 69.92 0 -2 0 21.23 2.07 0 2 0 28.53 2.20 0 2 0 28.60 1.97 -1 -2 0 3850.40 150.43 1 2 0 3923.87 151.75 -2 -2 0 4383.05 167.28 2 2 0 4241.90 167.48 -3 -2 0 255.03 11.63 3 2 0 243.79 11.49 -4 -2 0 297.66 14.29 4 2 0 298.77 13.94 -5 -2 0 1237.10 50.93 5 2 0 1240.17 50.67 -6 -2 0 423.95 21.10 6 2 0 435.34 21.32 6 -3 0 367.85 16.95 -6 3 0 357.42 20.21 5 -3 0 566.47 24.08 -5 3 0 568.26 26.42 4 -3 0 63.95 4.97 -4 3 0 57.29 6.75 3 -3 0 879.28 35.01 -3 3 0 866.47 36.21 2 -3 0 3281.31 129.51 -2 3 0 3384.82 130.26 -1 3 0 6371.20 246.72 0 3 0 2048.37 88.66 0 3 0 2435.87 87.40 -1 -3 0 930.93 34.72 1 3 0 806.23 34.60 -2 -3 0 3476.28 138.28 2 3 0 3647.15 138.83 -3 -3 0 729.16 29.24 3 3 0 699.70 29.57 -4 -3 0 316.06 15.15 4 3 0 334.11 15.33 -5 -3 0 897.74 37.67 5 3 0 898.27 37.81 5 -4 0 1003.00 40.86 -5 4 0 1007.08 48.98 4 -4 0 829.04 33.93 -4 4 0 840.84 36.01 3 -4 0 402.47 17.04 -3 4 0 394.02 18.39 2 -4 0 157.80 7.69 -2 4 0 147.42 8.18 -1 4 0 4065.59 158.12 0 4 0 2350.60 91.25 0 4 0 2325.10 91.36 1 4 0 2007.64 78.89 -2 -4 0 2145.51 85.64 2 4 0 2242.70 86.41 -3 -4 0 792.88 31.74 3 4 0 771.38 32.48 -4 -4 0 668.07 28.01 4 4 0 664.27 28.60 -5 -4 0 551.39 24.34 5 4 0 554.67 25.01 5 -5 0 11.98 3.14 -5 5 0 -2.49 5.00 4 -5 0 810.27 33.95 -4 5 0 853.18 36.10 3 -5 0 457.36 19.74 -3 5 0 470.19 21.14 2 -5 0 3.63 2.51 -2 5 0 -1.16 2.41 -1 5 0 1469.79 58.33 0 5 0 1913.77 73.21 0 5 0 1817.30 73.51 1 5 0 1572.21 62.47 -2 -5 0 244.66 10.63 2 5 0 241.29 11.72 -3 -5 0 1068.79 42.87 3 5 0 1080.13 44.12 -4 -5 0 1114.06 44.18 4 5 0 1068.47 45.29 -5 -5 0 304.98 14.94 5 -6 0 249.66 12.23 -5 6 0 240.80 15.51 4 -6 0 269.67 12.94 -4 6 0 273.83 15.13 3 -6 0 636.93 25.68 -3 6 0 577.32 26.68 2 -6 0 87.53 6.29 -2 6 0 78.63 6.40 -1 6 0 217.17 10.50 0 6 0 1454.19 59.28 0 6 0 1523.34 58.90 1 6 0 838.95 34.60 -2 -6 0 459.25 19.00 2 6 0 463.49 20.51 -3 -6 0 543.60 22.31 3 6 0 534.33 23.93 -4 -6 0 381.56 16.96 4 6 0 384.24 18.65 -5 -6 0 645.73 27.08 5 6 0 615.82 29.01 5 -7 0 151.62 9.01 -5 7 0 128.23 12.62 4 -7 0 121.74 7.71 -4 7 0 101.98 9.28 3 -7 0 341.60 16.14 -3 7 0 361.65 17.47 2 -7 0 900.73 37.17 -2 7 0 900.10 37.61 -1 7 0 317.76 14.65 0 7 0 758.35 30.55 0 7 0 728.72 30.99 1 7 0 1762.43 70.54 -2 -7 0 450.61 18.73 2 7 0 452.31 20.59 -3 -7 0 923.02 37.45 3 7 0 952.74 39.75 -4 -7 0 183.50 9.57 4 7 0 157.10 15.90 4 -8 0 246.29 12.52 -4 8 0 235.62 15.15 3 -8 0 213.75 11.49 -3 8 0 197.45 12.36 2 -8 0 873.13 36.47 -2 8 0 870.98 36.75 -1 8 0 1739.15 69.49 0 8 0 654.91 27.38 1 8 0 418.77 19.31 -2 -8 0 503.22 20.54 2 8 0 484.59 22.66 -3 -8 0 140.36 7.58 3 8 0 129.76 9.61 -4 -8 0 127.03 7.92 4 8 0 133.54 10.87 4 -9 0 158.35 10.12 -4 9 0 158.95 12.89 3 -9 0 71.39 7.55 -3 9 0 74.59 8.21 2 -9 0 636.12 27.28 -2 9 0 597.72 27.23 -1 9 0 464.27 20.85 0 9 0 237.58 11.93 1 9 0 204.64 11.77 -2 -9 0 408.26 17.57 2 9 0 423.01 20.10 3 9 0 257.46 15.04 3 -10 0 30.52 5.72 -3 10 0 37.50 6.60 2 -10 0 273.60 15.08 -2 10 0 279.62 14.86 -1 10 0 157.94 9.83 0 10 0 1101.14 45.01 1 10 0 320.97 16.49 2 10 0 283.86 16.09 3 10 0 94.09 10.38 2 -11 0 178.92 12.53 -2 11 0 207.16 12.49 -1 11 0 390.89 19.10 0 11 0 457.22 20.80 -1 -11 0 220.72 42.90 2 11 0 51.86 7.79 2 11 -1 152.19 12.19 -2 -11 1 152.27 9.74 1 11 -1 590.00 27.51 0 11 -1 1433.50 58.25 -1 11 -1 471.65 22.26 -2 11 -1 41.41 5.75 2 -11 1 34.25 6.23 3 10 -1 520.02 25.63 2 10 -1 44.01 6.81 -2 -10 1 49.32 4.71 1 10 -1 27.54 5.10 0 10 -1 477.07 21.37 -1 10 -1 251.78 13.44 -2 10 -1 783.01 33.98 2 -10 1 771.26 33.57 -3 10 -1 34.54 6.87 3 -10 1 30.36 5.72 3 9 -1 17.99 5.39 -3 -9 1 27.57 4.01 2 9 -1 217.72 12.73 -2 -9 1 218.91 10.68 1 9 -1 216.65 12.19 0 9 -1 698.55 29.48 -1 9 -1 355.39 16.90 -2 9 -1 803.15 35.04 2 -9 1 834.09 34.70 -3 9 -1 209.70 12.85 3 -9 1 209.16 11.77 -4 9 -1 117.70 12.15 4 -9 1 141.34 9.13 4 8 -1 70.05 7.86 -4 -8 1 81.31 6.80 3 8 -1 230.47 12.99 -3 -8 1 221.20 10.87 2 8 -1 2508.92 99.80 -2 -8 1 2492.67 97.85 1 8 -1 2047.91 81.92 0 8 -1 178.27 9.71 0 8 -1 184.61 10.04 -1 8 -1 332.76 15.63 -2 8 -1 469.89 21.17 2 -8 1 456.17 20.66 -3 8 -1 251.13 14.00 3 -8 1 236.82 12.44 -4 8 -1 127.77 11.54 4 -8 1 126.29 8.44 4 7 -1 405.70 22.81 -4 -7 1 445.24 18.96 3 7 -1 850.60 36.48 -3 -7 1 857.84 34.61 2 7 -1 642.45 27.45 -2 -7 1 615.53 25.70 1 7 -1 768.87 32.26 0 7 -1 361.76 16.76 0 7 -1 387.68 16.90 -1 7 -1 847.64 35.00 -2 7 -1 223.59 12.16 2 -7 1 231.93 11.68 -3 7 -1 381.82 18.68 3 -7 1 378.30 17.01 -4 7 -1 209.83 15.15 4 -7 1 236.18 11.46 -5 7 -1 121.58 12.57 5 -7 1 136.72 8.42 5 6 -1 184.18 12.16 -5 -6 1 167.28 10.35 4 6 -1 373.67 17.99 -4 -6 1 354.73 16.42 3 6 -1 776.25 33.06 -3 -6 1 778.47 31.69 2 6 -1 12.70 3.19 -2 -6 1 15.23 2.67 1 6 -1 704.11 29.38 0 6 -1 3543.58 137.50 0 6 -1 3505.13 137.69 -1 6 -1 1588.47 63.24 -2 6 -1 158.99 9.17 2 -6 1 153.80 8.53 -3 6 -1 1499.19 61.26 3 -6 1 1505.44 59.73 -4 6 -1 478.89 23.47 4 -6 1 515.75 21.32 -5 6 -1 395.45 21.42 5 -6 1 409.38 17.84 5 5 -1 120.42 11.91 -5 -5 1 139.17 9.03 4 5 -1 945.80 39.81 -4 -5 1 919.46 38.09 3 5 -1 645.67 27.19 -3 -5 1 619.51 26.10 2 5 -1 736.97 31.16 -2 -5 1 766.39 30.30 1 5 -1 276.04 12.58 0 5 -1 2320.48 89.11 0 5 -1 2221.31 89.03 -1 5 -1 1483.90 59.02 -2 5 -1 357.15 15.82 2 -5 1 332.69 14.92 -3 5 -1 393.77 18.33 3 -5 1 383.72 16.70 4 -5 1 280.56 12.79 -5 5 -1 143.90 12.04 5 -5 1 143.13 8.16 5 4 -1 382.13 18.81 -5 -4 1 400.34 18.41 4 4 -1 269.68 13.56 -4 -4 1 271.57 13.09 3 4 -1 510.58 22.53 -3 -4 1 535.40 21.96 2 4 -1 1502.05 59.64 -2 -4 1 1495.77 58.96 1 4 -1 1148.35 45.73 0 4 -1 447.56 18.23 0 4 -1 435.84 18.29 -1 4 -1 945.61 38.00 -2 4 -1 1340.06 52.19 2 -4 1 1257.93 51.21 -3 4 -1 169.89 9.74 3 -4 1 163.42 8.17 -4 4 -1 955.36 40.65 4 -4 1 963.57 38.53 5 -4 1 704.63 29.18 5 3 -1 793.10 33.82 -5 -3 1 787.11 33.64 4 3 -1 547.60 23.58 -4 -3 1 534.60 23.34 3 3 -1 159.53 8.52 -3 -3 1 162.86 8.37 2 3 -1 4251.69 164.54 -2 -3 1 4204.64 164.07 1 3 -1 3441.16 133.88 0 3 -1 52.22 3.32 0 3 -1 49.19 3.24 -1 3 -1 137.87 6.80 -2 3 -1 1809.78 70.88 2 -3 1 1770.39 70.12 -3 3 -1 428.41 18.94 3 -3 1 408.99 17.38 -4 3 -1 7.96 4.01 4 -3 1 5.21 2.22 -5 3 -1 887.57 38.08 5 -3 1 854.99 35.52 -6 3 -1 119.69 12.07 6 -3 1 130.34 8.40 6 2 -1 208.63 17.21 5 2 -1 581.58 25.35 -5 -2 1 576.54 25.81 4 2 -1 579.16 24.53 -4 -2 1 564.73 24.65 3 2 -1 660.88 27.45 -3 -2 1 668.34 27.45 2 2 -1 3975.43 153.72 -2 -2 1 3932.87 153.55 -1 -2 1 3604.56 139.66 -1 2 -1 162.12 7.54 1 -2 1 157.22 7.03 -2 2 -1 402.01 17.02 2 -2 1 389.97 16.14 -3 2 -1 1892.48 75.62 3 -2 1 1912.32 74.45 -4 2 -1 1093.41 44.66 4 -2 1 1058.33 42.99 -5 2 -1 579.81 25.69 5 -2 1 524.27 23.22 -6 2 -1 456.17 22.68 6 -2 1 420.28 19.60 6 1 -1 346.90 17.08 -6 -1 1 355.10 19.25 5 1 -1 277.91 13.72 -5 -1 1 276.65 14.58 4 1 -1 778.77 31.01 -4 -1 1 713.32 31.45 3 1 -1 1958.04 79.31 -3 -1 1 2075.92 79.63 2 1 -1 162.07 7.72 -2 -1 1 173.93 7.92 1 1 -1 9101.52 325.15 -1 -1 1 7731.86 325.04 -1 1 -1 922.97 36.69 -1 1 -1 907.78 36.23 1 -1 1 954.37 36.22 -2 1 -1 1462.95 57.51 2 -1 1 1446.17 56.82 -3 1 -1 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20 74.26 7.81 2 -3 -20 349.70 18.55 -2 3 20 320.29 18.52 -1 3 20 68.87 7.37 0 -3 -20 606.15 27.31 0 3 20 600.42 27.36 -1 -3 -20 385.20 19.07 1 3 20 369.83 18.79 1 -4 -20 8.43 6.36 -1 4 20 23.36 5.56 0 -4 -20 175.75 15.34 0 4 20 229.46 12.99 1 3 -21 21.84 5.16 0 3 -21 161.22 9.82 1 2 -21 372.58 18.16 -1 -2 21 373.51 21.15 0 2 -21 1359.12 54.91 2 1 -21 273.34 15.64 -2 -1 21 275.01 17.38 1 1 -21 27.12 5.26 -1 -1 21 17.87 6.27 0 1 -21 536.20 23.60 2 0 -21 228.76 13.99 -2 0 21 222.05 15.34 1 0 -21 40.51 6.01 -1 0 21 36.73 7.18 0 0 -21 134.42 9.54 2 -1 -21 116.51 10.58 -2 1 21 114.98 11.61 1 -1 -21 512.27 23.80 -1 1 21 510.86 25.41 0 -1 -21 151.74 10.61 0 1 21 130.72 15.47 1 -2 -21 284.74 22.09 -1 2 21 357.56 19.09 0 -2 -21 387.88 19.24 0 2 21 382.76 19.64 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6598 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71080 5.012 9.591 17.349 91.236 96.048 92.854 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 25980 _shelx_res_file ; TITL S_a.res in P-1 S_a.res created by SHELXL-2016/6 at 20:11:30 on 14-Mar-2019 REM Old TITL S in P-1 REM SHELXT solution in P-1 REM R1 0.103, Rweak 0.077, Alpha 0.091, Orientation as input REM Formula found by SHELXT: C54 Cd N6 O8 CELL 0.71073 5.0100 9.5930 17.3488 91.192 96.049 92.858 ZERR 1.000 0.0002 0.0004 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H CD N O UNIT 44 28 1 6 4 TEMP 0 L.S. 10 BOND $H LIST 4 EADP C18A C18B EADP C22A C22B EXYZ C18A C18B EXYZ C22A C22B acta HTAB C21B N1B_$3 HTAB C14 O2_$6 EQIV $3 x-1, y, z EQIV $6 -x+3, -y+1, -z+2 EADP C16A C16B EADP C17A C17B EADP O1A O1B size 0.2 0.15 0.1 FMAP 2 PLAN 20 WGHT 0.024400 0.270600 FVAR 1.09029 0.49928 0.50019 0.53805 0.48304 CD1 3 0.500000 0.000000 1.000000 10.50000 0.01142 0.01436 = 0.01246 0.00505 -0.00156 -0.00200 C1 1 1.030800 0.212321 0.969145 11.00000 0.01737 0.00995 = 0.01264 -0.00012 -0.00036 -0.00195 O2 5 1.205403 0.173520 1.020032 11.00000 0.02104 0.03036 = 0.01226 0.00709 0.00105 0.00943 N2 4 2.332025 0.985042 0.868113 11.00000 0.01625 0.01475 = 0.01433 -0.00190 0.00132 -0.00387 C2 1 1.116825 0.322879 0.914576 11.00000 0.01181 0.01312 = 0.01433 0.00173 0.00055 -0.00018 N3 4 1.694100 0.794428 0.661231 11.00000 0.01593 0.01920 = 0.01265 0.00435 -0.00173 -0.00374 C7 1 1.317647 0.516303 0.812973 11.00000 0.02032 0.01784 = 0.01249 0.00263 -0.00173 -0.00705 C8 1 1.441400 0.614436 0.760150 11.00000 0.01840 0.01893 = 0.01334 0.00245 -0.00188 -0.00567 C9 1 1.656637 0.705894 0.788119 11.00000 0.01750 0.01940 = 0.01268 0.00381 -0.00340 -0.00402 AFIX 43 H9 2 1.718309 0.709015 0.840630 11.00000 -1.20000 AFIX 0 C10 1 1.778663 0.792307 0.737354 11.00000 0.01347 0.01627 = 0.01344 0.00232 -0.00358 -0.00124 C11 1 1.482220 0.709658 0.634456 11.00000 0.01618 0.02119 = 0.01182 0.00141 -0.00215 -0.00304 C12 1 1.352779 0.617289 0.681010 11.00000 0.01755 0.02429 = 0.01364 0.00207 -0.00344 -0.00883 AFIX 43 H12 2 1.209557 0.558388 0.659790 11.00000 -1.20000 AFIX 0 C13 1 2.014055 0.888786 0.764154 11.00000 0.01291 0.01155 = 0.01374 0.00055 0.00022 -0.00046 C14 1 2.119056 0.901169 0.841794 11.00000 0.01424 0.01610 = 0.01477 0.00368 -0.00158 -0.00356 AFIX 43 H14 2 2.035985 0.847856 0.877505 11.00000 -1.20000 AFIX 0 C15 1 2.139829 0.969548 0.711684 11.00000 0.03096 0.02826 = 0.01177 -0.00109 0.00169 -0.01390 AFIX 3 H15 2 2.064183 0.977275 0.660752 11.00000 -1.20000 AFIX 0 PART 1 C3A 1 0.961878 0.364465 0.852136 21.00000 0.01209 0.01387 = 0.02048 0.00194 -0.00141 -0.00337 AFIX 43 H3A 2 0.782249 0.333101 0.843929 21.00000 -1.20000 AFIX 0 C4A 1 1.068202 0.454429 0.799408 21.00000 0.01685 0.01775 = 0.01237 0.00477 -0.00448 0.00050 AFIX 43 H4A 2 0.963827 0.472302 0.753466 21.00000 -1.20000 AFIX 0 C5A 1 1.385634 0.376150 0.930606 21.00000 0.01712 0.01506 = 0.01281 0.00204 -0.00181 -0.00023 AFIX 43 H5A 2 1.491225 0.349445 0.974614 21.00000 -1.20000 AFIX 0 C6A 1 1.489336 0.468629 0.879845 21.00000 0.01237 0.01834 = 0.01735 0.00331 -0.00111 -0.00061 AFIX 43 H6A 2 1.668591 0.500606 0.888215 21.00000 -1.20000 AFIX 0 PART 2 C3B 1 1.084703 0.298160 0.832636 -21.00000 0.01424 0.01077 = 0.01598 0.00014 -0.00304 -0.00469 AFIX 43 H3B 2 0.997962 0.215743 0.811842 -21.00000 -1.20000 AFIX 0 C4B 1 1.183257 0.397478 0.783632 -21.00000 0.01634 0.01878 = 0.00923 0.00134 -0.00118 -0.00105 AFIX 43 H4B 2 1.156407 0.381948 0.730220 -21.00000 -1.20000 AFIX 0 C5B 1 1.220822 0.452006 0.941860 -21.00000 0.01409 0.01610 = 0.01089 0.00230 -0.00092 -0.00187 AFIX 43 H5B 2 1.230328 0.472651 0.994723 -21.00000 -1.20000 AFIX 0 C6B 1 1.312279 0.552786 0.893060 -21.00000 0.01486 0.01075 = 0.01435 0.00113 -0.00305 -0.00370 AFIX 43 H6B 2 1.368693 0.641934 0.912107 -21.00000 -1.20000 AFIX 0 PART 1 N1A 4 1.188412 0.623881 0.428235 31.00000 0.03127 0.03252 = 0.01456 0.00091 -0.00650 -0.01252 C18A 1 1.387519 0.721716 0.550864 31.00000 0.01806 0.02207 = 0.01158 0.00305 -0.00223 -0.00241 C19A 1 1.278979 0.614045 0.503614 31.00000 0.02489 0.02536 = 0.01719 0.00549 -0.00349 -0.00960 AFIX 43 H19A 2 1.266320 0.526348 0.525207 31.00000 -1.20000 AFIX 0 C20A 1 1.411554 0.856040 0.516900 31.00000 0.02473 0.02419 = 0.01549 0.00169 -0.00216 -0.00306 AFIX 43 H20A 2 1.488323 0.933101 0.546027 31.00000 -1.20000 AFIX 0 C21A 1 1.317070 0.867922 0.439327 31.00000 0.03115 0.02610 = 0.01619 0.00776 -0.00417 -0.00174 AFIX 43 H21A 2 1.317850 0.954052 0.415694 31.00000 -1.20000 AFIX 0 C22A 1 1.218869 0.743623 0.397169 31.00000 0.03925 0.04345 = 0.01240 0.00683 -0.00656 -0.00796 AFIX 43 H22A 2 1.174002 0.749258 0.343968 31.00000 -1.20000 AFIX 0 PART 2 N1B 4 1.491974 0.761725 0.420988 -31.00000 0.03690 0.03827 = 0.01364 0.00662 0.00138 -0.00951 C18B 1 1.387519 0.721716 0.550864 -31.00000 0.01806 0.02207 = 0.01158 0.00305 -0.00223 -0.00241 C19B 1 1.563827 0.752211 0.497235 -31.00000 0.02253 0.02440 = 0.01689 0.00495 -0.00136 -0.00606 AFIX 43 H19B 2 1.744861 0.767223 0.515047 -31.00000 -1.20000 AFIX 0 C20B 1 1.114704 0.693168 0.523684 -31.00000 0.02037 0.03965 = 0.01452 0.00119 -0.00131 -0.00270 AFIX 43 H20B 2 0.989380 0.669399 0.557744 -31.00000 -1.20000 AFIX 0 C21B 1 1.038131 0.701473 0.444770 -31.00000 0.02492 0.04814 = 0.01934 0.00091 -0.00919 -0.00126 AFIX 43 H21B 2 0.861629 0.677839 0.424875 -31.00000 -1.20000 AFIX 0 C22B 1 1.218869 0.743623 0.397169 -31.00000 0.03925 0.04345 = 0.01240 0.00683 -0.00656 -0.00796 AFIX 43 H22B 2 1.158523 0.761499 0.345963 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C16A 1 2.387885 1.040284 0.738977 41.00000 0.02005 0.01469 = 0.01613 0.00185 0.00428 -0.00364 AFIX 43 H16A 2 2.492199 1.082883 0.703969 41.00000 -1.20000 AFIX 0 C17A 1 2.476205 1.046442 0.817515 41.00000 0.01076 0.01733 = 0.01685 -0.00226 0.00109 -0.00229 AFIX 43 H17A 2 2.638292 1.094169 0.834805 41.00000 -1.20000 AFIX 0 PART 2 C16B 1 2.318513 1.078738 0.737916 -41.00000 0.02005 0.01469 = 0.01613 0.00185 0.00428 -0.00364 AFIX 43 H16B 2 2.371949 1.147443 0.704885 -41.00000 -1.20000 AFIX 0 C17B 1 2.414013 1.080960 0.815587 -41.00000 0.01076 0.01733 = 0.01685 -0.00226 0.00109 -0.00229 AFIX 43 H17B 2 2.541193 1.151142 0.833782 -41.00000 -1.20000 AFIX 0 PART 0 PART 1 O1A 5 0.814750 0.149746 0.954650 51.00000 0.01300 0.01666 = 0.02040 0.00583 -0.00112 -0.00437 PART 2 O1B 5 0.769889 0.186434 0.964652 -51.00000 0.01300 0.01666 = 0.02040 0.00583 -0.00112 -0.00437 PART 0 HKLF 4 REM S_a.res in P-1 REM R1 = 0.0227 for 3329 Fo > 4sig(Fo) and 0.0232 for all 3379 data REM 335 parameters refined using 0 restraints END WGHT 0.0244 0.2706 REM Highest difference peak 0.556, deepest hole -0.806, 1-sigma level 0.068 Q1 1 0.4033 0.0348 1.0415 11.00000 0.05 0.56 Q2 1 1.4284 0.7148 0.5930 11.00000 0.05 0.39 Q3 1 1.0774 0.2772 0.9398 11.00000 0.05 0.36 Q4 1 2.1464 0.9403 0.6627 11.00000 0.05 0.34 Q5 1 1.4388 0.6608 0.6536 11.00000 0.05 0.33 Q6 1 1.2519 0.0375 1.0756 11.00000 0.05 0.31 Q7 1 1.3521 0.5798 0.7868 11.00000 0.05 0.30 Q8 1 1.3671 0.5110 0.8515 11.00000 0.05 0.28 Q9 1 1.4446 0.6004 0.7189 11.00000 0.05 0.26 Q10 1 1.9369 0.8955 0.8857 11.00000 0.05 0.26 Q11 1 2.0885 0.8933 0.7997 11.00000 0.05 0.26 Q12 1 2.0411 0.9341 0.7373 11.00000 0.05 0.25 Q13 1 2.4370 1.1334 0.6981 11.00000 0.05 0.25 Q14 1 2.0961 0.9081 0.7358 11.00000 0.05 0.24 Q15 1 1.7556 0.7261 0.7571 11.00000 0.05 0.24 Q16 1 2.4325 0.9906 0.8391 11.00000 0.05 0.24 Q17 1 2.4181 1.0332 0.7773 11.00000 0.05 0.24 Q18 1 1.1423 0.2999 0.8820 11.00000 0.05 0.23 Q19 1 1.4379 0.7768 0.5309 11.00000 0.05 0.23 Q20 1 1.2320 0.3620 0.9285 11.00000 0.05 0.22 ; _shelx_res_checksum 12066