#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:22:16 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293309 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572112.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_1572112 loop_ _publ_author_name 'Minko, Yury' 'Fetrow, Taylor V.' 'Sharma, Shikha' 'Cashman, Brenna K.' 'Tondreau, Aaron M.' _publ_section_title ; Flexible interactions of the rare-earth elements Y, La, and Lu with phosphorus in metallacyclohexane rings ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02077D _journal_year 2024 _chemical_formula_moiety 'C34 H55 I Lu N2 O3 P' _chemical_formula_sum 'C34 H55 I Lu N2 O3 P' _chemical_formula_weight 872.64 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2022-01-03 _audit_creation_method ; Olex2 1.2 (compiled Apr 3 2018 11:26:26 for OlexSys, GUI svn.r5486) ; _audit_update_record ; 2024-01-24 deposited with the CCDC. 2024-06-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.4115(9) _cell_length_b 14.1878(10) _cell_length_c 19.0912(14) _cell_measurement_reflns_used 9823 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 28.32 _cell_measurement_theta_min 2.35 _cell_volume 3632.7(4) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _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 0.0318 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 35210 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.335 _diffrn_reflns_theta_min 3.063 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.645 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.0661 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.8078. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.596 _exptl_crystal_description plate _exptl_crystal_F_000 1744 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.957 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.090 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.290(6) _refine_ls_extinction_coef 0.00021(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 9000 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0215 _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^)+4.4545P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0447 _reflns_Friedel_coverage 0.806 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 8672 _reflns_number_total 9000 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02077d2.cif _cod_data_source_block 2ndintlui _cod_database_code 1572112 _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_estimated_absorpt_t_max 0.899 _shelx_estimated_absorpt_t_min 0.501 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.710(6) 0.290(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C29(H29A,H29B), C32(H32A,H32B), C28(H28A,H28B), C30(H30A,H30B), C25(H25A,H25B), C24(H24A,H24B), C31(H31A,H31B), C27(H27A,H27B), C21(H21A,H21B), C26(H26A,H26B), C23(H23A,H23B), C22(H22A,H22B) 3.b Aromatic/amide H refined with riding coordinates: C20(H20), C12(H12), C8(H8), C16(H16), C18(H18), C10(H10) 3.c Idealised Me refined as rotating group: C00M(H00A,H00B,H00C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C13(H13A,H13B, H13C), C4(H4A,H4B,H4C), C012(H01A,H01B,H01C), C5(H5A,H5B,H5C) ; _shelx_res_file ; TITL 2ndintlui_a.res in P2(1)2(1)2(1) 2ndintlui.res created by SHELXL-2018/3 at 10:17:32 on 03-Jan-2022 REM Old TITL 2ndIntLuI_a.res in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.061, Rweak 0.036, Alpha 0.014 REM 1.286 for 29 systematic absences, Orientation as input REM Flack x = 0.305 ( 0.003 ) from 3148 Parsons quotients REM Formula found by SHELXT: C43 N13 O P I Lu CELL 0.71073 13.4115 14.1878 19.0912 90 90 90 ZERR 4 0.0009 0.001 0.0014 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H I Lu N O P UNIT 136 220 4 4 8 12 4 L.S. 4 PLAN 20 SIZE 0.22 0.12 0.03 TEMP -173.15 BOND list 4 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 0 2 OMIT 1 1 5 OMIT 8 3 7 OMIT 2 5 4 OMIT 0 6 5 OMIT 5 0 1 OMIT -2 -2 -3 OMIT 4 0 2 OMIT 8 0 6 REM REM REM WGHT 0.000000 4.454501 EXTI 0.000206 BASF 0.29018 FVAR 0.17609 LU1 4 0.346098 0.571854 0.415956 11.00000 0.01250 0.01074 = 0.01107 0.00055 -0.00016 0.00026 I1 3 0.535858 0.630421 0.492013 11.00000 0.02023 0.02194 = 0.02769 -0.00260 -0.00882 -0.00031 P1 7 0.142015 0.589692 0.343563 11.00000 0.01363 0.02081 = 0.01339 0.00188 0.00063 0.00250 O1 6 0.449055 0.448509 0.380488 11.00000 0.01559 0.01461 = 0.01672 -0.00050 -0.00143 0.00354 O2 6 0.274234 0.596933 0.528207 11.00000 0.02491 0.02106 = 0.01216 -0.00104 0.00254 -0.00078 N2 5 0.329517 0.599119 0.301015 11.00000 0.01029 0.01579 = 0.01465 0.00305 0.00139 0.00102 O3 6 0.321359 0.737434 0.420208 11.00000 0.02295 0.01246 = 0.01663 0.00076 0.00035 0.00065 N1 5 0.235967 0.452854 0.412906 11.00000 0.01261 0.01730 = 0.01209 0.00240 -0.00074 -0.00006 C20 1 0.506078 0.617074 0.279757 11.00000 0.01561 0.01385 = 0.01567 -0.00113 -0.00302 -0.00012 AFIX 43 H20 2 0.516928 0.615044 0.328908 11.00000 -1.20000 AFIX 0 C1 1 0.154557 0.462856 0.362278 11.00000 0.01540 0.02164 = 0.01568 0.00291 -0.00037 -0.00093 AFIX 23 H1A 2 0.091714 0.437760 0.382084 11.00000 -1.20000 H1B 2 0.170091 0.427778 0.318799 11.00000 -1.20000 AFIX 0 C2 1 0.229708 0.601218 0.269870 11.00000 0.01548 0.01960 = 0.01321 0.00210 0.00122 0.00088 AFIX 23 H2A 2 0.221192 0.548469 0.236455 11.00000 -1.20000 H2B 2 0.218634 0.661321 0.244701 11.00000 -1.20000 AFIX 0 C29 1 0.417128 0.388997 0.321564 11.00000 0.01733 0.01481 = 0.02235 -0.00799 -0.00338 0.00086 AFIX 23 H29A 2 0.368361 0.422733 0.291784 11.00000 -1.20000 H29B 2 0.386248 0.329981 0.338737 11.00000 -1.20000 AFIX 0 C32 1 0.541993 0.404933 0.402448 11.00000 0.02268 0.02730 = 0.03191 -0.00525 -0.01012 0.01118 AFIX 23 H32A 2 0.529007 0.347547 0.430503 11.00000 -1.20000 H32B 2 0.582269 0.449291 0.430766 11.00000 -1.20000 AFIX 0 C28 1 0.309234 0.795760 0.358626 11.00000 0.07129 0.01465 = 0.02334 0.00608 0.01083 0.00606 AFIX 23 H28A 2 0.248859 0.776631 0.332394 11.00000 -1.20000 H28B 2 0.367745 0.789156 0.327393 11.00000 -1.20000 AFIX 0 C19 1 0.586619 0.625506 0.235796 11.00000 0.01488 0.01363 = 0.01993 -0.00022 -0.00262 0.00057 C30 1 0.511444 0.368189 0.281130 11.00000 0.02608 0.01872 = 0.02702 -0.00523 0.00808 -0.00055 AFIX 23 H30A 2 0.519462 0.412799 0.241655 11.00000 -1.20000 H30B 2 0.510428 0.303113 0.262431 11.00000 -1.20000 AFIX 0 C12 1 0.309955 0.351211 0.499087 11.00000 0.01540 0.01594 = 0.01556 -0.00058 0.00056 -0.00090 AFIX 43 H12 2 0.347918 0.403293 0.515423 11.00000 -1.20000 AFIX 0 C15 1 0.407152 0.611308 0.253861 11.00000 0.01449 0.00982 = 0.01549 -0.00012 0.00232 0.00095 C7 1 0.246143 0.364325 0.441549 11.00000 0.01351 0.01638 = 0.01281 -0.00085 0.00542 -0.00230 C3 1 0.014255 0.600126 0.305421 11.00000 0.01432 0.04218 = 0.02387 0.00566 0.00062 0.00820 C25 1 0.325355 0.798426 0.481773 11.00000 0.02764 0.01771 = 0.01939 -0.00652 -0.00261 0.00077 AFIX 23 H25A 2 0.376029 0.775772 0.515513 11.00000 -1.20000 H25B 2 0.259756 0.800920 0.505478 11.00000 -1.20000 AFIX 0 C00M 1 0.691093 0.630252 0.264925 11.00000 0.01604 0.02847 = 0.02688 0.00210 -0.00011 -0.00465 AFIX 137 H00A 2 0.688180 0.634740 0.316108 11.00000 -1.50000 H00B 2 0.725175 0.685811 0.246031 11.00000 -1.50000 H00C 2 0.727775 0.573287 0.251553 11.00000 -1.50000 AFIX 0 C24 1 0.167700 0.612651 0.533777 11.00000 0.02175 0.03324 = 0.02367 -0.00621 0.00704 -0.00488 AFIX 23 H24A 2 0.130550 0.556002 0.518426 11.00000 -1.20000 H24B 2 0.147302 0.666601 0.504175 11.00000 -1.20000 AFIX 0 C8 1 0.194621 0.283833 0.417747 11.00000 0.01607 0.02026 = 0.01359 0.00065 0.00454 -0.00245 AFIX 43 H8 2 0.151809 0.289157 0.378301 11.00000 -1.20000 AFIX 0 C17 1 0.477448 0.626519 0.135747 11.00000 0.01757 0.01433 = 0.01544 -0.00115 0.00141 0.00042 C31 1 0.595405 0.380267 0.334362 11.00000 0.01677 0.02205 = 0.04540 -0.00670 0.00495 0.00419 AFIX 23 H31A 2 0.634072 0.321223 0.339446 11.00000 -1.20000 H31B 2 0.641150 0.431564 0.320109 11.00000 -1.20000 AFIX 0 C16 1 0.395533 0.617367 0.180253 11.00000 0.01615 0.01524 = 0.01348 0.00176 -0.00102 0.00018 AFIX 43 H16 2 0.330415 0.615144 0.160737 11.00000 -1.20000 AFIX 0 C27 1 0.299538 0.895698 0.383107 11.00000 0.03990 0.01451 = 0.03415 0.00365 0.00353 0.00389 AFIX 23 H27A 2 0.228710 0.913707 0.388955 11.00000 -1.20000 H27B 2 0.331844 0.939914 0.350027 11.00000 -1.20000 AFIX 0 C21 1 0.311139 0.579231 0.598335 11.00000 0.04206 0.03431 = 0.01632 0.00249 0.00307 0.00486 AFIX 23 H21A 2 0.382924 0.594714 0.602030 11.00000 -1.20000 H21B 2 0.301070 0.512533 0.611831 11.00000 -1.20000 AFIX 0 C14 1 0.148625 0.113166 0.421319 11.00000 0.02822 0.02096 = 0.03087 -0.00238 0.00265 -0.00490 AFIX 137 H14A 2 0.076762 0.123585 0.426467 11.00000 -1.50000 H14B 2 0.167904 0.056281 0.447096 11.00000 -1.50000 H14C 2 0.164897 0.105274 0.371621 11.00000 -1.50000 AFIX 0 C6 1 0.000652 0.702014 0.280919 11.00000 0.02968 0.04975 = 0.03254 0.01381 0.00371 0.01778 AFIX 137 H6A 2 0.002315 0.744262 0.321513 11.00000 -1.50000 H6B 2 -0.063640 0.708291 0.256973 11.00000 -1.50000 H6C 2 0.054570 0.718738 0.248579 11.00000 -1.50000 AFIX 0 C26 1 0.353500 0.893911 0.452996 11.00000 0.03608 0.01617 = 0.04575 -0.00368 -0.00541 0.00162 AFIX 23 H26A 2 0.426531 0.899438 0.446657 11.00000 -1.20000 H26B 2 0.330106 0.945237 0.484045 11.00000 -1.20000 AFIX 0 C13 1 0.386070 0.255266 0.596317 11.00000 0.03408 0.02862 = 0.01682 0.00535 -0.00288 0.00170 AFIX 137 H13A 2 0.445764 0.219236 0.583685 11.00000 -1.50000 H13B 2 0.349888 0.222212 0.633539 11.00000 -1.50000 H13C 2 0.405702 0.317955 0.612882 11.00000 -1.50000 AFIX 0 C4 1 -0.004934 0.531064 0.245952 11.00000 0.02533 0.05975 = 0.02626 -0.00198 -0.01232 -0.00003 AFIX 137 H4A 2 0.041774 0.543540 0.207580 11.00000 -1.50000 H4B 2 -0.073458 0.538680 0.229046 11.00000 -1.50000 H4C 2 0.004521 0.466493 0.262928 11.00000 -1.50000 AFIX 0 C9 1 0.204824 0.197296 0.450375 11.00000 0.01533 0.01802 = 0.01782 -0.00235 0.00641 -0.00102 C18 1 0.572586 0.630196 0.162730 11.00000 0.01856 0.01361 = 0.01731 0.00200 0.00704 -0.00147 AFIX 43 H18 2 0.628334 0.635851 0.132319 11.00000 -1.20000 AFIX 0 C11 1 0.319745 0.265097 0.533047 11.00000 0.01694 0.02092 = 0.01488 0.00077 0.00220 0.00356 C012 1 0.462045 0.634457 0.057780 11.00000 0.02358 0.02605 = 0.01656 0.00234 0.00509 -0.00099 AFIX 137 H01A 2 0.467389 0.571853 0.036415 11.00000 -1.50000 H01B 2 0.512983 0.676074 0.037830 11.00000 -1.50000 H01C 2 0.395745 0.660605 0.048391 11.00000 -1.50000 AFIX 0 C23 1 0.146581 0.633559 0.611136 11.00000 0.04070 0.03374 = 0.02245 0.00427 0.01490 0.00746 AFIX 23 H23A 2 0.107637 0.692415 0.616380 11.00000 -1.20000 H23B 2 0.109420 0.581109 0.633234 11.00000 -1.20000 AFIX 0 C10 1 0.265813 0.187453 0.507948 11.00000 0.02167 0.01733 = 0.01735 0.00258 0.00638 0.00338 AFIX 43 H10 2 0.271343 0.128095 0.530645 11.00000 -1.20000 AFIX 0 C5 1 -0.058951 0.581890 0.366208 11.00000 0.01462 0.06401 = 0.03720 0.01143 0.00413 0.00953 AFIX 137 H5A 2 -0.052496 0.516421 0.381932 11.00000 -1.50000 H5B 2 -0.127330 0.593186 0.350175 11.00000 -1.50000 H5C 2 -0.043552 0.624474 0.405150 11.00000 -1.50000 AFIX 0 C22 1 0.249450 0.643825 0.643208 11.00000 0.05518 0.03127 = 0.01781 -0.00226 0.00762 0.00497 AFIX 23 H22A 2 0.273478 0.709681 0.640224 11.00000 -1.20000 H22B 2 0.249897 0.623427 0.692798 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2ndintlui_a.res in P2(1)2(1)2(1) REM wR2 = 0.0447, GooF = S = 1.126, Restrained GooF = 1.126 for all data REM R1 = 0.0215 for 8672 Fo > 4sig(Fo) and 0.0232 for all 9000 data REM 388 parameters refined using 0 restraints END WGHT 0.0000 4.4548 REM Highest difference peak 0.957, deepest hole -0.866, 1-sigma level 0.090 Q1 1 0.6518 0.5833 0.4226 11.00000 0.05 0.96 Q2 1 0.4623 0.6314 0.5025 11.00000 0.05 0.61 Q3 1 0.2948 0.5902 0.4207 11.00000 0.05 0.59 Q4 1 0.3494 0.5976 0.4495 11.00000 0.05 0.51 Q5 1 0.3961 0.5955 0.4247 11.00000 0.05 0.50 Q6 1 0.3528 0.6025 0.3833 11.00000 0.05 0.48 Q7 1 0.2968 0.6375 0.4892 11.00000 0.05 0.46 Q8 1 0.7347 0.5681 0.4165 11.00000 0.05 0.43 Q9 1 0.4603 0.6384 0.3465 11.00000 0.05 0.43 Q10 1 0.1575 0.6378 0.4907 11.00000 0.05 0.43 Q11 1 -0.1568 0.4276 0.2430 11.00000 0.05 0.42 Q12 1 0.4224 0.8672 0.5119 11.00000 0.05 0.42 Q13 1 0.4619 0.5265 0.4944 11.00000 0.05 0.39 Q14 1 0.1562 0.9301 0.4086 11.00000 0.05 0.37 Q15 1 -0.0363 0.8582 0.3340 11.00000 0.05 0.37 Q16 1 0.1143 0.5779 0.4171 11.00000 0.05 0.36 Q17 1 -0.0215 0.6773 0.4183 11.00000 0.05 0.36 Q18 1 0.2742 0.2788 0.3204 11.00000 0.05 0.36 Q19 1 0.1054 0.6229 0.3723 11.00000 0.05 0.35 Q20 1 0.6600 0.2692 0.4167 11.00000 0.05 0.35 ; _shelx_res_checksum 11993 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.34610(2) 0.57185(2) 0.41596(2) 0.01144(4) Uani 1 1 d . . . . . I1 I 0.53586(2) 0.63042(2) 0.49201(2) 0.02329(8) Uani 1 1 d . . . . . P1 P 0.14202(9) 0.58969(8) 0.34356(6) 0.0159(2) Uani 1 1 d . . . . . O1 O 0.4491(2) 0.4485(2) 0.38049(16) 0.0156(7) Uani 1 1 d . . . . . O2 O 0.2742(3) 0.5969(2) 0.52821(17) 0.0194(7) Uani 1 1 d . . . . . N2 N 0.3295(3) 0.5991(3) 0.30102(19) 0.0136(8) Uani 1 1 d . . . . . O3 O 0.3214(2) 0.7374(2) 0.42021(18) 0.0173(6) Uani 1 1 d . . . . . N1 N 0.2360(3) 0.4529(2) 0.4129(2) 0.0140(7) Uani 1 1 d . . . . . C20 C 0.5061(3) 0.6171(3) 0.2798(2) 0.0150(9) Uani 1 1 d . . . . . H20 H 0.516928 0.615044 0.328908 0.018 Uiso 1 1 calc R . . . . C1 C 0.1546(4) 0.4629(3) 0.3623(2) 0.0176(8) Uani 1 1 d . . . . . H1A H 0.091714 0.437760 0.382084 0.021 Uiso 1 1 calc R . . . . H1B H 0.170091 0.427778 0.318799 0.021 Uiso 1 1 calc R . . . . C2 C 0.2297(3) 0.6012(3) 0.2699(2) 0.0161(9) Uani 1 1 d . . . . . H2A H 0.221192 0.548469 0.236455 0.019 Uiso 1 1 calc R . . . . H2B H 0.218634 0.661321 0.244701 0.019 Uiso 1 1 calc R . . . . C29 C 0.4171(4) 0.3890(3) 0.3216(3) 0.0182(10) Uani 1 1 d . . . . . H29A H 0.368361 0.422733 0.291784 0.022 Uiso 1 1 calc R . . . . H29B H 0.386248 0.329981 0.338737 0.022 Uiso 1 1 calc R . . . . C32 C 0.5420(4) 0.4049(4) 0.4024(3) 0.0273(12) Uani 1 1 d . . . . . H32A H 0.529007 0.347547 0.430503 0.033 Uiso 1 1 calc R . . . . H32B H 0.582269 0.449291 0.430766 0.033 Uiso 1 1 calc R . . . . C28 C 0.3092(6) 0.7958(4) 0.3586(3) 0.0364(16) Uani 1 1 d . . . . . H28A H 0.248859 0.776631 0.332394 0.044 Uiso 1 1 calc R . . . . H28B H 0.367745 0.789156 0.327393 0.044 Uiso 1 1 calc R . . . . C19 C 0.5866(3) 0.6255(3) 0.2358(2) 0.0161(9) Uani 1 1 d . . . . . C30 C 0.5114(4) 0.3682(4) 0.2811(3) 0.0239(11) Uani 1 1 d . . . . . H30A H 0.519462 0.412799 0.241655 0.029 Uiso 1 1 calc R . . . . H30B H 0.510428 0.303113 0.262431 0.029 Uiso 1 1 calc R . . . . C12 C 0.3100(3) 0.3512(3) 0.4991(2) 0.0156(9) Uani 1 1 d . . . . . H12 H 0.347918 0.403293 0.515423 0.019 Uiso 1 1 calc R . . . . C15 C 0.4072(3) 0.6113(3) 0.2539(2) 0.0133(9) Uani 1 1 d . . . . . C7 C 0.2461(3) 0.3643(3) 0.4415(2) 0.0142(9) Uani 1 1 d . . . . . C3 C 0.0143(4) 0.6001(4) 0.3054(3) 0.0268(12) Uani 1 1 d . . . . . C25 C 0.3254(4) 0.7984(3) 0.4818(3) 0.0216(11) Uani 1 1 d . . . . . H25A H 0.376029 0.775772 0.515513 0.026 Uiso 1 1 calc R . . . . H25B H 0.259756 0.800920 0.505478 0.026 Uiso 1 1 calc R . . . . C00M C 0.6911(4) 0.6303(4) 0.2649(3) 0.0238(11) Uani 1 1 d . . . . . H00A H 0.688180 0.634740 0.316108 0.036 Uiso 1 1 calc GR . . . . H00B H 0.725175 0.685811 0.246031 0.036 Uiso 1 1 calc GR . . . . H00C H 0.727775 0.573287 0.251553 0.036 Uiso 1 1 calc GR . . . . C24 C 0.1677(4) 0.6127(4) 0.5338(3) 0.0262(11) Uani 1 1 d . . . . . H24A H 0.130550 0.556002 0.518426 0.031 Uiso 1 1 calc R . . . . H24B H 0.147302 0.666601 0.504175 0.031 Uiso 1 1 calc R . . . . C8 C 0.1946(3) 0.2838(3) 0.4177(3) 0.0166(8) Uani 1 1 d . . . . . H8 H 0.151809 0.289157 0.378301 0.020 Uiso 1 1 calc R . . . . C17 C 0.4774(3) 0.6265(3) 0.1357(2) 0.0158(9) Uani 1 1 d . . . . . C31 C 0.5954(4) 0.3803(4) 0.3344(3) 0.0281(12) Uani 1 1 d . . . . . H31A H 0.634072 0.321223 0.339446 0.034 Uiso 1 1 calc R . . . . H31B H 0.641150 0.431564 0.320109 0.034 Uiso 1 1 calc R . . . . C16 C 0.3955(3) 0.6174(3) 0.1803(2) 0.0150(9) Uani 1 1 d . . . . . H16 H 0.330415 0.615144 0.160737 0.018 Uiso 1 1 calc R . . . . C27 C 0.2995(5) 0.8957(4) 0.3831(3) 0.0295(13) Uani 1 1 d . . . . . H27A H 0.228710 0.913707 0.388955 0.035 Uiso 1 1 calc R . . . . H27B H 0.331844 0.939914 0.350027 0.035 Uiso 1 1 calc R . . . . C21 C 0.3111(4) 0.5792(4) 0.5983(2) 0.0309(12) Uani 1 1 d . . . . . H21A H 0.382924 0.594714 0.602030 0.037 Uiso 1 1 calc R . . . . H21B H 0.301070 0.512533 0.611831 0.037 Uiso 1 1 calc R . . . . C14 C 0.1486(4) 0.1132(3) 0.4213(3) 0.0267(10) Uani 1 1 d . . . . . H14A H 0.076762 0.123585 0.426467 0.040 Uiso 1 1 calc GR . . . . H14B H 0.167904 0.056281 0.447096 0.040 Uiso 1 1 calc GR . . . . H14C H 0.164897 0.105274 0.371621 0.040 Uiso 1 1 calc GR . . . . C6 C 0.0007(4) 0.7020(5) 0.2809(3) 0.0373(15) Uani 1 1 d . . . . . H6A H 0.002315 0.744262 0.321513 0.056 Uiso 1 1 calc GR . . . . H6B H -0.063640 0.708291 0.256973 0.056 Uiso 1 1 calc GR . . . . H6C H 0.054570 0.718738 0.248579 0.056 Uiso 1 1 calc GR . . . . C26 C 0.3535(5) 0.8939(3) 0.4530(3) 0.0327(12) Uani 1 1 d . . . . . H26A H 0.426531 0.899438 0.446657 0.039 Uiso 1 1 calc R . . . . H26B H 0.330106 0.945237 0.484045 0.039 Uiso 1 1 calc R . . . . C13 C 0.3861(4) 0.2553(4) 0.5963(3) 0.0265(12) Uani 1 1 d . . . . . H13A H 0.445764 0.219236 0.583685 0.040 Uiso 1 1 calc GR . . . . H13B H 0.349888 0.222212 0.633539 0.040 Uiso 1 1 calc GR . . . . H13C H 0.405702 0.317955 0.612882 0.040 Uiso 1 1 calc GR . . . . C4 C -0.0049(4) 0.5311(5) 0.2460(3) 0.0371(14) Uani 1 1 d . . . . . H4A H 0.041774 0.543540 0.207580 0.056 Uiso 1 1 calc GR . . . . H4B H -0.073458 0.538680 0.229046 0.056 Uiso 1 1 calc GR . . . . H4C H 0.004521 0.466493 0.262928 0.056 Uiso 1 1 calc GR . . . . C9 C 0.2048(3) 0.1973(3) 0.4504(2) 0.0171(10) Uani 1 1 d . . . . . C18 C 0.5726(3) 0.6302(3) 0.1627(2) 0.0165(9) Uani 1 1 d . . . . . H18 H 0.628334 0.635851 0.132319 0.020 Uiso 1 1 calc R . . . . C11 C 0.3197(3) 0.2651(3) 0.5330(2) 0.0176(10) Uani 1 1 d . . . . . C012 C 0.4620(4) 0.6345(4) 0.0578(2) 0.0221(10) Uani 1 1 d . . . . . H01A H 0.467389 0.571853 0.036415 0.033 Uiso 1 1 calc GR . . . . H01B H 0.512983 0.676074 0.037830 0.033 Uiso 1 1 calc GR . . . . H01C H 0.395745 0.660605 0.048391 0.033 Uiso 1 1 calc GR . . . . C23 C 0.1466(5) 0.6336(4) 0.6111(3) 0.0323(12) Uani 1 1 d . . . . . H23A H 0.107637 0.692415 0.616380 0.039 Uiso 1 1 calc R . . . . H23B H 0.109420 0.581109 0.633234 0.039 Uiso 1 1 calc R . . . . C10 C 0.2658(4) 0.1875(3) 0.5079(3) 0.0188(9) Uani 1 1 d . . . . . H10 H 0.271343 0.128095 0.530645 0.023 Uiso 1 1 calc R . . . . C5 C -0.0590(4) 0.5819(5) 0.3662(3) 0.0386(15) Uani 1 1 d . . . . . H5A H -0.052496 0.516421 0.381932 0.058 Uiso 1 1 calc GR . . . . H5B H -0.127330 0.593186 0.350175 0.058 Uiso 1 1 calc GR . . . . H5C H -0.043552 0.624474 0.405150 0.058 Uiso 1 1 calc GR . . . . C22 C 0.2495(5) 0.6438(4) 0.6432(3) 0.0348(14) Uani 1 1 d . . . . . H22A H 0.273478 0.709681 0.640224 0.042 Uiso 1 1 calc R . . . . H22B H 0.249897 0.623427 0.692798 0.042 Uiso 1 1 calc R . . . . 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 Lu1 0.01250(7) 0.01074(7) 0.01107(7) 0.00055(7) -0.00016(8) 0.00026(7) I1 0.02023(15) 0.02194(16) 0.02769(17) -0.00260(13) -0.00882(14) -0.00031(13) P1 0.0136(5) 0.0208(6) 0.0134(5) 0.0019(4) 0.0006(5) 0.0025(5) O1 0.0156(15) 0.0146(17) 0.0167(15) -0.0005(12) -0.0014(13) 0.0035(12) O2 0.0249(17) 0.0211(18) 0.0122(15) -0.0010(12) 0.0025(14) -0.0008(14) N2 0.0103(18) 0.0158(18) 0.0147(17) 0.0031(13) 0.0014(15) 0.0010(14) O3 0.0229(16) 0.0125(14) 0.0166(15) 0.0008(14) 0.0003(15) 0.0007(11) N1 0.0126(16) 0.0173(18) 0.0121(16) 0.0024(16) -0.0007(17) -0.0001(13) C20 0.016(2) 0.014(2) 0.016(2) -0.0011(17) -0.0030(18) -0.0001(18) C1 0.0154(19) 0.022(2) 0.0157(19) 0.0029(16) 0.000(2) -0.001(2) C2 0.015(2) 0.020(2) 0.013(2) 0.0021(17) 0.0012(18) 0.0009(18) C29 0.017(2) 0.015(2) 0.022(2) -0.0080(19) -0.003(2) 0.0009(18) C32 0.023(2) 0.027(3) 0.032(3) -0.005(2) -0.010(2) 0.011(2) C28 0.071(5) 0.015(3) 0.023(3) 0.006(2) 0.011(3) 0.006(3) C19 0.015(2) 0.014(2) 0.020(2) -0.0002(18) -0.0026(18) 0.0006(18) C30 0.026(3) 0.019(2) 0.027(3) -0.005(2) 0.008(2) -0.001(2) C12 0.0154(19) 0.016(2) 0.016(2) -0.0006(18) 0.0006(18) -0.0009(17) C15 0.014(2) 0.010(2) 0.015(2) -0.0001(16) 0.0023(18) 0.0009(16) C7 0.014(2) 0.016(2) 0.0128(19) -0.0009(17) 0.0054(17) -0.0023(18) C3 0.014(2) 0.042(3) 0.024(3) 0.006(2) 0.001(2) 0.008(2) C25 0.028(3) 0.018(2) 0.019(2) -0.0065(19) -0.003(2) 0.0008(19) C00M 0.016(2) 0.028(3) 0.027(3) 0.002(2) 0.000(2) -0.005(2) C24 0.022(3) 0.033(3) 0.024(2) -0.006(2) 0.007(2) -0.005(2) C8 0.0161(19) 0.020(2) 0.0136(19) 0.001(2) 0.005(2) -0.0025(17) C17 0.018(2) 0.014(2) 0.015(2) -0.0011(18) 0.0014(18) 0.0004(19) C31 0.017(2) 0.022(3) 0.045(3) -0.007(2) 0.005(2) 0.004(2) C16 0.016(2) 0.015(2) 0.013(2) 0.0018(17) -0.0010(18) 0.0002(18) C27 0.040(3) 0.015(2) 0.034(3) 0.004(2) 0.004(3) 0.004(2) C21 0.042(3) 0.034(3) 0.016(2) 0.002(2) 0.003(2) 0.005(3) C14 0.028(2) 0.021(2) 0.031(2) -0.002(2) 0.003(3) -0.005(2) C6 0.030(3) 0.050(4) 0.033(3) 0.014(3) 0.004(3) 0.018(3) C26 0.036(3) 0.016(2) 0.046(3) -0.004(2) -0.005(3) 0.002(3) C13 0.034(3) 0.029(3) 0.017(3) 0.005(2) -0.003(2) 0.002(2) C4 0.025(3) 0.060(4) 0.026(3) -0.002(3) -0.012(2) 0.000(3) C9 0.015(2) 0.018(2) 0.018(2) -0.0024(18) 0.0064(19) -0.0010(18) C18 0.019(2) 0.014(2) 0.017(2) 0.0020(18) 0.0070(18) -0.0015(18) C11 0.017(2) 0.021(2) 0.015(2) 0.0008(18) 0.0022(18) 0.0036(18) C012 0.024(2) 0.026(3) 0.017(2) 0.002(2) 0.005(2) -0.001(2) C23 0.041(3) 0.034(3) 0.022(2) 0.004(2) 0.015(3) 0.007(3) C10 0.022(2) 0.017(2) 0.017(2) 0.0026(19) 0.006(2) 0.0034(18) C5 0.015(2) 0.064(4) 0.037(3) 0.011(3) 0.004(2) 0.010(3) C22 0.055(4) 0.031(3) 0.018(3) -0.002(2) 0.008(3) 0.005(3) 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 '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 I1 Lu1 P1 159.25(2) . . ? O1 Lu1 I1 81.27(8) . . ? O1 Lu1 P1 117.29(8) . . ? O1 Lu1 O2 127.95(11) . . ? O1 Lu1 O3 146.73(11) . . ? O2 Lu1 I1 82.42(9) . . ? O2 Lu1 P1 91.83(9) . . ? N2 Lu1 I1 120.20(9) . . ? N2 Lu1 P1 57.13(9) . . ? N2 Lu1 O1 84.48(12) . . ? N2 Lu1 O2 144.84(13) . . ? N2 Lu1 O3 81.30(13) . . ? N2 Lu1 N1 92.25(14) . . ? O3 Lu1 I1 80.24(8) . . ? O3 Lu1 P1 79.03(8) . . ? O3 Lu1 O2 76.37(11) . . ? N1 Lu1 I1 140.14(10) . . ? N1 Lu1 P1 57.63(9) . . ? N1 Lu1 O1 79.48(12) . . ? N1 Lu1 O2 82.48(13) . . ? N1 Lu1 O3 130.80(12) . . ? C1 P1 Lu1 75.60(16) . . ? C1 P1 C3 103.7(2) . . ? C2 P1 Lu1 77.42(15) . . ? C2 P1 C1 100.2(2) . . ? C2 P1 C3 106.3(2) . . ? C3 P1 Lu1 176.24(17) . . ? C29 O1 Lu1 118.8(3) . . ? C32 O1 Lu1 138.1(3) . . ? C32 O1 C29 103.1(3) . . ? C24 O2 Lu1 119.3(3) . . ? C21 O2 Lu1 132.0(3) . . ? C21 O2 C24 107.2(4) . . ? C2 N2 Lu1 119.5(3) . . ? C15 N2 Lu1 125.7(3) . . ? C15 N2 C2 114.8(4) . . ? C28 O3 Lu1 123.6(3) . . ? C28 O3 C25 108.6(3) . . ? C25 O3 Lu1 127.5(3) . . ? C1 N1 Lu1 115.8(3) . . ? C7 N1 Lu1 127.7(3) . . ? C7 N1 C1 115.1(3) . . ? C19 C20 C15 121.9(4) . . ? N1 C1 P1 106.9(3) . . ? N2 C2 P1 105.8(3) . . ? O1 C29 C30 105.0(4) . . ? O1 C32 C31 104.8(4) . . ? O3 C28 C27 107.3(4) . . ? C20 C19 C00M 120.6(4) . . ? C20 C19 C18 120.3(4) . . ? C18 C19 C00M 119.1(4) . . ? C29 C30 C31 104.8(4) . . ? C11 C12 C7 122.6(4) . . ? N2 C15 C20 118.9(4) . . ? N2 C15 C16 124.7(4) . . ? C16 C15 C20 116.4(4) . . ? N1 C7 C12 119.5(4) . . ? N1 C7 C8 124.2(4) . . ? C12 C7 C8 116.3(4) . . ? C6 C3 P1 107.7(4) . . ? C6 C3 C5 108.2(5) . . ? C4 C3 P1 113.3(4) . . ? C4 C3 C6 111.1(5) . . ? C4 C3 C5 110.2(5) . . ? C5 C3 P1 106.1(4) . . ? O3 C25 C26 104.4(4) . . ? O2 C24 C23 106.4(4) . . ? C9 C8 C7 121.7(5) . . ? C16 C17 C012 120.0(4) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 C012 119.6(4) . . ? C32 C31 C30 104.3(4) . . ? C17 C16 C15 121.6(4) . . ? C28 C27 C26 102.5(4) . . ? O2 C21 C22 103.5(4) . . ? C25 C26 C27 102.5(4) . . ? C8 C9 C14 119.0(4) . . ? C10 C9 C8 120.5(4) . . ? C10 C9 C14 120.5(4) . . ? C17 C18 C19 119.5(4) . . ? C12 C11 C13 120.8(4) . . ? C12 C11 C10 118.9(4) . . ? C10 C11 C13 120.4(4) . . ? C22 C23 C24 103.9(5) . . ? C9 C10 C11 120.0(4) . . ? C21 C22 C23 102.2(5) . . ? 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 Lu1 I1 3.0456(4) . ? Lu1 P1 3.0766(12) . ? Lu1 O1 2.330(3) . ? Lu1 O2 2.377(3) . ? Lu1 N2 2.239(4) . ? Lu1 O3 2.374(3) . ? Lu1 N1 2.244(3) . ? P1 C1 1.842(5) . ? P1 C2 1.841(5) . ? P1 C3 1.868(5) . ? O1 C29 1.470(5) . ? O1 C32 1.453(6) . ? O2 C24 1.450(6) . ? O2 C21 1.449(6) . ? N2 C2 1.465(6) . ? N2 C15 1.387(6) . ? O3 C28 1.447(6) . ? O3 C25 1.461(6) . ? N1 C1 1.465(6) . ? N1 C7 1.377(6) . ? C20 C19 1.373(6) . ? C20 C15 1.418(6) . ? C29 C30 1.511(6) . ? C32 C31 1.525(7) . ? C28 C27 1.499(7) . ? C19 C00M 1.509(6) . ? C19 C18 1.409(6) . ? C30 C31 1.526(7) . ? C12 C7 1.405(6) . ? C12 C11 1.389(6) . ? C15 C16 1.416(6) . ? C7 C8 1.410(6) . ? C3 C6 1.530(8) . ? C3 C4 1.522(8) . ? C3 C5 1.542(7) . ? C25 C26 1.510(7) . ? C24 C23 1.533(7) . ? C8 C9 1.384(7) . ? C17 C16 1.395(6) . ? C17 C18 1.377(6) . ? C17 C012 1.507(6) . ? C27 C26 1.518(8) . ? C21 C22 1.503(8) . ? C14 C9 1.517(6) . ? C13 C11 1.507(7) . ? C9 C10 1.377(7) . ? C11 C10 1.402(7) . ? C23 C22 1.516(9) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.710(6) 2 0.290(6)