#------------------------------------------------------------------------------ #$Date: 2021-07-31 11:27:07 +0300 (Sat, 31 Jul 2021) $ #$Revision: 267856 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564291.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_1564291 loop_ _publ_author_name 'Boukhemis, Ouafa' 'Bendjeddou, Lamia' 'Platas-Iglesias, Carlos' 'Esteban-G\'omez, David' 'Carcelli, Mauro' 'Merazig, Hocine' _publ_section_title ; Hydrothermal synthesis of six new lanthanides coordination polymers based on 1-H-benzimidazole-5-carboxylic acid: Structure, Hirshfeld analysis, thermal and spectroscopic properties ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119740 _journal_paper_doi 10.1016/j.ica.2020.119740 _journal_volume 510 _journal_year 2020 _chemical_absolute_configuration . _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C24 H17 Gd N6 O7' _chemical_formula_sum 'C24 H17 Gd N6 O7' _chemical_formula_weight 658.69 _chemical_name_systematic ; Catena-Poly [aqua( \m3-1H-benzimidazole-5-carboxylato \k4 N:O^5^ ,O^5^', O^5^') ( \m2-1H-benzimidazole-5-carboxylato \k2 O^5^ ,O^5^') ( \m2-1H-benzimidazole-5-carboxylato \k2 O^5^ ,O^5^')gadolinium(III)] ; _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 103.662(1) _cell_angle_beta 97.485(1) _cell_angle_gamma 109.596(1) _cell_formula_units_Z 2 _cell_length_a 8.8513(2) _cell_length_b 11.7031(2) _cell_length_c 12.2157(3) _cell_measurement_reflns_used 9908 _cell_measurement_temperature 296 _cell_measurement_theta_max 36.39 _cell_measurement_theta_min 2.52 _cell_volume 1127.64(4) _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPIII (Farrugia, 2012)' _computing_publication_material ; WinGX (Farrugia, 2012), Mercury (Version 1.4; Macrae et al., 2006) and POVRay (Persistence of Vision Team, 2004) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SIR2002 (Burla et al, 2003)' _diffrn_ambient_temperature 296 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_unetI/netI 0.0098 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 25021 _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 3.58 _exptl_absorpt_coefficient_mu 3.003 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.6197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0632 before and 0.0252 after correction. The Ratio of minimum to maximum transmission is 0.8295. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.94 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 646 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.706 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 349 _refine_ls_number_reflns 5575 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0127 _refine_ls_R_factor_gt 0.0123 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'W=1/[\S^2^(FO^2^)+(0.0147P)^2^+0.6688P] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0314 _reflns_number_gt 5460 _reflns_number_total 5575 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ICA-2020-510-119740.cif _cod_data_source_block 6 _cod_original_formula_sum 'C24 H17 Gd N6 O7 ' _cod_database_code 1564291 _shelx_res_file ; TITL Lamia_Gd_0m_a.res in P-1 lamia_Gd_0m_a.res created by SHELXL-2018/3 at 05:59:22 on 31-Oct-2019 REM Old TITL Lamia_Gd_0m in P-1 REM SHELXT solution in P-1 REM R1 0.058, Rweak 0.009, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C28 N2 O7 Gd CELL 0.71073 8.8513 11.7031 12.2157 103.662 97.485 109.596 ZERR 2 0.0002 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H Gd N O UNIT 48 34 2 12 14 DFIX 0.85 0.01 H1W O1W DFIX 0.85 0.01 H2W O1W DFIX 1.39 H1W H2W L.S. 4 PLAN 20 TEMP 23 BOND $H LIST 4 fmap 2 acta SHEL 50 0.75 OMIT 0 0 1 OMIT 0 1 0 OMIT -1 1 0 OMIT 0 1 1 OMIT 0 -1 2 OMIT 0 0 2 OMIT -1 2 0 OMIT -1 0 2 OMIT -1 -2 1 OMIT 1 -1 1 OMIT 1 1 0 OMIT 0 -2 1 OMIT 0 2 0 OMIT 0 -2 4 WGHT 0.014700 0.668800 FVAR 0.62235 GD1 5 0.232840 0.116822 0.512058 11.00000 0.01076 0.01307 = 0.01912 0.00725 0.00179 0.00445 O3 4 0.494157 0.159802 0.637120 11.00000 0.01555 0.01898 = 0.02432 0.00602 -0.00010 0.00645 O7 4 0.108974 0.265436 0.505309 11.00000 0.01396 0.02034 = 0.03528 0.01033 0.00250 0.00853 O2 4 -0.067820 -0.052129 0.680229 11.00000 0.01631 0.03067 = 0.02139 0.00820 0.00010 0.00626 O1W 4 0.355966 0.008422 0.376438 11.00000 0.02360 0.01995 = 0.02517 0.00912 0.00740 0.01203 AFIX 2 H2W 2 0.355775 0.016841 0.310967 11.00000 -1.50000 H1W 2 0.399251 -0.039906 0.377730 11.00000 -1.50000 AFIX 0 O1 4 0.147491 0.120187 0.688562 11.00000 0.02484 0.02316 = 0.02117 0.00988 0.00518 0.00858 O5 4 -0.109547 0.096013 0.492476 11.00000 0.02434 0.01595 = 0.02794 0.01112 0.00646 0.00901 O4 4 0.434689 0.330039 0.683368 11.00000 0.01901 0.02132 = 0.03818 0.01324 0.00401 0.00936 N5 3 -0.574764 0.275809 0.431569 11.00000 0.01479 0.01827 = 0.02815 0.01154 0.00627 0.00810 C16 1 1.258787 0.471880 0.875552 11.00000 0.01743 0.03307 = 0.03268 0.01006 -0.00048 0.00356 AFIX 43 H16 2 1.369132 0.482538 0.891717 11.00000 -1.20000 AFIX 0 N1 3 0.540554 0.188443 1.075085 11.00000 0.02206 0.02641 = 0.02361 0.00435 -0.00256 0.00220 AFIX 43 H1N 2 0.616743 0.251442 1.065533 11.00000 -1.20000 AFIX 0 N3 3 1.136993 0.358797 0.815635 11.00000 0.01843 0.02613 = 0.03470 0.00667 0.00086 0.00791 AFIX 43 H3N 2 1.147598 0.287900 0.787944 11.00000 -1.20000 AFIX 0 C22 1 -0.410851 0.295804 0.428463 11.00000 0.01363 0.01543 = 0.02029 0.00783 0.00372 0.00545 N4 3 1.208655 0.565363 0.909039 11.00000 0.02016 0.02691 = 0.02814 0.00615 -0.00152 -0.00032 C7 1 0.313977 0.121326 0.896136 11.00000 0.02103 0.02336 = 0.02189 0.00942 0.00272 0.00420 AFIX 43 H7 2 0.366530 0.183233 0.863112 11.00000 -1.20000 AFIX 0 C19 1 -0.090581 0.372925 0.399119 11.00000 0.01408 0.01827 = 0.02417 0.00981 0.00491 0.00466 AFIX 43 H19 2 0.017006 0.397018 0.389494 11.00000 -1.20000 AFIX 0 C8 1 0.546822 0.140337 1.165043 11.00000 0.02861 0.03239 = 0.01979 0.00216 -0.00234 0.01177 AFIX 43 H8 2 0.638706 0.172455 1.226204 11.00000 -1.20000 AFIX 0 N2 3 0.412203 0.044372 1.158856 11.00000 0.03285 0.03314 = 0.01919 0.00757 -0.00018 0.01223 C20 1 -0.185471 0.437859 0.368838 11.00000 0.01834 0.01591 = 0.02337 0.01055 0.00488 0.00464 AFIX 43 H20 2 -0.144295 0.505136 0.338890 11.00000 -1.20000 AFIX 0 C18 1 -0.153094 0.270600 0.444446 11.00000 0.01334 0.01474 = 0.01948 0.00697 0.00178 0.00594 N6 3 -0.472554 0.438789 0.361618 11.00000 0.01957 0.01923 = 0.03089 0.01435 0.00570 0.01034 AFIX 43 H6N 2 -0.469069 0.500224 0.333565 11.00000 -1.20000 AFIX 0 C3 1 0.080935 -0.065699 0.892273 11.00000 0.02134 0.02450 = 0.02535 0.00913 0.00090 0.00130 AFIX 43 H3 2 -0.021757 -0.128083 0.853061 11.00000 -1.20000 AFIX 0 C15 1 0.830151 0.300689 0.752376 11.00000 0.01921 0.01640 = 0.02561 0.00393 -0.00020 0.00446 AFIX 43 H15 2 0.802043 0.215145 0.713973 11.00000 -1.20000 AFIX 0 C10 1 0.712068 0.354519 0.756711 11.00000 0.01741 0.01897 = 0.02059 0.00625 0.00113 0.00435 C23 1 -0.313685 0.230491 0.458084 11.00000 0.01459 0.01615 = 0.02141 0.01020 0.00411 0.00556 AFIX 43 H23 2 -0.355570 0.161854 0.486237 11.00000 -1.20000 AFIX 0 C24 1 -0.603396 0.363338 0.391221 11.00000 0.01756 0.02231 = 0.03164 0.01304 0.00580 0.01092 AFIX 43 H24 2 -0.704378 0.372350 0.383804 11.00000 -1.20000 AFIX 0 C9 1 0.537333 0.277735 0.690564 11.00000 0.01636 0.01986 = 0.01993 0.00984 0.00365 0.00576 C1 1 0.072085 0.031384 0.729227 11.00000 0.01774 0.02204 = 0.01744 0.00587 0.00378 0.00959 C14 1 0.991939 0.380086 0.807840 11.00000 0.01813 0.02062 = 0.02279 0.00699 0.00187 0.00589 C2 1 0.157787 0.029266 0.842141 11.00000 0.01881 0.02221 = 0.01904 0.00683 0.00179 0.00657 C12 1 0.918763 0.562648 0.872026 11.00000 0.02874 0.01734 = 0.02920 0.00125 0.00161 0.00547 AFIX 43 H12 2 0.946687 0.647903 0.911412 11.00000 -1.20000 AFIX 0 C4 1 0.154429 -0.068144 0.997862 11.00000 0.02909 0.02643 = 0.02706 0.01382 0.00360 0.00354 AFIX 43 H4 2 0.102194 -0.130449 1.030583 11.00000 -1.20000 AFIX 0 C11 1 0.757662 0.484520 0.817037 11.00000 0.02421 0.02120 = 0.02879 0.00532 0.00315 0.01027 AFIX 43 H11 2 0.676556 0.518421 0.819738 11.00000 -1.20000 AFIX 0 C5 1 0.309718 0.025680 1.054391 11.00000 0.02565 0.02415 = 0.01927 0.00715 0.00247 0.00980 C13 1 1.038535 0.509699 0.866684 11.00000 0.02041 0.01963 = 0.02117 0.00505 0.00030 0.00165 C6 1 0.387824 0.116624 1.001483 11.00000 0.01915 0.02163 = 0.02118 0.00398 0.00079 0.00469 C21 1 -0.345601 0.398412 0.385007 11.00000 0.01720 0.01469 = 0.01945 0.00737 0.00213 0.00755 C17 1 -0.045015 0.206734 0.482775 11.00000 0.01674 0.01656 = 0.01917 0.00673 0.00445 0.00904 HKLF 4 REM Lamia_Gd_0m_a.res in P-1 REM wR2 = 0.0314, GooF = S = 1.077, Restrained GooF = 1.077 for all data REM R1 = 0.0123 for 5460 Fo > 4sig(Fo) and 0.0127 for all 5575 data REM 349 parameters refined using 0 restraints END WGHT 0.0147 0.6689 REM Highest difference peak 0.706, deepest hole -0.284, 1-sigma level 0.057 Q1 1 -0.2950 0.3531 0.5389 11.00000 0.05 0.71 Q2 1 -0.1016 0.2458 0.4632 11.00000 0.05 0.42 Q3 1 -0.3808 0.3393 0.3998 11.00000 0.05 0.41 Q4 1 0.2518 0.0731 0.4553 11.00000 0.05 0.41 Q5 1 0.2339 0.1661 0.5755 11.00000 0.05 0.39 Q6 1 0.6220 0.3218 0.7191 11.00000 0.05 0.38 Q7 1 0.1174 0.0405 0.7954 11.00000 0.05 0.37 Q8 1 -0.2361 0.2458 0.4415 11.00000 0.05 0.37 Q9 1 1.0046 0.4385 0.8426 11.00000 0.05 0.35 Q10 1 0.3462 0.0629 1.0209 11.00000 0.05 0.34 Q11 1 -0.1263 0.3163 0.4115 11.00000 0.05 0.33 Q12 1 -0.3652 0.2628 0.4382 11.00000 0.05 0.33 Q13 1 -0.1442 0.4028 0.3819 11.00000 0.05 0.32 Q14 1 -0.4000 0.4244 0.3725 11.00000 0.05 0.32 Q15 1 -0.4929 0.2777 0.4264 11.00000 0.05 0.32 Q16 1 -0.2676 0.4229 0.3758 11.00000 0.05 0.30 Q17 1 0.2243 0.0793 0.8775 11.00000 0.05 0.30 Q18 1 0.2311 -0.0124 1.0345 11.00000 0.05 0.29 Q19 1 -0.5440 0.3919 0.3679 11.00000 0.05 0.29 Q20 1 0.1122 -0.0393 0.9602 11.00000 0.05 0.29 ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z 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 Gd1 Gd 0.23284(2) 0.11682(2) 0.51206(2) 0.01405(2) Uani 1 1 d . . . . . O3 O 0.49416(12) 0.15980(9) 0.63712(9) 0.02020(19) Uani 1 1 d . . . . . O7 O 0.10897(12) 0.26544(10) 0.50531(10) 0.0226(2) Uani 1 1 d . . . . . O2 O -0.06782(12) -0.05213(11) 0.68023(9) 0.0239(2) Uani 1 1 d . . . . . O1W O 0.35597(13) 0.00842(10) 0.37644(10) 0.0213(2) Uani 1 1 d . . . . . H2W H 0.356(3) 0.017(2) 0.311(2) 0.032 Uiso 1 1 d . . . . . H1W H 0.399(3) -0.040(2) 0.3777(18) 0.032 Uiso 1 1 d . . . . . O1 O 0.14749(13) 0.12019(10) 0.68856(9) 0.0226(2) Uani 1 1 d . . . . . O5 O -0.10955(13) 0.09601(9) 0.49248(9) 0.0215(2) Uani 1 1 d . . . . . O4 O 0.43469(13) 0.33004(10) 0.68337(10) 0.0252(2) Uani 1 1 d . . . . . N5 N -0.57476(14) 0.27581(11) 0.43157(11) 0.0189(2) Uani 1 1 d . . . . . C16 C 1.25879(19) 0.47188(16) 0.87555(15) 0.0299(3) Uani 1 1 d . . . . . H16 H 1.369132 0.482538 0.891717 0.036 Uiso 1 1 calc R . . . . N1 N 0.54055(17) 0.18844(13) 1.07508(12) 0.0273(3) Uani 1 1 d . . . . . H1N H 0.616743 0.251442 1.065533 0.033 Uiso 1 1 calc R . . . . N3 N 1.13699(16) 0.35880(13) 0.81563(12) 0.0275(3) Uani 1 1 d . . . . . H3N H 1.147598 0.287900 0.787944 0.033 Uiso 1 1 calc R . . . . C22 C -0.41085(16) 0.29580(12) 0.42846(12) 0.0160(2) Uani 1 1 d . . . . . N4 N 1.20865(16) 0.56536(13) 0.90904(12) 0.0287(3) Uani 1 1 d . . . . . C7 C 0.31398(18) 0.12133(14) 0.89614(13) 0.0230(3) Uani 1 1 d . . . . . H7 H 0.366530 0.183233 0.863112 0.028 Uiso 1 1 calc R . . . . C19 C -0.09058(16) 0.37293(13) 0.39912(12) 0.0186(3) Uani 1 1 d . . . . . H19 H 0.017006 0.397018 0.389494 0.022 Uiso 1 1 calc R . . . . C8 C 0.5468(2) 0.14034(16) 1.16504(13) 0.0287(3) Uani 1 1 d . . . . . H8 H 0.638706 0.172455 1.226204 0.034 Uiso 1 1 calc R . . . . N2 N 0.41220(18) 0.04437(14) 1.15886(11) 0.0291(3) Uani 1 1 d . . . . . C20 C -0.18547(17) 0.43786(13) 0.36884(12) 0.0188(3) Uani 1 1 d . . . . . H20 H -0.144295 0.505136 0.338890 0.023 Uiso 1 1 calc R . . . . C18 C -0.15309(16) 0.27060(12) 0.44445(11) 0.0155(2) Uani 1 1 d . . . . . N6 N -0.47255(15) 0.43879(11) 0.36162(11) 0.0212(2) Uani 1 1 d . . . . . H6N H -0.469069 0.500224 0.333565 0.025 Uiso 1 1 calc R . . . . C3 C 0.08093(19) -0.06570(15) 0.89227(14) 0.0259(3) Uani 1 1 d . . . . . H3 H -0.021757 -0.128083 0.853061 0.031 Uiso 1 1 calc R . . . . C15 C 0.83015(18) 0.30069(13) 0.75238(13) 0.0220(3) Uani 1 1 d . . . . . H15 H 0.802043 0.215145 0.713973 0.026 Uiso 1 1 calc R . . . . C10 C 0.71207(17) 0.35452(13) 0.75671(12) 0.0199(3) Uani 1 1 d . . . . . C23 C -0.31368(16) 0.23049(12) 0.45808(12) 0.0166(2) Uani 1 1 d . . . . . H23 H -0.355570 0.161854 0.486237 0.020 Uiso 1 1 calc R . . . . C24 C -0.60340(18) 0.36334(14) 0.39122(13) 0.0220(3) Uani 1 1 d . . . . . H24 H -0.704378 0.372350 0.383804 0.026 Uiso 1 1 calc R . . . . C9 C 0.53733(17) 0.27773(13) 0.69056(12) 0.0184(2) Uani 1 1 d . . . . . C1 C 0.07208(17) 0.03138(13) 0.72923(12) 0.0186(3) Uani 1 1 d . . . . . C14 C 0.99194(17) 0.38009(14) 0.80784(13) 0.0211(3) Uani 1 1 d . . . . . C2 C 0.15779(17) 0.02927(14) 0.84214(12) 0.0205(3) Uani 1 1 d . . . . . C12 C 0.9188(2) 0.56265(14) 0.87203(14) 0.0275(3) Uani 1 1 d . . . . . H12 H 0.946687 0.647903 0.911412 0.033 Uiso 1 1 calc R . . . . C4 C 0.1544(2) -0.06814(15) 0.99786(14) 0.0286(3) Uani 1 1 d . . . . . H4 H 0.102194 -0.130449 1.030583 0.034 Uiso 1 1 calc R . . . . C11 C 0.75766(19) 0.48452(14) 0.81704(14) 0.0250(3) Uani 1 1 d . . . . . H11 H 0.676556 0.518421 0.819738 0.030 Uiso 1 1 calc R . . . . C5 C 0.30972(19) 0.02568(14) 1.05439(13) 0.0231(3) Uani 1 1 d . . . . . C13 C 1.03853(18) 0.50970(14) 0.86668(13) 0.0227(3) Uani 1 1 d . . . . . C6 C 0.38782(18) 0.11662(14) 1.00148(13) 0.0223(3) Uani 1 1 d . . . . . C21 C -0.34560(16) 0.39841(12) 0.38501(12) 0.0165(2) Uani 1 1 d . . . . . C17 C -0.04502(16) 0.20673(12) 0.48278(12) 0.0165(2) Uani 1 1 d . . . . . 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 Gd1 0.01076(3) 0.01307(3) 0.01912(4) 0.00725(2) 0.00179(2) 0.00445(2) O3 0.0155(4) 0.0190(5) 0.0243(5) 0.0060(4) -0.0001(4) 0.0065(4) O7 0.0140(4) 0.0203(5) 0.0353(6) 0.0103(4) 0.0025(4) 0.0085(4) O2 0.0163(5) 0.0307(5) 0.0214(5) 0.0082(4) 0.0001(4) 0.0063(4) O1W 0.0236(5) 0.0200(5) 0.0252(5) 0.0091(4) 0.0074(4) 0.0120(4) O1 0.0248(5) 0.0232(5) 0.0212(5) 0.0099(4) 0.0052(4) 0.0086(4) O5 0.0243(5) 0.0160(4) 0.0279(5) 0.0111(4) 0.0065(4) 0.0090(4) O4 0.0190(5) 0.0213(5) 0.0382(6) 0.0132(4) 0.0040(4) 0.0094(4) N5 0.0148(5) 0.0183(5) 0.0281(6) 0.0115(5) 0.0063(4) 0.0081(4) C16 0.0174(7) 0.0331(8) 0.0327(8) 0.0101(7) -0.0005(6) 0.0036(6) N1 0.0221(6) 0.0264(6) 0.0236(6) 0.0044(5) -0.0026(5) 0.0022(5) N3 0.0184(6) 0.0261(6) 0.0347(7) 0.0067(5) 0.0009(5) 0.0079(5) C22 0.0136(6) 0.0154(6) 0.0203(6) 0.0078(5) 0.0037(5) 0.0054(5) N4 0.0202(6) 0.0269(6) 0.0281(7) 0.0062(5) -0.0015(5) -0.0003(5) C7 0.0210(7) 0.0234(7) 0.0219(7) 0.0094(5) 0.0027(5) 0.0042(6) C19 0.0141(6) 0.0183(6) 0.0242(7) 0.0098(5) 0.0049(5) 0.0047(5) C8 0.0286(8) 0.0324(8) 0.0198(7) 0.0022(6) -0.0023(6) 0.0118(7) N2 0.0329(7) 0.0331(7) 0.0192(6) 0.0076(5) -0.0002(5) 0.0122(6) C20 0.0183(6) 0.0159(6) 0.0234(7) 0.0105(5) 0.0049(5) 0.0046(5) C18 0.0133(6) 0.0147(5) 0.0195(6) 0.0070(5) 0.0018(5) 0.0059(5) N6 0.0196(6) 0.0192(5) 0.0309(6) 0.0144(5) 0.0057(5) 0.0103(5) C3 0.0213(7) 0.0245(7) 0.0254(7) 0.0091(6) 0.0009(6) 0.0013(6) C15 0.0192(6) 0.0164(6) 0.0256(7) 0.0039(5) -0.0002(5) 0.0045(5) C10 0.0174(6) 0.0190(6) 0.0206(6) 0.0062(5) 0.0011(5) 0.0043(5) C23 0.0146(6) 0.0162(6) 0.0214(6) 0.0102(5) 0.0041(5) 0.0056(5) C24 0.0176(6) 0.0223(6) 0.0316(8) 0.0130(6) 0.0058(5) 0.0109(5) C9 0.0164(6) 0.0199(6) 0.0199(6) 0.0098(5) 0.0036(5) 0.0058(5) C1 0.0177(6) 0.0220(6) 0.0174(6) 0.0059(5) 0.0038(5) 0.0096(5) C14 0.0181(6) 0.0206(6) 0.0228(7) 0.0070(5) 0.0019(5) 0.0059(5) C2 0.0188(6) 0.0222(6) 0.0190(6) 0.0068(5) 0.0018(5) 0.0066(5) C12 0.0287(8) 0.0173(6) 0.0292(8) 0.0013(6) 0.0016(6) 0.0055(6) C4 0.0291(8) 0.0264(7) 0.0271(8) 0.0138(6) 0.0036(6) 0.0035(6) C11 0.0242(7) 0.0212(7) 0.0288(7) 0.0053(6) 0.0032(6) 0.0103(6) C5 0.0256(7) 0.0241(7) 0.0193(7) 0.0072(5) 0.0025(5) 0.0098(6) C13 0.0204(7) 0.0196(6) 0.0212(7) 0.0051(5) 0.0003(5) 0.0017(5) C6 0.0191(6) 0.0216(7) 0.0212(7) 0.0040(5) 0.0008(5) 0.0047(5) C21 0.0172(6) 0.0147(6) 0.0194(6) 0.0074(5) 0.0021(5) 0.0076(5) C17 0.0167(6) 0.0166(6) 0.0192(6) 0.0067(5) 0.0044(5) 0.0090(5) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O1W 142.51(4) . . . yes O1 Gd1 O3 81.06(4) . . . yes O1 Gd1 O4 69.23(4) . . . yes O1 Gd1 O7 83.95(4) . . . yes O1 Gd1 N5 136.64(4) . . 1_655 yes O1 Gd1 O2 128.98(4) . . 2_556 yes O1 Gd1 O5 73.70(4) . . 2_556 yes O1W Gd1 O3 79.38(4) . . . yes O1W Gd1 O4 118.37(4) . . . yes O1W Gd1 O7 133.21(4) . . . yes O1W Gd1 N5 70.17(4) . . 1_655 yes O1W Gd1 O2 70.69(4) . . 2_556 yes O1W Gd1 O5 76.96(4) . . 2_556 yes O3 Gd1 O4 50.18(4) . . . yes O3 Gd1 O7 125.61(4) . . . yes O3 Gd1 N5 80.27(4) . . 1_655 yes O2 Gd1 O3 148.68(4) 2_556 . . yes O3 Gd1 O5 96.13(4) . . 2_556 yes O4 Gd1 O7 75.60(4) . . . yes O4 Gd1 N5 68.72(4) . . 1_655 yes O2 Gd1 O4 140.69(4) 2_556 . . yes O4 Gd1 O5 132.54(4) . . 2_556 yes O7 Gd1 N5 75.96(4) . . 1_655 yes O2 Gd1 O7 73.02(4) 2_556 . . yes O5 Gd1 O7 128.72(4) 2_556 . . yes O2 Gd1 N5 81.08(4) 2_556 . 1_655 yes O5 Gd1 N5 147.06(4) 2_556 . 1_655 yes O2 Gd1 O5 86.16(4) 2_556 . 2_556 yes Gd1 O1 C1 132.26(10) . . . yes Gd1 O2 C1 132.31(10) 2_556 . . yes Gd1 O3 C9 101.02(9) . . . yes Gd1 O4 C9 87.80(9) . . . yes Gd1 O5 C17 173.60(10) 2_556 . . yes Gd1 O7 C17 107.83(9) . . . yes C6 N1 C8 106.53(14) . . . yes Gd1 O1W H1W 134.6(16) . . . no H2W O1W H1W 103(2) . . . no Gd1 O1W H2W 122.1(18) . . . no C5 N2 C8 104.08(14) . . . yes C14 N3 C16 106.20(14) . . . yes C13 N4 C16 104.14(14) . . . yes Gd1 N5 C24 127.88(11) 1_455 . . yes C22 N5 C24 104.46(13) . . . yes Gd1 N5 C22 127.51(9) 1_455 . . yes C21 N6 C24 106.88(13) . . . yes O1 C1 O2 123.78(14) . . . yes O1 C1 C2 117.25(13) . . . yes C6 N1 H1N 127.00 . . . no C8 N1 H1N 127.00 . . . no O2 C1 C2 118.97(13) . . . yes C1 C2 C3 120.14(14) . . . no C1 C2 C7 119.02(14) . . . no C3 C2 C7 120.84(14) . . . no C16 N3 H3N 127.00 . . . no C14 N3 H3N 127.00 . . . no C2 C3 C4 121.61(16) . . . no C3 C4 C5 118.11(16) . . . no N2 C5 C6 109.91(15) . . . yes N2 C5 C4 130.29(15) . . . yes C4 C5 C6 119.74(14) . . . no N1 C6 C5 105.10(13) . . . yes N1 C6 C7 132.25(15) . . . yes C5 C6 C7 122.64(15) . . . no C21 N6 H6N 127.00 . . . no C24 N6 H6N 127.00 . . . no C2 C7 C6 116.99(15) . . . no N1 C8 N2 114.36(15) . . . yes O3 C9 O4 119.75(14) . . . yes O3 C9 C10 119.84(14) . . . yes O4 C9 C10 120.34(13) . . . yes C9 C10 C11 119.28(14) . . . no C9 C10 C15 120.27(13) . . . no C11 C10 C15 120.31(14) . . . no C10 C11 C12 122.07(16) . . . no C11 C12 C13 117.96(15) . . . no C12 C13 C14 119.62(15) . . . no N4 C13 C14 109.71(14) . . . yes N4 C13 C12 130.64(15) . . . yes N3 C14 C15 131.72(15) . . . yes C13 C14 C15 122.84(15) . . . no N3 C14 C13 105.39(14) . . . yes C10 C15 C14 117.19(14) . . . no N3 C16 N4 114.57(16) . . . yes O5 C17 O7 121.96(14) . . . yes O7 C17 C18 118.46(13) . . . yes O5 C17 C18 119.58(13) . . . yes C17 C18 C19 120.41(13) . . . no C17 C18 C23 118.63(12) . . . no C19 C18 C23 120.93(13) . . . no C18 C19 C20 121.47(14) . . . no C19 C20 C21 117.14(14) . . . no C20 C21 C22 122.28(14) . . . no N6 C21 C22 105.42(13) . . . yes N6 C21 C20 132.25(13) . . . yes N5 C22 C23 130.62(13) . . . yes N5 C22 C21 109.43(13) . . . yes C21 C22 C23 119.94(14) . . . no C18 C23 C22 118.23(13) . . . no N5 C24 N6 113.82(15) . . . yes C2 C3 H3 119.00 . . . no C4 C3 H3 119.00 . . . no C3 C4 H4 121.00 . . . no C5 C4 H4 121.00 . . . no C2 C7 H7 122.00 . . . no C6 C7 H7 122.00 . . . no N1 C8 H8 123.00 . . . no N2 C8 H8 123.00 . . . no C10 C11 H11 119.00 . . . no C12 C11 H11 119.00 . . . no C11 C12 H12 121.00 . . . no C13 C12 H12 121.00 . . . no C10 C15 H15 121.00 . . . no C14 C15 H15 121.00 . . . no N3 C16 H16 123.00 . . . no N4 C16 H16 123.00 . . . no C18 C19 H19 119.00 . . . no C20 C19 H19 119.00 . . . no C19 C20 H20 121.00 . . . no C21 C20 H20 121.00 . . . no C18 C23 H23 121.00 . . . no C22 C23 H23 121.00 . . . no N5 C24 H24 123.00 . . . no N6 C24 H24 123.00 . . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.3717(11) . . yes Gd1 O1W 2.4386(12) . . yes Gd1 O3 2.4234(11) . . yes Gd1 O4 2.7142(12) . . yes Gd1 O7 2.3574(12) . . yes Gd1 N5 2.5503(13) . 1_655 yes Gd1 O2 2.3976(11) . 2_556 yes Gd1 O5 2.3439(11) . 2_556 yes Gd1 O5 2.9308(11) . . yes O1 C1 1.2797(19) . . yes O2 C1 1.2512(19) . . yes O3 C9 1.2777(18) . . yes O4 C9 1.259(2) . . yes O5 C17 1.2700(17) . . yes O7 C17 1.2611(19) . . yes N1 C6 1.381(2) . . yes N1 C8 1.351(2) . . yes O1W H2W 0.83(2) . . no O1W H1W 0.78(3) . . no N2 C8 1.314(2) . . yes N2 C5 1.390(2) . . yes N3 C14 1.383(2) . . yes N3 C16 1.353(2) . . yes N4 C16 1.313(2) . . yes N4 C13 1.393(2) . . yes N5 C22 1.397(2) . . yes N5 C24 1.318(2) . . yes N6 C21 1.380(2) . . yes N6 C24 1.351(2) . . yes N1 H1N 0.8600 . . no C1 C2 1.495(2) . . no C2 C7 1.391(2) . . no C2 C3 1.413(2) . . no C3 C4 1.378(2) . . no N3 H3N 0.8600 . . no C4 C5 1.398(2) . . no C5 C6 1.406(2) . . no N6 H6N 0.8600 . . no C6 C7 1.387(2) . . no C9 C10 1.501(2) . . no C10 C11 1.415(2) . . no C10 C15 1.390(2) . . no C11 C12 1.381(2) . . no C12 C13 1.397(2) . . no C13 C14 1.406(2) . . no C14 C15 1.389(2) . . no C17 C18 1.490(2) . . no C18 C19 1.413(2) . . no C18 C23 1.386(2) . . no C19 C20 1.378(2) . . no C20 C21 1.392(2) . . no C21 C22 1.405(2) . . no C22 C23 1.395(2) . . no C3 H3 0.9300 . . no C4 H4 0.9300 . . no C7 H7 0.9300 . . no C8 H8 0.9300 . . no C11 H11 0.9300 . . no C12 H12 0.9300 . . no C15 H15 0.9300 . . no C16 H16 0.9300 . . no C19 H19 0.9300 . . no C20 H20 0.9300 . . no C23 H23 0.9300 . . no C24 H24 0.9300 . . no 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 N1 H1N N4 0.8600 2.1000 2.933(2) 162.00 2_767 yes N3 H3N O1 0.8600 2.0500 2.8948(19) 168.00 1_655 yes N6 H6N O4 0.8600 1.9700 2.8064(17) 163.00 2_566 yes O1W H1W O3 0.78(3) 1.93(3) 2.7052(16) 174.00 2_656 yes O1W H2W N2 0.83(2) 2.05(2) 2.8673(18) 167.00 1_554 yes C15 H15 O1W 0.9300 2.4100 3.3038(19) 162.00 2_656 yes C23 H23 O3 0.9300 2.4100 3.0399(18) 125.00 1_455 yes C8 H8 Cg6 0.9300 2.4300 3.1959(17) 139.00 1_656 yes C20 H20 Cg2 0.9300 2.5200 3.2832(16) 139.00 2_666 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Gd1 O1 C1 -41.28(17) . . . . no O3 Gd1 O1 C1 -100.52(14) . . . . no O4 Gd1 O1 C1 -151.19(15) . . . . no O7 Gd1 O1 C1 131.94(14) . . . . no N5 Gd1 O1 C1 -165.94(12) 1_655 . . . no O2 Gd1 O1 C1 69.56(15) 2_556 . . . no O5 Gd1 O1 C1 -1.39(13) 2_556 . . . no O1 Gd1 O3 C9 -76.70(9) . . . . no O1W Gd1 O3 C9 135.45(9) . . . . no O4 Gd1 O3 C9 -6.35(8) . . . . no O7 Gd1 O3 C9 -0.82(10) . . . . no N5 Gd1 O3 C9 63.99(9) 1_655 . . . no O2 Gd1 O3 C9 118.23(10) 2_556 . . . no O5 Gd1 O3 C9 -149.09(9) 2_556 . . . no O1 Gd1 O4 C9 102.06(9) . . . . no O1W Gd1 O4 C9 -37.36(10) . . . . no O3 Gd1 O4 C9 6.33(8) . . . . no O7 Gd1 O4 C9 -169.03(9) . . . . no N5 Gd1 O4 C9 -88.75(9) 1_655 . . . no O2 Gd1 O4 C9 -131.17(9) 2_556 . . . no O5 Gd1 O4 C9 61.12(10) 2_556 . . . no O1 Gd1 O7 C17 -72.22(10) . . . . no O1W Gd1 O7 C17 102.13(10) . . . . no O3 Gd1 O7 C17 -146.66(9) . . . . no O4 Gd1 O7 C17 -142.28(10) . . . . no N5 Gd1 O7 C17 146.51(10) 1_655 . . . no O2 Gd1 O7 C17 61.71(9) 2_556 . . . no O5 Gd1 O7 C17 -8.74(11) 2_556 . . . no O1 Gd1 N5 C22 96.10(12) . . 1_655 1_655 no O1 Gd1 N5 C24 -78.67(14) . . 1_655 1_655 no O1W Gd1 N5 C22 -51.75(11) . . 1_655 1_655 no O1W Gd1 N5 C24 133.49(13) . . 1_655 1_655 no O3 Gd1 N5 C22 30.39(11) . . 1_655 1_655 no O3 Gd1 N5 C24 -144.38(13) . . 1_655 1_655 no O4 Gd1 N5 C22 81.30(12) . . 1_655 1_655 no O4 Gd1 N5 C24 -93.46(13) . . 1_655 1_655 no O7 Gd1 N5 C22 161.07(12) . . 1_655 1_655 no O7 Gd1 N5 C24 -13.70(12) . . 1_655 1_655 no O1 Gd1 O2 C1 -33.43(16) . . 2_556 2_556 no O1W Gd1 O2 C1 109.50(14) . . 2_556 2_556 no O3 Gd1 O2 C1 127.46(13) . . 2_556 2_556 no O4 Gd1 O2 C1 -138.97(13) . . 2_556 2_556 no O7 Gd1 O2 C1 -100.55(14) . . 2_556 2_556 no Gd1 O1 C1 O2 -58.9(2) . . . . no Gd1 O1 C1 C2 121.37(13) . . . . no Gd1 O2 C1 O1 14.0(2) 2_556 . . . no Gd1 O2 C1 C2 -166.28(10) 2_556 . . . no Gd1 O3 C9 O4 12.18(15) . . . . no Gd1 O3 C9 C10 -164.84(11) . . . . no Gd1 O4 C9 O3 -10.66(13) . . . . no Gd1 O4 C9 C10 166.34(12) . . . . no Gd1 O7 C17 O5 15.62(16) . . . . no Gd1 O7 C17 C18 -164.78(10) . . . . no C8 N1 C6 C5 -0.38(18) . . . . no C8 N1 C6 C7 -179.29(18) . . . . no C6 N1 C8 N2 -0.7(2) . . . . no C8 N2 C5 C4 175.40(19) . . . . no C8 N2 C5 C6 -1.65(19) . . . . no C5 N2 C8 N1 1.5(2) . . . . no C16 N3 C14 C13 -0.36(17) . . . . no C16 N3 C14 C15 176.88(17) . . . . no C14 N3 C16 N4 0.6(2) . . . . no C16 N4 C13 C12 -177.83(17) . . . . no C16 N4 C13 C14 0.32(18) . . . . no C13 N4 C16 N3 -0.6(2) . . . . no C24 N5 C22 C21 0.13(17) . . . . no C24 N5 C22 C23 -178.37(15) . . . . no Gd1 N5 C22 C21 -175.61(9) 1_455 . . . no Gd1 N5 C22 C23 5.9(2) 1_455 . . . no C22 N5 C24 N6 0.17(17) . . . . no Gd1 N5 C24 N6 175.88(9) 1_455 . . . no C24 N6 C21 C20 177.80(15) . . . . no C24 N6 C21 C22 0.45(16) . . . . no C21 N6 C24 N5 -0.40(18) . . . . no O1 C1 C2 C3 179.56(15) . . . . no O1 C1 C2 C7 -0.9(2) . . . . no O2 C1 C2 C3 -0.2(2) . . . . no O2 C1 C2 C7 179.39(15) . . . . no C1 C2 C3 C4 -178.04(16) . . . . no C7 C2 C3 C4 2.4(3) . . . . no C1 C2 C7 C6 179.18(14) . . . . no C3 C2 C7 C6 -1.3(2) . . . . no C2 C3 C4 C5 -0.8(3) . . . . no C3 C4 C5 N2 -178.54(17) . . . . no C3 C4 C5 C6 -1.7(3) . . . . no N2 C5 C6 N1 1.27(19) . . . . no N2 C5 C6 C7 -179.68(15) . . . . no C4 C5 C6 N1 -176.14(16) . . . . no C4 C5 C6 C7 2.9(3) . . . . no N1 C6 C7 C2 177.42(17) . . . . no C5 C6 C7 C2 -1.3(2) . . . . no O3 C9 C10 C11 -178.99(14) . . . . no O3 C9 C10 C15 5.3(2) . . . . no O4 C9 C10 C11 4.0(2) . . . . no O4 C9 C10 C15 -171.73(14) . . . . no C9 C10 C11 C12 -174.91(14) . . . . no C15 C10 C11 C12 0.8(2) . . . . no C9 C10 C15 C14 174.83(13) . . . . no C11 C10 C15 C14 -0.9(2) . . . . no C10 C11 C12 C13 0.1(2) . . . . no C11 C12 C13 N4 177.09(16) . . . . no C11 C12 C13 C14 -0.9(2) . . . . no N4 C13 C14 N3 0.03(18) . . . . no N4 C13 C14 C15 -177.52(14) . . . . no C12 C13 C14 N3 178.41(14) . . . . no C12 C13 C14 C15 0.9(2) . . . . no N3 C14 C15 C10 -176.80(16) . . . . no C13 C14 C15 C10 0.0(2) . . . . no O5 C17 C18 C19 -160.44(13) . . . . no O5 C17 C18 C23 21.83(19) . . . . no O7 C17 C18 C19 20.0(2) . . . . no O7 C17 C18 C23 -157.78(13) . . . . no C17 C18 C19 C20 -176.51(13) . . . . no C23 C18 C19 C20 1.2(2) . . . . no C17 C18 C23 C22 176.20(12) . . . . no C19 C18 C23 C22 -1.5(2) . . . . no C18 C19 C20 C21 0.1(2) . . . . no C19 C20 C21 N6 -177.98(15) . . . . no C19 C20 C21 C22 -1.0(2) . . . . no N6 C21 C22 N5 -0.36(16) . . . . no N6 C21 C22 C23 178.32(13) . . . . no C20 C21 C22 N5 -178.05(13) . . . . no C20 C21 C22 C23 0.6(2) . . . . no N5 C22 C23 C18 179.00(14) . . . . no C21 C22 C23 C18 0.6(2) . . . . no