#------------------------------------------------------------------------------ #$Date: 2020-06-30 07:22:57 +0300 (Tue, 30 Jun 2020) $ #$Revision: 253552 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/07/7240797.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_7240797 loop_ _publ_author_name 'Olyshevets, Iryna' 'Ovchynnikov, Vladimir' 'Kariaka, Nataliia' 'Dyakonenko, Viktoriya' 'Shishkina, Svitlana' 'Sliva, Tatiana' 'Ostrowska, Ma\/lgorzata' 'Jedy\'nczuk, Aleksandra' 'Gumienna-Kontecka, El\.zbieta' 'Amirkhanov, Vladimir' _publ_section_title ; Lanthanide complexes based on a new bis-chelating carbacylamidophosphate (CAPh) scorpionate-like ligand ; _journal_issue 42 _journal_name_full 'RSC Advances' _journal_page_first 24808 _journal_paper_doi 10.1039/D0RA04714G _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C22 H36 N11 O19 P4 Tb, C3 H8 O' _chemical_formula_sum 'C25 H44 N11 O20 P4 Tb' _chemical_formula_weight 1101.51 _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 dual _audit_creation_date 2020-02-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-02-16 deposited with the CCDC. 2020-06-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.506(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.134(2) _cell_length_b 17.152(2) _cell_length_c 19.453(3) _cell_measurement_reflns_used 934 _cell_measurement_temperature 110 _cell_measurement_theta_max 18.6650 _cell_measurement_theta_min 3.2450 _cell_volume 4179.3(11) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 110 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1827 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 9.00 94.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 57.0000 150.0000 85 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 69.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -99.0000 -120.0000 78 #__ type_ start__ end____ width___ exp.time_ 3 omega 26.00 69.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -99.0000 30.0000 43 #__ type_ start__ end____ width___ exp.time_ 4 omega -38.00 11.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -57.0000 -90.0000 49 #__ type_ start__ end____ width___ exp.time_ 5 omega 12.00 38.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -57.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega -14.00 44.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -57.0000 -60.0000 58 #__ type_ start__ end____ width___ exp.time_ 7 omega 36.00 61.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -178.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 8 omega 27.00 57.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 -77.0000 120.0000 30 #__ type_ start__ end____ width___ exp.time_ 9 omega -4.00 99.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 26.7645 19.0000 90.0000 103 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0192364000 _diffrn_orient_matrix_UB_12 0.0071071000 _diffrn_orient_matrix_UB_13 -0.0375927000 _diffrn_orient_matrix_UB_21 -0.0442989000 _diffrn_orient_matrix_UB_22 -0.0246795000 _diffrn_orient_matrix_UB_23 -0.0024423000 _diffrn_orient_matrix_UB_31 -0.0294480000 _diffrn_orient_matrix_UB_32 0.0324787000 _diffrn_orient_matrix_UB_33 0.0063158000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1810 _diffrn_reflns_av_unetI/netI 0.1656 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 33047 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.901 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.935 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.51474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.751 _exptl_crystal_description block _exptl_crystal_F_000 2224 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.858 _refine_diff_density_min -1.602 _refine_diff_density_rms 0.183 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 560 _refine_ls_number_reflns 7352 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.983 _refine_ls_R_factor_all 0.1448 _refine_ls_R_factor_gt 0.0790 _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^)+(0.0753P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1684 _refine_ls_wR_factor_ref 0.2067 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4081 _reflns_number_total 7352 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ra04714g2.cif _cod_data_source_block kiev301_lt _cod_original_cell_volume 4179.6(12) _cod_database_code 7240797 _shelx_shelxl_version_number 2018/1 _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_max 0.698 _shelx_estimated_absorpt_t_min 0.445 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _olex2_refinement_description ; 1. Twinned data refinement Scales: -1(10) 2(10) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 3. Restrained distances O10-C13B 1.45 with sigma of 0.002 O10-C13A 1.45 with sigma of 0.002 4. Uiso/Uaniso restraints and constraints Uanis(C13B) = Uanis(C13A) Uanis(C25) = Uanis(C24) 5. Others Fixed Sof: C13A(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C13B(0.5) H13D(0.5) H13E(0.5) H13F(0.5) 6.a Ternary CH refined with riding coordinates: C23(H23) 6.b Aromatic/amide H refined with riding coordinates: N2(H2), N4(H4), N5(H5), N7(H7), N9(H9), N10(H10), C5(H5A), C6(H6), C7(H7A), C16(H16), C17(H17), C18(H18) 6.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C21(H21A,H21B, H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C) 6.d Idealised tetrahedral OH refined as rotating group: O20(H20) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' '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_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 Tb1 Tb 0.39196(5) 0.20773(3) 0.65651(3) 0.0336(2) Uani 1 1 d . . . . . P1 P 0.4673(3) 0.36753(16) 0.76906(17) 0.0319(7) Uani 1 1 d . . . . . P2 P 0.5030(3) 0.04011(16) 0.76432(17) 0.0334(7) Uani 1 1 d . . . . . P3 P 0.5452(3) 0.1472(2) 0.5476(2) 0.0574(11) Uani 1 1 d . . . . . P4 P 0.2078(3) 0.34581(17) 0.53981(19) 0.0379(8) Uani 1 1 d . . . . . O1 O 0.4623(7) 0.3624(4) 0.8502(4) 0.039(2) Uani 1 1 d . . . . . O2 O 0.4412(6) 0.4556(4) 0.7467(4) 0.0324(18) Uani 1 1 d . . . . . O3 O 0.3816(7) 0.3137(4) 0.7271(4) 0.039(2) Uani 1 1 d . . . . . O4 O 0.5667(6) 0.2273(4) 0.7349(4) 0.0311(18) Uani 1 1 d . . . . . O5 O 0.6659(6) -0.0723(4) 0.7393(4) 0.0352(19) Uani 1 1 d . . . . . O6 O 0.4530(7) -0.0414(4) 0.7384(4) 0.039(2) Uani 1 1 d . . . . . O7 O 0.5452(7) 0.0290(4) 0.8464(4) 0.040(2) Uani 1 1 d . . . . . O8 O 0.4282(7) 0.1052(4) 0.7393(4) 0.035(2) Uani 1 1 d . . . . . O9 O 0.4889(8) 0.1292(6) 0.4660(5) 0.069(3) Uani 1 1 d . . . . . O10 O 0.6370(8) 0.0854(6) 0.5681(6) 0.084(4) Uani 1 1 d D . . . . O11 O 0.4732(7) 0.1312(4) 0.5913(4) 0.040(2) Uani 1 1 d . . . . . O12 O 0.4757(7) 0.2964(4) 0.5961(4) 0.0349(19) Uani 1 1 d . . . . . O13 O 0.1822(7) 0.5212(4) 0.5319(5) 0.045(2) Uani 1 1 d . . . . . O14 O 0.2586(7) 0.2710(4) 0.5672(4) 0.042(2) Uani 1 1 d . . . . . O15 O 0.1060(8) 0.3639(5) 0.5605(5) 0.056(3) Uani 1 1 d . . . . . O16 O 0.1681(8) 0.3495(5) 0.4545(4) 0.052(2) Uani 1 1 d . . . . . O17 O 0.2178(7) 0.1754(4) 0.6775(4) 0.040(2) Uani 1 1 d . . . . . O18 O 0.0975(8) 0.0999(5) 0.6073(6) 0.064(3) Uani 1 1 d . . . . . O19 O 0.2593(7) 0.1077(4) 0.5959(5) 0.042(2) Uani 1 1 d . . . . . N1 N 0.5867(7) 0.3573(4) 0.7663(5) 0.024(2) Uani 1 1 d . . . . . N2 N 0.7244(7) 0.2883(5) 0.7492(5) 0.033(2) Uani 1 1 d . . . . . H2 H 0.757567 0.333134 0.761301 0.039 Uiso 1 1 calc R . . . . N3 N 0.7522(8) 0.1564(5) 0.7324(5) 0.027(2) Uani 1 1 d . . . . . N4 N 0.7753(8) 0.0215(5) 0.7238(5) 0.034(2) Uani 1 1 d . . . . . H4 H 0.817921 -0.015608 0.717679 0.041 Uiso 1 1 calc R . . . . N5 N 0.6115(8) 0.0529(4) 0.7404(5) 0.032(2) Uani 1 1 d . . . . . H5 H 0.626083 0.101054 0.730964 0.038 Uiso 1 1 calc R . . . . N6 N 0.6005(9) 0.2323(6) 0.5543(6) 0.046(3) Uani 1 1 d . . . . . N7 N 0.6237(8) 0.3600(7) 0.5823(6) 0.050(3) Uani 1 1 d . . . . . H7 H 0.689196 0.351978 0.580893 0.060 Uiso 1 1 calc R . . . . N8 N 0.4918(8) 0.4543(5) 0.5839(5) 0.035(2) Uani 1 1 d . . . . . N9 N 0.3580(9) 0.5444(5) 0.5740(5) 0.041(3) Uani 1 1 d . . . . . H9 H 0.342436 0.593129 0.580855 0.049 Uiso 1 1 calc R . . . . N10 N 0.2947(7) 0.4163(5) 0.5632(5) 0.033(2) Uani 1 1 d . . . . . H10 H 0.361785 0.403318 0.583929 0.039 Uiso 1 1 calc R . . . . N11 N 0.1892(9) 0.1276(6) 0.6269(7) 0.049(3) Uani 1 1 d . . . . . C1 C 0.5308(11) 0.4112(6) 0.9041(7) 0.046(3) Uani 1 1 d . . . . . H1A H 0.508190 0.465611 0.894805 0.069 Uiso 1 1 calc GR . . . . H1B H 0.604436 0.405695 0.902692 0.069 Uiso 1 1 calc GR . . . . H1C H 0.526842 0.395655 0.951686 0.069 Uiso 1 1 calc GR . . . . C2 C 0.3365(9) 0.4868(7) 0.7453(7) 0.040(3) Uani 1 1 d . . . . . H2A H 0.280885 0.463007 0.705487 0.061 Uiso 1 1 calc GR . . . . H2B H 0.335893 0.543466 0.738575 0.061 Uiso 1 1 calc GR . . . . H2C H 0.322843 0.474828 0.791010 0.061 Uiso 1 1 calc GR . . . . C3 C 0.6204(9) 0.2889(6) 0.7492(5) 0.024(2) Uani 1 1 d . . . . . C4 C 0.7880(10) 0.2296(6) 0.7336(6) 0.034(3) Uani 1 1 d . . . . . C5 C 0.8822(9) 0.2487(6) 0.7204(6) 0.033(3) Uani 1 1 d . . . . . H5A H 0.903829 0.301410 0.719693 0.040 Uiso 1 1 calc R . . . . C6 C 0.9441(11) 0.1880(7) 0.7084(7) 0.043(3) Uani 1 1 d . . . . . H6 H 1.010397 0.198713 0.700054 0.052 Uiso 1 1 calc R . . . . C7 C 0.9093(10) 0.1116(6) 0.7084(6) 0.037(3) Uani 1 1 d . . . . . H7A H 0.949769 0.069079 0.699199 0.044 Uiso 1 1 calc R . . . . C8 C 0.8141(9) 0.1001(6) 0.7224(6) 0.029(3) Uani 1 1 d . . . . . C9 C 0.6817(10) -0.0033(6) 0.7334(7) 0.036(3) Uani 1 1 d . . . . . C10 C 0.4086(12) -0.0558(8) 0.6612(7) 0.057(4) Uani 1 1 d . . . . . H10A H 0.439093 -0.018519 0.634631 0.085 Uiso 1 1 calc GR . . . . H10B H 0.330900 -0.049403 0.646903 0.085 Uiso 1 1 calc GR . . . . H10C H 0.426066 -0.108977 0.650312 0.085 Uiso 1 1 calc GR . . . . C11 C 0.4719(11) 0.0338(7) 0.8907(7) 0.046(3) Uani 1 1 d . . . . . H11A H 0.421204 -0.009639 0.878673 0.069 Uiso 1 1 calc GR . . . . H11B H 0.432826 0.083275 0.881068 0.069 Uiso 1 1 calc GR . . . . H11C H 0.513026 0.031059 0.941866 0.069 Uiso 1 1 calc GR . . . . C12 C 0.3950(14) 0.1699(9) 0.4314(9) 0.080(5) Uani 1 1 d . . . . . H12A H 0.380004 0.165426 0.379041 0.119 Uiso 1 1 calc GR . . . . H12B H 0.403850 0.224972 0.445328 0.119 Uiso 1 1 calc GR . . . . H12C H 0.335520 0.147772 0.445537 0.119 Uiso 1 1 calc GR . . . . C13A C 0.633(3) 0.0102(9) 0.5335(15) 0.088(9) Uani 0.5 1 d D . P A 1 H13A H 0.595945 -0.027236 0.555593 0.133 Uiso 0.5 1 calc GR . P A 1 H13B H 0.705858 -0.008134 0.539511 0.133 Uiso 0.5 1 calc GR . P A 1 H13C H 0.594628 0.015150 0.482043 0.133 Uiso 0.5 1 calc GR . P A 1 C13B C 0.716(2) 0.0638(18) 0.5330(16) 0.088(9) Uani 0.5 1 d D . P A 2 H13D H 0.679694 0.041418 0.485537 0.133 Uiso 0.5 1 calc GR . P A 2 H13E H 0.764792 0.025204 0.562493 0.133 Uiso 0.5 1 calc GR . P A 2 H13F H 0.755994 0.110145 0.527144 0.133 Uiso 0.5 1 calc GR . P A 2 C14 C 0.5584(10) 0.2927(7) 0.5764(6) 0.040(3) Uani 1 1 d . . . . . C15 C 0.5957(10) 0.4373(7) 0.5899(7) 0.041(3) Uani 1 1 d . . . . . C16 C 0.6726(12) 0.4948(9) 0.5982(7) 0.054(4) Uani 1 1 d . . . . . H16 H 0.743406 0.481936 0.599361 0.065 Uiso 1 1 calc R . . . . C17 C 0.6442(13) 0.5703(9) 0.6046(7) 0.060(4) Uani 1 1 d . . . . . H17 H 0.696853 0.610063 0.613551 0.072 Uiso 1 1 calc R . . . . C18 C 0.5399(13) 0.5894(7) 0.5983(7) 0.052(4) Uani 1 1 d . . . . . H18 H 0.519176 0.641780 0.602469 0.062 Uiso 1 1 calc R . . . . C19 C 0.4663(11) 0.5288(7) 0.5857(7) 0.040(3) Uani 1 1 d . . . . . C20 C 0.2718(10) 0.4940(6) 0.5533(7) 0.038(3) Uani 1 1 d . . . . . C21 C 0.0888(13) 0.3346(7) 0.6240(8) 0.058(4) Uani 1 1 d . . . . . H21A H 0.091146 0.277547 0.623512 0.086 Uiso 1 1 calc GR . . . . H21B H 0.018718 0.351791 0.626330 0.086 Uiso 1 1 calc GR . . . . H21C H 0.144501 0.354284 0.666120 0.086 Uiso 1 1 calc GR . . . . C22 C 0.1070(11) 0.2882(6) 0.4138(6) 0.045(3) Uani 1 1 d . . . . . H22A H 0.082075 0.303211 0.362807 0.068 Uiso 1 1 calc GR . . . . H22B H 0.045477 0.277653 0.430902 0.068 Uiso 1 1 calc GR . . . . H22C H 0.151237 0.241222 0.419243 0.068 Uiso 1 1 calc GR . . . . O20 O 0.6741(11) 0.2890(6) 0.4414(7) 0.089(4) Uani 1 1 d . . . . . H20 H 0.651926 0.262985 0.470543 0.133 Uiso 1 1 calc GR . . . . C23 C 0.7523(13) 0.2469(9) 0.4228(8) 0.063(4) Uani 1 1 d . . . . . H23 H 0.733399 0.190280 0.417148 0.075 Uiso 1 1 calc R . . . . C24 C 0.7596(17) 0.2804(11) 0.3532(9) 0.100(5) Uani 1 1 d . . . . . H24A H 0.687550 0.289978 0.320807 0.151 Uiso 1 1 calc GR . . . . H24B H 0.796582 0.243438 0.330516 0.151 Uiso 1 1 calc GR . . . . H24C H 0.799345 0.329534 0.362727 0.151 Uiso 1 1 calc GR . . . . C25 C 0.8463(17) 0.2594(12) 0.4845(10) 0.100(5) Uani 1 1 d . . . . . H25A H 0.826241 0.288894 0.521533 0.151 Uiso 1 1 calc GR . . . . H25B H 0.899810 0.288745 0.469217 0.151 Uiso 1 1 calc GR . . . . H25C H 0.876240 0.208899 0.504189 0.151 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 Tb1 0.0297(4) 0.0360(3) 0.0335(4) -0.0004(3) 0.0071(3) 0.0000(3) P1 0.0301(19) 0.0308(15) 0.0334(18) -0.0016(13) 0.0072(16) 0.0019(13) P2 0.0335(19) 0.0327(15) 0.0334(18) 0.0014(13) 0.0092(17) -0.0016(13) P3 0.050(3) 0.080(3) 0.042(2) -0.0113(19) 0.012(2) 0.019(2) P4 0.031(2) 0.0397(17) 0.044(2) 0.0004(15) 0.0121(18) -0.0026(14) O1 0.036(5) 0.050(5) 0.029(5) -0.003(4) 0.007(4) -0.003(4) O2 0.027(5) 0.037(4) 0.031(4) -0.005(3) 0.005(4) -0.002(3) O3 0.041(6) 0.042(4) 0.038(5) -0.011(4) 0.017(5) 0.001(4) O4 0.026(5) 0.036(4) 0.031(5) 0.009(3) 0.007(4) 0.000(3) O5 0.020(5) 0.030(4) 0.054(5) 0.001(4) 0.008(4) -0.004(3) O6 0.043(6) 0.036(4) 0.037(5) -0.003(4) 0.010(5) -0.002(4) O7 0.038(5) 0.051(5) 0.030(5) 0.010(4) 0.010(4) 0.009(4) O8 0.041(5) 0.033(4) 0.033(5) 0.004(3) 0.015(4) 0.002(4) O9 0.040(6) 0.123(8) 0.033(6) -0.016(6) -0.005(5) 0.012(6) O10 0.047(7) 0.124(9) 0.065(7) -0.025(7) -0.006(6) 0.043(6) O11 0.039(5) 0.046(4) 0.041(5) -0.016(4) 0.020(5) 0.008(4) O12 0.032(5) 0.044(4) 0.033(5) 0.003(4) 0.016(4) 0.000(4) O13 0.045(6) 0.051(5) 0.045(6) 0.006(4) 0.023(5) 0.009(4) O14 0.036(6) 0.048(5) 0.041(5) 0.009(4) 0.007(5) 0.008(4) O15 0.059(7) 0.047(5) 0.072(7) 0.007(5) 0.034(6) 0.001(4) O16 0.062(7) 0.048(5) 0.028(5) 0.002(4) -0.014(5) -0.005(4) O17 0.034(5) 0.043(4) 0.036(5) -0.006(4) 0.001(5) -0.004(4) O18 0.047(7) 0.066(6) 0.072(7) -0.008(5) 0.008(6) -0.026(5) O19 0.035(6) 0.038(4) 0.046(5) -0.013(4) 0.002(5) 0.001(4) N1 0.014(5) 0.021(4) 0.034(5) -0.005(4) 0.000(5) 0.002(3) N2 0.023(6) 0.031(5) 0.040(6) 0.003(4) 0.004(5) -0.002(4) N3 0.031(6) 0.034(5) 0.019(5) -0.001(4) 0.013(5) 0.009(4) N4 0.027(6) 0.025(4) 0.043(6) -0.003(4) 0.001(5) 0.006(4) N5 0.045(7) 0.012(4) 0.042(6) -0.008(4) 0.018(6) -0.004(4) N6 0.045(8) 0.057(6) 0.040(7) 0.009(5) 0.019(6) 0.013(5) N7 0.015(6) 0.085(8) 0.044(7) 0.009(6) -0.001(6) -0.009(6) N8 0.028(6) 0.047(6) 0.025(5) 0.002(4) -0.001(5) -0.008(5) N9 0.050(8) 0.042(5) 0.034(6) 0.000(5) 0.016(6) -0.004(5) N10 0.012(5) 0.044(5) 0.038(6) 0.009(4) 0.002(5) 0.007(4) N11 0.034(7) 0.039(6) 0.068(9) 0.008(6) 0.004(7) -0.014(5) C1 0.051(9) 0.036(6) 0.046(8) -0.002(6) 0.007(8) 0.006(6) C2 0.015(7) 0.054(7) 0.048(8) -0.005(6) 0.004(6) 0.000(5) C3 0.021(6) 0.033(6) 0.016(5) -0.001(5) 0.002(5) -0.001(5) C4 0.032(8) 0.030(6) 0.034(7) 0.008(5) 0.000(6) 0.005(5) C5 0.025(7) 0.035(6) 0.047(8) -0.001(5) 0.022(7) 0.006(5) C6 0.041(8) 0.052(7) 0.038(8) -0.007(6) 0.014(7) -0.016(6) C7 0.050(9) 0.032(6) 0.028(7) 0.012(5) 0.012(7) 0.007(5) C8 0.020(6) 0.032(6) 0.032(7) 0.000(5) 0.003(6) 0.002(5) C9 0.031(8) 0.031(6) 0.042(8) -0.001(5) 0.007(7) -0.002(5) C10 0.071(12) 0.057(8) 0.045(9) 0.005(7) 0.022(9) -0.003(7) C11 0.042(9) 0.056(8) 0.049(8) -0.002(6) 0.027(8) -0.001(6) C12 0.072(14) 0.096(12) 0.059(11) -0.002(9) 0.001(11) 0.019(10) C13A 0.11(3) 0.068(16) 0.092(18) 0.044(15) 0.036(19) 0.056(15) C13B 0.11(3) 0.068(16) 0.092(18) 0.044(15) 0.036(19) 0.056(15) C14 0.023(7) 0.078(9) 0.024(7) 0.028(6) 0.013(6) 0.021(7) C15 0.034(8) 0.062(8) 0.034(7) 0.015(6) 0.021(7) -0.007(6) C16 0.035(9) 0.082(10) 0.048(9) 0.010(8) 0.016(8) -0.020(7) C17 0.045(10) 0.095(12) 0.032(8) 0.004(8) 0.001(8) -0.039(9) C18 0.066(11) 0.056(8) 0.036(8) -0.005(6) 0.019(9) -0.015(7) C19 0.037(8) 0.050(7) 0.035(8) 0.000(6) 0.015(7) -0.007(6) C20 0.031(8) 0.031(6) 0.048(8) 0.020(6) 0.008(7) 0.009(6) C21 0.058(11) 0.061(8) 0.057(10) 0.012(7) 0.022(9) 0.009(7) C22 0.061(10) 0.044(7) 0.027(7) -0.002(6) 0.006(7) 0.000(6) O20 0.129(12) 0.077(7) 0.095(9) 0.036(6) 0.087(9) 0.044(7) C23 0.056(11) 0.092(11) 0.049(9) -0.006(8) 0.029(9) 0.027(9) C24 0.093(12) 0.149(12) 0.068(9) 0.027(9) 0.037(10) 0.000(9) C25 0.093(12) 0.149(12) 0.068(9) 0.027(9) 0.037(10) 0.000(9) 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O4 74.0(3) . . ? O3 Tb1 O8 102.7(3) . . ? O3 Tb1 O12 84.8(3) . . ? O3 Tb1 O14 84.9(3) . . ? O3 Tb1 O17 81.8(3) . . ? O3 Tb1 O19 132.1(3) . . ? O3 Tb1 N11 106.1(3) . . ? O4 Tb1 O12 74.0(3) . . ? O4 Tb1 O17 133.1(3) . . ? O4 Tb1 O19 144.3(2) . . ? O4 Tb1 N11 148.3(3) . . ? O8 Tb1 O4 72.9(3) . . ? O8 Tb1 O12 142.4(3) . . ? O8 Tb1 O17 74.2(3) . . ? O8 Tb1 O19 77.0(3) . . ? O8 Tb1 N11 76.4(3) . . ? O11 Tb1 O3 154.0(3) . . ? O11 Tb1 O4 85.1(3) . . ? O11 Tb1 O8 85.3(3) . . ? O11 Tb1 O12 74.5(3) . . ? O11 Tb1 O14 103.0(3) . . ? O11 Tb1 O17 124.2(3) . . ? O11 Tb1 O19 73.7(3) . . ? O11 Tb1 N11 99.8(3) . . ? O12 Tb1 O17 143.3(3) . . ? O12 Tb1 O19 124.8(3) . . ? O12 Tb1 N11 137.5(3) . . ? O14 Tb1 O4 141.2(3) . . ? O14 Tb1 O8 144.7(3) . . ? O14 Tb1 O12 72.0(3) . . ? O14 Tb1 O17 72.9(3) . . ? O14 Tb1 O19 72.8(3) . . ? O14 Tb1 N11 68.5(3) . . ? O17 Tb1 N11 25.5(3) . . ? O19 Tb1 O17 51.5(3) . . ? O19 Tb1 N11 26.3(3) . . ? O2 P1 O1 104.7(4) . . ? O2 P1 N1 103.3(4) . . ? O3 P1 O1 104.9(4) . . ? O3 P1 O2 112.0(5) . . ? O3 P1 N1 120.0(4) . . ? N1 P1 O1 111.1(5) . . ? O6 P2 N5 110.1(4) . . ? O7 P2 O6 102.1(4) . . ? O7 P2 N5 103.8(5) . . ? O8 P2 O6 113.5(5) . . ? O8 P2 O7 115.8(4) . . ? O8 P2 N5 110.8(4) . . ? O9 P3 N6 108.8(6) . . ? O10 P3 O9 102.5(6) . . ? O10 P3 N6 107.3(6) . . ? O11 P3 O9 111.0(6) . . ? O11 P3 O10 107.8(6) . . ? O11 P3 N6 118.1(5) . . ? O14 P4 O15 114.6(5) . . ? O14 P4 O16 112.7(5) . . ? O14 P4 N10 110.0(5) . . ? O15 P4 O16 103.2(6) . . ? O15 P4 N10 111.6(5) . . ? O16 P4 N10 104.2(5) . . ? C1 O1 P1 119.1(7) . . ? C2 O2 P1 118.5(7) . . ? P1 O3 Tb1 130.0(5) . . ? C3 O4 Tb1 129.3(7) . . ? C10 O6 P2 118.8(7) . . ? C11 O7 P2 120.4(8) . . ? P2 O8 Tb1 141.0(4) . . ? C12 O9 P3 117.9(9) . . ? C13A O10 P3 124.6(15) . . ? C13B O10 P3 131.1(14) . . ? P3 O11 Tb1 134.1(4) . . ? C14 O12 Tb1 133.4(7) . . ? P4 O14 Tb1 146.5(5) . . ? C21 O15 P4 122.5(9) . . ? C22 O16 P4 120.8(7) . . ? N11 O17 Tb1 95.1(7) . . ? N11 O19 Tb1 95.4(6) . . ? C3 N1 P1 120.7(7) . . ? C3 N2 H2 114.1 . . ? C3 N2 C4 131.9(9) . . ? C4 N2 H2 114.1 . . ? C8 N3 C4 117.5(10) . . ? C8 N4 H4 115.4 . . ? C9 N4 H4 115.4 . . ? C9 N4 C8 129.2(9) . . ? P2 N5 H5 116.5 . . ? C9 N5 P2 127.1(7) . . ? C9 N5 H5 116.5 . . ? C14 N6 P3 121.2(10) . . ? C14 N7 H7 116.3 . . ? C15 N7 H7 116.3 . . ? C15 N7 C14 127.4(11) . . ? C19 N8 C15 117.3(10) . . ? C19 N9 H9 115.5 . . ? C20 N9 H9 115.5 . . ? C20 N9 C19 129.1(10) . . ? P4 N10 H10 117.4 . . ? C20 N10 P4 125.2(9) . . ? C20 N10 H10 117.4 . . ? O17 N11 Tb1 59.4(6) . . ? O17 N11 O19 117.0(10) . . ? O18 N11 Tb1 172.0(9) . . ? O18 N11 O17 121.8(12) . . ? O18 N11 O19 121.2(12) . . ? O19 N11 Tb1 58.3(5) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 N1 126.2(10) . . ? O4 C3 N2 119.3(9) . . ? N1 C3 N2 114.5(9) . . ? N3 C4 N2 116.7(10) . . ? N3 C4 C5 123.4(10) . . ? C5 C4 N2 119.9(9) . . ? C4 C5 H5A 121.3 . . ? C4 C5 C6 117.5(10) . . ? C6 C5 H5A 121.3 . . ? C5 C6 H6 120.0 . . ? C5 C6 C7 120.0(12) . . ? C7 C6 H6 120.0 . . ? C6 C7 H7A 121.4 . . ? C8 C7 C6 117.1(11) . . ? C8 C7 H7A 121.4 . . ? N3 C8 N4 116.4(10) . . ? N3 C8 C7 124.4(10) . . ? C7 C8 N4 119.2(9) . . ? O5 C9 N4 120.2(10) . . ? O5 C9 N5 122.6(11) . . ? N4 C9 N5 117.1(9) . . ? O6 C10 H10A 109.5 . . ? O6 C10 H10B 109.5 . . ? O6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O7 C11 H11A 109.5 . . ? O7 C11 H11B 109.5 . . ? O7 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 H12A 109.5 . . ? O9 C12 H12B 109.5 . . ? O9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13A H13A 109.5 . . ? O10 C13A H13B 109.5 . . ? O10 C13A H13C 109.5 . . ? H13A C13A H13B 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? O10 C13B H13D 109.5 . . ? O10 C13B H13E 109.5 . . ? O10 C13B H13F 109.5 . . ? H13D C13B H13E 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? O12 C14 N6 129.1(12) . . ? O12 C14 N7 119.4(11) . . ? N6 C14 N7 111.4(11) . . ? N8 C15 N7 118.8(10) . . ? N8 C15 C16 122.1(12) . . ? C16 C15 N7 118.9(12) . . ? C15 C16 H16 120.8 . . ? C17 C16 C15 118.5(14) . . ? C17 C16 H16 120.8 . . ? C16 C17 H17 119.7 . . ? C16 C17 C18 120.6(13) . . ? C18 C17 H17 119.7 . . ? C17 C18 H18 121.4 . . ? C17 C18 C19 117.3(13) . . ? C19 C18 H18 121.4 . . ? N8 C19 N9 115.8(10) . . ? N8 C19 C18 123.9(13) . . ? C18 C19 N9 120.3(11) . . ? O13 C20 N9 118.8(10) . . ? O13 C20 N10 124.9(11) . . ? N10 C20 N9 116.2(11) . . ? O15 C21 H21A 109.5 . . ? O15 C21 H21B 109.5 . . ? O15 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O16 C22 H22A 109.5 . . ? O16 C22 H22B 109.5 . . ? O16 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 O20 H20 109.5 . . ? O20 C23 H23 110.8 . . ? O20 C23 C24 106.8(13) . . ? O20 C23 C25 102.6(13) . . ? C24 C23 H23 110.8 . . ? C25 C23 H23 110.8 . . ? C25 C23 C24 114.8(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 Tb1 O3 2.307(7) . ? Tb1 O4 2.366(8) . ? Tb1 O8 2.335(7) . ? Tb1 O11 2.298(6) . ? Tb1 O12 2.384(7) . ? Tb1 O14 2.331(8) . ? Tb1 O17 2.504(8) . ? Tb1 O19 2.476(8) . ? Tb1 N11 2.897(10) . ? P1 O1 1.602(8) . ? P1 O2 1.582(7) . ? P1 O3 1.494(9) . ? P1 N1 1.595(9) . ? P2 O6 1.562(8) . ? P2 O7 1.537(8) . ? P2 O8 1.470(8) . ? P2 N5 1.642(9) . ? P3 O9 1.567(10) . ? P3 O10 1.565(10) . ? P3 O11 1.475(8) . ? P3 N6 1.618(11) . ? P4 O14 1.470(8) . ? P4 O15 1.540(9) . ? P4 O16 1.584(8) . ? P4 N10 1.632(9) . ? O1 C1 1.428(14) . ? O2 C2 1.469(13) . ? O4 C3 1.254(12) . ? O5 C9 1.213(11) . ? O6 C10 1.459(14) . ? O7 C11 1.475(12) . ? O9 C12 1.400(17) . ? O10 C13A 1.449(2) . ? O10 C13B 1.449(2) . ? O12 C14 1.256(13) . ? O13 C20 1.217(14) . ? O15 C21 1.412(14) . ? O16 C22 1.412(13) . ? O17 N11 1.250(13) . ? O18 N11 1.243(13) . ? O19 N11 1.289(13) . ? N1 C3 1.332(12) . ? N2 H2 0.8800 . ? N2 C3 1.366(13) . ? N2 C4 1.398(13) . ? N3 C4 1.339(13) . ? N3 C8 1.315(12) . ? N4 H4 0.8800 . ? N4 C8 1.444(12) . ? N4 C9 1.366(14) . ? N5 H5 0.8800 . ? N5 C9 1.367(13) . ? N6 C14 1.307(14) . ? N7 H7 0.8800 . ? N7 C14 1.422(16) . ? N7 C15 1.395(15) . ? N8 C15 1.365(15) . ? N8 C19 1.324(14) . ? N9 H9 0.8800 . ? N9 C19 1.397(15) . ? N9 C20 1.386(15) . ? N10 H10 0.8800 . ? N10 C20 1.366(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C5 1.375(15) . ? C5 H5A 0.9500 . ? C5 C6 1.383(15) . ? C6 H6 0.9500 . ? C6 C7 1.389(14) . ? C7 H7A 0.9500 . ? C7 C8 1.371(15) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C15 C16 1.386(17) . ? C16 H16 0.9500 . ? C16 C17 1.363(19) . ? C17 H17 0.9500 . ? C17 C18 1.38(2) . ? C18 H18 0.9500 . ? C18 C19 1.390(17) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O20 H20 0.8400 . ? O20 C23 1.390(15) . ? C23 H23 1.0000 . ? C23 C24 1.500(19) . ? C23 C25 1.46(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2 O5 0.88 1.91 2.765(11) 163.6 2_656 yes N5 H5 N3 0.88 1.90 2.601(12) 135.1 . yes N9 H9 O20 0.88 2.06 2.891(13) 155.9 3_666 yes N10 H10 N8 0.88 1.92 2.581(13) 130.7 . yes C13A H13A O9 0.98 2.05 2.88(3) 141.4 3_656 yes O20 H20 N6 0.84 2.01 2.826(13) 162.7 . yes loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 -1(10) 2 2(10)