#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572196.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_1572196 loop_ _publ_author_name 'Delano, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular \s-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03786C _journal_year 2024 _chemical_formula_moiety 'C24 H30 Gd I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Gd I4 N' _chemical_formula_weight 1082.26 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-05-10 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.314(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3396(2) _cell_length_b 14.3064(3) _cell_length_c 21.2014(4) _cell_measurement_reflns_used 21684 _cell_measurement_temperature 99.8(6) _cell_measurement_theta_max 31.5720 _cell_measurement_theta_min 2.8430 _cell_volume 3075.22(11) _computing_cell_refinement 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.8(6) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.828 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -28.00 19.00 0.50 1.56 -- -7.98 78.00 174.00 94 2 \w -28.00 -2.00 0.50 1.56 -- -7.98 -78.00 49.00 52 3 \w -15.00 14.00 0.50 1.56 -- -7.98 -77.00 0.00 58 4 \w -38.00 7.00 0.50 1.56 -- -7.98 -57.00 -60.00 90 5 \w -16.00 9.00 0.50 1.56 -- -7.98 -77.00 -90.00 50 6 \w -14.00 11.00 0.50 1.56 -- -7.98 -77.00-150.00 50 7 \w 1.00 39.00 0.50 1.56 -- 6.58 -99.00-180.00 76 8 \w -16.00 24.00 0.50 1.56 -- 6.58 -77.00 -30.00 80 9 \w -26.00 15.00 0.50 1.56 -- 6.58 -78.00 49.00 82 10 \w -6.00 31.00 0.50 1.56 -- 6.58 57.00-150.00 74 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0066257000 _diffrn_orient_matrix_UB_12 0.0153735000 _diffrn_orient_matrix_UB_13 0.0322888000 _diffrn_orient_matrix_UB_21 0.0407485000 _diffrn_orient_matrix_UB_22 -0.0390476000 _diffrn_orient_matrix_UB_23 0.0105795000 _diffrn_orient_matrix_UB_31 0.0564934000 _diffrn_orient_matrix_UB_32 0.0263781000 _diffrn_orient_matrix_UB_33 -0.0031281000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.828 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 36647 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.828 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.690 _diffrn_reflns_theta_min 2.462 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.361 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.065 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.338 _exptl_crystal_description plate _exptl_crystal_F_000 1996 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _refine_diff_density_max 2.135 _refine_diff_density_min -2.207 _refine_diff_density_rms 0.179 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 8616 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0301 _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^)+(0.0297P)^2^+5.4165P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.0719 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7408 _reflns_number_total 8616 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2GdTIP _cod_database_code 1572196 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C25H32Cl2GdI4N _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.630 _shelx_estimated_absorpt_t_min 0.196 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C25(H25A,H25B) 2.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C23(H23A,H23B, H23C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C14(H14A, H14B,H14C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C) ; _shelx_res_file ; TITL fed765_040523_final_a.res in P2(1)/c fed765_040523_final.res created by SHELXL-2018/3 at 12:14:01 on 10-May-2023 REM Old TITL FED765_040523_Final in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.085, Rweak 0.002, Alpha 0.027 REM 0.685 for 264 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N2 Cl2 I4 Gd CELL 0.71073 10.3396 14.3064 21.2014 90 101.314 90 ZERR 4 0.0002 0.0003 0.0004 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Gd I N UNIT 100 128 8 4 16 4 L.S. 4 0 0 PLAN 20 SIZE 0.08 0.22 0.38 TEMP -173 BOND list 4 fmap 2 53 ACTA REM REM REM WGHT 0.029700 5.416501 FVAR 0.12521 GD1 4 0.803476 0.286995 0.339682 11.00000 0.01419 0.01362 = 0.01495 0.00055 -0.00011 -0.00245 I1 5 0.522322 0.386535 0.281839 11.00000 0.01916 0.01638 = 0.02071 -0.00099 0.00289 0.00409 I4 5 0.817746 0.060195 0.201038 11.00000 0.01814 0.01896 = 0.02655 -0.00266 0.00367 0.00417 I3 5 0.479732 0.063467 0.081083 11.00000 0.02359 0.02240 = 0.01901 -0.00495 0.00205 -0.00589 I2 5 0.289084 0.280960 0.130288 11.00000 0.01652 0.02896 = 0.04086 -0.00399 -0.00835 0.00394 CL1 3 0.608456 0.372441 0.080817 11.00000 0.03572 0.03774 = 0.03047 -0.00431 0.00645 -0.01011 CL2 3 0.695558 0.557421 0.050756 11.00000 0.06225 0.03226 = 0.12583 0.00163 0.03342 -0.00512 N1 6 0.673950 0.226551 0.241119 11.00000 0.01470 0.01740 = 0.01615 -0.00156 0.00057 -0.00100 C4 1 0.664671 0.155103 0.197871 11.00000 0.01572 0.01478 = 0.01714 -0.00209 0.00239 -0.00198 C1 1 0.556677 0.272968 0.225185 11.00000 0.01652 0.01650 = 0.02023 -0.00024 0.00274 0.00104 C2 1 0.472944 0.232999 0.173491 11.00000 0.01370 0.01744 = 0.02068 0.00012 0.00170 0.00019 C3 1 0.544372 0.155714 0.155502 11.00000 0.01591 0.01529 = 0.01852 -0.00319 0.00469 -0.00346 C19 1 0.889090 0.432425 0.279279 11.00000 0.01755 0.01576 = 0.02370 0.00196 0.00424 -0.00337 C15 1 0.958982 0.353679 0.262450 11.00000 0.01769 0.01763 = 0.02111 -0.00122 0.00475 -0.00410 C5 1 0.684906 0.144665 0.388308 11.00000 0.02859 0.01915 = 0.01284 0.00062 0.00251 -0.00829 C9 1 0.822471 0.129172 0.406791 11.00000 0.03148 0.01708 = 0.02022 0.00445 0.00736 -0.00215 C6 1 0.653651 0.225240 0.422086 11.00000 0.01967 0.01784 = 0.01635 0.00245 0.00229 -0.00484 C18 1 0.932680 0.449126 0.346113 11.00000 0.02840 0.01737 = 0.02668 -0.00414 0.00829 -0.01123 C10 1 0.587753 0.083015 0.345739 11.00000 0.03612 0.02789 = 0.02596 -0.00401 0.00606 -0.01728 AFIX 137 H10A 2 0.517874 0.121526 0.320490 11.00000 -1.50000 H10B 2 0.548988 0.039071 0.372257 11.00000 -1.50000 H10C 2 0.632866 0.048130 0.316632 11.00000 -1.50000 AFIX 0 C17 1 1.029772 0.382307 0.370374 11.00000 0.02765 0.02782 = 0.02403 0.00142 -0.00100 -0.01701 C7 1 0.771855 0.259042 0.461075 11.00000 0.02255 0.01906 = 0.01683 -0.00032 0.00178 -0.00200 C8 1 0.876217 0.198982 0.452079 11.00000 0.01979 0.02200 = 0.01651 0.00437 0.00022 -0.00014 C11 1 0.516510 0.258917 0.425301 11.00000 0.02082 0.03146 = 0.02731 0.00803 0.00526 -0.00353 AFIX 137 H11A 2 0.516754 0.327207 0.428944 11.00000 -1.50000 H11B 2 0.488968 0.231381 0.462889 11.00000 -1.50000 H11C 2 0.454906 0.239993 0.386156 11.00000 -1.50000 AFIX 0 C16 1 1.045883 0.322105 0.318678 11.00000 0.01621 0.01962 = 0.03313 0.00586 0.00398 -0.00378 C20 1 0.950956 0.318314 0.194934 11.00000 0.02914 0.03566 = 0.02560 -0.00571 0.01170 -0.00655 AFIX 137 H20A 2 0.993457 0.256925 0.196255 11.00000 -1.50000 H20B 2 0.995957 0.362212 0.171025 11.00000 -1.50000 H20C 2 0.858226 0.312778 0.173561 11.00000 -1.50000 AFIX 0 C23 1 0.891348 0.529393 0.383365 11.00000 0.05109 0.02679 = 0.04950 -0.01751 0.03194 -0.01709 AFIX 137 H23A 2 0.799344 0.545620 0.365565 11.00000 -1.50000 H23B 2 0.947854 0.583510 0.380232 11.00000 -1.50000 H23C 2 0.899887 0.511404 0.428595 11.00000 -1.50000 AFIX 0 C12 1 0.781279 0.338418 0.508681 11.00000 0.02962 0.02325 = 0.02500 -0.00769 0.00421 -0.00143 AFIX 137 H12A 2 0.871805 0.362405 0.518093 11.00000 -1.50000 H12B 2 0.757277 0.315808 0.548480 11.00000 -1.50000 H12C 2 0.720872 0.388567 0.490371 11.00000 -1.50000 AFIX 0 C24 1 0.801013 0.493881 0.231706 11.00000 0.02271 0.03040 = 0.04220 0.01655 0.00716 0.00388 AFIX 137 H24A 2 0.737271 0.455079 0.202763 11.00000 -1.50000 H24B 2 0.854554 0.529134 0.206577 11.00000 -1.50000 H24C 2 0.753789 0.537499 0.254762 11.00000 -1.50000 AFIX 0 C21 1 1.146495 0.246241 0.320398 11.00000 0.02225 0.02998 = 0.07265 0.01450 0.01193 0.00594 AFIX 137 H21A 2 1.166456 0.218574 0.363502 11.00000 -1.50000 H21B 2 1.227206 0.272623 0.309956 11.00000 -1.50000 H21C 2 1.111604 0.197923 0.288861 11.00000 -1.50000 AFIX 0 C14 1 0.898878 0.045385 0.389957 11.00000 0.04213 0.02249 = 0.03303 0.00282 0.01131 0.00605 AFIX 137 H14A 2 0.846719 0.012991 0.352769 11.00000 -1.50000 H14B 2 0.916917 0.002586 0.426727 11.00000 -1.50000 H14C 2 0.982381 0.066424 0.379493 11.00000 -1.50000 AFIX 0 C13 1 1.010794 0.195826 0.494237 11.00000 0.02323 0.03600 = 0.02795 0.01010 0.00092 0.00055 AFIX 137 H13A 2 1.077010 0.185165 0.467676 11.00000 -1.50000 H13B 2 1.014469 0.144892 0.525446 11.00000 -1.50000 H13C 2 1.028843 0.255360 0.517136 11.00000 -1.50000 AFIX 0 C22 1 1.122145 0.387774 0.435140 11.00000 0.05195 0.05738 = 0.03451 0.00944 -0.01101 -0.03545 AFIX 137 H22A 2 1.070567 0.394067 0.469066 11.00000 -1.50000 H22B 2 1.180239 0.442077 0.435999 11.00000 -1.50000 H22C 2 1.175460 0.330717 0.442303 11.00000 -1.50000 AFIX 0 C25 1 0.703506 0.441550 0.041079 11.00000 0.18471 0.02683 = 0.10025 -0.01793 0.11832 -0.02438 AFIX 23 H25A 2 0.796674 0.422234 0.055043 11.00000 -1.20000 H25B 2 0.678033 0.427874 -0.005482 11.00000 -1.20000 AFIX 0 HKLF 4 REM fed765_040523_final_a.res in P2(1)/c REM wR2 = 0.0719, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0301 for 7408 Fo > 4sig(Fo) and 0.0375 for all 8616 data REM 308 parameters refined using 0 restraints END WGHT 0.0297 5.4107 REM Highest difference peak 2.135, deepest hole -2.207, 1-sigma level 0.179 Q1 1 0.7004 0.5424 0.0114 11.00000 0.05 2.14 Q2 1 0.7798 0.5192 0.0545 11.00000 0.05 1.41 Q3 1 0.3366 0.2792 0.1032 11.00000 0.05 1.11 Q4 1 0.8048 0.0471 0.2363 11.00000 0.05 1.08 Q5 1 0.8486 0.2855 0.3041 11.00000 0.05 0.99 Q6 1 0.7625 0.2815 0.3758 11.00000 0.05 0.87 Q7 1 0.8947 0.2948 0.3798 11.00000 0.05 0.86 Q8 1 0.7745 0.0203 0.1603 11.00000 0.05 0.86 Q9 1 0.5717 0.3788 0.2563 11.00000 0.05 0.85 Q10 1 0.7396 0.4269 0.0394 11.00000 0.05 0.80 Q11 1 0.8571 0.3181 0.3803 11.00000 0.05 0.80 Q12 1 0.5461 0.0787 0.0544 11.00000 0.05 0.79 Q13 1 0.7735 0.2413 0.2966 11.00000 0.05 0.78 Q14 1 0.7735 0.1010 0.1578 11.00000 0.05 0.78 Q15 1 0.3022 0.2541 0.1603 11.00000 0.05 0.77 Q16 1 0.7717 0.3255 0.2965 11.00000 0.05 0.76 Q17 1 0.4776 0.3919 0.3177 11.00000 0.05 0.71 Q18 1 0.8690 0.3815 0.4024 11.00000 0.05 0.70 Q19 1 0.4892 0.3423 0.2396 11.00000 0.05 0.69 Q20 1 0.4823 0.4218 0.2384 11.00000 0.05 0.67 ; _shelx_res_checksum 75907 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.298 _oxdiff_exptl_absorpt_empirical_full_min 0.679 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.80348(2) 0.28699(2) 0.33968(2) 0.01466(5) Uani 1 1 d . . . . . I1 I 0.52232(2) 0.38653(2) 0.28184(2) 0.01889(6) Uani 1 1 d . . . . . I4 I 0.81775(2) 0.06019(2) 0.20104(2) 0.02132(6) Uani 1 1 d . . . . . I3 I 0.47973(2) 0.06347(2) 0.08108(2) 0.02196(6) Uani 1 1 d . . . . . I2 I 0.28908(3) 0.28096(2) 0.13029(2) 0.03068(7) Uani 1 1 d . . . . . Cl1 Cl 0.60846(12) 0.37244(8) 0.08082(6) 0.0347(2) Uani 1 1 d . . . . . Cl2 Cl 0.69556(18) 0.55742(10) 0.05076(12) 0.0714(5) Uani 1 1 d . . . . . N1 N 0.6740(3) 0.2266(2) 0.24112(15) 0.0164(6) Uani 1 1 d . . . . . C4 C 0.6647(3) 0.1551(2) 0.19787(17) 0.0160(7) Uani 1 1 d . . . . . C1 C 0.5567(4) 0.2730(2) 0.22518(18) 0.0179(7) Uani 1 1 d . . . . . C2 C 0.4729(3) 0.2330(2) 0.17349(18) 0.0175(7) Uani 1 1 d . . . . . C3 C 0.5444(3) 0.1557(2) 0.15550(18) 0.0164(7) Uani 1 1 d . . . . . C19 C 0.8891(4) 0.4324(2) 0.27928(19) 0.0190(7) Uani 1 1 d . . . . . C15 C 0.9590(4) 0.3537(3) 0.26245(18) 0.0187(7) Uani 1 1 d . . . . . C5 C 0.6849(4) 0.1447(3) 0.38831(17) 0.0204(7) Uani 1 1 d . . . . . C9 C 0.8225(4) 0.1292(3) 0.40679(19) 0.0226(8) Uani 1 1 d . . . . . C6 C 0.6537(4) 0.2252(3) 0.42209(18) 0.0181(7) Uani 1 1 d . . . . . C18 C 0.9327(4) 0.4491(3) 0.3461(2) 0.0238(8) Uani 1 1 d . . . . . C10 C 0.5878(5) 0.0830(3) 0.3457(2) 0.0300(9) Uani 1 1 d . . . . . H10A H 0.517874 0.121526 0.320490 0.045 Uiso 1 1 calc R U . . . H10B H 0.548988 0.039071 0.372257 0.045 Uiso 1 1 calc R U . . . H10C H 0.632866 0.048130 0.316632 0.045 Uiso 1 1 calc R U . . . C17 C 1.0298(4) 0.3823(3) 0.3704(2) 0.0273(9) Uani 1 1 d . . . . . C7 C 0.7719(4) 0.2590(3) 0.46108(18) 0.0198(7) Uani 1 1 d . . . . . C8 C 0.8762(4) 0.1990(3) 0.45208(18) 0.0199(7) Uani 1 1 d . . . . . C11 C 0.5165(4) 0.2589(3) 0.4253(2) 0.0265(9) Uani 1 1 d . . . . . H11A H 0.516754 0.327207 0.428944 0.040 Uiso 1 1 calc R U . . . H11B H 0.488968 0.231381 0.462889 0.040 Uiso 1 1 calc R U . . . H11C H 0.454906 0.239993 0.386156 0.040 Uiso 1 1 calc R U . . . C16 C 1.0459(4) 0.3221(3) 0.3187(2) 0.0231(8) Uani 1 1 d . . . . . C20 C 0.9510(4) 0.3183(3) 0.1949(2) 0.0293(9) Uani 1 1 d . . . . . H20A H 0.993457 0.256925 0.196255 0.044 Uiso 1 1 calc R U . . . H20B H 0.995957 0.362212 0.171025 0.044 Uiso 1 1 calc R U . . . H20C H 0.858226 0.312778 0.173561 0.044 Uiso 1 1 calc R U . . . C23 C 0.8913(5) 0.5294(3) 0.3834(3) 0.0395(12) Uani 1 1 d . . . . . H23A H 0.799344 0.545620 0.365565 0.059 Uiso 1 1 calc R U . . . H23B H 0.947854 0.583510 0.380232 0.059 Uiso 1 1 calc R U . . . H23C H 0.899887 0.511404 0.428595 0.059 Uiso 1 1 calc R U . . . C12 C 0.7813(4) 0.3384(3) 0.5087(2) 0.0261(8) Uani 1 1 d . . . . . H12A H 0.871805 0.362405 0.518093 0.039 Uiso 1 1 calc R U . . . H12B H 0.757277 0.315808 0.548480 0.039 Uiso 1 1 calc R U . . . H12C H 0.720872 0.388567 0.490371 0.039 Uiso 1 1 calc R U . . . C24 C 0.8010(4) 0.4939(3) 0.2317(2) 0.0317(10) Uani 1 1 d . . . . . H24A H 0.737271 0.455079 0.202763 0.047 Uiso 1 1 calc R U . . . H24B H 0.854554 0.529134 0.206577 0.047 Uiso 1 1 calc R U . . . H24C H 0.753789 0.537499 0.254762 0.047 Uiso 1 1 calc R U . . . C21 C 1.1465(4) 0.2462(3) 0.3204(3) 0.0413(12) Uani 1 1 d . . . . . H21A H 1.166456 0.218574 0.363502 0.062 Uiso 1 1 calc R U . . . H21B H 1.227206 0.272623 0.309956 0.062 Uiso 1 1 calc R U . . . H21C H 1.111604 0.197923 0.288861 0.062 Uiso 1 1 calc R U . . . C14 C 0.8989(5) 0.0454(3) 0.3900(2) 0.0320(10) Uani 1 1 d . . . . . H14A H 0.846719 0.012991 0.352769 0.048 Uiso 1 1 calc R U . . . H14B H 0.916917 0.002586 0.426727 0.048 Uiso 1 1 calc R U . . . H14C H 0.982381 0.066424 0.379493 0.048 Uiso 1 1 calc R U . . . C13 C 1.0108(4) 0.1958(3) 0.4942(2) 0.0296(9) Uani 1 1 d . . . . . H13A H 1.077010 0.185165 0.467676 0.044 Uiso 1 1 calc R U . . . H13B H 1.014469 0.144892 0.525446 0.044 Uiso 1 1 calc R U . . . H13C H 1.028843 0.255360 0.517136 0.044 Uiso 1 1 calc R U . . . C22 C 1.1221(6) 0.3878(4) 0.4351(3) 0.0506(15) Uani 1 1 d . . . . . H22A H 1.070567 0.394067 0.469066 0.076 Uiso 1 1 calc R U . . . H22B H 1.180239 0.442077 0.435999 0.076 Uiso 1 1 calc R U . . . H22C H 1.175460 0.330717 0.442303 0.076 Uiso 1 1 calc R U . . . C25 C 0.7035(10) 0.4416(4) 0.0411(4) 0.092(3) Uani 1 1 d . . . . . H25A H 0.796674 0.422234 0.055043 0.110 Uiso 1 1 calc R U . . . H25B H 0.678033 0.427874 -0.005482 0.110 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 0.01419(9) 0.01362(9) 0.01495(9) 0.00055(6) -0.00011(7) -0.00245(6) I1 0.01916(12) 0.01638(12) 0.02071(12) -0.00099(8) 0.00289(9) 0.00409(8) I4 0.01814(12) 0.01896(12) 0.02655(13) -0.00266(9) 0.00367(10) 0.00417(8) I3 0.02359(13) 0.02240(13) 0.01901(12) -0.00495(9) 0.00205(10) -0.00589(9) I2 0.01652(13) 0.02896(15) 0.04086(17) -0.00399(11) -0.00835(11) 0.00394(10) Cl1 0.0357(6) 0.0377(6) 0.0305(5) -0.0043(4) 0.0064(5) -0.0101(5) Cl2 0.0622(10) 0.0323(7) 0.1258(17) 0.0016(8) 0.0334(11) -0.0051(6) N1 0.0147(14) 0.0174(15) 0.0162(15) -0.0016(11) 0.0006(12) -0.0010(11) C4 0.0157(16) 0.0148(16) 0.0171(17) -0.0021(13) 0.0024(14) -0.0020(12) C1 0.0165(17) 0.0165(17) 0.0202(18) -0.0002(13) 0.0027(15) 0.0010(13) C2 0.0137(16) 0.0174(17) 0.0207(18) 0.0001(14) 0.0017(14) 0.0002(13) C3 0.0159(16) 0.0153(16) 0.0185(17) -0.0032(13) 0.0047(14) -0.0035(12) C19 0.0175(17) 0.0158(17) 0.0237(19) 0.0020(14) 0.0042(15) -0.0034(13) C15 0.0177(17) 0.0176(18) 0.0211(18) -0.0012(14) 0.0047(15) -0.0041(13) C5 0.029(2) 0.0192(18) 0.0128(16) 0.0006(13) 0.0025(15) -0.0083(15) C9 0.031(2) 0.0171(18) 0.0202(18) 0.0045(14) 0.0074(17) -0.0021(15) C6 0.0197(18) 0.0178(17) 0.0163(17) 0.0024(13) 0.0023(15) -0.0048(13) C18 0.028(2) 0.0174(18) 0.027(2) -0.0041(15) 0.0083(17) -0.0112(15) C10 0.036(2) 0.028(2) 0.026(2) -0.0040(17) 0.0061(19) -0.0173(18) C17 0.028(2) 0.028(2) 0.024(2) 0.0014(16) -0.0010(17) -0.0170(16) C7 0.0226(18) 0.0191(18) 0.0168(17) -0.0003(14) 0.0018(15) -0.0020(14) C8 0.0198(18) 0.0220(18) 0.0165(17) 0.0044(14) 0.0002(15) -0.0001(14) C11 0.021(2) 0.031(2) 0.027(2) 0.0080(17) 0.0053(17) -0.0035(16) C16 0.0162(17) 0.0196(19) 0.033(2) 0.0059(16) 0.0040(16) -0.0038(14) C20 0.029(2) 0.036(2) 0.026(2) -0.0057(18) 0.0117(18) -0.0065(18) C23 0.051(3) 0.027(2) 0.049(3) -0.018(2) 0.032(3) -0.017(2) C12 0.030(2) 0.023(2) 0.025(2) -0.0077(16) 0.0042(17) -0.0014(16) C24 0.023(2) 0.030(2) 0.042(3) 0.0166(19) 0.0072(19) 0.0039(16) C21 0.022(2) 0.030(2) 0.073(4) 0.014(2) 0.012(2) 0.0059(18) C14 0.042(3) 0.022(2) 0.033(2) 0.0028(17) 0.011(2) 0.0060(18) C13 0.023(2) 0.036(2) 0.028(2) 0.0101(18) 0.0009(17) 0.0006(17) C22 0.052(3) 0.057(3) 0.035(3) 0.009(2) -0.011(2) -0.035(3) C25 0.185(9) 0.027(3) 0.100(6) -0.018(3) 0.118(7) -0.024(4) 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' Cl Cl 0.1484 0.1585 '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' I I -0.4742 1.8119 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 2 -1 0.1088 -2 -2 1 0.1153 -1 1 1 0.1367 1 -1 -1 0.1264 0 0 -1 0.0115 0 0 1 0.0640 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 N1 Gd1 I1 61.76(7) . . ? N1 Gd1 C19 92.50(11) . . ? N1 Gd1 C15 84.04(11) . . ? N1 Gd1 C5 80.96(11) . . ? N1 Gd1 C9 97.45(11) . . ? N1 Gd1 C6 98.73(11) . . ? N1 Gd1 C18 122.95(12) . . ? N1 Gd1 C17 134.77(12) . . ? N1 Gd1 C7 128.73(11) . . ? N1 Gd1 C8 128.02(11) . . ? N1 Gd1 C16 107.58(12) . . ? C19 Gd1 I1 80.49(8) . . ? C19 Gd1 C15 30.71(11) . . ? C19 Gd1 C5 171.81(12) . . ? C19 Gd1 C6 147.92(11) . . ? C19 Gd1 C7 133.33(12) . . ? C15 Gd1 I1 102.26(8) . . ? C15 Gd1 C6 177.17(11) . . ? C15 Gd1 C7 146.81(12) . . ? C5 Gd1 I1 92.01(9) . . ? C5 Gd1 C15 151.26(12) . . ? C5 Gd1 C6 30.73(11) . . ? C5 Gd1 C7 50.86(11) . . ? C9 Gd1 I1 122.74(9) . . ? C9 Gd1 C19 156.72(12) . . ? C9 Gd1 C15 129.69(12) . . ? C9 Gd1 C5 30.76(12) . . ? C9 Gd1 C6 50.71(12) . . ? C9 Gd1 C18 136.76(13) . . ? C9 Gd1 C17 109.50(13) . . ? C9 Gd1 C7 50.98(12) . . ? C9 Gd1 C8 30.95(12) . . ? C9 Gd1 C16 105.98(12) . . ? C6 Gd1 I1 78.67(8) . . ? C18 Gd1 I1 92.30(10) . . ? C18 Gd1 C19 30.79(12) . . ? C18 Gd1 C15 50.82(12) . . ? C18 Gd1 C5 154.41(12) . . ? C18 Gd1 C6 126.63(12) . . ? C18 Gd1 C17 30.57(13) . . ? C18 Gd1 C7 103.55(12) . . ? C18 Gd1 C8 108.30(12) . . ? C18 Gd1 C16 50.91(12) . . ? C17 Gd1 I1 122.87(10) . . ? C17 Gd1 C19 50.67(12) . . ? C17 Gd1 C15 50.77(12) . . ? C17 Gd1 C5 137.43(12) . . ? C17 Gd1 C6 126.48(12) . . ? C17 Gd1 C7 96.19(12) . . ? C17 Gd1 C16 30.97(13) . . ? C7 Gd1 I1 99.12(8) . . ? C7 Gd1 C6 30.54(11) . . ? C8 Gd1 I1 128.13(8) . . ? C8 Gd1 C19 136.92(12) . . ? C8 Gd1 C15 127.91(12) . . ? C8 Gd1 C5 50.91(12) . . ? C8 Gd1 C6 50.59(11) . . ? C8 Gd1 C17 86.76(12) . . ? C8 Gd1 C7 30.77(12) . . ? C8 Gd1 C16 97.35(12) . . ? C16 Gd1 I1 130.66(8) . . ? C16 Gd1 C19 50.79(12) . . ? C16 Gd1 C15 30.68(12) . . ? C16 Gd1 C5 135.97(12) . . ? C16 Gd1 C6 147.49(12) . . ? C16 Gd1 C7 118.74(12) . . ? C1 I1 Gd1 68.69(10) . . ? C4 N1 Gd1 143.7(2) . . ? C4 N1 C1 104.8(3) . . ? C1 N1 Gd1 110.8(2) . . ? N1 C4 I4 121.0(3) . . ? N1 C4 C3 111.5(3) . . ? C3 C4 I4 127.4(3) . . ? N1 C1 I1 118.6(3) . . ? N1 C1 C2 112.5(3) . . ? C2 C1 I1 128.8(3) . . ? C1 C2 I2 126.6(3) . . ? C1 C2 C3 104.9(3) . . ? C3 C2 I2 128.5(3) . . ? C4 C3 I3 127.4(3) . . ? C4 C3 C2 106.2(3) . . ? C2 C3 I3 126.5(3) . . ? C15 C19 Gd1 74.7(2) . . ? C15 C19 C24 124.5(4) . . ? C18 C19 Gd1 74.0(2) . . ? C18 C19 C15 107.8(3) . . ? C18 C19 C24 127.1(4) . . ? C24 C19 Gd1 124.1(3) . . ? C19 C15 Gd1 74.6(2) . . ? C19 C15 C20 124.7(4) . . ? C16 C15 Gd1 74.4(2) . . ? C16 C15 C19 108.1(3) . . ? C16 C15 C20 126.9(4) . . ? C20 C15 Gd1 122.2(2) . . ? C9 C5 Gd1 73.5(2) . . ? C9 C5 C6 107.5(3) . . ? C9 C5 C10 126.3(4) . . ? C6 C5 Gd1 75.3(2) . . ? C6 C5 C10 125.9(4) . . ? C10 C5 Gd1 121.2(3) . . ? C5 C9 Gd1 75.8(2) . . ? C5 C9 C8 108.4(3) . . ? C5 C9 C14 126.9(4) . . ? C8 C9 Gd1 75.1(2) . . ? C8 C9 C14 124.2(4) . . ? C14 C9 Gd1 122.2(3) . . ? C5 C6 Gd1 74.0(2) . . ? C5 C6 C11 125.9(3) . . ? C7 C6 Gd1 74.2(2) . . ? C7 C6 C5 108.3(3) . . ? C7 C6 C11 125.0(3) . . ? C11 C6 Gd1 125.9(2) . . ? C19 C18 Gd1 75.2(2) . . ? C19 C18 C23 125.8(4) . . ? C17 C18 Gd1 75.1(2) . . ? C17 C18 C19 108.3(3) . . ? C17 C18 C23 125.6(4) . . ? C23 C18 Gd1 120.0(3) . . ? C18 C17 Gd1 74.4(2) . . ? C18 C17 C16 108.1(4) . . ? C18 C17 C22 125.0(4) . . ? C16 C17 Gd1 74.6(2) . . ? C16 C17 C22 125.4(5) . . ? C22 C17 Gd1 127.8(3) . . ? C6 C7 Gd1 75.3(2) . . ? C6 C7 C8 107.8(3) . . ? C6 C7 C12 125.5(4) . . ? C8 C7 Gd1 73.9(2) . . ? C8 C7 C12 126.4(4) . . ? C12 C7 Gd1 121.6(3) . . ? C9 C8 Gd1 74.0(2) . . ? C9 C8 C7 108.0(3) . . ? C9 C8 C13 125.2(4) . . ? C7 C8 Gd1 75.3(2) . . ? C7 C8 C13 125.3(4) . . ? C13 C8 Gd1 127.7(3) . . ? C15 C16 Gd1 74.9(2) . . ? C15 C16 C17 107.6(4) . . ? C15 C16 C21 125.0(4) . . ? C17 C16 Gd1 74.4(2) . . ? C17 C16 C21 127.0(4) . . ? C21 C16 Gd1 121.9(3) . . ? Cl2 C25 Cl1 117.5(4) . . ? 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 I1 3.2533(3) . ? Gd1 N1 2.410(3) . ? Gd1 C19 2.683(4) . ? Gd1 C15 2.685(4) . ? Gd1 C5 2.685(4) . ? Gd1 C9 2.655(4) . ? Gd1 C6 2.701(4) . ? Gd1 C18 2.667(4) . ? Gd1 C17 2.676(4) . ? Gd1 C7 2.687(4) . ? Gd1 C8 2.670(4) . ? Gd1 C16 2.678(4) . ? I1 C1 2.092(4) . ? I4 C4 2.076(4) . ? I3 C3 2.065(4) . ? I2 C2 2.059(4) . ? Cl1 C25 1.726(6) . ? Cl2 C25 1.674(6) . ? N1 C4 1.364(4) . ? N1 C1 1.366(5) . ? C4 C3 1.384(5) . ? C1 C2 1.380(5) . ? C2 C3 1.423(5) . ? C19 C15 1.421(5) . ? C19 C18 1.420(6) . ? C19 C24 1.503(6) . ? C15 C16 1.419(6) . ? C15 C20 1.505(5) . ? C5 C9 1.417(6) . ? C5 C6 1.427(5) . ? C5 C10 1.499(5) . ? C9 C8 1.421(6) . ? C9 C14 1.516(6) . ? C6 C7 1.419(5) . ? C6 C11 1.512(5) . ? C18 C17 1.408(6) . ? C18 C23 1.502(6) . ? C17 C16 1.429(6) . ? C17 C22 1.513(6) . ? C7 C8 1.421(5) . ? C7 C12 1.510(5) . ? C8 C13 1.500(6) . ? C16 C21 1.499(6) . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.0000 2.0000 -1.0000 0.0117 -0.0072 0.1689 -2.0000 -2.0000 1.0000 -0.0117 0.0072 -0.1689 -1.0000 1.0000 1.0000 0.0410 -0.0692 -0.0332 1.0000 -1.0000 -1.0000 -0.0410 0.0692 0.0332 0.0000 0.0000 -1.0000 -0.0323 -0.0106 0.0031 -0.0000 -0.0000 1.0000 0.0323 0.0106 -0.0031