#------------------------------------------------------------------------------ #$Date: 2016-06-14 11:04:59 +0300 (Tue, 14 Jun 2016) $ #$Revision: 183455 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/55/7225520.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_7225520 loop_ _publ_author_name 'Jiang, Y.' 'Holmberg, R. J.' 'Habib, F.' 'Ungur, L.' 'Korobkov, I.' 'Chibotaru, L. F.' 'Murugesu, M.' _publ_section_title ; Probing the structural and magnetic properties of a new family of centrosymmetric dinuclear lanthanide complexes ; _journal_issue 61 _journal_name_full 'RSC Adv.' _journal_page_first 56668 _journal_paper_doi 10.1039/C6RA12070A _journal_volume 6 _journal_year 2016 _chemical_formula_sum 'C38 H60 Gd2 N6 O14' _chemical_formula_weight 1139.42 _chemical_name_systematic 1 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2015-09-22 deposited with the CCDC. 2016-06-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.8720(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.3263(3) _cell_length_b 8.3727(2) _cell_length_c 20.7908(5) _cell_measurement_reflns_used 9832 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 28.31 _cell_measurement_theta_min 2.26 _cell_volume 2261.48(9) _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_collection 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0205 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 29945 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.312 _diffrn_reflns_theta_min 2.257 _exptl_absorpt_coefficient_mu 2.976 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 1140 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.141 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 5567 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0200 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+3.1676P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0510 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5333 _reflns_number_total 5567 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ra12070a2.cif _cod_data_source_block mm421 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_database_code 7225520 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.647 _shelx_estimated_absorpt_t_max 0.755 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mm421 in P2(1)/c CELL 0.71073 13.32630 8.37270 20.79080 90.0000 102.8720 90.0000 ZERR 2.00 0.00030 0.00020 0.00050 0.0000 0.0011 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O GD UNIT 76 120 12 28 4 TEMP -73.150 SIZE 0.10 0.11 0.16 L.S. 80 ACTA CONF LIST 0 BOND FMAP 2 PLAN 5 OMIT -5 1 14 OMIT -8 8 6 OMIT -9 6 2 OMIT -4 3 9 OMIT 4 1 13 OMIT -6 1 6 OMIT -5 1 4 OMIT -6 3 2 OMIT -4 1 7 OMIT 8 1 8 OMIT 0 1 18 OMIT 5 5 8 OMIT 2 1 12 OMIT -4 1 2 OMIT 4 5 2 OMIT -12 1 14 OMIT -6 2 27 OMIT -2 6 20 OMIT -11 1 4 OMIT -5 2 6 OMIT -7 4 3 OMIT -12 8 2 OMIT 0 1 12 OMIT -12 7 5 OMIT -6 2 23 OMIT 6 9 5 OMIT -6 1 4 OMIT 9 6 2 OMIT 1 1 12 OMIT -10 4 5 OMIT -8 1 18 OMIT -9 1 1 OMIT 3 3 7 OMIT -2 7 19 OMIT -7 1 24 OMIT -5 2 9 OMIT -12 5 5 OMIT -9 7 1 OMIT -4 2 7 OMIT -7 1 20 OMIT -9 2 7 OMIT -4 2 1 OMIT -4 1 20 OMIT 7 3 9 OMIT -8 2 17 OMIT -9 1 6 OMIT 4 8 12 OMIT -9 8 2 OMIT 4 7 2 OMIT -4 2 17 WGHT 0.023900 3.167600 FVAR 0.10477 GD1 5 0.364278 0.972621 0.524774 11.00000 0.01098 0.01925 = 0.01491 0.00080 0.00618 -0.00001 O1 4 0.295526 0.974382 0.617064 11.00000 0.01962 0.02396 = 0.02122 -0.00113 0.01177 -0.00240 O2 4 0.144528 1.077886 0.667503 11.00000 0.02747 0.03172 = 0.04058 -0.00014 0.02200 0.00481 O3 4 0.532398 0.871130 0.535104 11.00000 0.01433 0.01772 = 0.01890 0.00236 0.00830 0.00051 O4 4 0.194866 0.886301 0.488562 11.00000 0.01570 0.04132 = 0.02567 -0.00154 0.00758 -0.00380 O5 4 0.349844 0.823780 0.424272 11.00000 0.01687 0.03036 = 0.02145 -0.00450 0.00698 -0.00398 O6 4 0.456998 1.168973 0.596743 11.00000 0.02204 0.03282 = 0.02200 -0.00744 0.01018 -0.00707 AFIX 3 H6A 2 0.442896 1.211754 0.636404 11.00000 -1.50000 H6B 2 0.531426 1.184977 0.596025 11.00000 -1.50000 AFIX 0 N4 3 0.401412 0.711580 0.581797 11.00000 0.01664 0.01912 = 0.02154 0.00186 0.00900 0.00087 N5 3 0.490558 0.627289 0.575106 11.00000 0.01963 0.01888 = 0.02903 0.00374 0.01289 0.00393 N6 3 0.723187 0.768517 0.532266 11.00000 0.01506 0.02777 = 0.02870 0.00650 0.01163 0.00460 C1 1 0.236782 0.865284 0.634750 11.00000 0.01482 0.02960 = 0.01444 0.00031 0.00681 -0.00204 C2 1 0.151618 0.915201 0.661667 11.00000 0.01959 0.03125 = 0.02084 0.00068 0.00902 0.00081 C3 1 0.085309 0.806110 0.679665 11.00000 0.02153 0.04397 = 0.03627 0.00065 0.01974 -0.00100 AFIX 43 H3A 2 0.027615 0.842450 0.695387 11.00000 -1.20000 AFIX 0 C4 1 0.102584 0.642661 0.674887 11.00000 0.03170 0.04119 = 0.05198 0.00108 0.02900 -0.01044 AFIX 43 H4A 2 0.056391 0.567796 0.686886 11.00000 -1.20000 AFIX 0 C5 1 0.186577 0.590357 0.652782 11.00000 0.03236 0.02752 = 0.04261 0.00245 0.02292 -0.00357 AFIX 43 H5A 2 0.199665 0.479027 0.651348 11.00000 -1.20000 AFIX 0 C6 1 0.253877 0.699697 0.632122 11.00000 0.02053 0.02687 = 0.02212 0.00120 0.01192 -0.00238 C7 1 0.075206 1.136086 0.705150 11.00000 0.03763 0.04483 = 0.04567 0.00007 0.02641 0.01161 AFIX 33 H7A 2 0.076518 1.253114 0.705475 11.00000 -1.50000 H7B 2 0.095985 1.096197 0.750487 11.00000 -1.50000 H7C 2 0.005383 1.099018 0.685412 11.00000 -1.50000 AFIX 0 C8 1 0.344684 0.633664 0.613733 11.00000 0.02280 0.02161 = 0.02600 0.00111 0.01216 -0.00127 AFIX 43 H8A 2 0.363237 0.526564 0.626039 11.00000 -1.20000 AFIX 0 C9 1 0.549063 0.720145 0.549280 11.00000 0.01579 0.02121 = 0.01860 -0.00014 0.00739 0.00185 C10 1 0.642797 0.647867 0.531297 11.00000 0.02028 0.02022 = 0.03303 0.00467 0.01435 0.00423 AFIX 23 H10A 2 0.670244 0.561640 0.562919 11.00000 -1.20000 H10B 2 0.623017 0.600084 0.486707 11.00000 -1.20000 AFIX 0 C11 1 0.774459 0.806361 0.600932 11.00000 0.02593 0.04856 = 0.03190 0.01422 -0.00323 -0.00080 AFIX 33 H11A 2 0.723601 0.847378 0.624314 11.00000 -1.50000 H11B 2 0.827624 0.887391 0.601217 11.00000 -1.50000 H11C 2 0.806256 0.709485 0.622938 11.00000 -1.50000 AFIX 0 C12 1 0.799110 0.708416 0.496456 11.00000 0.02809 0.04078 = 0.06441 0.01170 0.03195 0.01275 AFIX 33 H12A 2 0.764497 0.683745 0.450827 11.00000 -1.50000 H12B 2 0.831486 0.611473 0.518061 11.00000 -1.50000 H12C 2 0.851892 0.790019 0.496638 11.00000 -1.50000 AFIX 0 C13 1 0.146106 0.783477 0.449404 11.00000 0.01236 0.03603 = 0.02796 0.00625 0.00197 -0.00203 C14 1 0.182854 0.713500 0.397950 11.00000 0.01695 0.03072 = 0.03343 -0.00428 0.00072 -0.00591 AFIX 43 H14A 2 0.138280 0.643693 0.368742 11.00000 -1.20000 AFIX 0 C15 1 0.281066 0.740246 0.387046 11.00000 0.01942 0.02295 = 0.02041 0.00079 0.00164 0.00051 C16 1 0.041731 0.738684 0.459900 11.00000 0.01811 0.06778 = 0.04568 -0.00208 0.01055 -0.01179 AFIX 137 H16A 2 0.047375 0.709998 0.506268 11.00000 -1.50000 H16B 2 0.015009 0.647343 0.431795 11.00000 -1.50000 H16C 2 -0.005258 0.829499 0.448481 11.00000 -1.50000 AFIX 0 C17 1 0.310874 0.663014 0.328292 11.00000 0.03315 0.03945 = 0.02630 -0.01122 0.00620 -0.00398 AFIX 137 H17A 2 0.373521 0.599571 0.343294 11.00000 -1.50000 H17B 2 0.323498 0.746001 0.297804 11.00000 -1.50000 H17C 2 0.254931 0.593393 0.305683 11.00000 -1.50000 AFIX 0 O7 4 0.351478 1.251442 0.684827 11.00000 0.04397 0.03297 = 0.02971 -0.01128 0.02120 -0.01066 AFIX 83 H7D 2 0.322400 1.164654 0.671692 11.00000 0.04865 AFIX 0 C18 1 0.368457 1.260039 0.754460 11.00000 0.06610 0.05085 = 0.02788 -0.00451 0.01769 -0.01655 AFIX 23 H18A 2 0.402933 1.161255 0.774240 11.00000 -1.20000 H18B 2 0.301640 1.268936 0.767533 11.00000 -1.20000 AFIX 0 C19 1 0.432970 1.399258 0.779178 11.00000 0.07313 0.05147 = 0.03404 -0.00392 -0.00387 -0.01499 AFIX 33 H19A 2 0.444740 1.403425 0.827387 11.00000 -1.50000 H19B 2 0.397993 1.497065 0.760300 11.00000 -1.50000 H19C 2 0.499144 1.390008 0.766308 11.00000 -1.50000 AFIX 0 HKLF 4 REM mm421 in P2(1)/c REM R1 = 0.0200 for 5333 Fo > 4sig(Fo) and 0.0214 for all 5567 data REM 274 parameters refined using 0 restraints END WGHT 0.0099 2.3797 REM Highest difference peak 1.141, deepest hole -0.583, 1-sigma level 0.076 Q1 1 0.3647 0.8705 0.5278 11.00000 0.05 1.14 Q2 1 0.0942 0.9227 0.5765 11.00000 0.05 0.79 Q3 1 0.3463 1.0661 0.5199 11.00000 0.05 0.65 Q4 1 0.6997 0.8617 0.5222 11.00000 0.05 0.52 Q5 1 0.3492 0.9710 0.4805 11.00000 0.05 0.49 ; _shelx_res_checksum 59642 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Gd1 Gd 0.36428(2) 0.97262(2) 0.52477(2) 0.01453(4) Uani 1 1 d . . O1 O 0.29553(12) 0.97438(18) 0.61706(8) 0.0205(3) Uani 1 1 d . . O2 O 0.14453(14) 1.0779(2) 0.66750(9) 0.0310(4) Uani 1 1 d . . O3 O 0.53240(11) 0.87113(17) 0.53510(7) 0.0163(3) Uani 1 1 d . . O4 O 0.19487(12) 0.8863(2) 0.48856(8) 0.0271(4) Uani 1 1 d . . O5 O 0.34984(12) 0.8238(2) 0.42427(7) 0.0225(3) Uani 1 1 d . . O6 O 0.45700(13) 1.1690(2) 0.59674(8) 0.0248(3) Uani 1 1 d . . H6A H 0.4429 1.2118 0.6364 0.037 Uiso 1 1 d R U H6B H 0.5314 1.1850 0.5960 0.037 Uiso 1 1 d R U N4 N 0.40141(14) 0.7116(2) 0.58180(9) 0.0184(3) Uani 1 1 d . . N5 N 0.49056(14) 0.6273(2) 0.57511(9) 0.0213(4) Uani 1 1 d . . N6 N 0.72319(14) 0.7685(2) 0.53227(9) 0.0228(4) Uani 1 1 d . . C1 C 0.23678(16) 0.8653(3) 0.63475(10) 0.0191(4) Uani 1 1 d . . C2 C 0.15162(17) 0.9152(3) 0.66167(10) 0.0232(4) Uani 1 1 d . . C3 C 0.08531(19) 0.8061(3) 0.67967(13) 0.0318(5) Uani 1 1 d . . H3A H 0.0276 0.8424 0.6954 0.038 Uiso 1 1 calc R U C4 C 0.1026(2) 0.6427(4) 0.67489(15) 0.0385(6) Uani 1 1 d . . H4A H 0.0564 0.5678 0.6869 0.046 Uiso 1 1 calc R U C5 C 0.1866(2) 0.5904(3) 0.65278(13) 0.0319(5) Uani 1 1 d . . H5A H 0.1997 0.4790 0.6513 0.038 Uiso 1 1 calc R U C6 C 0.25388(17) 0.6997(3) 0.63212(11) 0.0221(4) Uani 1 1 d . . C7 C 0.0752(2) 1.1361(4) 0.70515(15) 0.0400(6) Uani 1 1 d . . H7A H 0.0765 1.2531 0.7055 0.060 Uiso 1 1 calc R U H7B H 0.0960 1.0962 0.7505 0.060 Uiso 1 1 calc R U H7C H 0.0054 1.0990 0.6854 0.060 Uiso 1 1 calc R U C8 C 0.34468(17) 0.6337(3) 0.61373(11) 0.0224(4) Uani 1 1 d . . H8A H 0.3632 0.5266 0.6260 0.027 Uiso 1 1 calc R U C9 C 0.54906(16) 0.7201(3) 0.54928(10) 0.0180(4) Uani 1 1 d . . C10 C 0.64280(17) 0.6479(3) 0.53130(12) 0.0232(4) Uani 1 1 d . . H10A H 0.6702 0.5616 0.5629 0.028 Uiso 1 1 calc R U H10B H 0.6230 0.6001 0.4867 0.028 Uiso 1 1 calc R U C11 C 0.7745(2) 0.8064(4) 0.60093(13) 0.0370(6) Uani 1 1 d . . H11A H 0.7236 0.8474 0.6243 0.055 Uiso 1 1 calc R U H11B H 0.8276 0.8874 0.6012 0.055 Uiso 1 1 calc R U H11C H 0.8063 0.7095 0.6229 0.055 Uiso 1 1 calc R U C12 C 0.7991(2) 0.7084(4) 0.49646(16) 0.0410(7) Uani 1 1 d . . H12A H 0.7645 0.6837 0.4508 0.062 Uiso 1 1 calc R U H12B H 0.8315 0.6115 0.5181 0.062 Uiso 1 1 calc R U H12C H 0.8519 0.7900 0.4966 0.062 Uiso 1 1 calc R U C13 C 0.14611(17) 0.7835(3) 0.44940(12) 0.0258(5) Uani 1 1 d . . C14 C 0.18285(18) 0.7135(3) 0.39795(12) 0.0278(5) Uani 1 1 d . . H14A H 0.1383 0.6437 0.3687 0.033 Uiso 1 1 calc R U C15 C 0.28107(17) 0.7402(3) 0.38705(10) 0.0214(4) Uani 1 1 d . . C16 C 0.0417(2) 0.7387(4) 0.45990(15) 0.0433(7) Uani 1 1 d . . H16A H 0.0474 0.7100 0.5063 0.065 Uiso 1 1 calc R U H16B H 0.0150 0.6473 0.4318 0.065 Uiso 1 1 calc R U H16C H -0.0053 0.8295 0.4485 0.065 Uiso 1 1 calc R U C17 C 0.3109(2) 0.6630(3) 0.32829(12) 0.0330(5) Uani 1 1 d . . H17A H 0.3735 0.5996 0.3433 0.050 Uiso 1 1 calc R U H17B H 0.3235 0.7460 0.2978 0.050 Uiso 1 1 calc R U H17C H 0.2549 0.5934 0.3057 0.050 Uiso 1 1 calc R U O7 O 0.35148(15) 1.2514(2) 0.68483(9) 0.0335(4) Uani 1 1 d . . H7D H 0.3224 1.1647 0.6717 0.049(10) Uiso 1 1 calc R . C18 C 0.3685(3) 1.2600(4) 0.75446(14) 0.0471(8) Uani 1 1 d . . H18A H 0.4029 1.1613 0.7742 0.057 Uiso 1 1 calc R U H18B H 0.3016 1.2689 0.7675 0.057 Uiso 1 1 calc R U C19 C 0.4330(3) 1.3993(4) 0.77918(16) 0.0553(9) Uani 1 1 d . . H19A H 0.4447 1.4034 0.8274 0.083 Uiso 1 1 calc R U H19B H 0.3980 1.4971 0.7603 0.083 Uiso 1 1 calc R U H19C H 0.4991 1.3900 0.7663 0.083 Uiso 1 1 calc R U 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 0.01098(6) 0.01925(6) 0.01491(5) 0.00080(3) 0.00618(4) -0.00001(3) O1 0.0196(8) 0.0240(8) 0.0212(7) -0.0011(6) 0.0118(6) -0.0024(6) O2 0.0275(9) 0.0317(9) 0.0406(10) -0.0001(8) 0.0220(8) 0.0048(7) O3 0.0143(7) 0.0177(7) 0.0189(6) 0.0024(5) 0.0083(5) 0.0005(5) O4 0.0157(8) 0.0413(10) 0.0257(8) -0.0015(7) 0.0076(6) -0.0038(7) O5 0.0169(7) 0.0304(9) 0.0215(7) -0.0045(6) 0.0070(6) -0.0040(6) O6 0.0220(8) 0.0328(9) 0.0220(7) -0.0074(6) 0.0102(6) -0.0071(7) N4 0.0166(8) 0.0191(8) 0.0215(8) 0.0019(7) 0.0090(7) 0.0009(7) N5 0.0196(9) 0.0189(9) 0.0290(9) 0.0037(7) 0.0129(7) 0.0039(7) N6 0.0151(9) 0.0278(10) 0.0287(9) 0.0065(7) 0.0116(7) 0.0046(7) C1 0.0148(9) 0.0296(11) 0.0144(8) 0.0003(8) 0.0068(7) -0.0020(8) C2 0.0196(10) 0.0313(11) 0.0208(9) 0.0007(9) 0.0090(8) 0.0008(9) C3 0.0215(12) 0.0440(15) 0.0363(13) 0.0006(11) 0.0197(10) -0.0010(10) C4 0.0317(14) 0.0412(15) 0.0520(16) 0.0011(12) 0.0290(13) -0.0104(11) C5 0.0324(13) 0.0275(12) 0.0426(14) 0.0025(10) 0.0229(11) -0.0036(10) C6 0.0205(11) 0.0269(11) 0.0221(10) 0.0012(8) 0.0119(8) -0.0024(8) C7 0.0376(15) 0.0448(16) 0.0457(15) 0.0001(12) 0.0264(13) 0.0116(12) C8 0.0228(11) 0.0216(10) 0.0260(10) 0.0011(8) 0.0122(9) -0.0013(8) C9 0.0158(10) 0.0212(10) 0.0186(9) -0.0001(7) 0.0074(7) 0.0019(7) C10 0.0203(10) 0.0202(10) 0.0330(11) 0.0047(9) 0.0144(9) 0.0042(8) C11 0.0259(13) 0.0486(16) 0.0319(13) 0.0142(11) -0.0032(10) -0.0008(11) C12 0.0281(14) 0.0408(15) 0.0644(19) 0.0117(13) 0.0320(13) 0.0127(11) C13 0.0124(10) 0.0360(13) 0.0280(11) 0.0062(9) 0.0020(8) -0.0020(9) C14 0.0170(11) 0.0307(12) 0.0334(12) -0.0043(9) 0.0007(9) -0.0059(9) C15 0.0194(10) 0.0229(11) 0.0204(10) 0.0008(8) 0.0016(8) 0.0005(8) C16 0.0181(12) 0.068(2) 0.0457(16) -0.0021(14) 0.0106(11) -0.0118(12) C17 0.0332(14) 0.0394(15) 0.0263(11) -0.0112(10) 0.0062(10) -0.0040(11) O7 0.0440(11) 0.0330(10) 0.0297(9) -0.0113(7) 0.0212(8) -0.0107(8) C18 0.066(2) 0.0509(18) 0.0279(13) -0.0045(12) 0.0177(13) -0.0165(16) C19 0.073(2) 0.051(2) 0.0340(15) -0.0039(14) -0.0039(15) -0.0150(18) 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' Gd Gd -0.1653 3.9035 '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 O1 Gd1 O4 74.61(6) . . O1 Gd1 O3 118.17(5) . . O4 Gd1 O3 138.53(6) . . O1 Gd1 O6 73.65(5) . . O4 Gd1 O6 138.48(6) . . O3 Gd1 O6 80.90(5) . . O1 Gd1 O5 139.28(5) . . O4 Gd1 O5 70.98(5) . . O3 Gd1 O5 77.47(5) . . O6 Gd1 O5 146.72(5) . . O1 Gd1 O3 142.96(5) . 3_676 O4 Gd1 O3 128.28(5) . 3_676 O3 Gd1 O3 66.82(6) . 3_676 O6 Gd1 O3 71.10(5) . 3_676 O5 Gd1 O3 77.22(5) . 3_676 O1 Gd1 N4 71.45(6) . . O4 Gd1 N4 87.53(6) . . O3 Gd1 N4 63.61(5) . . O6 Gd1 N4 106.74(6) . . O5 Gd1 N4 85.84(6) . . O3 Gd1 N4 129.96(5) 3_676 . O1 Gd1 N6 98.78(6) . 3_676 O4 Gd1 N6 78.97(6) . 3_676 O3 Gd1 N6 131.09(5) . 3_676 O6 Gd1 N6 80.15(6) . 3_676 O5 Gd1 N6 95.40(6) . 3_676 O3 Gd1 N6 64.44(5) 3_676 3_676 N4 Gd1 N6 165.18(6) . 3_676 O1 Gd1 Gd1 139.80(4) . 3_676 O4 Gd1 Gd1 144.95(4) . 3_676 O3 Gd1 Gd1 33.98(3) . 3_676 O6 Gd1 Gd1 73.13(4) . 3_676 O5 Gd1 Gd1 74.78(4) . 3_676 O3 Gd1 Gd1 32.84(3) 3_676 3_676 N4 Gd1 Gd1 97.37(4) . 3_676 N6 Gd1 Gd1 97.20(4) 3_676 3_676 C1 O1 Gd1 127.15(13) . . C2 O2 C7 117.0(2) . . C9 O3 Gd1 118.64(12) . . C9 O3 Gd1 123.29(12) . 3_676 Gd1 O3 Gd1 113.18(6) . 3_676 C13 O4 Gd1 138.00(15) . . C15 O5 Gd1 136.27(14) . . C8 N4 N5 113.56(18) . . C8 N4 Gd1 127.88(15) . . N5 N4 Gd1 118.32(12) . . C9 N5 N4 109.66(17) . . C10 N6 C12 109.8(2) . . C10 N6 C11 109.90(18) . . C12 N6 C11 109.9(2) . . C10 N6 Gd1 108.27(13) . 3_676 C12 N6 Gd1 109.93(15) . 3_676 C11 N6 Gd1 108.94(16) . 3_676 O1 C1 C6 124.38(19) . . O1 C1 C2 118.8(2) . . C6 C1 C2 116.79(19) . . O2 C2 C3 124.9(2) . . O2 C2 C1 113.55(19) . . C3 C2 C1 121.5(2) . . C2 C3 C4 120.3(2) . . C5 C4 C3 119.8(2) . . C4 C5 C6 121.0(2) . . C1 C6 C5 120.4(2) . . C1 C6 C8 122.34(19) . . C5 C6 C8 117.0(2) . . N4 C8 C6 124.0(2) . . N5 C9 O3 125.82(19) . . N5 C9 C10 117.96(19) . . O3 C9 C10 116.18(18) . . N6 C10 C9 111.25(18) . . O4 C13 C14 124.1(2) . . O4 C13 C16 115.9(2) . . C14 C13 C16 119.9(2) . . C15 C14 C13 123.9(2) . . O5 C15 C14 124.4(2) . . O5 C15 C17 116.4(2) . . C14 C15 C17 119.2(2) . . O7 C18 C19 110.2(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Gd1 O1 2.3032(14) . Gd1 O4 2.3300(16) . Gd1 O3 2.3608(14) . Gd1 O6 2.3758(16) . Gd1 O5 2.4035(15) . Gd1 O3 2.4333(14) 3_676 Gd1 N4 2.4831(18) . Gd1 N6 2.6166(19) 3_676 Gd1 Gd1 4.0021(2) 3_676 O1 C1 1.308(3) . O2 C2 1.373(3) . O2 C7 1.423(3) . O3 C9 1.306(3) . O3 Gd1 2.4333(13) 3_676 O4 C13 1.261(3) . O5 C15 1.270(3) . N4 C8 1.289(3) . N4 N5 1.415(2) . N5 C9 1.299(3) . N6 C10 1.469(3) . N6 C12 1.472(3) . N6 C11 1.473(3) . N6 Gd1 2.6166(19) 3_676 C1 C6 1.408(3) . C1 C2 1.435(3) . C2 C3 1.379(3) . C3 C4 1.395(4) . C4 C5 1.373(3) . C5 C6 1.414(3) . C6 C8 1.457(3) . C9 C10 1.508(3) . C13 C14 1.400(3) . C13 C16 1.503(3) . C14 C15 1.395(3) . C15 C17 1.511(3) . O7 C18 1.416(3) . C18 C19 1.471(4) . 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 C8 N4 N5 C9 -172.7(2) . Gd1 N4 N5 C9 12.4(2) . Gd1 O1 C1 C6 43.5(3) . Gd1 O1 C1 C2 -139.61(16) . C7 O2 C2 C3 11.5(4) . C7 O2 C2 C1 -168.2(2) . O1 C1 C2 O2 -2.0(3) . C6 C1 C2 O2 175.14(19) . O1 C1 C2 C3 178.3(2) . C6 C1 C2 C3 -4.5(3) . O2 C2 C3 C4 -176.6(2) . C1 C2 C3 C4 3.0(4) . C2 C3 C4 C5 0.7(4) . C3 C4 C5 C6 -2.6(4) . O1 C1 C6 C5 179.5(2) . C2 C1 C6 C5 2.6(3) . O1 C1 C6 C8 4.8(3) . C2 C1 C6 C8 -172.2(2) . C4 C5 C6 C1 0.9(4) . C4 C5 C6 C8 175.9(3) . N5 N4 C8 C6 174.4(2) . Gd1 N4 C8 C6 -11.3(3) . C1 C6 C8 N4 -19.7(4) . C5 C6 C8 N4 165.4(2) . N4 N5 C9 O3 3.9(3) . N4 N5 C9 C10 -173.61(18) . Gd1 O3 C9 N5 -19.2(3) . Gd1 O3 C9 N5 -172.67(17) 3_676 Gd1 O3 C9 C10 158.36(14) . Gd1 O3 C9 C10 4.9(2) 3_676 C12 N6 C10 C9 -163.4(2) . C11 N6 C10 C9 75.5(2) . Gd1 N6 C10 C9 -43.4(2) 3_676 N5 C9 C10 N6 -153.8(2) . O3 C9 C10 N6 28.4(3) . Gd1 O4 C13 C14 -20.4(4) . Gd1 O4 C13 C16 160.5(2) . O4 C13 C14 C15 5.1(4) . C16 C13 C14 C15 -175.9(2) . Gd1 O5 C15 C14 0.6(4) . Gd1 O5 C15 C17 -177.88(16) . C13 C14 C15 O5 3.9(4) . C13 C14 C15 C17 -177.7(2) .