#------------------------------------------------------------------------------ #$Date: 2019-11-17 12:09:43 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229792 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045421.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_7045421 loop_ _publ_author_name 'Cadman, Laura K.' 'Mahon, Mary F.' 'Burrows, Andrew D.' _publ_section_title ; The effect of metal distribution on the luminescence properties of mixed-lanthanide metal-organic frameworks. ; _journal_issue 7 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2360 _journal_page_last 2367 _journal_paper_doi 10.1039/c7dt04583b _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C16 H9 Gd O10, H2 O, O' _chemical_formula_sum 'C16 H13 Gd O12' _chemical_formula_weight 554.51 _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2017-11-21 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2017-11-21 deposited with the CCDC. 2018-01-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.753(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8450(5) _cell_length_b 12.7548(6) _cell_length_c 13.9951(8) _cell_measurement_reflns_used 3535 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 72.4560 _cell_measurement_theta_min 5.3050 _cell_volume 1753.61(16) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 150.00(10) _diffrn_detector_area_resol_mean 8.1150 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0458 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5691 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.850 _diffrn_reflns_theta_min 4.695 _exptl_absorpt_coefficient_mu 25.113 _exptl_absorpt_correction_T_max 0.708 _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.100 _exptl_crystal_description block _exptl_crystal_F_000 1076 _exptl_crystal_size_max 0.078 _exptl_crystal_size_mid 0.019 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.829 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 279 _refine_ls_number_reflns 5691 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.892 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0282 _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^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.0718 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4080 _reflns_number_total 5691 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL CELL 1.54184 9.84503 12.754782 13.995133 90 93.7533 90 ZERR 4 0.0005 0.000601 0.000792 0 0.0046 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Gd O UNIT 64 52 4 48 ISOR 0.001 0.001 C4 L.S. 12 PLAN 3 MORE -1 BOND $H CONF fmap 2 acta OMIT -2 -2 2 OMIT -1 -3 2 OMIT 2 -2 -2 OMIT -1 3 2 REM REM REM WGHT 0.043600 BASF 0.25421 FVAR 2.67057 GD1 3 0.227816 0.002791 0.416132 11.00000 0.00699 0.00607 = 0.00694 0.00073 0.00075 0.00203 O1 4 0.077328 -0.020516 0.275922 11.00000 0.01894 0.00671 = 0.01386 0.00587 -0.00405 -0.00355 O2 4 0.209028 0.118587 0.270389 11.00000 0.01448 0.00932 = 0.01130 0.00192 0.00030 -0.00186 O3 4 0.106509 0.386970 0.015186 11.00000 0.01236 0.01073 = 0.01386 0.00436 -0.00293 -0.00620 O4 4 -0.089865 0.378074 -0.070960 11.00000 0.01043 0.00862 = 0.01013 0.00293 -0.00036 0.00051 O5 4 -0.247713 0.009996 -0.021493 11.00000 0.01520 0.01207 = 0.00849 -0.00148 -0.00044 -0.00719 O6 4 -0.402577 -0.363826 -0.042166 11.00000 0.01195 0.00983 = 0.01663 -0.00569 0.00472 -0.00202 O7 4 -0.569813 -0.371825 0.056296 11.00000 0.01379 0.01262 = 0.02042 -0.00342 0.00659 -0.00679 O8 4 -0.632200 -0.068211 0.285494 11.00000 0.01222 0.01176 = 0.01013 -0.00185 0.00402 0.00051 O9 4 -0.465527 0.051323 0.285395 11.00000 0.02176 0.01928 = 0.02072 -0.01618 0.00917 -0.00676 AFIX 147 0.9500 H9 2 -0.518097 0.085421 0.330735 11.00000 -1.20000 AFIX 0 O10 4 0.240607 0.037477 0.586657 11.00000 0.02792 0.03007 = 0.00989 -0.00245 -0.00076 0.01650 AFIX 7 H10A 2 0.319226 0.011196 0.617797 11.00000 0.06104 H10B 2 0.168936 0.007777 0.617277 11.00000 0.12155 AFIX 6 O11 4 0.062412 -0.232551 0.237944 11.00000 0.07467 0.03062 = 0.06386 -0.01269 0.02861 -0.01067 H11A 2 0.104897 -0.174715 0.243907 11.00000 -1.50000 H11B 2 -0.008712 -0.230197 0.269260 11.00000 -1.50000 AFIX 0 PART 1 O12 4 -0.178305 -0.222675 0.326378 10.80000 0.04987 0.02930 = 0.04515 -0.01102 0.02843 -0.00195 PART 0 C1 1 0.110264 0.065068 0.236097 11.00000 0.01097 0.01020 = 0.00909 0.00028 0.00154 0.00023 C2 1 0.025658 0.103335 0.150785 11.00000 0.00766 0.00710 = 0.01297 0.00094 0.00199 -0.00060 C3 1 0.049166 0.201614 0.112814 11.00000 0.00959 0.00933 = 0.01055 0.00002 -0.00176 -0.00106 AFIX 43 H3 2 0.117690 0.244255 0.140299 11.00000 -1.20000 AFIX 0 C4 1 -0.031103 0.235950 0.032859 11.00000 0.00848 0.00757 = 0.00908 -0.00070 0.00146 -0.00095 C5 1 -0.131748 0.173334 -0.009447 11.00000 0.00912 0.00985 = 0.01031 0.00394 0.00217 -0.00060 AFIX 43 H5 2 -0.185226 0.197115 -0.062277 11.00000 -1.20000 AFIX 0 C6 1 -0.152456 0.073608 0.028046 11.00000 0.00911 0.00755 = 0.00928 0.00055 0.00298 -0.00322 C7 1 -0.074939 0.037992 0.107497 11.00000 0.01035 0.00799 = 0.00918 0.00129 0.00159 -0.00023 AFIX 43 H7 2 -0.089432 -0.028598 0.131915 11.00000 -1.20000 AFIX 0 C8 1 -0.002024 0.341610 -0.009600 11.00000 0.01199 0.00766 = 0.00368 -0.00191 0.00275 -0.00201 C9 1 -0.329196 -0.050630 0.032619 11.00000 0.01210 0.00890 = 0.01021 0.00291 0.00050 -0.00121 C10 1 -0.359020 -0.152198 0.000858 11.00000 0.01501 0.01059 = 0.00813 -0.00191 0.00074 -0.00065 AFIX 43 H10 2 -0.319598 -0.178659 -0.052720 11.00000 -1.20000 AFIX 0 C11 1 -0.448342 -0.213733 0.050017 11.00000 0.00803 0.00844 = 0.01301 -0.00119 0.00260 -0.00134 C12 1 -0.506403 -0.174993 0.131030 11.00000 0.00941 0.00865 = 0.00995 -0.00060 0.00275 -0.00307 AFIX 43 H12 2 -0.566630 -0.215828 0.163520 11.00000 -1.20000 AFIX 0 C13 1 -0.472718 -0.073835 0.162685 11.00000 0.01295 0.00892 = 0.00645 -0.00140 0.00284 0.00040 C14 1 -0.385112 -0.011103 0.113623 11.00000 0.01085 0.00700 = 0.01346 -0.00129 -0.00216 -0.00136 AFIX 43 H14 2 -0.364278 0.056463 0.134834 11.00000 -1.20000 AFIX 0 C15 1 -0.475701 -0.324893 0.018262 11.00000 0.00715 0.00881 = 0.01159 -0.00053 0.00046 -0.00174 C16 1 -0.533686 -0.030421 0.248942 11.00000 0.01376 0.00985 = 0.01432 -0.00073 0.00067 0.00380 PART 2 O12A 4 -0.148619 -0.177299 0.287085 10.20000 0.04165 0.06535 = 0.02554 -0.02092 0.01621 -0.00528 HKLF 5 REM REM R1 = 0.0282 for 4080 Fo > 4sig(Fo) and 0.0419 for all 5691 data REM 279 parameters refined using 6 restraints END WGHT 0.0436 0.0000 REM Highest difference peak 0.829, deepest hole -0.596, 1-sigma level 0.120 Q1 1 0.0995 0.4924 0.0825 11.00000 0.05 0.83 Q2 1 0.4164 0.0009 0.5821 11.00000 0.05 0.82 Q3 1 0.0565 -0.0042 0.4199 11.00000 0.05 0.82 REM The information below was added by Olex2. REM REM R1 = 0.0282 for 4080 Fo > 4sig(Fo) and 0.0419 for all 5696 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.83, deepest hole -0.60 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0419 REM R1_gt = 0.0282 REM wR_ref = 0.0718 REM GOOF = 0.892 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 5696 REM Reflections_gt = 4080 REM Parameters = n/a REM Hole = -0.60 REM Peak = 0.83 REM Flack = n/a ; _cod_data_source_file c7dt04583b2.cif _cod_data_source_block s16lkc18-Cpd-3 _cod_depositor_comments 'Adding full bibliography for 7045418--7045423.cif.' _cod_original_cell_volume 1753.62(16) _cod_database_code 7045421 _shelxl_version_number 2014-3 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7458(6) 0.2542(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups At 1.5 times of: All O(H,H) groups 3. Uiso/Uaniso restraints and constraints Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001 4. Others Fixed Sof: O12(0.8) O12A(0.2) 5.a Free rotating group: O11(H11A,H11B) 5.b Rotating group: O10(H10A,H10B) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14) 5.d Idealised tetrahedral OH refined as rotating group: O9(H9) ; _olex2_submission_special_instructions 'No special instructions were received' _twin_special_details ; Component 2 rotated by -179.8907\% around [1.00 0.00 -0.09] (reciprocal) or [1.00 0.00 0.00] (direct) ; 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 Gd1 Gd 0.22782(2) 0.00279(3) 0.41613(2) 0.00665(8) Uani 1 1 d . . . . . O1 O 0.0773(4) -0.0205(3) 0.2759(3) 0.0134(8) Uani 1 1 d . . . . . O2 O 0.2090(4) 0.1186(3) 0.2704(2) 0.0117(7) Uani 1 1 d . . . . . O3 O 0.1065(4) 0.3870(3) 0.0152(3) 0.0125(7) Uani 1 1 d . . . . . O4 O -0.0899(4) 0.3781(3) -0.0710(3) 0.0098(7) Uani 1 1 d . . . . . O5 O -0.2477(4) 0.0100(3) -0.0215(2) 0.0120(7) Uani 1 1 d . . . . . O6 O -0.4026(4) -0.3638(3) -0.0422(3) 0.0126(8) Uani 1 1 d . . . . . O7 O -0.5698(4) -0.3718(3) 0.0563(3) 0.0154(9) Uani 1 1 d . . . . . O8 O -0.6322(4) -0.0682(3) 0.2855(2) 0.0112(7) Uani 1 1 d . . . . . O9 O -0.4655(4) 0.0513(3) 0.2854(3) 0.0202(9) Uani 1 1 d . . . . . H9 H -0.5181 0.0854 0.3307 0.024 Uiso 1 1 calc GR . . . . O10 O 0.2406(5) 0.0375(3) 0.5867(3) 0.0227(10) Uani 1 1 d . . . . . H10A H 0.3192 0.0112 0.6178 0.06(3) Uiso 1 1 d GR . . . . H10B H 0.1689 0.0078 0.6173 0.12(5) Uiso 1 1 d GR . . . . O11 O 0.0624(8) -0.2326(5) 0.2379(5) 0.0553(18) Uani 1 1 d . . . . . H11A H 0.1049 -0.1747 0.2439 0.083 Uiso 1 1 d G . . . . H11B H -0.0087 -0.2302 0.2693 0.083 Uiso 1 1 d G . . . . O12 O -0.1783(8) -0.2227(5) 0.3264(5) 0.0403(17) Uani 0.8 1 d . . P A 1 C1 C 0.1103(5) 0.0651(4) 0.2361(4) 0.0100(10) Uani 1 1 d . . . . . C2 C 0.0257(5) 0.1033(4) 0.1508(4) 0.0092(10) Uani 1 1 d . . . . . C3 C 0.0492(5) 0.2016(4) 0.1128(3) 0.0099(10) Uani 1 1 d . . . . . H3 H 0.1177 0.2443 0.1403 0.012 Uiso 1 1 calc R . . . . C4 C -0.0311(5) 0.2360(4) 0.0329(4) 0.0083(9) Uani 1 1 d . U . . . C5 C -0.1317(5) 0.1733(4) -0.0094(3) 0.0097(10) Uani 1 1 d . . . . . H5 H -0.1852 0.1971 -0.0623 0.012 Uiso 1 1 calc R . . . . C6 C -0.1525(5) 0.0736(4) 0.0280(3) 0.0085(9) Uani 1 1 d . . . . . C7 C -0.0749(5) 0.0380(4) 0.1075(3) 0.0091(10) Uani 1 1 d . . . . . H7 H -0.0894 -0.0286 0.1319 0.011 Uiso 1 1 calc R . . . . C8 C -0.0020(7) 0.3416(4) -0.0096(4) 0.0077(9) Uani 1 1 d . . . . . C9 C -0.3292(5) -0.0506(4) 0.0326(4) 0.0104(10) Uani 1 1 d . . . . . C10 C -0.3590(6) -0.1522(4) 0.0009(3) 0.0112(10) Uani 1 1 d . . . . . H10 H -0.3196 -0.1787 -0.0527 0.013 Uiso 1 1 calc R . . . . C11 C -0.4483(5) -0.2137(4) 0.0500(4) 0.0097(10) Uani 1 1 d . . . . . C12 C -0.5064(5) -0.1750(4) 0.1310(3) 0.0092(10) Uani 1 1 d . . . . . H12 H -0.5666 -0.2158 0.1635 0.011 Uiso 1 1 calc R . . . . C13 C -0.4727(5) -0.0738(4) 0.1627(3) 0.0093(10) Uani 1 1 d . . . . . C14 C -0.3851(5) -0.0111(4) 0.1136(3) 0.0106(9) Uani 1 1 d . . . . . H14 H -0.3643 0.0565 0.1348 0.013 Uiso 1 1 calc R . . . . C15 C -0.4757(5) -0.3249(4) 0.0183(3) 0.0092(10) Uani 1 1 d . . . . . C16 C -0.5337(6) -0.0304(4) 0.2489(4) 0.0127(11) Uani 1 1 d . . . . . O12A O -0.149(3) -0.177(3) 0.2871(19) 0.044(7) Uani 0.2 1 d . . P B 2 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 0.00699(12) 0.00607(11) 0.00694(11) 0.00073(14) 0.00075(7) 0.00203(16) O1 0.019(2) 0.0067(19) 0.0139(17) 0.0059(14) -0.0040(14) -0.0035(14) O2 0.014(2) 0.0093(16) 0.0113(17) 0.0019(13) 0.0003(14) -0.0019(15) O3 0.0124(19) 0.0107(17) 0.0139(18) 0.0044(14) -0.0029(14) -0.0062(14) O4 0.0104(18) 0.0086(16) 0.0101(17) 0.0029(14) -0.0004(14) 0.0005(14) O5 0.0152(17) 0.0121(16) 0.0085(13) -0.0015(15) -0.0004(12) -0.0072(17) O6 0.012(2) 0.0098(18) 0.0166(19) -0.0057(14) 0.0047(15) -0.0020(15) O7 0.014(2) 0.0126(19) 0.020(2) -0.0034(15) 0.0066(16) -0.0068(16) O8 0.0122(19) 0.0118(17) 0.0101(16) -0.0018(13) 0.0040(14) 0.0005(14) O9 0.022(2) 0.019(2) 0.021(2) -0.0162(17) 0.0092(17) -0.0068(18) O10 0.028(2) 0.030(2) 0.0099(17) -0.0025(15) -0.0008(17) 0.0165(18) O11 0.075(5) 0.031(3) 0.064(4) -0.013(3) 0.029(4) -0.011(3) O12 0.050(5) 0.029(3) 0.045(4) -0.011(3) 0.028(4) -0.002(3) C1 0.011(3) 0.010(2) 0.009(2) 0.0003(19) 0.0015(19) 0.000(2) C2 0.008(2) 0.007(2) 0.013(2) 0.0009(19) 0.0020(19) -0.0006(18) C3 0.010(3) 0.009(2) 0.011(2) 0.0000(18) -0.0018(19) -0.0011(19) C4 0.0085(14) 0.0076(13) 0.0091(13) -0.0007(11) 0.0015(11) -0.0009(11) C5 0.009(3) 0.010(2) 0.010(2) 0.0039(18) 0.0022(19) -0.0006(19) C6 0.009(2) 0.008(2) 0.009(2) 0.0006(18) 0.0030(18) -0.0032(18) C7 0.010(3) 0.008(2) 0.009(2) 0.0013(17) 0.0016(19) -0.0002(18) C8 0.012(2) 0.008(2) 0.004(2) -0.0019(19) 0.0028(18) -0.002(2) C9 0.012(3) 0.009(2) 0.010(2) 0.0029(19) 0.0005(19) -0.001(2) C10 0.015(3) 0.011(2) 0.008(2) -0.0019(18) 0.0007(19) -0.001(2) C11 0.008(2) 0.008(2) 0.013(2) -0.0012(18) 0.0026(19) -0.0013(18) C12 0.009(3) 0.009(2) 0.010(2) -0.0006(18) 0.0027(18) -0.0031(18) C13 0.013(3) 0.009(2) 0.006(2) -0.0014(18) 0.0028(18) 0.0004(19) C14 0.011(2) 0.007(2) 0.013(2) -0.001(2) -0.0022(17) -0.001(2) C15 0.007(3) 0.009(2) 0.012(3) -0.0005(18) 0.0005(19) -0.0017(18) C16 0.014(3) 0.010(2) 0.014(2) -0.0007(18) 0.001(2) 0.0038(19) O12A 0.042(17) 0.07(2) 0.026(14) -0.021(14) 0.016(12) -0.005(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O2 53.18(11) . . O1 Gd1 O8 72.59(13) . 1_655 O1 Gd1 O10 144.90(14) . . O1 Gd1 C1 26.84(13) . . O2 Gd1 O8 68.81(12) . 1_655 O2 Gd1 C1 26.50(13) . . O3 Gd1 O1 129.01(12) 2_545 . O3 Gd1 O2 135.28(13) 2_545 . O3 Gd1 O8 71.04(12) 2_545 1_655 O3 Gd1 O10 73.91(13) 2_545 . O3 Gd1 C1 140.70(14) 2_545 . O4 Gd1 O1 124.81(12) 4_666 . O4 Gd1 O2 72.41(12) 4_666 . O4 Gd1 O3 82.49(13) 4_666 2_545 O4 Gd1 O8 80.64(12) 4_666 1_655 O4 Gd1 O10 79.39(14) 4_666 . O4 Gd1 C1 98.83(14) 4_666 . O6 Gd1 O1 77.63(13) 4_656 . O6 Gd1 O2 130.50(13) 4_656 . O6 Gd1 O3 78.19(14) 4_656 2_545 O6 Gd1 O4 157.00(13) 4_656 4_666 O6 Gd1 O8 104.40(13) 4_656 1_655 O6 Gd1 O10 83.34(15) 4_656 . O6 Gd1 C1 104.02(15) 4_656 . O7 Gd1 O1 80.43(14) 2_455 . O7 Gd1 O2 73.19(13) 2_455 . O7 Gd1 O3 146.22(13) 2_455 2_545 O7 Gd1 O4 93.41(13) 2_455 4_666 O7 Gd1 O6 95.73(13) 2_455 4_656 O7 Gd1 O8 141.57(13) 2_455 1_655 O7 Gd1 O10 72.38(14) 2_455 . O7 Gd1 C1 73.08(14) 2_455 . O8 Gd1 C1 70.47(13) 1_655 . O10 Gd1 O2 133.47(13) . . O10 Gd1 O8 141.47(13) . 1_655 O10 Gd1 C1 145.23(13) . . C1 O1 Gd1 95.2(3) . . C1 O2 Gd1 90.3(3) . . C8 O3 Gd1 164.4(4) . 2 C8 O4 Gd1 140.7(3) . 4_565 C9 O5 C6 116.9(4) . . C15 O6 Gd1 147.1(4) . 4 C15 O7 Gd1 160.0(4) . 2_445 C16 O8 Gd1 130.2(3) . 1_455 C16 O9 H9 109.5 . . Gd1 O10 H10A 112.7 . . Gd1 O10 H10B 112.8 . . H10A O10 H10B 105.8 . . H11A O11 H11B 109.6 . . O1 C1 Gd1 58.0(2) . . O1 C1 C2 119.0(5) . . O2 C1 Gd1 63.2(3) . . O2 C1 O1 120.6(5) . . O2 C1 C2 120.3(5) . . C2 C1 Gd1 169.3(4) . . C3 C2 C1 120.2(5) . . C3 C2 C7 120.2(5) . . C7 C2 C1 119.5(5) . . C2 C3 H3 120.3 . . C2 C3 C4 119.4(5) . . C4 C3 H3 120.3 . . C3 C4 C8 118.9(5) . . C5 C4 C3 121.1(5) . . C5 C4 C8 119.9(5) . . C4 C5 H5 120.5 . . C4 C5 C6 119.1(5) . . C6 C5 H5 120.5 . . O5 C6 C5 117.0(4) . . C7 C6 O5 121.9(4) . . C7 C6 C5 121.0(5) . . C2 C7 H7 120.4 . . C6 C7 C2 119.3(5) . . C6 C7 H7 120.4 . . O3 C8 O4 123.6(5) . . O3 C8 C4 119.2(5) . . O4 C8 C4 117.2(5) . . O5 C9 C10 117.7(5) . . O5 C9 C14 121.5(5) . . C14 C9 C10 120.8(5) . . C9 C10 H10 120.3 . . C11 C10 C9 119.5(5) . . C11 C10 H10 120.3 . . C10 C11 C15 119.4(5) . . C12 C11 C10 120.5(5) . . C12 C11 C15 120.0(5) . . C11 C12 H12 120.5 . . C11 C12 C13 119.0(5) . . C13 C12 H12 120.5 . . C12 C13 C16 120.0(5) . . C14 C13 C12 121.1(5) . . C14 C13 C16 118.8(5) . . C9 C14 C13 119.1(5) . . C9 C14 H14 120.4 . . C13 C14 H14 120.4 . . O6 C15 O7 125.0(5) . . O6 C15 C11 118.3(5) . . O7 C15 C11 116.6(5) . . O8 C16 O9 123.0(5) . . O8 C16 C13 124.4(5) . . O9 C16 C13 112.6(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Gd1 O1 2.399(4) . Gd1 O2 2.515(3) . Gd1 O3 2.358(4) 2_545 Gd1 O4 2.350(4) 4_666 Gd1 O6 2.287(4) 4_656 Gd1 O7 2.281(4) 2_455 Gd1 O8 2.528(3) 1_655 Gd1 O10 2.422(4) . Gd1 C1 2.817(5) . O1 C1 1.277(6) . O2 C1 1.257(6) . O3 Gd1 2.358(4) 2 O3 C8 1.244(7) . O4 Gd1 2.350(3) 4_565 O4 C8 1.267(7) . O5 C6 1.390(6) . O5 C9 1.376(6) . O6 Gd1 2.287(4) 4 O6 C15 1.249(6) . O7 Gd1 2.281(4) 2_445 O7 C15 1.251(6) . O8 Gd1 2.528(3) 1_455 O8 C16 1.225(7) . O9 H9 0.9501 . O9 C16 1.324(6) . O10 H10A 0.9259 . O10 H10B 0.9298 . O11 H11A 0.8494 . O11 H11B 0.8506 . C1 C2 1.492(7) . C2 C3 1.387(7) . C2 C7 1.401(7) . C3 H3 0.9300 . C3 C4 1.397(7) . C4 C5 1.376(7) . C4 C8 1.508(7) . C5 H5 0.9300 . C5 C6 1.396(6) . C6 C7 1.383(7) . C7 H7 0.9300 . C9 C10 1.395(7) . C9 C14 1.387(7) . C10 H10 0.9300 . C10 C11 1.394(7) . C11 C12 1.393(7) . C11 C15 1.505(7) . C12 H12 0.9300 . C12 C13 1.397(7) . C13 C14 1.390(7) . C13 C16 1.490(7) . C14 H14 0.9300 . 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 Gd1 O1 C1 O2 9.0(5) . Gd1 O1 C1 C2 -168.1(4) . Gd1 O2 C1 O1 -8.5(5) . Gd1 O2 C1 C2 168.6(4) . Gd1 O3 C8 O4 73.3(15) 2 Gd1 O3 C8 C4 -108.4(13) 2 Gd1 O4 C8 O3 -82.3(8) 4_565 Gd1 O4 C8 C4 99.3(5) 4_565 Gd1 O6 C15 O7 -47.7(9) 4 Gd1 O6 C15 C11 131.1(5) 4 Gd1 O7 C15 O6 -12.4(14) 2_445 Gd1 O7 C15 C11 168.8(9) 2_445 Gd1 O8 C16 O9 12.6(8) 1_455 Gd1 O8 C16 C13 -170.8(3) 1_455 Gd1 C1 C2 C3 102.1(19) . Gd1 C1 C2 C7 -80(2) . O1 C1 C2 C3 172.5(5) . O1 C1 C2 C7 -9.5(7) . O2 C1 C2 C3 -4.6(8) . O2 C1 C2 C7 173.4(5) . O5 C6 C7 C2 175.9(4) . O5 C9 C10 C11 -175.8(5) . O5 C9 C14 C13 176.5(5) . C1 C2 C3 C4 179.9(5) . C1 C2 C7 C6 -179.6(5) . C2 C3 C4 C5 -0.8(8) . C2 C3 C4 C8 -178.2(5) . C3 C2 C7 C6 -1.5(8) . C3 C4 C5 C6 -0.6(8) . C3 C4 C8 O3 13.3(8) . C3 C4 C8 O4 -168.2(5) . C4 C5 C6 O5 -175.0(4) . C4 C5 C6 C7 1.0(8) . C5 C4 C8 O3 -164.1(5) . C5 C4 C8 O4 14.3(8) . C5 C6 C7 C2 0.1(8) . C6 O5 C9 C10 -140.8(5) . C6 O5 C9 C14 42.1(7) . C7 C2 C3 C4 1.9(8) . C8 C4 C5 C6 176.8(5) . C9 O5 C6 C5 -141.1(5) . C9 O5 C6 C7 43.0(7) . C9 C10 C11 C12 -0.8(8) . C9 C10 C11 C15 -177.4(4) . C10 C9 C14 C13 -0.6(8) . C10 C11 C12 C13 -0.6(8) . C10 C11 C15 O6 10.4(7) . C10 C11 C15 O7 -170.7(5) . C11 C12 C13 C14 1.4(8) . C11 C12 C13 C16 179.8(5) . C12 C11 C15 O6 -166.2(5) . C12 C11 C15 O7 12.7(7) . C12 C13 C14 C9 -0.8(8) . C12 C13 C16 O8 -14.6(8) . C12 C13 C16 O9 162.2(5) . C14 C9 C10 C11 1.4(8) . C14 C13 C16 O8 163.8(5) . C14 C13 C16 O9 -19.3(7) . C15 C11 C12 C13 176.0(4) . C16 C13 C14 C9 -179.3(5) . loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7458(6) 2 0.2542(6)