#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:22:16 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293309 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572116.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_1572116 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 'C43 H62 Lu N2 O P, C4 H8 O' _chemical_formula_sum 'C47 H70 Lu N2 O2 P' _chemical_formula_weight 900.99 _chemical_properties_physical Air-sensitive,Moisture-sensitive _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 _audit_creation_date 2021-10-26 _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 99.117(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0585(4) _cell_length_b 28.9336(10) _cell_length_c 15.5726(6) _cell_measurement_reflns_used 9818 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.12 _cell_measurement_theta_min 2.37 _cell_volume 4474.8(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0538 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 99041 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.283 _diffrn_reflns_theta_min 1.933 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.6515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.1431 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8736. 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 1.337 _exptl_crystal_description plate _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.714 _refine_diff_density_min -2.602 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef 0.00013(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 1.237 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 11121 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.237 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0350 _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^)+(0.0177P)^2^+11.7801P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.0747 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10065 _reflns_number_total 11121 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02077d2.cif _cod_data_source_block lubiampind _cod_database_code 1572116 _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 0.935 _shelx_estimated_absorpt_t_min 0.698 _olex2_refinement_description ; 1. 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 2.a Ternary CH refined with riding coordinates: C31(H31), C28(H28) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C1(H1A,H1B), C43(H43A,H43B), C42(H42A,H42B), C41(H41A,H41B), C40(H40A,H40B), C46(H46A,H46B), C45(H45A,H45B), C44(H44A,H44B), C47(H47A,H47B) 2.c Aromatic/amide H refined with riding coordinates: C23(H23), C35(H35), C36(H36), C16(H16), C18(H18), C20(H20), C8(H8), C10(H10), C12(H12) 2.d Idealised Me refined as rotating group: C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,H30B, H30C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C21(H21A,H21B,H21C), C22(H22A, H22B,H22C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C5(H5A, H5B,H5C), C4(H4A,H4B,H4C) ; _shelx_res_file ; TITL LuBiAMPInd_a.res in P2(1)/c lubiampind.res created by SHELXL-2018/3 at 11:03:22 on 26-Oct-2021 CELL 0.71073 10.0585 28.9336 15.5726 90 99.117 90 ZERR 4 0.0004 0.001 0.0006 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Lu N O P UNIT 188 280 4 8 8 4 L.S. 4 PLAN 12 SIZE 0.17 0.12 0.03 TEMP -173.15 HTAB C20 O1 BOND $H CONF HTAB fmap 2 acta SHEL 999 0.75 OMIT 1 0 6 OMIT 0 1 6 OMIT 0 2 12 OMIT 2 1 17 REM REM REM WGHT 0.017700 11.780100 EXTI 0.000129 FVAR 0.24369 LU1 3 0.228863 0.378628 0.247221 11.00000 0.00948 0.01271 = 0.01157 0.00070 0.00198 -0.00096 P1 6 -0.019707 0.419550 0.169175 11.00000 0.00947 0.01806 = 0.01653 0.00193 0.00183 -0.00025 O1 5 0.271110 0.325853 0.355466 11.00000 0.01646 0.01545 = 0.01554 0.00414 0.00290 -0.00132 O2 5 0.801020 0.230476 0.343593 11.00000 0.04979 0.02762 = 0.08728 0.00304 0.01755 0.00283 C23 1 0.332399 0.427519 0.133698 11.00000 0.01169 0.01372 = 0.01202 0.00232 0.00148 -0.00154 AFIX 43 H23 2 0.271500 0.444105 0.091918 11.00000 -1.20000 AFIX 0 N2 4 0.068184 0.333109 0.178293 11.00000 0.01107 0.01741 = 0.01363 -0.00129 0.00081 -0.00181 N1 4 0.107285 0.416457 0.329959 11.00000 0.01372 0.01661 = 0.01296 -0.00135 0.00344 -0.00054 C25 1 0.480439 0.410472 0.256123 11.00000 0.00998 0.01530 = 0.01435 0.00220 0.00223 -0.00179 C26 1 0.470144 0.370424 0.198950 11.00000 0.00995 0.01207 = 0.01511 -0.00059 0.00175 -0.00092 C27 1 0.374768 0.381668 0.122371 11.00000 0.01554 0.01454 = 0.01091 0.00125 0.00543 -0.00252 C31 1 0.339485 0.354327 0.038188 11.00000 0.01954 0.01774 = 0.01511 -0.00290 0.00245 -0.00056 AFIX 13 H31 2 0.341078 0.320694 0.053106 11.00000 -1.20000 AFIX 0 C32 1 0.199271 0.366151 -0.010563 11.00000 0.02139 0.02376 = 0.01633 -0.00434 -0.00011 -0.00139 AFIX 137 H32A 2 0.131523 0.358831 0.026190 11.00000 -1.50000 H32B 2 0.181467 0.348024 -0.064318 11.00000 -1.50000 H32C 2 0.195058 0.399169 -0.024772 11.00000 -1.50000 AFIX 0 C33 1 0.443910 0.362927 -0.021738 11.00000 0.02621 0.04744 = 0.01774 -0.01013 0.00719 -0.00594 AFIX 137 H33A 2 0.441566 0.395540 -0.038899 11.00000 -1.50000 H33B 2 0.423149 0.343531 -0.073727 11.00000 -1.50000 H33C 2 0.533818 0.355211 0.009074 11.00000 -1.50000 AFIX 0 C24 1 0.392069 0.445580 0.215031 11.00000 0.00852 0.01216 = 0.01469 0.00188 0.00282 -0.00226 C28 1 0.380910 0.495857 0.241026 11.00000 0.01820 0.01409 = 0.01284 0.00019 0.00157 0.00069 AFIX 13 H28 2 0.413992 0.498293 0.304893 11.00000 -1.20000 AFIX 0 C29 1 0.472611 0.525608 0.193985 11.00000 0.01988 0.01577 = 0.02828 -0.00002 0.00560 -0.00200 AFIX 137 H29A 2 0.566273 0.515711 0.210929 11.00000 -1.50000 H29B 2 0.463854 0.558107 0.209915 11.00000 -1.50000 H29C 2 0.446421 0.522056 0.130990 11.00000 -1.50000 AFIX 0 C30 1 0.236363 0.514359 0.223886 11.00000 0.01908 0.01765 = 0.02310 -0.00062 0.00759 0.00251 AFIX 137 H30A 2 0.200863 0.511854 0.161720 11.00000 -1.50000 H30B 2 0.235812 0.546831 0.241721 11.00000 -1.50000 H30C 2 0.179982 0.496223 0.257256 11.00000 -1.50000 AFIX 0 C34 1 0.556644 0.331338 0.220632 11.00000 0.01261 0.01716 = 0.01922 0.00182 0.00703 0.00106 C39 1 0.553044 0.288910 0.164088 11.00000 0.02208 0.01952 = 0.02913 -0.00231 0.00587 0.00604 AFIX 137 H39A 2 0.573947 0.297596 0.106879 11.00000 -1.50000 H39B 2 0.463096 0.275040 0.157233 11.00000 -1.50000 H39C 2 0.619751 0.266519 0.191401 11.00000 -1.50000 AFIX 0 C35 1 0.649642 0.334086 0.295520 11.00000 0.01437 0.01851 = 0.02408 0.00547 0.00301 0.00326 AFIX 43 H35 2 0.709551 0.308919 0.310331 11.00000 -1.20000 AFIX 0 C36 1 0.659334 0.372861 0.351093 11.00000 0.01414 0.02005 = 0.01977 0.00563 0.00125 -0.00043 AFIX 43 H36 2 0.724409 0.372571 0.402462 11.00000 -1.20000 AFIX 0 C37 1 0.579312 0.410523 0.333982 11.00000 0.01194 0.01710 = 0.02231 0.00102 0.00167 -0.00356 C38 1 0.602494 0.452333 0.393974 11.00000 0.01801 0.02226 = 0.01629 0.00015 -0.00250 -0.00400 AFIX 137 H38A 2 0.670586 0.444801 0.444287 11.00000 -1.50000 H38B 2 0.517982 0.460677 0.413873 11.00000 -1.50000 H38C 2 0.633824 0.478412 0.362349 11.00000 -1.50000 AFIX 0 C2 1 -0.057898 0.357700 0.147447 11.00000 0.01411 0.01999 = 0.01949 -0.00034 0.00185 -0.00023 AFIX 23 H2A 2 -0.130191 0.347207 0.179236 11.00000 -1.20000 H2B 2 -0.086993 0.352341 0.084485 11.00000 -1.20000 AFIX 0 C15 1 0.067052 0.286712 0.160264 11.00000 0.01735 0.01893 = 0.01423 -0.00179 0.00398 -0.00456 C16 1 -0.042461 0.262725 0.112009 11.00000 0.02305 0.02063 = 0.02856 -0.00364 -0.00343 -0.00556 AFIX 43 H16 2 -0.122126 0.279307 0.090035 11.00000 -1.20000 AFIX 0 C17 1 -0.037013 0.215587 0.095764 11.00000 0.03554 0.02479 = 0.03113 -0.00602 -0.00431 -0.00982 C21 1 -0.155788 0.192091 0.041309 11.00000 0.05380 0.02866 = 0.06350 -0.00856 -0.02378 -0.01242 AFIX 137 H21A 2 -0.172545 0.206244 -0.016572 11.00000 -1.50000 H21B 2 -0.235723 0.195651 0.069428 11.00000 -1.50000 H21C 2 -0.136055 0.159154 0.035786 11.00000 -1.50000 AFIX 0 C18 1 0.076567 0.190368 0.128994 11.00000 0.04383 0.01572 = 0.02998 -0.00588 0.00239 -0.00271 AFIX 43 H18 2 0.079503 0.158051 0.118677 11.00000 -1.20000 AFIX 0 C19 1 0.186946 0.212603 0.177786 11.00000 0.03088 0.01840 = 0.01716 -0.00093 0.00495 0.00089 C22 1 0.309433 0.185042 0.217119 11.00000 0.04128 0.02083 = 0.02882 -0.00124 0.00356 0.00908 AFIX 137 H22A 2 0.381408 0.206221 0.241944 11.00000 -1.50000 H22B 2 0.340338 0.166169 0.171886 11.00000 -1.50000 H22C 2 0.285879 0.164886 0.263002 11.00000 -1.50000 AFIX 0 C20 1 0.181955 0.259654 0.190779 11.00000 0.02067 0.01956 = 0.01506 -0.00089 0.00341 -0.00144 AFIX 43 H20 2 0.259184 0.274583 0.221626 11.00000 -1.20000 AFIX 0 C1 1 -0.030716 0.425954 0.286087 11.00000 0.01479 0.01975 = 0.02052 -0.00042 0.00515 0.00152 AFIX 23 H1A 2 -0.059036 0.457620 0.299117 11.00000 -1.20000 H1B 2 -0.095276 0.403523 0.304165 11.00000 -1.20000 AFIX 0 C7 1 0.133788 0.422918 0.418813 11.00000 0.01936 0.00993 = 0.01912 -0.00184 0.00560 -0.00154 C8 1 0.267909 0.418120 0.460233 11.00000 0.01779 0.01595 = 0.01870 -0.00306 0.00471 -0.00235 AFIX 43 H8 2 0.335851 0.412226 0.425664 11.00000 -1.20000 AFIX 0 C9 1 0.304547 0.421673 0.549556 11.00000 0.02633 0.01401 = 0.01832 -0.00254 0.00233 -0.00404 C13 1 0.449801 0.415370 0.590203 11.00000 0.03113 0.02753 = 0.01747 -0.00219 -0.00301 -0.00447 AFIX 137 H13A 2 0.490946 0.391339 0.558663 11.00000 -1.50000 H13B 2 0.454406 0.406147 0.651156 11.00000 -1.50000 H13C 2 0.498418 0.444530 0.587196 11.00000 -1.50000 AFIX 0 C10 1 0.204616 0.431455 0.600284 11.00000 0.03776 0.01582 = 0.01376 -0.00301 0.00757 -0.00527 AFIX 43 H10 2 0.228255 0.434373 0.661566 11.00000 -1.20000 AFIX 0 C11 1 0.071821 0.436890 0.561752 11.00000 0.03369 0.01213 = 0.02331 -0.00233 0.01464 -0.00199 C14 1 -0.037423 0.446490 0.616362 11.00000 0.04181 0.02501 = 0.02270 -0.00385 0.01824 -0.00147 AFIX 137 H14A 2 -0.080690 0.476108 0.598873 11.00000 -1.50000 H14B 2 0.002629 0.447812 0.677923 11.00000 -1.50000 H14C 2 -0.104742 0.421747 0.607549 11.00000 -1.50000 AFIX 0 C12 1 0.036324 0.432815 0.471746 11.00000 0.01941 0.01537 = 0.02035 0.00033 0.00712 -0.00109 AFIX 43 H12 2 -0.055012 0.436783 0.445840 11.00000 -1.20000 AFIX 0 C3 1 -0.164061 0.451791 0.107671 11.00000 0.01240 0.02698 = 0.02404 0.00745 0.00340 0.00264 C6 1 -0.296859 0.433610 0.129070 11.00000 0.01341 0.02660 = 0.03610 0.00704 0.00102 0.00086 AFIX 137 H6A 2 -0.371534 0.450877 0.095679 11.00000 -1.50000 H6B 2 -0.298792 0.437479 0.191379 11.00000 -1.50000 H6C 2 -0.305821 0.400758 0.113941 11.00000 -1.50000 AFIX 0 C5 1 -0.149434 0.503101 0.131394 11.00000 0.02159 0.02337 = 0.05505 0.01254 0.00049 0.00211 AFIX 137 H5A 2 -0.220981 0.520714 0.095658 11.00000 -1.50000 H5B 2 -0.061530 0.514263 0.120711 11.00000 -1.50000 H5C 2 -0.156432 0.507161 0.192995 11.00000 -1.50000 AFIX 0 C4 1 -0.158326 0.445887 0.010952 11.00000 0.04089 0.07259 = 0.01773 0.01585 0.00562 0.01990 AFIX 137 H4A 2 -0.172798 0.413324 -0.005181 11.00000 -1.50000 H4B 2 -0.069892 0.455747 -0.001067 11.00000 -1.50000 H4C 2 -0.228605 0.464800 -0.023011 11.00000 -1.50000 AFIX 0 C43 1 0.156401 0.305814 0.391283 11.00000 0.02186 0.02034 = 0.02205 0.00217 0.00808 -0.00473 AFIX 23 H43A 2 0.083469 0.296602 0.344003 11.00000 -1.20000 H43B 2 0.120037 0.328229 0.429624 11.00000 -1.20000 AFIX 0 C42 1 0.214694 0.264093 0.442290 11.00000 0.03139 0.02345 = 0.02266 0.00695 0.00596 -0.00530 AFIX 23 H42A 2 0.217547 0.236872 0.404109 11.00000 -1.20000 H42B 2 0.162817 0.256248 0.489273 11.00000 -1.20000 AFIX 0 C41 1 0.355957 0.280960 0.478963 11.00000 0.03441 0.03441 = 0.02419 0.01533 -0.00026 -0.00297 AFIX 23 H41A 2 0.354754 0.301729 0.529357 11.00000 -1.20000 H41B 2 0.417454 0.254751 0.496744 11.00000 -1.20000 AFIX 0 C40 1 0.396319 0.306693 0.402543 11.00000 0.01963 0.02458 = 0.02284 0.00890 -0.00094 0.00110 AFIX 23 H40A 2 0.460987 0.331675 0.422810 11.00000 -1.20000 H40B 2 0.438339 0.285424 0.364870 11.00000 -1.20000 AFIX 0 C46 1 0.851121 0.155084 0.304860 11.00000 0.06805 0.03985 = 0.09442 -0.01314 0.04063 -0.00799 AFIX 23 H46A 2 0.901663 0.130461 0.340193 11.00000 -1.20000 H46B 2 0.854029 0.149051 0.242608 11.00000 -1.20000 AFIX 0 C45 1 0.706014 0.157611 0.322082 11.00000 0.04074 0.05320 = 0.07037 -0.00746 0.00536 -0.01686 AFIX 23 H45A 2 0.641647 0.158954 0.267015 11.00000 -1.20000 H45B 2 0.683799 0.130755 0.356564 11.00000 -1.20000 AFIX 0 C44 1 0.704715 0.201233 0.372031 11.00000 0.04169 0.04210 = 0.08080 0.00286 0.02934 0.00261 AFIX 23 H44A 2 0.614341 0.215631 0.360789 11.00000 -1.20000 H44B 2 0.728379 0.195174 0.435174 11.00000 -1.20000 AFIX 0 C47 1 0.907984 0.202009 0.331279 11.00000 0.03175 0.03226 = 0.07577 0.00178 0.00987 -0.00173 AFIX 23 H47A 2 0.973361 0.199684 0.385766 11.00000 -1.20000 H47B 2 0.954921 0.214849 0.285324 11.00000 -1.20000 AFIX 0 HKLF 4 REM LuBiAMPInd_a.res in P2(1)/c REM wR2 = 0.0747, GooF = S = 1.237, Restrained GooF = 1.237 for all data REM R1 = 0.0350 for 10065 Fo > 4sig(Fo) and 0.0397 for all 11121 data REM 492 parameters refined using 0 restraints END WGHT 0.0178 11.7801 REM Instructions for potential hydrogen bonds HTAB C20 O1 REM Highest difference peak 1.714, deepest hole -2.602, 1-sigma level 0.109 Q1 1 0.2278 0.4134 0.2450 11.00000 0.05 1.71 Q2 1 0.2156 0.3788 0.1867 11.00000 0.05 1.54 Q3 1 0.2277 0.3436 0.2443 11.00000 0.05 1.49 Q4 1 0.1537 0.3782 0.2389 11.00000 0.05 1.39 Q5 1 0.2348 0.3801 0.3078 11.00000 0.05 1.26 Q6 1 0.7805 0.1682 0.2565 11.00000 0.05 0.87 Q7 1 -0.2320 0.3460 0.2185 11.00000 0.05 0.80 Q8 1 0.7792 0.3458 0.2842 11.00000 0.05 0.76 Q9 1 0.3212 0.3797 0.3014 11.00000 0.05 0.72 Q10 1 -0.2257 0.3869 0.2718 11.00000 0.05 0.71 Q11 1 -0.0171 0.3897 0.1606 11.00000 0.05 0.70 Q12 1 -0.2344 0.3842 0.2242 11.00000 0.05 0.67 ; _shelx_res_checksum 81969 _olex2_submission_special_instructions 'No special instructions were received' 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 Lu1 Lu 0.22886(2) 0.37863(2) 0.24722(2) 0.01122(4) Uani 1 1 d . . . . . P1 P -0.01971(8) 0.41955(3) 0.16917(5) 0.01471(16) Uani 1 1 d . . . . . O1 O 0.2711(2) 0.32585(8) 0.35547(14) 0.0158(4) Uani 1 1 d . . . . . O2 O 0.8010(4) 0.23048(11) 0.3436(3) 0.0542(10) Uani 1 1 d . . . . . C23 C 0.3324(3) 0.42752(10) 0.13370(19) 0.0125(6) Uani 1 1 d . . . . . H23 H 0.271500 0.444105 0.091918 0.015 Uiso 1 1 calc R . . . . N2 N 0.0682(3) 0.33311(9) 0.17829(17) 0.0142(5) Uani 1 1 d . . . . . N1 N 0.1073(3) 0.41646(9) 0.32996(17) 0.0143(5) Uani 1 1 d . . . . . C25 C 0.4804(3) 0.41047(10) 0.2561(2) 0.0132(6) Uani 1 1 d . . . . . C26 C 0.4701(3) 0.37042(10) 0.1989(2) 0.0124(6) Uani 1 1 d . . . . . C27 C 0.3748(3) 0.38167(11) 0.12237(19) 0.0133(6) Uani 1 1 d . . . . . C31 C 0.3395(3) 0.35433(11) 0.0382(2) 0.0175(6) Uani 1 1 d . . . . . H31 H 0.341078 0.320694 0.053106 0.021 Uiso 1 1 calc R . . . . C32 C 0.1993(3) 0.36615(12) -0.0106(2) 0.0208(7) Uani 1 1 d . . . . . H32A H 0.131523 0.358831 0.026190 0.031 Uiso 1 1 calc GR . . . . H32B H 0.181467 0.348024 -0.064318 0.031 Uiso 1 1 calc GR . . . . H32C H 0.195058 0.399169 -0.024772 0.031 Uiso 1 1 calc GR . . . . C33 C 0.4439(4) 0.36293(15) -0.0217(2) 0.0301(8) Uani 1 1 d . . . . . H33A H 0.441566 0.395540 -0.038899 0.045 Uiso 1 1 calc GR . . . . H33B H 0.423149 0.343531 -0.073727 0.045 Uiso 1 1 calc GR . . . . H33C H 0.533818 0.355211 0.009074 0.045 Uiso 1 1 calc GR . . . . C24 C 0.3921(3) 0.44558(10) 0.2150(2) 0.0117(5) Uani 1 1 d . . . . . C28 C 0.3809(3) 0.49586(11) 0.2410(2) 0.0151(6) Uani 1 1 d . . . . . H28 H 0.413992 0.498293 0.304893 0.018 Uiso 1 1 calc R . . . . C29 C 0.4726(3) 0.52561(11) 0.1940(2) 0.0211(7) Uani 1 1 d . . . . . H29A H 0.566273 0.515711 0.210929 0.032 Uiso 1 1 calc GR . . . . H29B H 0.463854 0.558107 0.209915 0.032 Uiso 1 1 calc GR . . . . H29C H 0.446421 0.522056 0.130990 0.032 Uiso 1 1 calc GR . . . . C30 C 0.2364(3) 0.51436(12) 0.2239(2) 0.0195(7) Uani 1 1 d . . . . . H30A H 0.200863 0.511854 0.161720 0.029 Uiso 1 1 calc GR . . . . H30B H 0.235812 0.546831 0.241721 0.029 Uiso 1 1 calc GR . . . . H30C H 0.179982 0.496223 0.257256 0.029 Uiso 1 1 calc GR . . . . C34 C 0.5566(3) 0.33134(11) 0.2206(2) 0.0158(6) Uani 1 1 d . . . . . C39 C 0.5530(4) 0.28891(12) 0.1641(2) 0.0234(7) Uani 1 1 d . . . . . H39A H 0.573947 0.297596 0.106879 0.035 Uiso 1 1 calc GR . . . . H39B H 0.463096 0.275040 0.157233 0.035 Uiso 1 1 calc GR . . . . H39C H 0.619751 0.266519 0.191401 0.035 Uiso 1 1 calc GR . . . . C35 C 0.6496(3) 0.33409(12) 0.2955(2) 0.0190(6) Uani 1 1 d . . . . . H35 H 0.709551 0.308919 0.310331 0.023 Uiso 1 1 calc R . . . . C36 C 0.6593(3) 0.37286(11) 0.3511(2) 0.0181(6) Uani 1 1 d . . . . . H36 H 0.724409 0.372571 0.402462 0.022 Uiso 1 1 calc R . . . . C37 C 0.5793(3) 0.41052(11) 0.3340(2) 0.0172(6) Uani 1 1 d . . . . . C38 C 0.6025(3) 0.45233(12) 0.3940(2) 0.0194(7) Uani 1 1 d . . . . . H38A H 0.670586 0.444801 0.444287 0.029 Uiso 1 1 calc GR . . . . H38B H 0.517982 0.460677 0.413873 0.029 Uiso 1 1 calc GR . . . . H38C H 0.633824 0.478412 0.362349 0.029 Uiso 1 1 calc GR . . . . C2 C -0.0579(3) 0.35770(11) 0.1474(2) 0.0180(6) Uani 1 1 d . . . . . H2A H -0.130191 0.347207 0.179236 0.022 Uiso 1 1 calc R . . . . H2B H -0.086993 0.352341 0.084485 0.022 Uiso 1 1 calc R . . . . C15 C 0.0671(3) 0.28671(11) 0.1603(2) 0.0167(6) Uani 1 1 d . . . . . C16 C -0.0425(4) 0.26272(12) 0.1120(2) 0.0249(7) Uani 1 1 d . . . . . H16 H -0.122126 0.279307 0.090035 0.030 Uiso 1 1 calc R . . . . C17 C -0.0370(4) 0.21559(14) 0.0958(3) 0.0315(9) Uani 1 1 d . . . . . C21 C -0.1558(5) 0.19209(16) 0.0413(4) 0.0522(14) Uani 1 1 d . . . . . H21A H -0.172545 0.206244 -0.016572 0.078 Uiso 1 1 calc GR . . . . H21B H -0.235723 0.195651 0.069428 0.078 Uiso 1 1 calc GR . . . . H21C H -0.136055 0.159154 0.035786 0.078 Uiso 1 1 calc GR . . . . C18 C 0.0766(4) 0.19037(13) 0.1290(3) 0.0302(8) Uani 1 1 d . . . . . H18 H 0.079503 0.158051 0.118677 0.036 Uiso 1 1 calc R . . . . C19 C 0.1869(4) 0.21260(12) 0.1778(2) 0.0220(7) Uani 1 1 d . . . . . C22 C 0.3094(4) 0.18504(13) 0.2171(3) 0.0305(8) Uani 1 1 d . . . . . H22A H 0.381408 0.206221 0.241944 0.046 Uiso 1 1 calc GR . . . . H22B H 0.340338 0.166169 0.171886 0.046 Uiso 1 1 calc GR . . . . H22C H 0.285879 0.164886 0.263002 0.046 Uiso 1 1 calc GR . . . . C20 C 0.1820(3) 0.25965(11) 0.1908(2) 0.0184(6) Uani 1 1 d . . . . . H20 H 0.259184 0.274583 0.221626 0.022 Uiso 1 1 calc R . . . . C1 C -0.0307(3) 0.42595(12) 0.2861(2) 0.0181(6) Uani 1 1 d . . . . . H1A H -0.059036 0.457620 0.299117 0.022 Uiso 1 1 calc R . . . . H1B H -0.095276 0.403523 0.304165 0.022 Uiso 1 1 calc R . . . . C7 C 0.1338(3) 0.42292(10) 0.4188(2) 0.0159(6) Uani 1 1 d . . . . . C8 C 0.2679(3) 0.41812(11) 0.4602(2) 0.0173(6) Uani 1 1 d . . . . . H8 H 0.335851 0.412226 0.425664 0.021 Uiso 1 1 calc R . . . . C9 C 0.3045(4) 0.42167(11) 0.5496(2) 0.0197(7) Uani 1 1 d . . . . . C13 C 0.4498(4) 0.41537(13) 0.5902(2) 0.0261(8) Uani 1 1 d . . . . . H13A H 0.490946 0.391339 0.558663 0.039 Uiso 1 1 calc GR . . . . H13B H 0.454406 0.406147 0.651156 0.039 Uiso 1 1 calc GR . . . . H13C H 0.498418 0.444530 0.587196 0.039 Uiso 1 1 calc GR . . . . C10 C 0.2046(4) 0.43145(11) 0.6003(2) 0.0221(7) Uani 1 1 d . . . . . H10 H 0.228255 0.434373 0.661566 0.026 Uiso 1 1 calc R . . . . C11 C 0.0718(4) 0.43689(11) 0.5618(2) 0.0219(7) Uani 1 1 d . . . . . C14 C -0.0374(4) 0.44649(13) 0.6164(2) 0.0284(8) Uani 1 1 d . . . . . H14A H -0.080690 0.476108 0.598873 0.043 Uiso 1 1 calc GR . . . . H14B H 0.002629 0.447812 0.677923 0.043 Uiso 1 1 calc GR . . . . H14C H -0.104742 0.421747 0.607549 0.043 Uiso 1 1 calc GR . . . . C12 C 0.0363(3) 0.43281(11) 0.4717(2) 0.0179(6) Uani 1 1 d . . . . . H12 H -0.055012 0.436783 0.445840 0.022 Uiso 1 1 calc R . . . . C3 C -0.1641(3) 0.45179(12) 0.1077(2) 0.0211(7) Uani 1 1 d . . . . . C6 C -0.2969(3) 0.43361(13) 0.1291(3) 0.0257(8) Uani 1 1 d . . . . . H6A H -0.371534 0.450877 0.095679 0.039 Uiso 1 1 calc GR . . . . H6B H -0.298792 0.437479 0.191379 0.039 Uiso 1 1 calc GR . . . . H6C H -0.305821 0.400758 0.113941 0.039 Uiso 1 1 calc GR . . . . C5 C -0.1494(4) 0.50310(13) 0.1314(3) 0.0339(9) Uani 1 1 d . . . . . H5A H -0.220981 0.520714 0.095658 0.051 Uiso 1 1 calc GR . . . . H5B H -0.061530 0.514263 0.120711 0.051 Uiso 1 1 calc GR . . . . H5C H -0.156432 0.507161 0.192995 0.051 Uiso 1 1 calc GR . . . . C4 C -0.1583(5) 0.44589(19) 0.0110(3) 0.0436(12) Uani 1 1 d . . . . . H4A H -0.172798 0.413324 -0.005181 0.065 Uiso 1 1 calc GR . . . . H4B H -0.069892 0.455747 -0.001067 0.065 Uiso 1 1 calc GR . . . . H4C H -0.228605 0.464800 -0.023011 0.065 Uiso 1 1 calc GR . . . . C43 C 0.1564(3) 0.30581(12) 0.3913(2) 0.0209(7) Uani 1 1 d . . . . . H43A H 0.083469 0.296602 0.344003 0.025 Uiso 1 1 calc R . . . . H43B H 0.120037 0.328229 0.429624 0.025 Uiso 1 1 calc R . . . . C42 C 0.2147(4) 0.26409(13) 0.4423(2) 0.0256(8) Uani 1 1 d . . . . . H42A H 0.217547 0.236872 0.404109 0.031 Uiso 1 1 calc R . . . . H42B H 0.162817 0.256248 0.489273 0.031 Uiso 1 1 calc R . . . . C41 C 0.3560(4) 0.28096(15) 0.4790(3) 0.0315(9) Uani 1 1 d . . . . . H41A H 0.354754 0.301729 0.529357 0.038 Uiso 1 1 calc R . . . . H41B H 0.417454 0.254751 0.496744 0.038 Uiso 1 1 calc R . . . . C40 C 0.3963(3) 0.30669(13) 0.4025(2) 0.0228(7) Uani 1 1 d . . . . . H40A H 0.460987 0.331675 0.422810 0.027 Uiso 1 1 calc R . . . . H40B H 0.438339 0.285424 0.364870 0.027 Uiso 1 1 calc R . . . . C46 C 0.8511(6) 0.15508(19) 0.3049(5) 0.0644(17) Uani 1 1 d . . . . . H46A H 0.901663 0.130461 0.340193 0.077 Uiso 1 1 calc R . . . . H46B H 0.854029 0.149051 0.242608 0.077 Uiso 1 1 calc R . . . . C45 C 0.7060(5) 0.15761(19) 0.3221(4) 0.0551(14) Uani 1 1 d . . . . . H45A H 0.641647 0.158954 0.267015 0.066 Uiso 1 1 calc R . . . . H45B H 0.683799 0.130755 0.356564 0.066 Uiso 1 1 calc R . . . . C44 C 0.7047(5) 0.20123(17) 0.3720(4) 0.0527(14) Uani 1 1 d . . . . . H44A H 0.614341 0.215631 0.360789 0.063 Uiso 1 1 calc R . . . . H44B H 0.728379 0.195174 0.435174 0.063 Uiso 1 1 calc R . . . . C47 C 0.9080(5) 0.20201(16) 0.3313(4) 0.0464(12) Uani 1 1 d . . . . . H47A H 0.973361 0.199684 0.385766 0.056 Uiso 1 1 calc R . . . . H47B H 0.954921 0.214849 0.285324 0.056 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 0.00948(6) 0.01271(6) 0.01157(6) 0.00070(5) 0.00198(4) -0.00096(5) P1 0.0095(4) 0.0181(4) 0.0165(4) 0.0019(3) 0.0018(3) -0.0003(3) O1 0.0165(11) 0.0155(11) 0.0155(11) 0.0041(8) 0.0029(8) -0.0013(8) O2 0.050(2) 0.0276(17) 0.087(3) 0.0030(17) 0.0175(19) 0.0028(14) C23 0.0117(14) 0.0137(14) 0.0120(14) 0.0023(11) 0.0015(11) -0.0015(11) N2 0.0111(12) 0.0174(13) 0.0136(12) -0.0013(10) 0.0008(9) -0.0018(10) N1 0.0137(13) 0.0166(13) 0.0130(12) -0.0014(10) 0.0034(10) -0.0005(10) C25 0.0100(13) 0.0153(14) 0.0143(14) 0.0022(11) 0.0022(11) -0.0018(11) C26 0.0099(13) 0.0121(14) 0.0151(14) -0.0006(11) 0.0017(11) -0.0009(10) C27 0.0155(14) 0.0145(14) 0.0109(13) 0.0013(11) 0.0054(10) -0.0025(11) C31 0.0195(16) 0.0177(16) 0.0151(15) -0.0029(12) 0.0024(12) -0.0006(12) C32 0.0214(17) 0.0238(17) 0.0163(15) -0.0043(13) -0.0001(12) -0.0014(13) C33 0.0262(19) 0.047(2) 0.0177(17) -0.0101(16) 0.0072(14) -0.0059(17) C24 0.0085(13) 0.0122(14) 0.0147(14) 0.0019(11) 0.0028(10) -0.0023(10) C28 0.0182(16) 0.0141(14) 0.0128(14) 0.0002(11) 0.0016(11) 0.0007(11) C29 0.0199(17) 0.0158(16) 0.0283(18) 0.0000(13) 0.0056(14) -0.0020(12) C30 0.0191(16) 0.0176(16) 0.0231(17) -0.0006(13) 0.0076(13) 0.0025(12) C34 0.0126(14) 0.0172(15) 0.0192(15) 0.0018(12) 0.0070(12) 0.0011(11) C39 0.0221(17) 0.0195(17) 0.0291(19) -0.0023(14) 0.0059(14) 0.0060(13) C35 0.0144(15) 0.0185(16) 0.0241(17) 0.0055(13) 0.0030(12) 0.0033(12) C36 0.0141(15) 0.0200(16) 0.0198(15) 0.0056(12) 0.0013(11) -0.0004(12) C37 0.0119(15) 0.0171(15) 0.0223(16) 0.0010(12) 0.0017(12) -0.0036(11) C38 0.0180(16) 0.0223(17) 0.0163(15) 0.0002(13) -0.0025(12) -0.0040(12) C2 0.0141(15) 0.0200(16) 0.0195(16) -0.0003(13) 0.0019(12) -0.0002(12) C15 0.0173(15) 0.0189(16) 0.0142(15) -0.0018(12) 0.0040(12) -0.0046(12) C16 0.0231(18) 0.0206(17) 0.0286(19) -0.0036(14) -0.0034(14) -0.0056(13) C17 0.036(2) 0.0248(19) 0.031(2) -0.0060(16) -0.0043(17) -0.0098(16) C21 0.054(3) 0.029(2) 0.063(3) -0.009(2) -0.024(3) -0.012(2) C18 0.044(2) 0.0157(17) 0.030(2) -0.0059(15) 0.0024(17) -0.0027(15) C19 0.0309(19) 0.0184(16) 0.0172(16) -0.0009(13) 0.0050(14) 0.0009(13) C22 0.041(2) 0.0208(18) 0.029(2) -0.0012(15) 0.0036(17) 0.0091(16) C20 0.0207(16) 0.0196(16) 0.0151(15) -0.0009(12) 0.0034(12) -0.0014(12) C1 0.0148(15) 0.0198(16) 0.0205(16) -0.0004(13) 0.0052(12) 0.0015(12) C7 0.0194(16) 0.0099(14) 0.0191(16) -0.0018(11) 0.0056(12) -0.0015(11) C8 0.0178(16) 0.0160(15) 0.0187(16) -0.0031(12) 0.0047(12) -0.0024(12) C9 0.0263(18) 0.0140(15) 0.0183(16) -0.0025(12) 0.0023(13) -0.0040(12) C13 0.031(2) 0.0275(19) 0.0175(17) -0.0022(14) -0.0030(14) -0.0045(15) C10 0.038(2) 0.0158(16) 0.0138(15) -0.0030(12) 0.0076(14) -0.0053(14) C11 0.034(2) 0.0121(15) 0.0233(17) -0.0023(13) 0.0146(14) -0.0020(13) C14 0.042(2) 0.0250(19) 0.0227(18) -0.0038(14) 0.0182(16) -0.0015(16) C12 0.0194(16) 0.0154(15) 0.0203(16) 0.0003(12) 0.0071(12) -0.0011(12) C3 0.0124(15) 0.0270(18) 0.0240(17) 0.0074(14) 0.0034(13) 0.0026(13) C6 0.0134(16) 0.0266(18) 0.036(2) 0.0070(15) 0.0010(14) 0.0009(13) C5 0.0216(19) 0.0234(19) 0.055(3) 0.0125(18) 0.0005(17) 0.0021(14) C4 0.041(3) 0.073(3) 0.0177(19) 0.016(2) 0.0056(17) 0.020(2) C43 0.0219(17) 0.0203(16) 0.0221(17) 0.0022(13) 0.0081(13) -0.0047(13) C42 0.031(2) 0.0234(18) 0.0227(18) 0.0069(14) 0.0060(15) -0.0053(14) C41 0.034(2) 0.034(2) 0.0242(19) 0.0153(16) -0.0003(16) -0.0030(16) C40 0.0196(17) 0.0246(17) 0.0228(17) 0.0089(14) -0.0009(13) 0.0011(13) C46 0.068(4) 0.040(3) 0.094(5) -0.013(3) 0.041(3) -0.008(3) C45 0.041(3) 0.053(3) 0.070(4) -0.007(3) 0.005(3) -0.017(2) C44 0.042(3) 0.042(3) 0.081(4) 0.003(3) 0.029(3) 0.003(2) C47 0.032(2) 0.032(2) 0.076(4) 0.002(2) 0.010(2) -0.0017(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Lu1 P1 130.12(6) . . ? O1 Lu1 C23 145.38(9) . . ? O1 Lu1 C25 97.43(9) . . ? O1 Lu1 C26 94.48(8) . . ? O1 Lu1 C27 120.98(9) . . ? O1 Lu1 C24 125.99(9) . . ? C23 Lu1 P1 84.45(7) . . ? C23 Lu1 C25 51.11(9) . . ? C23 Lu1 C26 51.46(9) . . ? C23 Lu1 C27 31.39(9) . . ? C23 Lu1 C24 31.25(9) . . ? N2 Lu1 P1 61.34(7) . . ? N2 Lu1 O1 89.79(9) . . ? N2 Lu1 C23 109.38(9) . . ? N2 Lu1 C25 146.89(9) . . ? N2 Lu1 C26 115.85(9) . . ? N2 Lu1 C27 96.40(9) . . ? N2 Lu1 C24 140.30(9) . . ? N1 Lu1 P1 60.89(7) . . ? N1 Lu1 O1 87.46(9) . . ? N1 Lu1 C23 116.46(10) . . ? N1 Lu1 N2 98.52(10) . . ? N1 Lu1 C25 114.00(10) . . ? N1 Lu1 C26 145.56(9) . . ? N1 Lu1 C27 147.85(10) . . ? N1 Lu1 C24 99.56(9) . . ? C25 Lu1 P1 129.48(7) . . ? C26 Lu1 P1 133.79(7) . . ? C26 Lu1 C25 31.63(9) . . ? C27 Lu1 P1 103.06(7) . . ? C27 Lu1 C25 52.39(9) . . ? C27 Lu1 C26 31.74(9) . . ? C27 Lu1 C24 52.77(9) . . ? C24 Lu1 P1 98.27(7) . . ? C24 Lu1 C25 31.26(9) . . ? C24 Lu1 C26 52.36(9) . . ? C2 P1 Lu1 79.59(10) . . ? C2 P1 C1 103.51(15) . . ? C2 P1 C3 105.58(16) . . ? C1 P1 Lu1 78.92(10) . . ? C1 P1 C3 107.04(15) . . ? C3 P1 Lu1 170.54(11) . . ? C43 O1 Lu1 118.69(18) . . ? C40 O1 Lu1 132.38(19) . . ? C40 O1 C43 108.9(2) . . ? C47 O2 C44 105.8(4) . . ? Lu1 C23 H23 117.1 . . ? C27 C23 Lu1 74.69(17) . . ? C27 C23 H23 124.3 . . ? C27 C23 C24 111.4(3) . . ? C24 C23 Lu1 75.60(17) . . ? C24 C23 H23 124.3 . . ? C2 N2 Lu1 113.27(19) . . ? C15 N2 Lu1 131.3(2) . . ? C15 N2 C2 115.4(3) . . ? C1 N1 Lu1 113.03(19) . . ? C7 N1 Lu1 128.1(2) . . ? C7 N1 C1 117.3(3) . . ? C26 C25 Lu1 73.68(16) . . ? C24 C25 Lu1 72.91(16) . . ? C24 C25 C26 108.2(3) . . ? C24 C25 C37 132.2(3) . . ? C37 C25 Lu1 124.4(2) . . ? C37 C25 C26 119.2(3) . . ? C25 C26 Lu1 74.69(16) . . ? C27 C26 Lu1 72.37(16) . . ? C27 C26 C25 107.4(3) . . ? C34 C26 Lu1 123.4(2) . . ? C34 C26 C25 120.1(3) . . ? C34 C26 C27 132.1(3) . . ? C23 C27 Lu1 73.92(17) . . ? C23 C27 C26 106.4(3) . . ? C23 C27 C31 124.1(3) . . ? C26 C27 Lu1 75.89(16) . . ? C26 C27 C31 128.8(3) . . ? C31 C27 Lu1 122.7(2) . . ? C27 C31 H31 108.2 . . ? C27 C31 C32 112.4(3) . . ? C27 C31 C33 110.5(3) . . ? C32 C31 H31 108.2 . . ? C32 C31 C33 109.2(3) . . ? C33 C31 H31 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C23 C24 Lu1 73.14(16) . . ? C23 C24 C25 106.5(3) . . ? C23 C24 C28 123.7(3) . . ? C25 C24 Lu1 75.82(17) . . ? C25 C24 C28 128.8(3) . . ? C28 C24 Lu1 125.3(2) . . ? C24 C28 H28 107.8 . . ? C24 C28 C29 109.6(3) . . ? C24 C28 C30 113.3(3) . . ? C29 C28 H28 107.8 . . ? C29 C28 C30 110.3(3) . . ? C30 C28 H28 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C34 C39 123.2(3) . . ? C35 C34 C26 117.3(3) . . ? C35 C34 C39 119.5(3) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C35 H35 118.8 . . ? C34 C35 C36 122.5(3) . . ? C36 C35 H35 118.8 . . ? C35 C36 H36 118.7 . . ? C37 C36 C35 122.5(3) . . ? C37 C36 H36 118.7 . . ? C25 C37 C38 122.3(3) . . ? C36 C37 C25 118.3(3) . . ? C36 C37 C38 119.3(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P1 C2 H2A 110.7 . . ? P1 C2 H2B 110.7 . . ? N2 C2 P1 105.4(2) . . ? N2 C2 H2A 110.7 . . ? N2 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N2 C15 C16 124.8(3) . . ? N2 C15 C20 119.6(3) . . ? C16 C15 C20 115.7(3) . . ? C15 C16 H16 119.0 . . ? C17 C16 C15 121.9(3) . . ? C17 C16 H16 119.0 . . ? C16 C17 C21 119.5(4) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 C21 120.3(4) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.8(3) . . ? C19 C18 H18 120.1 . . ? C18 C19 C22 120.2(3) . . ? C20 C19 C18 119.3(3) . . ? C20 C19 C22 120.5(3) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C15 C20 H20 118.5 . . ? C19 C20 C15 123.0(3) . . ? C19 C20 H20 118.5 . . ? P1 C1 H1A 111.0 . . ? P1 C1 H1B 111.0 . . ? N1 C1 P1 103.8(2) . . ? N1 C1 H1A 111.0 . . ? N1 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? N1 C7 C8 117.7(3) . . ? N1 C7 C12 125.0(3) . . ? C12 C7 C8 117.3(3) . . ? C7 C8 H8 118.8 . . ? C9 C8 C7 122.4(3) . . ? C9 C8 H8 118.8 . . ? C8 C9 C13 119.9(3) . . ? C8 C9 C10 118.7(3) . . ? C10 C9 C13 121.4(3) . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C10 C11 C14 120.8(3) . . ? C10 C11 C12 120.1(3) . . ? C12 C11 C14 119.0(3) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C12 H12 119.5 . . ? C11 C12 C7 121.0(3) . . ? C11 C12 H12 119.5 . . ? C6 C3 P1 110.8(2) . . ? C6 C3 C5 109.7(3) . . ? C6 C3 C4 110.5(3) . . ? C5 C3 P1 109.0(2) . . ? C4 C3 P1 107.7(3) . . ? C4 C3 C5 109.2(3) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C43 H43A 110.8 . . ? O1 C43 H43B 110.8 . . ? O1 C43 C42 104.5(3) . . ? H43A C43 H43B 108.9 . . ? C42 C43 H43A 110.8 . . ? C42 C43 H43B 110.8 . . ? C43 C42 H42A 111.4 . . ? C43 C42 H42B 111.4 . . ? C43 C42 C41 101.7(3) . . ? H42A C42 H42B 109.3 . . ? C41 C42 H42A 111.4 . . ? C41 C42 H42B 111.4 . . ? C42 C41 H41A 111.3 . . ? C42 C41 H41B 111.3 . . ? H41A C41 H41B 109.2 . . ? C40 C41 C42 102.3(3) . . ? C40 C41 H41A 111.3 . . ? C40 C41 H41B 111.3 . . ? O1 C40 C41 105.3(3) . . ? O1 C40 H40A 110.7 . . ? O1 C40 H40B 110.7 . . ? C41 C40 H40A 110.7 . . ? C41 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? H46A C46 H46B 109.0 . . ? C45 C46 H46A 111.0 . . ? C45 C46 H46B 111.0 . . ? C47 C46 H46A 111.0 . . ? C47 C46 H46B 111.0 . . ? C47 C46 C45 104.0(4) . . ? C46 C45 H45A 111.2 . . ? C46 C45 H45B 111.2 . . ? H45A C45 H45B 109.1 . . ? C44 C45 C46 102.8(4) . . ? C44 C45 H45A 111.2 . . ? C44 C45 H45B 111.2 . . ? O2 C44 C45 106.4(4) . . ? O2 C44 H44A 110.4 . . ? O2 C44 H44B 110.4 . . ? C45 C44 H44A 110.4 . . ? C45 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? O2 C47 C46 107.6(4) . . ? O2 C47 H47A 110.2 . . ? O2 C47 H47B 110.2 . . ? C46 C47 H47A 110.2 . . ? C46 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? 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 P1 2.8578(8) . ? Lu1 O1 2.264(2) . ? Lu1 C23 2.607(3) . ? Lu1 N2 2.225(3) . ? Lu1 N1 2.203(3) . ? Lu1 C25 2.676(3) . ? Lu1 C26 2.663(3) . ? Lu1 C27 2.616(3) . ? Lu1 C24 2.638(3) . ? P1 C2 1.850(3) . ? P1 C1 1.851(3) . ? P1 C3 1.859(3) . ? O1 C43 1.477(4) . ? O1 C40 1.462(4) . ? O2 C44 1.409(6) . ? O2 C47 1.392(6) . ? C23 H23 0.9500 . ? C23 C27 1.413(4) . ? C23 C24 1.413(4) . ? N2 C2 1.467(4) . ? N2 C15 1.371(4) . ? N1 C1 1.473(4) . ? N1 C7 1.380(4) . ? C25 C26 1.455(4) . ? C25 C24 1.432(4) . ? C25 C37 1.441(4) . ? C26 C27 1.444(4) . ? C26 C34 1.434(4) . ? C27 C31 1.524(4) . ? C31 H31 1.0000 . ? C31 C32 1.531(5) . ? C31 C33 1.532(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C24 C28 1.519(4) . ? C28 H28 1.0000 . ? C28 C29 1.531(4) . ? C28 C30 1.533(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C34 C39 1.508(5) . ? C34 C35 1.377(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C35 H35 0.9500 . ? C35 C36 1.411(5) . ? C36 H36 0.9500 . ? C36 C37 1.356(4) . ? C37 C38 1.524(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C15 C16 1.413(4) . ? C15 C20 1.414(5) . ? C16 H16 0.9500 . ? C16 C17 1.390(5) . ? C17 C21 1.512(5) . ? C17 C18 1.385(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C18 H18 0.9500 . ? C18 C19 1.399(5) . ? C19 C22 1.513(5) . ? C19 C20 1.378(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C20 H20 0.9500 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C7 C8 1.407(5) . ? C7 C12 1.407(4) . ? C8 H8 0.9500 . ? C8 C9 1.385(5) . ? C9 C13 1.508(5) . ? C9 C10 1.402(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C10 H10 0.9500 . ? C10 C11 1.384(5) . ? C11 C14 1.518(5) . ? C11 C12 1.395(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 H12 0.9500 . ? C3 C6 1.521(5) . ? C3 C5 1.531(5) . ? C3 C4 1.526(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C42 1.511(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C41 1.525(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C40 1.513(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C45 1.527(8) . ? C46 C47 1.505(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C44 1.484(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C20 H20 O1 0.95 2.55 3.213(4) 127.4 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Lu1 P1 C2 N2 -4.84(18) . . . . ? Lu1 P1 C1 N1 13.78(18) . . . . ? Lu1 O1 C43 C42 165.2(2) . . . . ? Lu1 O1 C40 C41 168.3(2) . . . . ? Lu1 C23 C27 C26 -69.6(2) . . . . ? Lu1 C23 C27 C31 118.9(3) . . . . ? Lu1 C23 C24 C25 69.1(2) . . . . ? Lu1 C23 C24 C28 -121.6(3) . . . . ? Lu1 N2 C2 P1 6.7(2) . . . . ? Lu1 N2 C15 C16 -177.2(3) . . . . ? Lu1 N2 C15 C20 2.6(4) . . . . ? Lu1 N1 C1 P1 -19.2(2) . . . . ? Lu1 N1 C7 C8 21.4(4) . . . . ? Lu1 N1 C7 C12 -156.9(2) . . . . ? Lu1 C25 C26 C27 65.5(2) . . . . ? Lu1 C25 C26 C34 -120.0(3) . . . . ? Lu1 C25 C24 C23 -67.3(2) . . . . ? Lu1 C25 C24 C28 124.2(3) . . . . ? Lu1 C25 C37 C36 89.5(3) . . . . ? Lu1 C25 C37 C38 -94.5(3) . . . . ? Lu1 C26 C27 C23 68.2(2) . . . . ? Lu1 C26 C27 C31 -120.8(3) . . . . ? Lu1 C26 C34 C39 89.8(3) . . . . ? Lu1 C26 C34 C35 -92.4(3) . . . . ? Lu1 C27 C31 C32 58.1(3) . . . . ? Lu1 C27 C31 C33 -179.6(2) . . . . ? Lu1 C24 C28 C29 -167.5(2) . . . . ? Lu1 C24 C28 C30 -43.7(3) . . . . ? O1 C43 C42 C41 35.5(4) . . . . ? C23 C27 C31 C32 -34.0(4) . . . . ? C23 C27 C31 C33 88.2(4) . . . . ? C23 C24 C28 C29 -74.9(4) . . . . ? C23 C24 C28 C30 48.8(4) . . . . ? N2 C15 C16 C17 179.8(4) . . . . ? N2 C15 C20 C19 177.8(3) . . . . ? N1 C7 C8 C9 -176.8(3) . . . . ? N1 C7 C12 C11 177.3(3) . . . . ? C25 C26 C27 Lu1 -67.0(2) . . . . ? C25 C26 C27 C23 1.1(3) . . . . ? C25 C26 C27 C31 172.1(3) . . . . ? C25 C26 C34 C39 -179.2(3) . . . . ? C25 C26 C34 C35 -1.4(4) . . . . ? C25 C24 C28 C29 91.9(4) . . . . ? C25 C24 C28 C30 -144.4(3) . . . . ? C26 C25 C24 Lu1 65.8(2) . . . . ? C26 C25 C24 C23 -1.5(3) . . . . ? C26 C25 C24 C28 -170.0(3) . . . . ? C26 C25 C37 C36 -0.1(4) . . . . ? C26 C25 C37 C38 175.9(3) . . . . ? C26 C27 C31 C32 156.4(3) . . . . ? C26 C27 C31 C33 -81.3(4) . . . . ? C26 C34 C35 C36 1.6(5) . . . . ? C27 C23 C24 Lu1 -66.8(2) . . . . ? C27 C23 C24 C25 2.3(3) . . . . ? C27 C23 C24 C28 171.6(3) . . . . ? C27 C26 C34 C39 -6.3(5) . . . . ? C27 C26 C34 C35 171.5(3) . . . . ? C24 C23 C27 Lu1 67.4(2) . . . . ? C24 C23 C27 C26 -2.2(3) . . . . ? C24 C23 C27 C31 -173.7(3) . . . . ? C24 C25 C26 Lu1 -65.3(2) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C24 C25 C26 C34 174.7(3) . . . . ? C24 C25 C37 C36 -172.5(3) . . . . ? C24 C25 C37 C38 3.6(5) . . . . ? C34 C26 C27 Lu1 119.4(3) . . . . ? C34 C26 C27 C23 -172.4(3) . . . . ? C34 C26 C27 C31 -1.5(5) . . . . ? C34 C35 C36 C37 -1.2(5) . . . . ? C39 C34 C35 C36 179.5(3) . . . . ? C35 C36 C37 C25 0.3(5) . . . . ? C35 C36 C37 C38 -175.8(3) . . . . ? C37 C25 C26 Lu1 120.7(3) . . . . ? C37 C25 C26 C27 -173.8(3) . . . . ? C37 C25 C26 C34 0.7(4) . . . . ? C37 C25 C24 Lu1 -121.3(3) . . . . ? C37 C25 C24 C23 171.5(3) . . . . ? C37 C25 C24 C28 2.9(5) . . . . ? C2 P1 C1 N1 90.1(2) . . . . ? C2 P1 C3 C6 52.0(3) . . . . ? C2 P1 C3 C5 172.8(3) . . . . ? C2 P1 C3 C4 -68.8(3) . . . . ? C2 N2 C15 C16 3.0(5) . . . . ? C2 N2 C15 C20 -177.2(3) . . . . ? C15 N2 C2 P1 -173.5(2) . . . . ? C15 C16 C17 C21 -178.1(4) . . . . ? C15 C16 C17 C18 1.7(6) . . . . ? C16 C15 C20 C19 -2.4(5) . . . . ? C16 C17 C18 C19 -1.1(6) . . . . ? C17 C18 C19 C22 177.8(4) . . . . ? C17 C18 C19 C20 -1.2(6) . . . . ? C21 C17 C18 C19 178.7(4) . . . . ? C18 C19 C20 C15 3.0(5) . . . . ? C22 C19 C20 C15 -175.9(3) . . . . ? C20 C15 C16 C17 0.0(5) . . . . ? C1 P1 C2 N2 -80.7(2) . . . . ? C1 P1 C3 C6 -57.8(3) . . . . ? C1 P1 C3 C5 63.0(3) . . . . ? C1 P1 C3 C4 -178.7(3) . . . . ? C1 N1 C7 C8 -174.2(3) . . . . ? C1 N1 C7 C12 7.5(5) . . . . ? C7 N1 C1 P1 174.1(2) . . . . ? C7 C8 C9 C13 178.9(3) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? C8 C7 C12 C11 -1.0(5) . . . . ? C8 C9 C10 C11 0.8(5) . . . . ? C9 C10 C11 C14 178.7(3) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C13 C9 C10 C11 -179.7(3) . . . . ? C10 C11 C12 C7 0.4(5) . . . . ? C14 C11 C12 C7 -178.6(3) . . . . ? C12 C7 C8 C9 1.6(5) . . . . ? C3 P1 C2 N2 167.0(2) . . . . ? C3 P1 C1 N1 -158.6(2) . . . . ? C43 O1 C40 C41 -10.0(4) . . . . ? C43 C42 C41 C40 -41.2(4) . . . . ? C42 C41 C40 O1 31.9(4) . . . . ? C40 O1 C43 C42 -16.3(3) . . . . ? C46 C45 C44 O2 29.7(6) . . . . ? C45 C46 C47 O2 -11.4(7) . . . . ? C44 O2 C47 C46 30.7(6) . . . . ? C47 O2 C44 C45 -38.4(6) . . . . ? C47 C46 C45 C44 -10.9(7) . . . . ?