#------------------------------------------------------------------------------ #$Date: 2023-05-05 04:48:24 +0300 (Fri, 05 May 2023) $ #$Revision: 283250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712196.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_7712196 loop_ _publ_author_name 'Pilichos, Evangelos' 'Tubau, Ànnia' 'Speed, Saskia' 'Font-Bardia, Mercè' 'Escuer, Albert' 'Grabulosa, Arnald' 'Mayans, Júlia' _publ_section_title ; Magnetic and optical studies of a new family of multidimensional and multiproperty PO-lanthanide(III) derived systems. ; _journal_issue 8 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2485 _journal_page_last 2494 _journal_paper_doi 10.1039/d2dt03621e _journal_volume 52 _journal_year 2023 _chemical_formula_moiety 'C29 H31 Gd N4 O12 P2' _chemical_formula_sum 'C29 H31 Gd N4 O12 P2' _chemical_formula_weight 846.77 _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 _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-12-22 deposited with the CCDC. 2023-01-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.076(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.0768(7) _cell_length_b 9.9525(5) _cell_length_c 20.5086(10) _cell_measurement_reflns_used 9491 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.50 _cell_measurement_theta_min 2.29 _cell_volume 3380.9(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX4' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 123942 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.549 _diffrn_reflns_theta_min 2.288 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 2.123 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.664 _exptl_crystal_description prism _exptl_crystal_F_000 1692 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: methanol / ether' _exptl_crystal_size_max 0.395 _exptl_crystal_size_mid 0.097 _exptl_crystal_size_min 0.063 _refine_diff_density_max 0.643 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 435 _refine_ls_number_reflns 10344 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0271 _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^)+(0.0151P)^2^+2.1688P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.0571 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8380 _reflns_number_total 10344 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt03621e2.cif _cod_data_source_block mo_I06AAB43A_0m_a _cod_depositor_comments 'Adding full bibliography for 7712194--7712196.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7712196 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_res_file ; TITL mo_I06AAB43A_0m_a.res in P2(1)/n mo_I06AAB43A_0m_a.res created by SHELXL-2018/3 at 11:42:52 on 19-Dec-2022 REM Old TITL mo_I06AAB43A_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.053, Rweak 0.003, Alpha 0.051 REM 0.588 for 421 systematic absences, Orientation as input REM Formula found by SHELXT: C29 Gd N4 O12 P2 CELL 0.71073 17.0768 9.9525 20.5086 90.000 104.076 90.000 ZERR 4.000 0.0007 0.0005 0.0010 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H GD N O P UNIT 116 124 4 16 48 8 TEMP -173.150 L.S. 10 BOND LIST 6 DELU 0.001 GD1 O5 DELU 0.0001 GD1 O8 DELU 0.001 GD1 O9 DELU 0.001 GD1 O11 DELU 0.001 GD1 O12 OMIT -7 0 29 OMIT -10 11 16 OMIT 0 0 2 OMIT -12 10 17 ACTA FMAP 2 PLAN 20 WGHT 0.015100 2.168800 FVAR 0.22065 GD1 3 0.736527 0.380723 0.441771 11.00000 0.01010 0.00941 = 0.01333 0.00008 0.00384 -0.00001 P1 6 0.945328 0.360739 0.417767 11.00000 0.01076 0.01036 = 0.01142 -0.00157 0.00335 -0.00045 P2 6 0.509405 0.363646 0.416416 11.00000 0.01099 0.01385 = 0.01257 -0.00180 0.00347 -0.00064 O1 5 0.855475 0.377688 0.406723 11.00000 0.01272 0.01524 = 0.01613 -0.00196 0.00488 -0.00031 O2 5 0.597149 0.367950 0.415717 11.00000 0.01197 0.01643 = 0.01680 -0.00325 0.00434 -0.00002 O3 5 0.708817 0.285580 0.545284 11.00000 0.02365 0.04882 = 0.02579 0.01705 0.01351 0.01550 O4 5 0.799342 0.194966 0.626982 11.00000 0.04146 0.03418 = 0.02003 0.01295 0.00623 0.00454 O5 5 0.832502 0.280747 0.539432 11.00000 0.01728 0.03209 = 0.02677 0.01499 0.00345 -0.00026 O6 5 0.696913 0.377517 0.314875 11.00000 0.01938 0.01476 = 0.01997 -0.00075 0.00458 -0.00353 O7 5 0.723621 0.570174 0.364483 11.00000 0.02823 0.01335 = 0.01663 -0.00116 0.00419 0.00154 O8 5 0.717403 0.552830 0.257359 11.00000 0.04786 0.02976 = 0.01505 0.00946 0.00535 -0.00219 O9 5 0.820311 0.567972 0.508437 11.00000 0.01306 0.02585 = 0.03352 -0.01597 0.00555 0.00000 O10 5 0.694605 0.569066 0.506972 11.00000 0.01690 0.02999 = 0.04301 -0.01992 0.01577 -0.01160 O11 5 0.775515 0.711451 0.570743 11.00000 0.02157 0.01968 = 0.02432 -0.01107 0.00426 -0.00166 O12 5 0.728658 0.151931 0.415225 11.00000 0.02147 0.01116 = 0.02206 -0.00209 0.00701 -0.00084 N1 4 0.780820 0.251701 0.572775 11.00000 0.02393 0.01442 = 0.01815 0.00144 0.00576 0.00141 N2 4 0.712523 0.501047 0.310219 11.00000 0.01814 0.01810 = 0.01497 0.00175 0.00147 0.00106 N3 4 0.764182 0.619293 0.530522 11.00000 0.01605 0.01373 = 0.01697 -0.00023 0.00443 0.00059 N4 4 0.698244 -0.052665 0.367891 11.00000 0.02734 0.01024 = 0.01781 0.00033 -0.00040 0.00022 C1 1 0.972707 0.187816 0.413164 11.00000 0.01512 0.01152 = 0.01326 -0.00087 0.00613 -0.00040 C2 1 0.914134 0.101009 0.376068 11.00000 0.01573 0.01516 = 0.01746 -0.00250 0.00409 -0.00132 AFIX 43 H2 2 0.862133 0.134294 0.354542 11.00000 -1.20000 AFIX 0 C3 1 0.932210 -0.034041 0.370786 11.00000 0.02373 0.01355 = 0.02070 -0.00548 0.00607 -0.00479 AFIX 43 H3 2 0.892579 -0.093135 0.345474 11.00000 -1.20000 AFIX 0 C4 1 1.008087 -0.082748 0.402435 11.00000 0.02731 0.01207 = 0.02042 -0.00208 0.00529 0.00101 AFIX 43 H4 2 1.020252 -0.175169 0.398767 11.00000 -1.20000 AFIX 0 C5 1 1.066320 0.003244 0.439474 11.00000 0.02065 0.01746 = 0.02059 -0.00005 0.00109 0.00449 AFIX 43 H5 2 1.118131 -0.030517 0.461202 11.00000 -1.20000 AFIX 0 C6 1 1.048869 0.138254 0.444743 11.00000 0.01726 0.01570 = 0.01754 -0.00209 0.00206 -0.00082 AFIX 43 H6 2 1.088819 0.197047 0.469881 11.00000 -1.20000 AFIX 0 C7 1 0.980824 0.455499 0.356092 11.00000 0.01462 0.01390 = 0.01051 -0.00192 0.00122 -0.00289 C8 1 0.938938 0.572030 0.329691 11.00000 0.01933 0.01487 = 0.01580 -0.00275 0.00206 -0.00083 AFIX 43 H8 2 0.890656 0.596223 0.341987 11.00000 -1.20000 AFIX 0 C9 1 0.968252 0.652092 0.285464 11.00000 0.03561 0.01553 = 0.01676 -0.00086 0.00243 -0.00323 AFIX 43 H9 2 0.939772 0.730895 0.267280 11.00000 -1.20000 AFIX 0 C10 1 1.038800 0.617415 0.267817 11.00000 0.03698 0.02944 = 0.01548 0.00277 0.00776 -0.01061 AFIX 43 H10 2 1.059045 0.673300 0.238110 11.00000 -1.20000 AFIX 0 C11 1 1.080094 0.501505 0.293276 11.00000 0.02388 0.03654 = 0.02276 0.00248 0.01302 -0.00279 AFIX 43 H11 2 1.128021 0.477315 0.280408 11.00000 -1.20000 AFIX 0 C12 1 1.051383 0.420664 0.337635 11.00000 0.01679 0.02540 = 0.01757 0.00251 0.00555 0.00002 AFIX 43 H12 2 1.079930 0.341616 0.355358 11.00000 -1.20000 AFIX 0 C13 1 0.471784 0.194059 0.407950 11.00000 0.01601 0.01547 = 0.01350 -0.00149 0.00475 -0.00279 C14 1 0.526738 0.088015 0.419987 11.00000 0.01968 0.01774 = 0.02977 0.00066 0.00911 -0.00075 AFIX 43 H14 2 0.583070 0.105727 0.432758 11.00000 -1.20000 AFIX 0 C15 1 0.498924 -0.043616 0.413260 11.00000 0.03207 0.01571 = 0.04061 0.00071 0.01397 0.00021 AFIX 43 H15 2 0.536369 -0.115917 0.420733 11.00000 -1.20000 AFIX 0 C16 1 0.416725 -0.069940 0.395681 11.00000 0.03697 0.01849 = 0.03004 -0.00439 0.01170 -0.01137 AFIX 43 H16 2 0.397980 -0.160129 0.390910 11.00000 -1.20000 AFIX 0 C17 1 0.362070 0.034923 0.385099 11.00000 0.02370 0.02611 = 0.03417 -0.00327 0.00605 -0.00986 AFIX 43 H17 2 0.305770 0.016713 0.373679 11.00000 -1.20000 AFIX 0 C18 1 0.389360 0.167264 0.391143 11.00000 0.01952 0.02121 = 0.02629 -0.00125 0.00449 -0.00071 AFIX 43 H18 2 0.351691 0.239240 0.383789 11.00000 -1.20000 AFIX 0 C19 1 0.450266 0.464519 0.349537 11.00000 0.01450 0.01427 = 0.01320 -0.00214 0.00198 -0.00030 C20 1 0.374118 0.514226 0.351170 11.00000 0.01625 0.02318 = 0.01735 0.00065 0.00502 -0.00024 AFIX 43 H20 2 0.352123 0.495119 0.388479 11.00000 -1.20000 AFIX 0 C21 1 0.330808 0.591339 0.298335 11.00000 0.01772 0.02783 = 0.02744 0.00343 0.00276 0.00522 AFIX 43 H21 2 0.279122 0.625107 0.299465 11.00000 -1.20000 AFIX 0 C22 1 0.362771 0.619273 0.243856 11.00000 0.03098 0.02731 = 0.01971 0.00716 0.00182 0.00663 AFIX 43 H22 2 0.332604 0.671250 0.207484 11.00000 -1.20000 AFIX 0 C23 1 0.438369 0.571846 0.242185 11.00000 0.03351 0.03075 = 0.01950 0.00616 0.01100 0.00536 AFIX 43 H23 2 0.460160 0.592099 0.204892 11.00000 -1.20000 AFIX 0 C24 1 0.482589 0.494623 0.294902 11.00000 0.02091 0.02185 = 0.01909 -0.00018 0.00796 0.00220 AFIX 43 H24 2 0.534615 0.462439 0.293769 11.00000 -1.20000 AFIX 0 C25 1 0.701681 0.079123 0.365195 11.00000 0.02300 0.01128 = 0.02076 0.00147 0.00557 0.00161 AFIX 43 H25 2 0.682554 0.121395 0.322770 11.00000 -1.20000 AFIX 0 C26 1 0.728025 -0.123018 0.431301 11.00000 0.04350 0.01546 = 0.02179 0.00326 -0.00316 -0.00074 AFIX 137 H26A 2 0.687676 -0.188619 0.437549 11.00000 -1.50000 H26B 2 0.738065 -0.058162 0.468363 11.00000 -1.50000 H26C 2 0.778386 -0.169646 0.430686 11.00000 -1.50000 AFIX 0 C27 1 0.665843 -0.133493 0.308300 11.00000 0.06536 0.01383 = 0.02418 -0.00110 -0.00975 -0.00098 PART 1 AFIX 137 H27A 2 0.627004 -0.198453 0.317918 10.50000 -1.50000 H27B 2 0.709975 -0.181568 0.295590 10.50000 -1.50000 H27C 2 0.638731 -0.074889 0.271265 10.50000 -1.50000 AFIX 137 PART 2 H27D 2 0.614506 -0.173669 0.311472 10.50000 -1.50000 H27E 2 0.704266 -0.204845 0.305064 10.50000 -1.50000 H27F 2 0.656938 -0.076395 0.268236 10.50000 -1.50000 AFIX 0 PART 0 C28 1 0.998514 0.422896 0.498950 11.00000 0.01535 0.01119 = 0.01084 -0.00205 0.00265 -0.00165 AFIX 23 H28A 2 0.971487 0.389944 0.533453 11.00000 -1.20000 H28B 2 1.054295 0.387180 0.509995 11.00000 -1.20000 AFIX 0 C29 1 0.491747 0.424656 0.494373 11.00000 0.01637 0.01390 = 0.01326 -0.00130 0.00517 0.00028 AFIX 23 H29A 2 0.434923 0.406328 0.494898 11.00000 -1.20000 H29B 2 0.526676 0.374346 0.532078 11.00000 -1.20000 REM ##### REM ##### AFIX 0 HKLF 4 REM mo_I06AAB43A_0m_a.res in P2(1)/n REM wR2 = 0.0571, GooF = S = 1.025, Restrained GooF = 1.026 for all data REM R1 = 0.0271 for 8380 Fo > 4sig(Fo) and 0.0428 for all 10344 data REM 435 parameters refined using 3 restraints END WGHT 0.0144 2.2332 REM Highest difference peak 0.643, deepest hole -0.996, 1-sigma level 0.115 Q1 1 0.7810 0.3912 0.4976 11.00000 0.05 0.64 Q2 1 0.6843 0.3906 0.3942 11.00000 0.05 0.62 Q3 1 0.6771 0.3438 0.3510 11.00000 0.05 0.51 Q4 1 0.7103 0.3804 0.4940 11.00000 0.05 0.50 Q5 1 0.3832 0.0960 0.3847 11.00000 0.05 0.50 Q6 1 0.9769 0.4207 0.3845 11.00000 0.05 0.49 Q7 1 0.6618 0.4136 0.3525 11.00000 0.05 0.46 Q8 1 0.4987 0.1527 0.4190 11.00000 0.05 0.46 Q9 1 0.8167 0.3668 0.5317 11.00000 0.05 0.46 Q10 1 0.9837 0.4037 0.4638 11.00000 0.05 0.45 Q11 1 0.4836 0.2478 0.4101 11.00000 0.05 0.45 Q12 1 0.8161 0.5007 0.5014 11.00000 0.05 0.45 Q13 1 0.7607 0.3918 0.3910 11.00000 0.05 0.44 Q14 1 0.6849 0.1424 0.4669 11.00000 0.05 0.43 Q15 1 0.5000 0.5000 0.5000 10.50000 0.05 0.43 Q16 1 0.9649 0.2580 0.4146 11.00000 0.05 0.43 Q17 1 0.4997 0.3927 0.4626 11.00000 0.05 0.43 Q18 1 0.8999 0.3610 0.4157 11.00000 0.05 0.42 Q19 1 0.2603 0.6834 0.3225 11.00000 0.05 0.41 Q20 1 0.4777 0.4174 0.3711 11.00000 0.05 0.41 ; _shelx_res_checksum 11644 _shelx_hkl_file ; -2 0 0 1057.49 77.49 2 0 0 1162.68 77.29 2 0 0 1137.09 76.79 2 0 0 1044.20 76.99 2 0 0 1067.79 77.49 -2 0 0 1129.79 76.79 -2 0 0 1054.09 76.99 -2 0 0 1167.18 77.39 -3 0 0 -0.20 1.20 -3 0 0 -0.10 0.90 -3 0 0 -0.40 1.50 -3 0 0 -0.70 3.70 3 0 0 -0.40 1.30 3 0 0 -0.70 0.70 3 0 0 -1.30 0.90 3 0 0 0.80 1.50 -3 0 0 1.10 1.00 4 0 0 9999.00 674.03 -4 0 0 9406.26 678.53 -5 0 0 -1.90 4.00 -5 0 0 2.20 2.10 5 0 0 0.70 2.10 -5 0 0 2.80 1.40 5 0 0 0.20 1.80 -5 0 0 2.20 1.00 -5 0 0 -0.10 1.80 5 0 0 2.40 1.00 6 0 0 741.83 57.19 -6 0 0 791.42 57.39 6 0 0 794.72 54.59 6 0 0 761.22 56.29 -6 0 0 842.32 56.69 -6 0 0 709.23 62.49 -6 0 0 764.82 55.19 -6 0 0 767.92 55.59 -7 0 0 2.90 3.10 -7 0 0 -5.10 5.90 -7 0 0 -1.00 1.80 7 0 0 1.30 1.10 -7 0 0 2.30 1.90 -7 0 0 1.70 2.90 8 0 0 316.47 22.30 -8 0 0 292.57 23.30 -8 0 0 302.97 26.10 -8 0 0 282.17 33.00 -8 0 0 297.67 23.90 -8 0 0 345.37 25.30 9 0 0 1.40 0.90 -9 0 0 3.50 2.40 -9 0 0 0.00 6.10 -9 0 0 -0.10 3.50 -9 0 0 13.50 8.90 -9 0 0 0.90 2.00 -9 0 0 2.90 3.30 -10 0 0 245.68 19.60 -10 0 0 194.38 17.00 -10 0 0 202.18 31.20 -10 0 0 207.48 20.50 -10 0 0 222.38 17.90 -11 0 0 1.40 6.90 -11 0 0 10.90 3.10 -11 0 0 12.10 5.10 -11 0 0 7.80 9.20 -11 0 0 13.00 7.80 -11 0 0 10.80 5.10 -11 0 0 5.10 2.50 -12 0 0 85.69 20.20 -12 0 0 107.99 10.50 -12 0 0 99.19 9.40 -12 0 0 96.39 11.90 -12 0 0 86.29 19.50 -12 0 0 121.99 15.80 -12 0 0 87.09 13.90 -13 0 0 21.70 8.30 -13 0 0 13.00 11.00 -13 0 0 20.90 6.20 -13 0 0 7.50 2.90 -13 0 0 4.50 3.30 -13 0 0 12.70 5.30 -13 0 0 4.70 2.70 -13 0 0 -2.20 6.80 -14 0 0 14.50 3.90 -14 0 0 17.40 7.40 -14 0 0 4.30 9.90 -14 0 0 18.00 4.80 -14 0 0 26.20 7.70 -14 0 0 6.70 4.00 -14 0 0 -4.80 12.10 -14 0 0 14.40 6.00 -15 0 0 4.50 18.70 -15 0 0 0.30 2.50 -15 0 0 9.00 10.80 -15 0 0 8.30 4.00 -15 0 0 -3.10 3.00 -15 0 0 -5.00 4.50 -16 0 0 90.09 12.00 -16 0 0 87.19 24.90 -16 0 0 85.89 15.00 -16 0 0 76.79 10.30 -17 0 0 8.30 3.80 -17 0 0 -1.50 12.50 -17 0 0 -1.60 2.60 -17 0 0 16.60 6.80 -17 0 0 6.90 4.60 -18 0 0 49.10 6.50 -18 0 0 36.60 7.90 -18 0 0 69.79 9.30 -18 0 0 65.19 27.40 -18 0 0 35.10 17.20 -18 0 0 42.70 11.80 -19 0 0 5.60 14.60 -19 0 0 1.90 5.20 -19 0 0 5.90 5.30 -19 0 0 3.20 2.30 -19 0 0 9.10 8.60 -20 0 0 4.40 18.10 -20 0 0 6.20 5.60 -20 0 0 12.50 11.20 -20 0 0 2.90 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140.89 19.80 8 -3 0 96.29 21.40 8 -3 0 160.88 15.20 8 3 0 160.48 17.40 -8 3 0 141.59 16.60 -8 3 0 133.29 13.90 -8 3 0 188.98 26.10 8 3 0 104.79 20.00 -8 3 0 140.89 13.90 8 3 0 125.09 13.10 -8 3 0 157.08 12.30 -8 3 0 145.09 22.70 9 -3 0 574.44 56.99 -9 -3 0 601.24 46.60 9 -3 0 611.94 48.00 9 -3 0 601.04 46.10 9 -3 0 625.04 46.20 -9 -3 0 611.64 46.40 -9 -3 0 631.64 43.70 -9 -3 0 579.64 52.19 -9 -3 0 605.74 60.19 -9 3 0 622.44 47.60 -9 3 0 622.34 46.80 -9 3 0 622.74 50.59 9 3 0 617.24 50.19 9 3 0 556.64 46.40 -9 3 0 696.23 55.39 -9 3 0 638.24 44.80 -9 3 0 684.13 57.59 10 -3 0 103.69 24.20 10 -3 0 141.39 12.80 -10 -3 0 109.59 20.30 -10 -3 0 122.79 19.40 10 -3 0 135.39 12.30 -10 -3 0 149.09 13.40 -10 -3 0 114.79 12.70 -10 -3 0 127.79 10.00 -10 3 0 131.29 12.90 -10 3 0 163.98 26.40 -10 3 0 165.28 23.10 10 3 0 129.59 17.80 -10 3 0 137.99 14.10 -10 3 0 121.49 17.60 10 3 0 115.69 13.00 10 3 0 102.59 21.20 -10 3 0 127.29 11.00 11 -3 0 38.50 14.20 11 -3 0 50.49 6.80 -11 -3 0 62.39 9.10 -11 -3 0 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221.88 37.70 -13 3 0 291.67 23.10 -13 3 0 190.28 25.70 -13 3 0 283.27 28.30 13 3 0 216.58 25.50 -14 -3 0 524.45 41.00 14 -3 0 525.65 38.20 -14 -3 0 478.15 53.29 -14 -3 0 510.75 36.60 14 -3 0 526.25 38.90 -14 -3 0 521.35 47.40 -14 -3 0 499.45 58.49 14 -3 0 501.15 43.40 -14 -3 0 538.95 36.80 -14 3 0 528.75 47.00 -14 3 0 589.94 59.19 -14 3 0 524.75 45.80 -14 3 0 512.85 37.00 -14 3 0 477.75 47.40 -14 3 0 511.75 40.70 -14 3 0 513.05 42.00 14 3 0 509.75 44.10 -15 -3 0 78.69 18.00 -15 -3 0 97.49 13.00 -15 -3 0 107.99 14.40 15 -3 0 97.19 8.00 -15 -3 0 107.79 26.60 -15 -3 0 90.19 6.90 15 -3 0 87.39 7.60 -15 -3 0 74.29 25.60 -15 3 0 103.79 19.80 -15 3 0 104.89 18.10 -15 3 0 105.79 18.20 -15 3 0 105.99 11.90 15 3 0 94.09 15.60 -15 3 0 106.89 14.20 -16 -3 0 532.55 59.29 -16 -3 0 522.45 42.00 -16 -3 0 433.36 53.39 -16 -3 0 450.65 38.90 -16 -3 0 493.35 45.00 -16 3 0 481.75 40.70 -16 3 0 527.15 45.60 -16 3 0 468.25 43.50 -16 3 0 496.65 39.10 16 3 0 500.05 41.50 -16 3 0 523.85 47.00 -17 -3 0 66.09 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659.43 59.09 3 -4 0 149.79 26.40 3 -4 0 156.88 14.40 -3 -4 0 144.99 14.50 -3 -4 0 138.59 12.60 3 -4 0 141.19 14.10 -3 -4 0 149.29 14.80 3 -4 0 169.88 14.90 3 -4 0 173.98 14.90 -3 -4 0 148.19 22.60 -3 4 0 126.59 13.90 -3 4 0 138.69 16.10 3 4 0 151.38 17.70 -3 4 0 119.69 22.00 -3 4 0 134.99 14.70 3 4 0 160.78 12.40 3 4 0 131.39 12.30 3 4 0 167.58 23.20 4 -4 0 2008.50 155.38 -4 -4 0 2193.08 153.68 -4 -4 0 2220.58 156.08 -4 -4 0 2288.97 164.28 -4 -4 0 2372.06 160.48 4 -4 0 2085.99 165.78 4 -4 0 2205.48 155.98 4 -4 0 2266.27 155.38 -4 -4 0 2173.08 156.38 -4 4 0 2306.37 156.58 -4 4 0 2093.79 155.38 -4 4 0 2358.56 165.28 4 4 0 2123.69 153.48 4 4 0 2091.29 153.38 4 4 0 2113.19 161.58 -4 4 0 2137.39 158.78 -5 -4 0 5.90 2.80 -5 -4 0 7.90 2.70 5 -4 0 -0.50 3.90 5 -4 0 5.60 3.70 5 -4 0 16.90 11.60 5 -4 0 3.40 3.50 -5 -4 0 15.20 9.20 5 -4 0 7.50 3.90 -5 -4 0 4.80 5.40 5 4 0 12.40 3.40 5 4 0 13.60 8.20 5 4 0 6.40 2.30 -5 4 0 3.90 8.30 -5 4 0 4.20 4.00 -5 4 0 1.40 3.50 -5 4 0 8.60 5.40 -6 -4 0 927.91 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28 85.09 22.60 3 1 -28 54.69 17.20 3 1 -28 46.80 65.59 3 1 -28 18.00 15.90 2 -1 -28 124.09 23.20 -2 -1 28 153.98 27.50 2 -1 -28 127.79 72.99 -2 -1 28 106.19 27.40 -2 1 28 130.99 29.70 -2 1 28 103.99 66.99 -2 1 28 142.29 29.80 2 1 -28 122.09 23.50 2 1 -28 149.88 71.39 -1 -1 28 5.60 15.30 -1 -1 28 14.60 20.90 1 -1 -28 -55.29 82.79 1 -1 -28 30.70 17.30 -1 1 28 41.10 17.30 -1 1 28 111.19 52.49 1 1 -28 41.20 15.90 1 1 -28 12.70 17.90 1 1 -28 -181.48 114.59 1 1 -28 2.30 19.60 -1 1 28 46.70 17.80 0 -1 28 16.90 16.30 0 -1 28 -9.90 15.90 0 -1 -28 -2.00 18.00 0 1 -28 -24.10 12.20 0 1 -28 3.90 18.30 0 1 -28 26.30 86.69 0 1 28 1.70 19.80 0 1 28 0.50 16.60 0 1 28 62.79 68.49 -1 -1 -28 107.79 21.80 -1 -1 -28 50.19 86.99 1 -1 28 124.19 29.20 -1 -1 -28 112.59 27.80 1 -1 28 95.99 23.80 1 1 28 114.79 24.20 -1 1 -28 -62.89 78.59 -1 1 -28 103.39 27.80 1 1 28 70.89 26.00 11 -2 -28 381.86 57.09 -11 -2 28 432.96 48.30 -11 2 28 363.26 43.20 -11 2 28 468.85 51.39 10 -2 -28 38.70 29.80 -10 2 28 54.29 21.50 9 -2 -28 91.89 31.70 -9 -2 28 100.49 27.10 -9 -2 28 107.79 26.60 9 2 -28 111.29 127.49 -9 2 28 146.09 26.70 8 -2 -28 4.40 24.90 -8 -2 28 -25.40 13.90 -8 -2 28 -19.70 14.40 -8 2 28 1.10 15.50 -8 2 28 11.70 17.50 -7 -2 28 301.37 41.70 -7 -2 28 285.67 40.60 7 -2 -28 327.77 46.70 -7 2 28 296.67 40.40 7 2 -28 43.90 114.19 -7 2 28 254.17 38.30 -6 -2 28 41.50 17.10 -6 -2 28 6.90 11.90 6 2 -28 19.50 113.19 -6 2 28 -4.60 15.00 -6 2 28 10.30 15.30 -5 -2 28 99.59 23.10 -5 2 28 70.39 22.10 -5 2 28 142.29 29.20 5 2 -28 -42.00 122.09 4 -2 -28 -53.49 68.99 -4 -2 28 3.40 16.10 -4 -2 28 5.40 11.80 4 -2 -28 -11.10 9.20 -4 2 28 -25.70 14.00 4 2 -28 -28.90 62.79 4 2 -28 -8.20 11.30 -4 2 28 45.10 66.49 4 2 -28 -0.60 12.90 4 2 -28 30.00 118.79 -4 2 28 -2.60 15.80 -3 -2 28 128.99 27.30 3 -2 -28 103.29 74.99 -3 -2 28 112.59 24.20 3 2 -28 -159.38 117.39 -3 2 28 124.69 24.90 -3 2 28 143.19 28.40 3 2 -28 62.99 17.70 3 2 -28 42.70 68.79 -3 2 28 126.69 65.79 2 -2 -28 15.20 78.49 -2 -2 28 12.60 15.70 2 -2 -28 30.20 16.00 -2 -2 28 11.50 19.30 2 2 -28 -39.60 135.19 2 2 -28 15.90 16.80 -2 2 28 21.10 19.60 -2 2 28 48.80 19.00 -2 2 28 86.69 64.89 2 2 -28 117.79 71.39 2 2 -28 16.40 13.90 1 -2 -28 82.69 21.90 1 -2 -28 34.90 86.09 -1 -2 28 118.69 27.20 -1 -2 28 117.19 25.30 -1 2 28 228.18 71.89 1 2 -28 127.79 27.20 -1 2 28 89.89 23.20 -1 2 28 108.99 26.90 1 2 -28 46.30 71.89 1 2 -28 -81.49 136.29 1 2 -28 156.38 25.20 0 -2 -28 -5.70 16.70 0 -2 28 10.00 19.60 0 -2 28 -12.70 15.60 0 2 -28 -4.20 19.40 0 2 -28 37.70 16.10 0 2 28 45.20 67.39 0 2 -28 -106.79 87.19 0 2 28 -20.90 15.30 0 2 28 7.40 21.00 -10 -3 28 -32.10 15.60 10 -3 -28 -68.89 31.60 -10 -3 28 13.20 18.00 -10 3 28 -18.20 14.20 -10 3 28 -6.00 16.10 9 -3 -28 -5.80 32.60 9 3 -28 -59.79 114.69 -9 3 28 29.80 17.20 8 -3 -28 -14.50 31.90 -8 -3 28 22.20 19.50 -8 -3 28 4.80 16.00 -8 3 28 36.60 22.10 -8 3 28 14.90 16.00 8 3 -28 -16.30 118.29 -7 -3 28 -7.80 16.00 -7 -3 28 27.50 18.20 7 3 -28 -59.09 122.19 -7 3 28 21.20 18.00 -6 -3 28 8.80 14.10 -6 -3 28 -12.60 14.90 -6 3 28 17.20 18.80 6 3 -28 -20.20 120.59 -6 3 28 4.00 15.60 -5 -3 28 -19.60 15.60 -5 -3 28 2.50 13.30 -5 3 28 -15.00 11.60 5 3 -28 63.59 128.49 -5 3 28 24.10 18.20 5 3 -28 13.50 10.50 4 -3 -28 80.39 90.09 4 -3 -28 1.60 12.10 -4 -3 28 -2.40 16.80 -4 -3 28 29.00 18.20 -4 3 28 -23.90 15.80 4 3 -28 -201.48 120.99 -4 3 28 3.70 15.20 3 -3 -28 216.88 85.29 -3 -3 28 38.00 24.40 3 -3 -28 84.39 18.20 -3 -3 28 57.59 19.90 3 3 -28 107.99 20.70 3 3 -28 44.70 17.60 3 3 -28 23.20 71.19 -3 3 28 14.00 18.70 -3 3 28 72.99 24.70 3 3 -28 -301.17 145.09 2 -3 -28 159.58 84.79 2 -3 -28 100.69 21.70 -2 -3 28 76.99 22.00 -2 -3 28 74.19 27.40 -2 3 28 157.18 68.09 2 3 -28 17.40 72.59 2 3 -28 94.09 19.20 2 3 -28 -49.30 142.09 2 3 -28 46.20 21.40 -2 3 28 70.29 21.00 -2 3 28 88.89 24.60 -1 -3 28 38.30 17.80 1 -3 -28 -26.00 86.89 -1 -3 28 42.30 18.60 -1 3 28 -0.60 17.80 -1 3 28 0.30 18.20 1 3 -28 -53.09 74.69 1 3 -28 8.30 19.40 -1 3 28 32.00 67.29 1 3 -28 44.80 14.70 -7 -4 28 5.00 17.80 -7 4 28 4.20 16.70 7 4 -28 -13.20 158.48 -7 4 28 -6.60 16.00 -6 -4 28 211.68 36.50 -6 -4 28 263.27 41.10 6 4 -28 142.89 140.29 -6 4 28 288.57 40.10 -6 4 28 232.88 34.00 -6 4 28 233.38 37.60 -5 -4 28 7.40 17.00 -5 -4 28 -8.40 18.40 5 -4 -28 0.90 10.20 -5 4 28 18.80 19.60 -5 4 28 -6.40 17.20 5 4 -28 -0.80 13.30 5 4 -28 22.30 154.18 -5 4 28 -8.80 14.00 -4 -4 28 102.39 24.10 -4 -4 28 85.19 26.10 -4 4 28 173.48 29.30 -4 4 28 132.19 23.20 4 4 -28 75.19 20.50 -4 4 28 110.99 25.30 4 4 -28 -103.39 137.79 -9 0 29 -28.20 15.20 8 0 -29 -27.90 16.70 -8 0 29 -2.40 16.30 7 0 -29 -2.80 15.60 -6 0 29 -12.10 16.60 6 0 -29 -30.00 23.60 -6 0 29 0.30 19.40 -5 0 29 -10.70 16.30 -5 0 29 16.70 17.00 4 0 -29 -6.70 27.40 -4 0 29 -9.30 16.40 -4 0 29 -17.90 17.20 4 0 -29 -7.10 10.30 -3 0 29 256.07 39.00 -3 0 29 149.59 30.50 -9 -1 29 76.99 20.50 -9 1 29 66.39 20.20 -8 -1 29 31.40 20.60 8 -1 -29 32.70 25.50 8 1 -29 182.88 151.78 -8 1 29 24.80 18.80 7 -1 -29 93.49 27.90 -7 -1 29 125.99 32.60 -7 1 29 92.09 24.80 7 1 -29 -14.40 137.69 -7 1 29 90.19 21.00 -6 -1 29 133.89 29.60 6 -1 -29 150.38 33.60 -6 -1 29 82.99 26.20 -6 1 29 191.58 32.40 6 1 -29 -190.78 129.19 -5 -1 29 117.29 24.90 -5 -1 29 81.69 25.30 -5 1 29 127.09 26.30 5 1 -29 -17.70 130.39 -4 -1 29 -11.80 17.00 4 -1 -29 -0.20 14.30 -4 -1 29 -21.40 16.70 4 1 -29 -38.60 139.59 -4 1 29 -9.40 16.70 -4 1 29 7.40 17.80 4 1 -29 -11.80 11.40 -3 -1 29 -9.80 18.60 -3 -1 29 23.30 19.10 -3 1 29 33.30 20.90 -3 1 29 -9.40 18.20 -6 -2 29 136.69 32.90 -6 -2 29 148.69 36.30 -6 2 29 112.59 28.30 -5 2 29 -8.70 13.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 30916 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 0.73653(2) 0.38072(2) 0.44177(2) 0.01078(3) Uani 1 1 d . U . . . P1 P 0.94533(3) 0.36074(5) 0.41777(3) 0.01074(10) Uani 1 1 d . . . . . P2 P 0.50941(3) 0.36365(5) 0.41642(3) 0.01237(10) Uani 1 1 d . . . . . O1 O 0.85547(8) 0.37769(14) 0.40672(7) 0.0145(3) Uani 1 1 d . . . . . O2 O 0.59715(8) 0.36795(14) 0.41572(7) 0.0149(3) Uani 1 1 d . . . . . O3 O 0.70882(10) 0.2856(2) 0.54528(9) 0.0315(4) Uani 1 1 d . . . . . O4 O 0.79934(11) 0.19497(19) 0.62698(9) 0.0321(4) Uani 1 1 d . . . . . O5 O 0.83250(9) 0.28075(17) 0.53943(9) 0.0257(4) Uani 1 1 d . U . . . O6 O 0.69691(9) 0.37752(15) 0.31487(8) 0.0181(3) Uani 1 1 d . . . . . O7 O 0.72362(9) 0.57017(15) 0.36448(8) 0.0196(3) Uani 1 1 d . . . . . O8 O 0.71740(11) 0.55283(18) 0.25736(8) 0.0313(4) Uani 1 1 d . . . . . O9 O 0.82031(9) 0.56797(17) 0.50844(9) 0.0242(4) Uani 1 1 d . U . . . O10 O 0.69460(9) 0.56907(18) 0.50697(9) 0.0285(4) Uani 1 1 d . . . . . O11 O 0.77551(9) 0.71145(16) 0.57074(8) 0.0221(3) Uani 1 1 d . . . . . O12 O 0.72866(9) 0.15193(15) 0.41522(8) 0.0179(3) Uani 1 1 d . U . . . N1 N 0.78082(11) 0.25170(18) 0.57278(9) 0.0187(4) Uani 1 1 d . . . . . N2 N 0.71252(11) 0.50105(18) 0.31022(9) 0.0175(4) Uani 1 1 d . . . . . N3 N 0.76418(10) 0.61929(18) 0.53052(9) 0.0155(3) Uani 1 1 d . . . . . N4 N 0.69824(11) -0.05267(18) 0.36789(9) 0.0195(4) Uani 1 1 d . . . . . C1 C 0.97271(12) 0.1878(2) 0.41316(10) 0.0128(4) Uani 1 1 d . . . . . C2 C 0.91413(12) 0.1010(2) 0.37607(11) 0.0161(4) Uani 1 1 d . . . . . H2 H 0.862133 0.134294 0.354542 0.019 Uiso 1 1 calc R U . . . C3 C 0.93221(13) -0.0340(2) 0.37079(11) 0.0192(4) Uani 1 1 d . . . . . H3 H 0.892579 -0.093135 0.345474 0.023 Uiso 1 1 calc R U . . . C4 C 1.00809(14) -0.0827(2) 0.40244(11) 0.0200(5) Uani 1 1 d . . . . . H4 H 1.020252 -0.175169 0.398767 0.024 Uiso 1 1 calc R U . . . C5 C 1.06632(13) 0.0032(2) 0.43947(11) 0.0202(5) Uani 1 1 d . . . . . H5 H 1.118131 -0.030517 0.461202 0.024 Uiso 1 1 calc R U . . . C6 C 1.04887(13) 0.1383(2) 0.44474(11) 0.0172(4) Uani 1 1 d . . . . . H6 H 1.088819 0.197047 0.469881 0.021 Uiso 1 1 calc R U . . . C7 C 0.98082(12) 0.4555(2) 0.35609(10) 0.0133(4) Uani 1 1 d . . . . . C8 C 0.93894(13) 0.5720(2) 0.32969(11) 0.0171(4) Uani 1 1 d . . . . . H8 H 0.890656 0.596223 0.341987 0.020 Uiso 1 1 calc R U . . . C9 C 0.96825(15) 0.6521(2) 0.28546(12) 0.0233(5) Uani 1 1 d . . . . . H9 H 0.939772 0.730895 0.267280 0.028 Uiso 1 1 calc R U . . . C10 C 1.03880(15) 0.6174(3) 0.26782(12) 0.0271(5) Uani 1 1 d . . . . . H10 H 1.059045 0.673300 0.238110 0.032 Uiso 1 1 calc R U . . . C11 C 1.08009(14) 0.5015(3) 0.29328(12) 0.0265(5) Uani 1 1 d . . . . . H11 H 1.128021 0.477315 0.280408 0.032 Uiso 1 1 calc R U . . . C12 C 1.05138(13) 0.4207(2) 0.33764(11) 0.0197(5) Uani 1 1 d . . . . . H12 H 1.079930 0.341616 0.355358 0.024 Uiso 1 1 calc R U . . . C13 C 0.47178(12) 0.1941(2) 0.40795(10) 0.0148(4) Uani 1 1 d . . . . . C14 C 0.52674(14) 0.0880(2) 0.41999(12) 0.0219(5) Uani 1 1 d . . . . . H14 H 0.583070 0.105727 0.432758 0.026 Uiso 1 1 calc R U . . . C15 C 0.49892(15) -0.0436(2) 0.41326(14) 0.0286(6) Uani 1 1 d . . . . . H15 H 0.536369 -0.115917 0.420733 0.034 Uiso 1 1 calc R U . . . C16 C 0.41672(16) -0.0699(2) 0.39568(13) 0.0279(5) Uani 1 1 d . . . . . H16 H 0.397980 -0.160129 0.390910 0.033 Uiso 1 1 calc R U . . . C17 C 0.36207(15) 0.0349(3) 0.38510(13) 0.0282(5) Uani 1 1 d . . . . . H17 H 0.305770 0.016713 0.373679 0.034 Uiso 1 1 calc R U . . . C18 C 0.38936(13) 0.1673(2) 0.39114(12) 0.0225(5) Uani 1 1 d . . . . . H18 H 0.351691 0.239240 0.383789 0.027 Uiso 1 1 calc R U . . . C19 C 0.45027(12) 0.4645(2) 0.34954(10) 0.0142(4) Uani 1 1 d . . . . . C20 C 0.37412(12) 0.5142(2) 0.35117(11) 0.0188(4) Uani 1 1 d . . . . . H20 H 0.352123 0.495119 0.388479 0.023 Uiso 1 1 calc R U . . . C21 C 0.33081(14) 0.5913(2) 0.29834(13) 0.0248(5) Uani 1 1 d . . . . . H21 H 0.279122 0.625107 0.299465 0.030 Uiso 1 1 calc R U . . . C22 C 0.36277(15) 0.6193(3) 0.24386(12) 0.0267(5) Uani 1 1 d . . . . . H22 H 0.332604 0.671250 0.207484 0.032 Uiso 1 1 calc R U . . . C23 C 0.43837(15) 0.5718(3) 0.24219(12) 0.0271(5) Uani 1 1 d . . . . . H23 H 0.460160 0.592099 0.204892 0.033 Uiso 1 1 calc R U . . . C24 C 0.48259(13) 0.4946(2) 0.29490(11) 0.0201(5) Uani 1 1 d . . . . . H24 H 0.534615 0.462439 0.293769 0.024 Uiso 1 1 calc R U . . . C25 C 0.70168(13) 0.0791(2) 0.36520(12) 0.0183(4) Uani 1 1 d . . . . . H25 H 0.682554 0.121395 0.322770 0.022 Uiso 1 1 calc R U . . . C26 C 0.72803(16) -0.1230(2) 0.43130(12) 0.0288(6) Uani 1 1 d . . . . . H26A H 0.687676 -0.188619 0.437549 0.043 Uiso 1 1 calc R U . . . H26B H 0.738065 -0.058162 0.468363 0.043 Uiso 1 1 calc R U . . . H26C H 0.778386 -0.169646 0.430686 0.043 Uiso 1 1 calc R U . . . C27 C 0.6658(2) -0.1335(2) 0.30830(13) 0.0380(7) Uani 1 1 d . . . . . H27A H 0.627004 -0.198453 0.317918 0.057 Uiso 0.5 1 calc R U P A 1 H27B H 0.709975 -0.181568 0.295590 0.057 Uiso 0.5 1 calc R U P A 1 H27C H 0.638731 -0.074889 0.271265 0.057 Uiso 0.5 1 calc R U P A 1 H27D H 0.614506 -0.173669 0.311472 0.057 Uiso 0.5 1 calc R U P B 2 H27E H 0.704266 -0.204845 0.305064 0.057 Uiso 0.5 1 calc R U P B 2 H27F H 0.656938 -0.076395 0.268236 0.057 Uiso 0.5 1 calc R U P B 2 C28 C 0.99851(12) 0.42290(19) 0.49895(10) 0.0126(4) Uani 1 1 d . . . . . H28A H 0.971487 0.389944 0.533453 0.015 Uiso 1 1 calc R U . . . H28B H 1.054295 0.387180 0.509995 0.015 Uiso 1 1 calc R U . . . C29 C 0.49175(12) 0.4247(2) 0.49437(10) 0.0142(4) Uani 1 1 d . . . . . H29A H 0.434923 0.406328 0.494898 0.017 Uiso 1 1 calc R U . . . H29B H 0.526676 0.374346 0.532078 0.017 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 0.01010(4) 0.00941(5) 0.01333(5) 0.00008(4) 0.00384(3) -0.00001(4) P1 0.0108(2) 0.0104(2) 0.0114(2) -0.00157(19) 0.00335(18) -0.00045(18) P2 0.0110(2) 0.0139(3) 0.0126(2) -0.0018(2) 0.00347(18) -0.00064(19) O1 0.0127(6) 0.0152(7) 0.0161(7) -0.0020(6) 0.0049(5) -0.0003(6) O2 0.0120(6) 0.0164(7) 0.0168(7) -0.0033(6) 0.0043(5) 0.0000(6) O3 0.0236(8) 0.0488(12) 0.0258(9) 0.0170(8) 0.0135(7) 0.0155(8) O4 0.0415(10) 0.0342(10) 0.0200(9) 0.0129(8) 0.0062(8) 0.0045(8) O5 0.0173(7) 0.0321(10) 0.0268(9) 0.0150(7) 0.0034(6) -0.0003(7) O6 0.0194(7) 0.0148(7) 0.0200(8) -0.0007(6) 0.0046(6) -0.0035(6) O7 0.0282(8) 0.0134(7) 0.0166(8) -0.0012(6) 0.0042(6) 0.0015(6) O8 0.0479(11) 0.0298(10) 0.0150(8) 0.0095(7) 0.0053(8) -0.0022(8) O9 0.0131(7) 0.0258(8) 0.0335(10) -0.0160(7) 0.0055(6) 0.0000(6) O10 0.0169(8) 0.0300(9) 0.0430(11) -0.0199(8) 0.0158(7) -0.0116(7) O11 0.0216(8) 0.0197(8) 0.0243(9) -0.0111(7) 0.0043(6) -0.0017(6) O12 0.0215(7) 0.0112(6) 0.0221(8) -0.0021(6) 0.0070(6) -0.0008(6) N1 0.0239(9) 0.0144(9) 0.0182(10) 0.0014(7) 0.0058(7) 0.0014(7) N2 0.0181(9) 0.0181(9) 0.0150(9) 0.0018(7) 0.0015(7) 0.0011(7) N3 0.0161(8) 0.0137(9) 0.0170(9) -0.0002(7) 0.0044(7) 0.0006(7) N4 0.0273(10) 0.0102(9) 0.0178(10) 0.0003(7) -0.0004(8) 0.0002(7) C1 0.0151(9) 0.0115(10) 0.0133(10) -0.0009(8) 0.0061(7) -0.0004(7) C2 0.0157(9) 0.0152(10) 0.0175(10) -0.0025(8) 0.0041(8) -0.0013(8) C3 0.0237(11) 0.0136(10) 0.0207(11) -0.0055(9) 0.0061(9) -0.0048(8) C4 0.0273(11) 0.0121(10) 0.0204(11) -0.0021(8) 0.0053(9) 0.0010(8) C5 0.0206(10) 0.0175(11) 0.0206(11) -0.0001(9) 0.0011(9) 0.0045(8) C6 0.0173(9) 0.0157(11) 0.0175(10) -0.0021(8) 0.0021(8) -0.0008(8) C7 0.0146(9) 0.0139(10) 0.0105(9) -0.0019(8) 0.0012(7) -0.0029(7) C8 0.0193(10) 0.0149(10) 0.0158(11) -0.0028(8) 0.0021(8) -0.0008(8) C9 0.0356(13) 0.0155(11) 0.0168(11) -0.0009(9) 0.0024(10) -0.0032(9) C10 0.0370(13) 0.0294(13) 0.0155(11) 0.0028(10) 0.0078(10) -0.0106(11) C11 0.0239(11) 0.0365(14) 0.0228(12) 0.0025(11) 0.0130(10) -0.0028(10) C12 0.0168(10) 0.0254(12) 0.0176(11) 0.0025(9) 0.0056(8) 0.0000(8) C13 0.0160(9) 0.0155(10) 0.0135(10) -0.0015(8) 0.0048(8) -0.0028(8) C14 0.0197(10) 0.0177(11) 0.0298(13) 0.0007(9) 0.0091(9) -0.0007(8) C15 0.0321(13) 0.0157(12) 0.0406(16) 0.0007(10) 0.0140(11) 0.0002(10) C16 0.0370(14) 0.0185(12) 0.0300(14) -0.0044(10) 0.0117(11) -0.0114(10) C17 0.0237(12) 0.0261(13) 0.0342(14) -0.0033(11) 0.0060(10) -0.0099(10) C18 0.0195(10) 0.0212(11) 0.0263(13) -0.0013(10) 0.0045(9) -0.0007(9) C19 0.0145(9) 0.0143(10) 0.0132(10) -0.0021(8) 0.0020(8) -0.0003(8) C20 0.0163(10) 0.0232(12) 0.0174(11) 0.0007(9) 0.0050(8) -0.0002(8) C21 0.0177(10) 0.0278(13) 0.0274(13) 0.0034(10) 0.0028(9) 0.0052(9) C22 0.0310(12) 0.0273(13) 0.0197(11) 0.0072(10) 0.0018(9) 0.0066(10) C23 0.0335(13) 0.0308(13) 0.0195(12) 0.0062(10) 0.0110(10) 0.0054(11) C24 0.0209(11) 0.0218(12) 0.0191(11) -0.0002(9) 0.0080(9) 0.0022(9) C25 0.0230(11) 0.0113(10) 0.0208(11) 0.0015(8) 0.0056(9) 0.0016(8) C26 0.0435(15) 0.0155(11) 0.0218(12) 0.0033(10) -0.0032(11) -0.0007(11) C27 0.065(2) 0.0138(12) 0.0242(13) -0.0011(10) -0.0098(13) -0.0010(12) C28 0.0153(9) 0.0112(9) 0.0108(9) -0.0021(7) 0.0026(7) -0.0016(7) C29 0.0164(9) 0.0139(10) 0.0133(10) -0.0013(8) 0.0052(8) 0.0003(8) 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' Gd Gd -0.1653 3.9035 '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' 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 O2 Gd1 O1 149.26(5) . . ? O2 Gd1 O12 83.97(5) . . ? O1 Gd1 O12 85.41(5) . . ? O2 Gd1 O7 88.11(5) . . ? O1 Gd1 O7 75.85(5) . . ? O12 Gd1 O7 127.65(5) . . ? O2 Gd1 O5 127.47(5) . . ? O1 Gd1 O5 77.70(5) . . ? O12 Gd1 O5 77.61(6) . . ? O7 Gd1 O5 140.94(5) . . ? O2 Gd1 O3 77.07(5) . . ? O1 Gd1 O3 128.86(5) . . ? O12 Gd1 O3 79.33(6) . . ? O7 Gd1 O3 148.01(6) . . ? O5 Gd1 O3 51.46(5) . . ? O2 Gd1 O10 75.69(5) . . ? O1 Gd1 O10 124.18(5) . . ? O12 Gd1 O10 147.70(5) . . ? O7 Gd1 O10 77.06(6) . . ? O5 Gd1 O10 95.05(6) . . ? O3 Gd1 O10 71.89(6) . . ? O2 Gd1 O6 76.02(5) . . ? O1 Gd1 O6 73.44(5) . . ? O12 Gd1 O6 76.22(5) . . ? O7 Gd1 O6 51.73(5) . . ? O5 Gd1 O6 142.18(5) . . ? O3 Gd1 O6 145.16(6) . . ? O10 Gd1 O6 121.32(6) . . ? O2 Gd1 O9 125.36(5) . . ? O1 Gd1 O9 75.78(5) . . ? O12 Gd1 O9 146.51(5) . . ? O7 Gd1 O9 74.47(6) . . ? O5 Gd1 O9 71.50(6) . . ? O3 Gd1 O9 91.10(6) . . ? O10 Gd1 O9 50.20(5) . . ? O6 Gd1 O9 122.64(5) . . ? O2 Gd1 N2 84.42(5) . . ? O1 Gd1 N2 69.58(5) . . ? O12 Gd1 N2 101.49(5) . . ? O7 Gd1 N2 26.16(5) . . ? O5 Gd1 N2 147.20(5) . . ? O3 Gd1 N2 161.31(5) . . ? O10 Gd1 N2 101.20(6) . . ? O6 Gd1 N2 25.96(5) . . ? O9 Gd1 N2 97.59(6) . . ? O2 Gd1 N1 102.19(5) . . ? O1 Gd1 N1 103.33(5) . . ? O12 Gd1 N1 76.84(5) . . ? O7 Gd1 N1 154.74(5) . . ? O5 Gd1 N1 25.80(5) . . ? O3 Gd1 N1 25.66(5) . . ? O10 Gd1 N1 83.17(6) . . ? O6 Gd1 N1 153.03(5) . . ? O9 Gd1 N1 80.82(6) . . ? N2 Gd1 N1 172.89(5) . . ? O2 Gd1 N3 100.81(5) . . ? O1 Gd1 N3 100.41(5) . . ? O12 Gd1 N3 156.42(5) . . ? O7 Gd1 N3 75.82(5) . . ? O5 Gd1 N3 81.32(5) . . ? O3 Gd1 N3 79.31(6) . . ? O10 Gd1 N3 25.19(5) . . ? O6 Gd1 N3 127.36(5) . . ? O9 Gd1 N3 25.10(5) . . ? N2 Gd1 N3 101.95(5) . . ? N1 Gd1 N3 79.58(5) . . ? O1 P1 C1 111.67(9) . . ? O1 P1 C7 109.96(9) . . ? C1 P1 C7 109.27(9) . . ? O1 P1 C28 111.53(9) . . ? C1 P1 C28 107.41(9) . . ? C7 P1 C28 106.85(9) . . ? O2 P2 C19 110.68(9) . . ? O2 P2 C13 111.06(9) . . ? C19 P2 C13 109.20(10) . . ? O2 P2 C29 112.40(9) . . ? C19 P2 C29 107.71(10) . . ? C13 P2 C29 105.59(10) . . ? P1 O1 Gd1 153.46(9) . . ? P2 O2 Gd1 166.43(9) . . ? N1 O3 Gd1 96.68(12) . . ? N1 O5 Gd1 96.72(12) . . ? N2 O6 Gd1 93.26(11) . . ? N2 O7 Gd1 96.90(11) . . ? N3 O9 Gd1 96.46(11) . . ? N3 O10 Gd1 97.76(12) . . ? C25 O12 Gd1 138.18(15) . . ? O4 N1 O3 122.54(19) . . ? O4 N1 O5 122.34(19) . . ? O3 N1 O5 115.12(17) . . ? O4 N1 Gd1 178.59(16) . . ? O3 N1 Gd1 57.66(10) . . ? O5 N1 Gd1 57.47(10) . . ? O8 N2 O6 122.52(19) . . ? O8 N2 O7 121.08(19) . . ? O6 N2 O7 116.40(17) . . ? O8 N2 Gd1 168.29(15) . . ? O6 N2 Gd1 60.78(10) . . ? O7 N2 Gd1 56.94(10) . . ? O11 N3 O9 122.56(17) . . ? O11 N3 O10 122.26(17) . . ? O9 N3 O10 115.17(17) . . ? O11 N3 Gd1 175.44(15) . . ? O9 N3 Gd1 58.43(10) . . ? O10 N3 Gd1 57.05(10) . . ? C25 N4 C27 121.9(2) . . ? C25 N4 C26 120.53(19) . . ? C27 N4 C26 117.60(18) . . ? C6 C1 C2 119.81(19) . . ? C6 C1 P1 122.76(16) . . ? C2 C1 P1 117.44(15) . . ? C3 C2 C1 119.8(2) . . ? C4 C3 C2 120.1(2) . . ? C3 C4 C5 120.2(2) . . ? C6 C5 C4 120.1(2) . . ? C5 C6 C1 120.0(2) . . ? C12 C7 C8 119.7(2) . . ? C12 C7 P1 121.55(16) . . ? C8 C7 P1 118.60(16) . . ? C9 C8 C7 119.8(2) . . ? C10 C9 C8 120.2(2) . . ? C9 C10 C11 120.3(2) . . ? C10 C11 C12 120.0(2) . . ? C11 C12 C7 120.0(2) . . ? C18 C13 C14 119.7(2) . . ? C18 C13 P2 121.32(17) . . ? C14 C13 P2 118.95(16) . . ? C15 C14 C13 119.8(2) . . ? C16 C15 C14 120.3(2) . . ? C17 C16 C15 120.0(2) . . ? C16 C17 C18 120.1(2) . . ? C13 C18 C17 120.0(2) . . ? C24 C19 C20 119.62(19) . . ? C24 C19 P2 118.25(16) . . ? C20 C19 P2 122.13(16) . . ? C21 C20 C19 120.0(2) . . ? C20 C21 C22 120.1(2) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C24 120.2(2) . . ? C23 C24 C19 119.8(2) . . ? O12 C25 N4 123.7(2) . . ? C28 C28 P1 112.02(19) 3_766 . ? C29 C29 P2 113.50(19) 3_666 . ? 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 Gd1 O2 2.3126(14) . ? Gd1 O1 2.3138(14) . ? Gd1 O12 2.3375(15) . ? Gd1 O7 2.4385(15) . ? Gd1 O5 2.4680(16) . ? Gd1 O3 2.4730(17) . ? Gd1 O10 2.5060(16) . ? Gd1 O6 2.5249(15) . ? Gd1 O9 2.5373(15) . ? Gd1 N2 2.8884(18) . ? Gd1 N1 2.9071(18) . ? Gd1 N3 2.9590(18) . ? P1 O1 1.5050(14) . ? P1 C1 1.792(2) . ? P1 C7 1.797(2) . ? P1 C28 1.801(2) . ? P2 O2 1.5025(14) . ? P2 C19 1.799(2) . ? P2 C13 1.799(2) . ? P2 C29 1.803(2) . ? O3 N1 1.267(2) . ? O4 N1 1.218(2) . ? O5 N1 1.274(2) . ? O6 N2 1.267(2) . ? O7 N2 1.283(2) . ? O8 N2 1.221(2) . ? O9 N3 1.263(2) . ? O10 N3 1.271(2) . ? O11 N3 1.217(2) . ? O12 C25 1.249(3) . ? N4 C25 1.315(3) . ? N4 C27 1.455(3) . ? N4 C26 1.455(3) . ? C1 C6 1.394(3) . ? C1 C2 1.398(3) . ? C2 C3 1.389(3) . ? C3 C4 1.388(3) . ? C4 C5 1.390(3) . ? C5 C6 1.386(3) . ? C7 C12 1.392(3) . ? C7 C8 1.401(3) . ? C8 C9 1.389(3) . ? C9 C10 1.383(4) . ? C10 C11 1.386(4) . ? C11 C12 1.390(3) . ? C13 C18 1.391(3) . ? C13 C14 1.394(3) . ? C14 C15 1.389(3) . ? C15 C16 1.387(3) . ? C16 C17 1.382(4) . ? C17 C18 1.393(3) . ? C19 C24 1.397(3) . ? C19 C20 1.399(3) . ? C20 C21 1.386(3) . ? C21 C22 1.386(4) . ? C22 C23 1.383(3) . ? C23 C24 1.390(3) . ? C28 C28 1.536(4) 3_766 ? C29 C29 1.533(4) 3_666 ?