data_compound9 #===================================================================== # corresponding information _publ_contact_author_name 'Professor Dr. Guo-Cong Guo & Ming-Sheng Wang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_phone '+86 591 8370 5882' _publ_contact_author_fax '+86 591 8371 4946' _publ_contact_author_email 'mswang@fjirsm.ac.cn & gcguo@fjirsm.ac.cn' #===================================================================== _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'Dy H8 N3 O13, C7 H7 N5' _chemical_formula_sum 'C7 H15 Dy N8 O13' _chemical_formula_weight 581.77 _chemical_melting_point ? 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' 'Dy' 'Dy' -0.1892 4.4098 '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' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _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 6.5293(4) _cell_length_b 10.7441(4) _cell_length_c 13.2901(7) _cell_angle_alpha 89.987(4) _cell_angle_beta 87.860(5) _cell_angle_gamma 79.349(5) _cell_volume 915.60(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7378 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.1390 _cell_measurement_theta_min 2.5320 _exptl_absorpt_coefficient_mu 4.165 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.58041 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.110 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 566 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_unetI/netI 0.0689 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9031 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.097 _diffrn_reflns_theta_min 1.929 _diffrn_ambient_temperature 298(2) _diffrn_detector PILT _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device_type 'Rigaku Pilatus 200K' _diffrn_measurement_method CCD_Profile_fitting _diffrn_measurement_specimen_support Fiber _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Rotating Anode' _diffrn_source_current 80.0 _diffrn_source_power 4.0 _diffrn_source_voltage 50.0 _diffrn_special_details ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3633 _reflns_number_total 4056 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015) ; _computing_data_collection ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.475 _refine_diff_density_min -2.459 _refine_diff_density_rms 0.242 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 4056 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0423 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0707P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1057 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances O17-H17B = O17-H17A = O15-H15A = O15-H15B = O16-H16A = O16-H16B = O14-H14B = O14-H14A 0.85 with sigma of 0.01 H14A-H14B 1.25 with sigma of 0.01 3.a Aromatic/amide H refined with riding coordinates: C23(H23), C24(H24), C25(H25), C26(H26) 3.b Idealised Me refined as rotating group: C27(H27A,H27B,H27C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.50713(3) 0.24163(2) 0.78668(2) 0.02592(11) Uani 1 1 d . . . . . O11A O 0.4242(6) 0.3785(4) 0.6275(3) 0.0465(9) Uani 1 1 d . . . . . O11B O 0.1670(5) 0.3444(3) 0.7231(3) 0.0361(8) Uani 1 1 d . . . . . O11C O 0.1078(8) 0.4701(5) 0.5952(4) 0.0698(15) Uani 1 1 d . . . . . O12A O 0.4659(8) 0.4732(4) 0.8143(4) 0.0583(12) Uani 1 1 d . . . . . O12B O 0.3098(8) 0.3860(4) 0.9286(3) 0.0605(12) Uani 1 1 d . . . . . O12C O 0.2803(9) 0.5921(4) 0.9271(4) 0.0716(15) Uani 1 1 d . . . . . O13A O 0.2174(7) 0.1453(4) 0.8582(3) 0.0431(9) Uani 1 1 d . . . . . O13B O 0.4526(6) 0.1401(4) 0.9672(3) 0.0482(10) Uani 1 1 d . . . . . O13C O 0.1486(7) 0.1014(5) 1.0132(4) 0.0683(15) Uani 1 1 d . . . . . O14 O 0.7809(7) 0.2791(4) 0.8913(3) 0.0500(10) Uani 1 1 d D . . . . H14B H 0.767(12) 0.290(6) 0.9548(10) 0.075 Uiso 1 1 d DR . . . . H14A H 0.787(13) 0.356(2) 0.880(4) 0.075 Uiso 1 1 d DR . . . . O15 O 0.7225(7) 0.0410(4) 0.8113(3) 0.0437(9) Uani 1 1 d D . . . . H15A H 0.801(9) -0.003(6) 0.767(4) 0.066 Uiso 1 1 d DR . . . . H15B H 0.741(11) 0.004(6) 0.868(3) 0.066 Uiso 1 1 d DR . . . . O16 O 0.8023(6) 0.2537(5) 0.6861(3) 0.0467(10) Uani 1 1 d D . . . . H16A H 0.842(11) 0.255(7) 0.6247(18) 0.070 Uiso 1 1 d DR . . . . H16B H 0.906(8) 0.282(7) 0.708(5) 0.070 Uiso 1 1 d DR . . . . O17 O 0.4450(6) 0.1087(3) 0.6543(3) 0.0394(8) Uani 1 1 d D . . . . H17B H 0.342(7) 0.129(6) 0.616(4) 0.059 Uiso 1 1 d DR . . . . H17A H 0.533(9) 0.048(5) 0.628(5) 0.059 Uiso 1 1 d DR . . . . N11 N 0.2301(7) 0.3999(4) 0.6451(3) 0.0355(9) Uani 1 1 d . . . . . N12 N 0.3475(8) 0.4860(4) 0.8932(4) 0.0470(12) Uani 1 1 d . . . . . N13 N 0.2721(7) 0.1271(4) 0.9485(3) 0.0402(10) Uani 1 1 d . . . . . N21 N 0.9471(6) 0.1903(4) 0.4912(3) 0.0336(9) Uani 1 1 d . . . . . N22 N 1.1430(7) 0.1323(4) 0.5032(3) 0.0354(9) Uani 1 1 d . . . . . N23 N 1.2218(7) 0.0788(4) 0.4178(3) 0.0375(9) Uani 1 1 d . . . . . N24 N 1.0757(6) 0.0993(4) 0.3485(3) 0.0347(9) Uani 1 1 d . . . . . N25 N 0.3493(7) 0.3104(4) 0.2513(3) 0.0367(10) Uani 1 1 d . . . . . C21 C 0.9091(7) 0.1686(4) 0.3959(3) 0.0281(9) Uani 1 1 d . . . . . C22 C 0.7113(8) 0.2166(4) 0.3478(3) 0.0292(9) Uani 1 1 d . . . . . C23 C 0.6767(9) 0.1726(5) 0.2516(4) 0.0399(12) Uani 1 1 d . . . . . H23 H 0.7757 0.1108 0.2191 0.048 Uiso 1 1 calc R . . . . C24 C 0.4935(9) 0.2224(6) 0.2059(4) 0.0418(12) Uani 1 1 d . . . . . H24 H 0.4701 0.1939 0.1420 0.050 Uiso 1 1 calc R . . . . C25 C 0.3779(9) 0.3523(5) 0.3441(4) 0.0396(12) Uani 1 1 d . . . . . H25 H 0.2746 0.4126 0.3754 0.048 Uiso 1 1 calc R . . . . C26 C 0.5573(8) 0.3075(5) 0.3933(4) 0.0344(10) Uani 1 1 d . . . . . H26 H 0.5757 0.3380 0.4572 0.041 Uiso 1 1 calc R . . . . C27 C 0.1583(10) 0.3649(6) 0.1981(5) 0.0542(16) Uani 1 1 d . . . . . H27A H 0.0699 0.3031 0.1943 0.081 Uiso 1 1 calc GR . . . . H27B H 0.1959 0.3889 0.1313 0.081 Uiso 1 1 calc GR . . . . H27C H 0.0852 0.4382 0.2342 0.081 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01998(15) 0.03405(16) 0.02238(14) -0.00632(9) -0.00188(9) -0.00126(10) O11A 0.037(2) 0.057(2) 0.042(2) 0.0026(17) 0.0069(17) -0.0027(19) O11B 0.0286(18) 0.044(2) 0.0339(18) 0.0059(15) -0.0052(14) -0.0030(15) O11C 0.058(3) 0.080(3) 0.064(3) 0.033(3) -0.019(2) 0.008(3) O12A 0.067(3) 0.051(2) 0.061(3) -0.022(2) 0.004(2) -0.020(2) O12B 0.077(3) 0.060(3) 0.042(2) -0.0007(19) 0.002(2) -0.007(2) O12C 0.104(4) 0.050(3) 0.054(3) -0.023(2) -0.002(3) 0.005(3) O13A 0.049(2) 0.054(2) 0.0297(18) 0.0082(15) -0.0089(17) -0.0177(19) O13B 0.031(2) 0.074(3) 0.035(2) -0.0018(18) -0.0047(16) 0.0017(19) O13C 0.046(3) 0.101(4) 0.057(3) 0.036(3) 0.009(2) -0.010(3) O14 0.038(2) 0.073(3) 0.038(2) -0.0238(18) -0.0090(17) -0.006(2) O15 0.048(2) 0.048(2) 0.0259(17) -0.0056(14) -0.0033(16) 0.0162(19) O16 0.0272(19) 0.088(3) 0.0288(18) -0.0127(19) 0.0054(16) -0.021(2) O17 0.0343(19) 0.042(2) 0.0363(19) -0.0148(15) -0.0127(16) 0.0097(16) N11 0.037(2) 0.038(2) 0.030(2) 0.0019(16) -0.0017(17) -0.0014(19) N12 0.063(3) 0.038(2) 0.039(2) -0.0088(19) -0.024(2) -0.005(2) N13 0.038(2) 0.045(2) 0.035(2) 0.0080(18) -0.0003(19) 0.000(2) N21 0.032(2) 0.041(2) 0.0250(18) -0.0061(15) -0.0013(16) 0.0011(18) N22 0.028(2) 0.044(2) 0.032(2) -0.0019(17) -0.0059(17) -0.0010(18) N23 0.034(2) 0.043(2) 0.032(2) -0.0058(17) -0.0035(18) 0.0023(19) N24 0.031(2) 0.042(2) 0.0261(19) -0.0033(16) -0.0018(16) 0.0060(18) N25 0.031(2) 0.042(2) 0.039(2) 0.0034(18) -0.0084(19) -0.0095(19) C21 0.030(2) 0.029(2) 0.025(2) -0.0027(16) 0.0003(18) -0.0032(18) C22 0.031(2) 0.031(2) 0.023(2) -0.0023(16) -0.0010(18) -0.0014(19) C23 0.043(3) 0.043(3) 0.031(3) -0.012(2) -0.008(2) -0.001(2) C24 0.045(3) 0.048(3) 0.032(3) -0.007(2) -0.009(2) -0.006(2) C25 0.037(3) 0.040(3) 0.039(3) -0.002(2) -0.004(2) 0.000(2) C26 0.032(3) 0.041(3) 0.028(2) -0.0059(19) -0.0002(19) -0.001(2) C27 0.040(3) 0.062(4) 0.060(4) 0.009(3) -0.023(3) -0.002(3) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O11A 2.592(4) . ? Dy1 O11B 2.469(3) . ? Dy1 O12A 2.479(4) . ? Dy1 O12B 2.589(5) . ? Dy1 O13A 2.479(4) . ? Dy1 O13B 2.674(4) . ? Dy1 O14 2.396(4) . ? Dy1 O15 2.376(4) . ? Dy1 O16 2.327(4) . ? Dy1 O17 2.360(3) . ? O11A N11 1.258(6) . ? O11B N11 1.288(5) . ? O11C N11 1.209(5) . ? O12A N12 1.271(7) . ? O12B N12 1.235(6) . ? O12C N12 1.223(6) . ? O13A N13 1.269(5) . ? O13B N13 1.246(6) . ? O13C N13 1.224(6) . ? O14 H14B 0.852(10) . ? O14 H14A 0.853(10) . ? O15 H15A 0.849(10) . ? O15 H15B 0.848(10) . ? O16 H16A 0.848(10) . ? O16 H16B 0.850(10) . ? O17 H17B 0.850(10) . ? O17 H17A 0.851(10) . ? N21 N22 1.330(5) . ? N21 C21 1.329(6) . ? N22 N23 1.316(6) . ? N23 N24 1.339(6) . ? N24 C21 1.336(6) . ? N25 C24 1.331(7) . ? N25 C25 1.345(7) . ? N25 C27 1.481(6) . ? C21 C22 1.469(6) . ? C22 C23 1.404(6) . ? C22 C26 1.387(7) . ? C23 H23 0.9300 . ? C23 C24 1.379(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C25 C26 1.371(7) . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? 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_3 _geom_angle_publ_flag O11A Dy1 O13B 159.49(13) . . ? O11B Dy1 O11A 50.29(12) . . ? O11B Dy1 O12A 71.56(15) . . ? O11B Dy1 O12B 72.11(13) . . ? O11B Dy1 O13A 68.17(12) . . ? O11B Dy1 O13B 109.94(11) . . ? O12A Dy1 O11A 64.99(15) . . ? O12A Dy1 O12B 49.20(16) . . ? O12A Dy1 O13A 114.73(16) . . ? O12A Dy1 O13B 106.42(15) . . ? O12B Dy1 O11A 102.52(13) . . ? O12B Dy1 O13B 61.44(13) . . ? O13A Dy1 O11A 115.71(12) . . ? O13A Dy1 O12B 70.43(15) . . ? O13A Dy1 O13B 48.99(12) . . ? O14 Dy1 O11A 119.31(16) . . ? O14 Dy1 O11B 142.13(13) . . ? O14 Dy1 O12A 71.90(16) . . ? O14 Dy1 O12B 76.77(15) . . ? O14 Dy1 O13A 120.29(14) . . ? O14 Dy1 O13B 71.68(15) . . ? O15 Dy1 O11A 132.26(13) . . ? O15 Dy1 O11B 142.90(14) . . ? O15 Dy1 O12A 145.47(16) . . ? O15 Dy1 O12B 125.11(13) . . ? O15 Dy1 O13A 86.18(15) . . ? O15 Dy1 O13B 65.70(13) . . ? O15 Dy1 O14 73.80(15) . . ? O16 Dy1 O11A 66.98(14) . . ? O16 Dy1 O11B 117.10(14) . . ? O16 Dy1 O12A 87.70(18) . . ? O16 Dy1 O12B 132.62(16) . . ? O16 Dy1 O13A 156.79(17) . . ? O16 Dy1 O13B 132.94(13) . . ? O16 Dy1 O14 70.77(14) . . ? O16 Dy1 O15 77.33(16) . . ? O16 Dy1 O17 82.06(14) . . ? O17 Dy1 O11A 71.48(13) . . ? O17 Dy1 O11B 75.36(12) . . ? O17 Dy1 O12A 135.83(14) . . ? O17 Dy1 O12B 140.76(15) . . ? O17 Dy1 O13A 77.55(14) . . ? O17 Dy1 O13B 111.92(14) . . ? O17 Dy1 O14 140.89(13) . . ? O17 Dy1 O15 73.15(12) . . ? N11 O11A Dy1 94.5(3) . . ? N11 O11B Dy1 99.6(3) . . ? N12 O12A Dy1 100.1(3) . . ? N12 O12B Dy1 95.7(3) . . ? N13 O13A Dy1 100.9(3) . . ? N13 O13B Dy1 92.1(3) . . ? Dy1 O14 H14B 124(5) . . ? Dy1 O14 H14A 103(5) . . ? H14B O14 H14A 93.7(14) . . ? Dy1 O15 H15A 126(5) . . ? Dy1 O15 H15B 125(5) . . ? H15A O15 H15B 108(7) . . ? Dy1 O16 H16A 141(5) . . ? Dy1 O16 H16B 123(5) . . ? H16A O16 H16B 95(7) . . ? Dy1 O17 H17B 122(5) . . ? Dy1 O17 H17A 126(5) . . ? H17B O17 H17A 110(7) . . ? O11A N11 O11B 115.5(4) . . ? O11C N11 O11A 123.7(5) . . ? O11C N11 O11B 120.8(5) . . ? O12B N12 O12A 114.9(5) . . ? O12C N12 O12A 119.4(5) . . ? O12C N12 O12B 125.7(6) . . ? O13B N13 O13A 116.9(4) . . ? O13C N13 O13A 120.3(5) . . ? O13C N13 O13B 122.8(5) . . ? C21 N21 N22 105.1(4) . . ? N23 N22 N21 109.7(4) . . ? N22 N23 N24 109.0(4) . . ? C21 N24 N23 105.0(4) . . ? C24 N25 C25 120.5(4) . . ? C24 N25 C27 119.7(5) . . ? C25 N25 C27 119.7(5) . . ? N21 C21 N24 111.2(4) . . ? N21 C21 C22 124.6(4) . . ? N24 C21 C22 124.1(4) . . ? C23 C22 C21 119.8(4) . . ? C26 C22 C21 122.0(4) . . ? C26 C22 C23 118.2(4) . . ? C22 C23 H23 120.5 . . ? C24 C23 C22 118.9(5) . . ? C24 C23 H23 120.5 . . ? N25 C24 C23 121.5(5) . . ? N25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? N25 C25 H25 119.5 . . ? N25 C25 C26 120.9(5) . . ? C26 C25 H25 119.5 . . ? C22 C26 H26 120.0 . . ? C25 C26 C22 119.9(5) . . ? C25 C26 H26 120.0 . . ? N25 C27 H27A 109.5 . . ? N25 C27 H27B 109.5 . . ? N25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ?