#------------------------------------------------------------------------------ #$Date: 2020-02-11 02:42:14 +0200 (Tue, 11 Feb 2020) $ #$Revision: 248012 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557279.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557279 loop_ _publ_author_name 'Wang, Hui-Feng' 'Ma, Xiong-Feng' 'Zhu, Zhong-Hong' 'Zou, Hua-Hong' 'Liang, Fu-Pei' _publ_section_title ; Regulation of the Metal Center and Coordinating Anion of Mononuclear Ln(III) Complexes to Promote an Efficient Luminescence Response to Various Organic Solvents ; _journal_name_full Langmuir _journal_paper_doi 10.1021/acs.langmuir.9b02990 _journal_year 2020 _chemical_formula_moiety 'C24 H20 Dy N9 O9' _chemical_formula_sum 'C24 H20 Dy N9 O9' _chemical_formula_weight 740.99 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2019-06-12 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90.00 _cell_angle_beta 111.576(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.4862(8) _cell_length_b 10.4198(5) _cell_length_c 18.1346(9) _cell_measurement_reflns_used 3643 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.7490 _cell_measurement_theta_min 3.7000 _cell_volume 2896.9(3) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9784 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 35.00 94.00 1.00 20.00 -- 17.61 178.00 120.00 59 2 \w 35.00 94.00 1.00 20.00 -- 17.61 178.00 30.00 59 3 \w -51.00 38.00 1.00 20.00 -- 17.61 -57.00 90.00 89 4 \w -50.00 50.00 1.00 20.00 -- -19.80 77.00 150.00 100 5 \w -12.00 76.00 1.00 20.00 -- 17.61 77.00-150.00 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0273901000 _diffrn_orient_matrix_UB_12 -0.0526181000 _diffrn_orient_matrix_UB_13 0.0179102000 _diffrn_orient_matrix_UB_21 0.0078467000 _diffrn_orient_matrix_UB_22 -0.0102241000 _diffrn_orient_matrix_UB_23 -0.0354896000 _diffrn_orient_matrix_UB_31 0.0364448000 _diffrn_orient_matrix_UB_32 0.0419050000 _diffrn_orient_matrix_UB_33 0.0137623000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_unetI/netI 0.1131 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19201 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 3.37 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.645 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1460 _refine_diff_density_max 1.530 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.137 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 5377 _refine_ls_number_restraints 302 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0692 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1660 _refine_ls_wR_factor_ref 0.2035 _reflns_number_gt 2934 _reflns_number_total 5377 _reflns_threshold_expression >2sigma(I) _cod_data_source_file la9b02990_si_002.cif _cod_data_source_block 1 _cod_original_cell_volume 2897.0(2) _cod_database_code 1557279 _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 2. Rigid bond restraints Dy1, N3 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001 Dy1, N4 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 4. Others Fixed Sof: C12(0.5) C11(0.5) H11(0.5) C13(0.5) C2AA(0.5) H2AA(0.5) C0AA(0.5) H0AA(0.5) C1AA(0.5) H1AA(0.5) 5.a Ternary CH refined with riding coordinates: C15(H15), C14(H14), C11(H11), C2AA(H2AA), C0AA(H0AA), C1AA(H1AA) 5.b Aromatic/amide H refined with riding coordinates: C6(H6), C16(H16), C9(H9), C5(H5), C4(H4), C3(H3), C21(H21), C22(H22), C20(H20), C23(H23) 5.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C18(H18A,H18B,H18C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.323 _oxdiff_exptl_absorpt_empirical_full_min 0.844 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Dy1 Dy 0.72063(3) 0.21816(5) 0.95167(3) 0.0593(3) Uani 1 d . U O2 O 0.7083(5) 0.3173(8) 0.8243(5) 0.0750(14) Uani 1 d . U C24 C 0.9480(8) 0.2053(12) 0.9649(8) 0.0761(10) Uani 1 d . U N4 N 0.7177(6) 0.0183(10) 0.8746(5) 0.0763(9) Uani 1 d . U N2 N 0.6020(6) 0.3817(10) 0.9209(5) 0.0727(10) Uani 1 d . U O4 O 0.7244(8) 0.3218(13) 1.0737(7) 0.140(3) Uani 1 d . U O1 O 0.7802(5) 0.4212(8) 0.9304(4) 0.0746(14) Uani 1 d . U N7 N 0.7454(6) 0.4178(11) 0.8562(6) 0.0752(13) Uani 1 d . U O3 O 0.7460(5) 0.5101(8) 0.8149(4) 0.0800(16) Uani 1 d . U N6 N 0.8634(6) 0.1587(10) 0.9415(5) 0.0753(10) Uani 1 d . U N8 N 0.8038(11) 0.3144(16) 1.1203(10) 0.141(3) Uani 1 d . U N1 N 0.4651(6) 0.4451(10) 0.8629(5) 0.0738(10) Uani 1 d . U O5 O 0.8487(8) 0.2815(13) 1.0866(7) 0.141(3) Uani 1 d . U O9 O 0.6789(6) -0.0208(10) 1.1113(6) 0.113(2) Uani 1 d . U N5 N 0.9411(6) 0.0319(10) 0.8919(6) 0.0758(10) Uani 1 d . U C6 C 0.6543(7) 0.5872(12) 0.9992(7) 0.0730(11) Uani 1 d . U H6 H 0.7122 0.5624 1.0242 0.088 Uiso 1 calc R . O8 O 0.7603(7) 0.0445(11) 1.0521(5) 0.1104(19) Uani 1 d . U C16 C 0.7845(7) -0.0199(12) 0.8630(7) 0.0758(10) Uani 1 d . U H16 H 0.7835 -0.0929 0.8332 0.091 Uiso 1 calc R . C9 C 0.5088(8) 0.2310(12) 0.8325(7) 0.0751(10) Uani 1 d . U H9 H 0.4538 0.2088 0.7968 0.090 Uiso 1 calc R . C5 C 0.6265(7) 0.7056(12) 1.0137(7) 0.0736(11) Uani 1 d . U H5 H 0.6659 0.7629 1.0479 0.088 Uiso 1 calc R . O7 O 0.6311(7) 0.1007(10) 1.0104(6) 0.1100(19) Uani 1 d . U C7 C 0.5942(7) 0.5056(13) 0.9466(7) 0.0727(10) Uani 1 d . U N9 N 0.6869(10) 0.0380(14) 1.0584(8) 0.1102(19) Uani 1 d . U C19 C 0.9958(8) 0.1236(12) 0.9327(7) 0.0762(10) Uani 1 d . U N3 N 0.5714(6) 0.1564(10) 0.8474(6) 0.0766(10) Uani 1 d . U C8 C 0.5235(7) 0.3490(13) 0.8710(7) 0.0737(9) Uani 1 d . U C17 C 0.8629(7) 0.0560(12) 0.8986(7) 0.0754(10) Uani 1 d . U C4 C 0.5404(8) 0.7386(12) 0.9775(7) 0.0737(11) Uani 1 d . U H4 H 0.5233 0.8185 0.9896 0.088 Uiso 1 calc R . C3 C 0.4815(7) 0.6678(13) 0.9283(7) 0.0734(11) Uani 1 d . U H3 H 0.4242 0.6961 0.9052 0.088 Uiso 1 calc R . C21 C 1.1173(8) 0.2539(12) 0.9947(7) 0.0781(11) Uani 1 d . U H21 H 1.1757 0.2730 1.0059 0.094 Uiso 1 calc R . C2 C 0.5067(7) 0.5430(13) 0.9097(7) 0.0732(10) Uani 1 d . U C22 C 1.0746(7) 0.3287(13) 1.0244(7) 0.0781(11) Uani 1 d . U H22 H 1.1037 0.3969 1.0563 0.094 Uiso 1 calc R . C20 C 1.0851(7) 0.1534(13) 0.9501(7) 0.0771(11) Uani 1 d . U H20 H 1.1194 0.1034 0.9305 0.093 Uiso 1 calc R . C23 C 0.9848(8) 0.3098(12) 1.0099(7) 0.0774(11) Uani 1 d . U H23 H 0.9533 0.3649 1.0297 0.093 Uiso 1 calc R . O6 O 0.8194(7) 0.3443(13) 1.1876(7) 0.144(3) Uani 1 d . U C1 C 0.3725(6) 0.4424(11) 0.8098(6) 0.0772(16) Uani 1 d . U H1A H 0.3587 0.5192 0.7784 0.116 Uiso 1 calc GR . H1B H 0.3364 0.4373 0.8410 0.116 Uiso 1 calc GR . H1C H 0.3620 0.3690 0.7756 0.116 Uiso 1 calc GR . C18 C 0.9592(7) -0.0684(12) 0.8441(7) 0.0775(16) Uani 1 d . U H18A H 0.9459 -0.0374 0.7911 0.116 Uiso 1 calc GR . H18B H 0.9240 -0.1422 0.8429 0.116 Uiso 1 calc GR . H18C H 1.0198 -0.0916 0.8668 0.116 Uiso 1 calc GR . C10 C 0.5623(7) 0.0265(12) 0.8056(7) 0.0783(10) Uani 1 d . U C15 C 0.6318(7) -0.0562(12) 0.8485(7) 0.0782(10) Uani 1 d . U H15 H 0.6224 -0.0808 0.8969 0.094 Uiso 1 calc R . C14 C 0.6331(8) -0.1827(12) 0.8031(8) 0.0793(10) Uani 1 d . U H14 H 0.6790 -0.2444 0.8308 0.095 Uiso 1 calc R . C12 C 0.5274(15) -0.089(3) 0.6818(14) 0.0791(11) Uani 0.50 d . U C11 C 0.4792(15) -0.026(2) 0.7720(13) 0.0788(11) Uani 0.50 d . U H11 H 0.4254 0.0145 0.7717 0.095 Uiso 0.50 calc R . C13 C 0.5491(16) -0.234(2) 0.7633(16) 0.0793(11) Uani 0.50 d . U C2AA C 0.6095(15) -0.182(2) 0.7323(15) 0.0793(11) Uani 0.50 d . U H2AA H 0.6379 -0.2363 0.7050 0.095 Uiso 0.50 calc R . C0AA C 0.4848(15) -0.164(3) 0.7314(14) 0.0792(11) Uani 0.50 d . U H0AA H 0.4293 -0.2064 0.7021 0.095 Uiso 0.50 calc R . C1AA C 0.5562(14) 0.046(3) 0.7316(14) 0.0788(11) Uani 0.50 d . U H1AA H 0.5481 0.1308 0.7066 0.095 Uiso 0.50 calc R . 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 0.0449(4) 0.0594(4) 0.0660(4) -0.0023(3) 0.0114(3) 0.0096(2) O2 0.070(3) 0.079(4) 0.076(3) -0.003(3) 0.027(2) 0.000(3) C24 0.0609(18) 0.075(2) 0.084(2) 0.0036(16) 0.0168(17) 0.0102(17) N4 0.0626(16) 0.0720(18) 0.0836(19) -0.0045(14) 0.0141(15) 0.0097(16) N2 0.0575(17) 0.076(2) 0.082(2) 0.0056(17) 0.0222(16) 0.0102(17) O4 0.121(5) 0.171(6) 0.108(5) -0.051(5) 0.018(4) 0.011(5) O1 0.069(3) 0.079(4) 0.076(3) -0.003(3) 0.027(3) 0.000(3) N7 0.070(3) 0.079(3) 0.076(3) -0.003(3) 0.027(2) 0.000(3) O3 0.076(3) 0.081(4) 0.080(3) -0.001(3) 0.026(3) -0.002(3) N6 0.0605(18) 0.074(2) 0.083(2) 0.0025(16) 0.0167(17) 0.0103(17) N8 0.121(5) 0.171(6) 0.108(5) -0.050(4) 0.018(4) 0.011(5) N1 0.0580(17) 0.077(2) 0.083(2) 0.0063(17) 0.0215(15) 0.0104(16) O5 0.121(5) 0.172(6) 0.109(5) -0.050(5) 0.018(4) 0.011(5) O9 0.131(5) 0.098(4) 0.112(5) 0.022(3) 0.048(4) 0.020(4) N5 0.0615(18) 0.074(2) 0.084(2) 0.0027(16) 0.0172(16) 0.0111(17) C6 0.0586(19) 0.076(2) 0.083(2) 0.0069(18) 0.0244(17) 0.0105(18) O8 0.126(5) 0.097(4) 0.112(4) 0.023(3) 0.048(4) 0.023(4) C16 0.0619(17) 0.0725(19) 0.0832(19) -0.0017(15) 0.0152(16) 0.0100(16) C9 0.0584(16) 0.075(2) 0.0834(19) 0.0013(16) 0.0166(15) 0.0085(16) C5 0.0593(19) 0.077(2) 0.083(2) 0.0068(19) 0.0245(18) 0.0104(19) O7 0.126(5) 0.097(4) 0.111(4) 0.023(3) 0.048(4) 0.022(4) C7 0.0580(17) 0.076(2) 0.082(2) 0.0067(17) 0.0236(16) 0.0106(17) N9 0.127(5) 0.097(4) 0.111(4) 0.023(3) 0.048(4) 0.022(4) C19 0.0612(18) 0.075(2) 0.084(2) 0.0039(16) 0.0170(17) 0.0106(17) N3 0.0595(15) 0.0750(19) 0.0842(19) -0.0017(15) 0.0135(14) 0.0074(15) C8 0.0577(16) 0.076(2) 0.0826(19) 0.0045(16) 0.0202(15) 0.0097(16) C17 0.0611(17) 0.0734(19) 0.083(2) 0.0011(15) 0.0165(16) 0.0105(16) C4 0.0595(19) 0.077(2) 0.083(2) 0.0072(19) 0.0245(18) 0.0105(19) C3 0.0589(19) 0.077(2) 0.083(2) 0.0073(18) 0.0244(17) 0.0107(18) C21 0.062(2) 0.076(2) 0.086(2) 0.0051(18) 0.0161(19) 0.0098(19) C2 0.0581(17) 0.076(2) 0.083(2) 0.0069(17) 0.0233(16) 0.0107(17) C22 0.062(2) 0.076(2) 0.086(2) 0.0046(18) 0.0158(19) 0.0095(19) C20 0.0615(19) 0.076(2) 0.085(2) 0.0050(18) 0.0166(18) 0.0104(18) C23 0.0616(19) 0.076(2) 0.086(2) 0.0041(18) 0.0162(18) 0.0097(18) O6 0.125(5) 0.174(6) 0.109(5) -0.048(5) 0.016(4) 0.011(5) C1 0.060(3) 0.080(3) 0.085(3) 0.007(2) 0.020(2) 0.011(2) C18 0.065(3) 0.076(3) 0.084(3) 0.003(2) 0.019(2) 0.014(2) C10 0.0625(16) 0.0746(19) 0.0854(19) -0.0036(15) 0.0126(15) 0.0078(15) C15 0.0633(16) 0.0738(18) 0.0852(19) -0.0043(14) 0.0127(15) 0.0085(15) C14 0.0642(17) 0.075(2) 0.086(2) -0.0043(16) 0.0120(16) 0.0081(17) C12 0.0637(17) 0.075(2) 0.086(2) -0.0040(17) 0.0123(16) 0.0077(17) C11 0.0631(17) 0.075(2) 0.086(2) -0.0039(16) 0.0124(16) 0.0077(17) C13 0.0640(18) 0.075(2) 0.086(2) -0.0041(17) 0.0122(17) 0.0078(17) C2AA 0.0641(18) 0.075(2) 0.086(2) -0.0042(17) 0.0123(17) 0.0079(17) C0AA 0.0637(17) 0.075(2) 0.086(2) -0.0041(17) 0.0123(16) 0.0076(17) C1AA 0.0632(17) 0.075(2) 0.086(2) -0.0039(16) 0.0125(16) 0.0078(17) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 Dy1 N4 81.2(3) O2 Dy1 N2 73.6(3) O2 Dy1 N7 26.0(3) O2 Dy1 N6 77.9(3) O2 Dy1 O5 121.4(4) O2 Dy1 O8 154.3(3) O2 Dy1 N9 158.0(3) O2 Dy1 N3 71.9(3) N4 Dy1 N7 104.4(3) N4 Dy1 N6 65.0(3) N4 Dy1 O5 124.5(3) N4 Dy1 N9 82.2(4) N4 Dy1 N3 64.2(3) N2 Dy1 N4 126.3(3) N2 Dy1 N7 68.9(3) N2 Dy1 N6 146.3(3) N2 Dy1 O5 109.1(4) N2 Dy1 N9 105.4(4) N2 Dy1 N3 63.1(3) O4 Dy1 O2 128.9(4) O4 Dy1 N4 149.8(4) O4 Dy1 N2 70.0(4) O4 Dy1 N7 105.5(4) O4 Dy1 N6 117.7(4) O4 Dy1 O5 46.4(4) O4 Dy1 O8 75.2(4) O4 Dy1 N9 68.2(4) O4 Dy1 N3 118.4(4) O1 Dy1 O2 52.0(3) O1 Dy1 N4 124.4(3) O1 Dy1 N2 72.4(3) O1 Dy1 O4 83.2(4) O1 Dy1 N7 26.2(2) O1 Dy1 N6 76.0(3) O1 Dy1 O5 72.4(4) O1 Dy1 O8 137.9(3) O1 Dy1 O7 148.5(3) O1 Dy1 N9 149.5(3) O1 Dy1 N3 115.8(3) N7 Dy1 N9 173.0(4) N6 Dy1 N7 77.6(3) N6 Dy1 O5 71.3(4) N6 Dy1 N9 107.8(4) N6 Dy1 N3 123.7(3) O5 Dy1 N7 97.8(4) O5 Dy1 N9 80.1(4) O8 Dy1 N4 75.4(3) O8 Dy1 N2 129.5(3) O8 Dy1 N7 158.0(3) O8 Dy1 N6 82.7(3) O8 Dy1 O5 66.4(4) O8 Dy1 N9 25.7(3) O8 Dy1 N3 106.3(3) O7 Dy1 O2 139.7(3) O7 Dy1 N4 86.3(4) O7 Dy1 N2 83.7(3) O7 Dy1 O4 69.2(4) O7 Dy1 N7 151.8(3) O7 Dy1 N6 130.0(3) O7 Dy1 O5 97.2(4) O7 Dy1 O8 49.7(3) O7 Dy1 N9 24.2(3) O7 Dy1 N3 68.1(3) N3 Dy1 N7 92.8(3) N3 Dy1 O5 163.5(4) N3 Dy1 N9 87.8(4) N7 O2 Dy1 93.4(7) N6 C24 C19 108.1(11) C23 C24 N6 129.7(13) C23 C24 C19 122.2(12) C16 N4 Dy1 121.3(9) C16 N4 C15 123.7(11) C15 N4 Dy1 114.9(7) C7 N2 Dy1 135.9(7) C8 N2 Dy1 117.8(8) C8 N2 C7 106.3(10) N8 O4 Dy1 104.6(11) N7 O1 Dy1 95.4(7) O2 N7 Dy1 60.6(6) O2 N7 O1 118.4(11) O1 N7 Dy1 58.4(6) O3 N7 Dy1 171.6(8) O3 N7 O2 119.4(11) O3 N7 O1 122.2(11) C24 N6 Dy1 139.2(9) C17 N6 Dy1 116.2(8) C17 N6 C24 104.6(10) O5 N8 O4 111.3(17) O5 N8 O6 132.2(18) O6 N8 O4 116.5(17) C8 N1 C1 125.4(10) C2 N1 C8 108.3(10) C2 N1 C1 126.3(10) N8 O5 Dy1 96.5(11) C19 N5 C17 106.7(11) C19 N5 C18 126.8(10) C17 N5 C18 126.3(10) C5 C6 C7 118.6(11) N9 O8 Dy1 95.9(9) N4 C16 C17 116.3(12) N3 C9 C8 117.9(12) C4 C5 C6 119.5(12) N9 O7 Dy1 99.4(10) N2 C7 C2 107.6(10) C6 C7 N2 131.9(10) C6 C7 C2 120.4(12) O9 N9 Dy1 169.2(11) O9 N9 O8 119.8(15) O9 N9 O7 125.8(16) O8 N9 Dy1 58.4(8) O7 N9 Dy1 56.4(9) O7 N9 O8 114.2(15) N5 C19 C24 107.1(11) N5 C19 C20 135.4(12) C20 C19 C24 117.5(12) C9 N3 Dy1 119.8(9) C9 N3 C10 121.6(10) C10 N3 Dy1 118.6(7) N2 C8 N1 111.1(11) N2 C8 C9 121.1(11) N1 C8 C9 127.7(11) N6 C17 N5 113.6(11) N6 C17 C16 121.1(11) N5 C17 C16 125.4(12) C3 C4 C5 125.0(13) C4 C3 C2 118.2(11) C22 C21 C20 125.5(14) N1 C2 C7 106.6(11) N1 C2 C3 135.2(11) C7 C2 C3 118.2(11) C21 C22 C23 122.0(13) C21 C20 C19 117.6(13) C24 C23 C22 115.2(12) C15 C10 N3 110.7(9) C11 C10 N3 117.7(14) C11 C10 C15 118.0(15) C1AA C10 N3 108.9(15) C1AA C10 C15 113.3(15) C1AA C10 C11 85.5(15) N4 C15 C14 113.7(10) C10 C15 N4 109.4(11) C10 C15 C14 112.9(10) C13 C14 C15 113.0(14) C2AA C14 C15 119.7(16) C2AA C14 C13 65.5(16) C2AA C12 C1AA 100.6(16) C0AA C12 C2AA 80.5(17) C0AA C12 C1AA 102(2) C10 C11 C0AA 109.4(19) C10 C11 C1AA 45.7(11) C0AA C11 C1AA 90.9(18) C14 C13 C2AA 50.0(14) C0AA C13 C14 121(3) C0AA C13 C2AA 101(3) C14 C2AA C12 119(2) C14 C2AA C13 64.5(18) C13 C2AA C12 83.9(19) C12 C0AA C11 86.1(19) C13 C0AA C12 94(2) C13 C0AA C11 119(2) C10 C1AA C12 109(2) C10 C1AA C11 48.8(12) C12 C1AA C11 76.7(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Dy1 O2 2.470(8) Dy1 N4 2.498(10) Dy1 N2 2.498(9) Dy1 O4 2.443(11) Dy1 O1 2.422(8) Dy1 N7 2.831(12) Dy1 N6 2.506(9) Dy1 O5 2.661(11) Dy1 O8 2.478(10) Dy1 O7 2.443(10) Dy1 N9 2.893(15) Dy1 N3 2.572(9) O2 N7 1.243(12) C24 N6 1.388(14) C24 C19 1.423(16) C24 C23 1.362(16) N4 C16 1.259(13) N4 C15 1.529(14) N2 C7 1.394(15) N2 C8 1.322(13) O4 N8 1.273(16) O1 N7 1.255(11) N7 O3 1.221(12) N6 C17 1.321(14) N8 O5 1.172(17) N8 O6 1.192(17) N1 C8 1.359(14) N1 C2 1.343(14) N1 C1 1.476(12) O9 N9 1.187(15) N5 C19 1.334(14) N5 C17 1.363(13) N5 C18 1.457(14) C6 C5 1.374(15) C6 C7 1.386(15) O8 N9 1.259(15) C16 C17 1.449(15) C9 N3 1.240(14) C9 C8 1.390(17) C5 C4 1.371(15) O7 N9 1.201(14) C7 C2 1.404(14) C19 C20 1.422(15) N3 C10 1.532(15) C4 C3 1.283(15) C3 C2 1.442(16) C21 C22 1.293(16) C21 C20 1.310(16) C22 C23 1.419(15) C10 C15 1.416(14) C10 C11 1.39(2) C10 C1AA 1.32(3) C15 C14 1.559(16) C14 C13 1.41(3) C14 C2AA 1.20(3) C12 C2AA 1.64(3) C12 C0AA 1.54(3) C12 C1AA 1.64(3) C11 C0AA 1.63(3) C11 C1AA 1.84(4) C13 C2AA 1.42(4) C13 C0AA 1.24(3)