#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:11:51 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293775 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572114.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_1572114 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_issue 30 _journal_name_full 'Chemical science' _journal_page_first 12138 _journal_page_last 12147 _journal_paper_doi 10.1039/d4sc02077d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C34 H55 I La N2 O3 P' _chemical_formula_sum 'C34 H55 I La N2 O3 P' _chemical_formula_weight 836.58 _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 13.352(2) _cell_length_b 14.546(3) _cell_length_c 19.171(4) _cell_measurement_reflns_used 9505 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 28.34 _cell_measurement_theta_min 2.80 _cell_volume 3723.4(12) _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 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0310 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 63378 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.373 _diffrn_reflns_theta_min 2.801 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6902 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.0646 before and 0.0574 after correction. The Ratio of minimum to maximum transmission is 0.9256. 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 1.492 _exptl_crystal_description block _exptl_crystal_F_000 1688 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 3.471 _refine_diff_density_min -2.008 _refine_diff_density_rms 0.090 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.020(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 387 _refine_ls_number_reflns 9274 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0262 _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^)+(0.0165P)^2^+8.9705P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.0619 _reflns_Friedel_coverage 0.808 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 9194 _reflns_number_total 9274 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02077d2.cif _cod_data_source_block 2ndintlai _cod_depositor_comments 'Adding full bibliography for 1572109--1572117.cif.' _cod_original_cell_volume 3723.2(12) _cod_database_code 1572114 _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 0.735 _shelx_estimated_absorpt_t_min 0.639 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.980(16) 0.020(16) 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: C24(H24A,H24B), C25(H25A,H25B), C23(H23A,H23B), C33(H33A,H33B), C1(H1A,H1B), C34(H34A,H34B), C2(H2A,H2B), C31(H31A,H31B), C32(H32A,H32B), C30(H30A,H30B), C29(H29A,H29B), C35(H35A,H35B), C26(H26A,H26B), C27(H27A,H27B) 3.b Aromatic/amide H refined with riding coordinates: C10(H10), C8(H8), C18(H18), C12(H12), C16(H16), C20(H20) 3.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C14(H14A,H14B, H14C), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C) ; _shelx_res_file ; TITL 2ndintlai_a.res in P2(1)2(1)2(1) 2ndintlai.res created by SHELXL-2018/3 at 10:12:45 on 03-Jan-2022 REM Old TITL 2ndIntLaI_a.res in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.098, Rweak 0.038, Alpha 0.008 REM 3.367 for 26 systematic absences, Orientation as input REM Flack x = 0.067 ( 0.004 ) from 3325 Parsons quotients REM Formula found by SHELXT: C32 N5 O2 P I La CELL 0.71073 13.3517 14.5457 19.1709 90 90 90 ZERR 4 0.0024 0.0027 0.0035 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 La N O P UNIT 136 220 4 4 8 12 4 L.S. 12 PLAN -24 0 0 SIZE 0.24 0.18 0.16 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 0 2 OMIT 1 1 0 OMIT 0 1 2 OMIT -1 1 1 OMIT 1 1 1 OMIT 0 2 1 OMIT 1 0 1 OMIT 0 1 1 OMIT 1 2 0 OMIT 0 2 3 REM REM REM WGHT 0.016500 8.970499 BASF 0.01997 FVAR 0.30809 LA1 4 0.350206 0.570226 0.416529 11.00000 0.01405 0.01432 = 0.01489 0.00175 -0.00347 -0.00061 I1 3 0.557564 0.625002 0.492280 11.00000 0.02864 0.02717 = 0.05177 -0.00035 -0.02388 -0.00107 P1 7 0.137077 0.579724 0.341467 11.00000 0.01350 0.02316 = 0.01422 0.00151 -0.00053 0.00233 O2 6 0.273870 0.605707 0.535588 11.00000 0.03625 0.03085 = 0.01598 -0.00169 0.00307 -0.00544 O1 6 0.457642 0.435803 0.377623 11.00000 0.02020 0.01977 = 0.02314 -0.00034 -0.00376 0.00412 O3 6 0.325333 0.745436 0.413123 11.00000 0.02897 0.01603 = 0.02217 -0.00039 -0.00480 0.00237 C13 1 0.385379 0.256604 0.596032 11.00000 0.02846 0.03313 = 0.02449 0.00501 -0.00017 0.00131 AFIX 137 H13A 2 0.351212 0.220184 0.631855 11.00000 -1.50000 H13B 2 0.400271 0.317925 0.614495 11.00000 -1.50000 H13C 2 0.447971 0.226048 0.582790 11.00000 -1.50000 AFIX 0 C3 1 0.006494 0.587734 0.306834 11.00000 0.01273 0.04204 = 0.02257 0.00239 -0.00096 0.00664 C10 1 0.268761 0.187901 0.507026 11.00000 0.02045 0.02109 = 0.02041 0.00350 0.00429 0.00129 AFIX 43 H10 2 0.276987 0.129974 0.529186 11.00000 -1.20000 AFIX 0 C17 1 0.471326 0.619747 0.129988 11.00000 0.02065 0.02188 = 0.01821 0.00404 -0.00046 0.00129 C24 1 0.518858 0.359722 0.278094 11.00000 0.02708 0.02263 = 0.03622 -0.00473 0.00558 0.00086 AFIX 23 H24A 2 0.527743 0.404271 0.239546 11.00000 -1.20000 H24B 2 0.516693 0.296808 0.258452 11.00000 -1.20000 AFIX 0 C11 1 0.318506 0.265334 0.532665 11.00000 0.01922 0.02567 = 0.01651 0.00389 0.00270 0.00206 N1 5 0.230174 0.447002 0.413996 11.00000 0.01527 0.01950 = 0.01628 0.00202 -0.00231 -0.00339 C6 1 -0.009718 0.686234 0.280937 11.00000 0.02252 0.04959 = 0.03446 0.00924 0.00473 0.01570 AFIX 137 H6A 2 0.007202 0.729620 0.318229 11.00000 -1.50000 H6B 2 -0.080007 0.694397 0.267581 11.00000 -1.50000 H6C 2 0.033280 0.697708 0.240433 11.00000 -1.50000 AFIX 0 C19 1 0.581315 0.619189 0.230088 11.00000 0.01519 0.01528 = 0.02433 -0.00061 -0.00054 -0.00042 C25 1 0.603276 0.368829 0.331828 11.00000 0.02348 0.02923 = 0.05045 -0.00800 0.00306 0.00461 AFIX 23 H25A 2 0.640557 0.310309 0.336423 11.00000 -1.20000 H25B 2 0.650660 0.418010 0.318216 11.00000 -1.20000 AFIX 0 C8 1 0.194790 0.280685 0.416225 11.00000 0.01572 0.02246 = 0.01558 -0.00215 0.00498 -0.00171 AFIX 43 H8 2 0.153236 0.284962 0.376132 11.00000 -1.20000 AFIX 0 C22 1 0.457061 0.627382 0.052454 11.00000 0.01980 0.04424 = 0.01959 0.00723 0.00050 -0.00091 AFIX 137 H22A 2 0.404570 0.672601 0.042476 11.00000 -1.50000 H22B 2 0.437372 0.567430 0.033586 11.00000 -1.50000 H22C 2 0.519939 0.647094 0.030734 11.00000 -1.50000 AFIX 0 C14 1 0.153119 0.113412 0.419901 11.00000 0.03039 0.01991 = 0.03409 -0.00336 0.00386 -0.00650 AFIX 137 H14A 2 0.177891 0.057739 0.442949 11.00000 -1.50000 H14B 2 0.165371 0.109017 0.369609 11.00000 -1.50000 H14C 2 0.081062 0.119681 0.428390 11.00000 -1.50000 AFIX 0 C23 1 0.424141 0.380520 0.319296 11.00000 0.02225 0.01967 = 0.02875 -0.00395 0.00050 0.00057 AFIX 23 H23A 2 0.375466 0.414888 0.290355 11.00000 -1.20000 H23B 2 0.392276 0.323037 0.335790 11.00000 -1.20000 AFIX 0 C18 1 0.567122 0.623847 0.157776 11.00000 0.01565 0.02064 = 0.02034 0.00333 0.00230 0.00067 AFIX 43 H18 2 0.623278 0.629830 0.127686 11.00000 -1.20000 AFIX 0 C12 1 0.305771 0.349263 0.500179 11.00000 0.01580 0.02165 = 0.02080 0.00086 -0.00085 -0.00275 AFIX 43 H12 2 0.340449 0.401331 0.517831 11.00000 -1.20000 AFIX 0 C33 1 0.291819 0.896625 0.371563 11.00000 0.03696 0.01834 = 0.03583 0.00551 0.01131 0.00592 AFIX 23 H33A 2 0.225685 0.921443 0.385374 11.00000 -1.20000 H33B 2 0.317271 0.932242 0.331286 11.00000 -1.20000 AFIX 0 C21 1 0.685305 0.625142 0.260255 11.00000 0.01535 0.03480 = 0.02990 -0.00318 -0.00133 -0.00149 AFIX 137 H21A 2 0.721830 0.568278 0.250032 11.00000 -1.50000 H21B 2 0.681000 0.633611 0.310880 11.00000 -1.50000 H21C 2 0.720728 0.677411 0.239476 11.00000 -1.50000 AFIX 0 C1 1 0.153220 0.455419 0.360808 11.00000 0.01638 0.02272 = 0.01933 0.00184 -0.00280 -0.00220 AFIX 23 H1A 2 0.089429 0.428914 0.377795 11.00000 -1.20000 H1B 2 0.173570 0.421991 0.318116 11.00000 -1.20000 AFIX 0 C9 1 0.206969 0.196108 0.448728 11.00000 0.01794 0.02005 = 0.02321 -0.00223 0.00775 -0.00334 C34 1 0.364955 0.900488 0.432076 11.00000 0.03522 0.01989 = 0.05874 -0.00377 -0.00677 -0.00465 AFIX 23 H34A 2 0.350558 0.953355 0.463015 11.00000 -1.20000 H34B 2 0.434936 0.904844 0.415332 11.00000 -1.20000 AFIX 0 C2 1 0.220852 0.593225 0.265402 11.00000 0.01274 0.02466 = 0.01612 0.00213 -0.00117 0.00240 AFIX 23 H2A 2 0.211758 0.541788 0.232184 11.00000 -1.20000 H2B 2 0.207026 0.651774 0.240895 11.00000 -1.20000 AFIX 0 C16 1 0.388579 0.610358 0.173837 11.00000 0.01370 0.02033 = 0.01872 0.00057 -0.00234 0.00147 AFIX 43 H16 2 0.323333 0.607898 0.154158 11.00000 -1.20000 AFIX 0 C31 1 0.169474 0.625318 0.541279 11.00000 0.03509 0.03550 = 0.02521 -0.00172 -0.00019 -0.00214 AFIX 23 H31A 2 0.129113 0.572447 0.524928 11.00000 -1.20000 H31B 2 0.151766 0.680003 0.513117 11.00000 -1.20000 AFIX 0 C20 1 0.499103 0.610644 0.272971 11.00000 0.01823 0.01770 = 0.01976 0.00184 -0.00020 0.00041 AFIX 43 H20 2 0.509247 0.608834 0.322000 11.00000 -1.20000 AFIX 0 C32 1 0.284407 0.796006 0.353910 11.00000 0.03647 0.01869 = 0.03013 0.00876 -0.00417 0.00082 AFIX 23 H32A 2 0.213677 0.778489 0.345939 11.00000 -1.20000 H32B 2 0.323139 0.782307 0.311120 11.00000 -1.20000 AFIX 0 C4 1 -0.014312 0.518908 0.248152 11.00000 0.01807 0.05886 = 0.02904 -0.00319 -0.00693 0.00241 AFIX 137 H4A 2 0.031157 0.530867 0.209062 11.00000 -1.50000 H4B 2 -0.083771 0.525552 0.232416 11.00000 -1.50000 H4C 2 -0.003637 0.456257 0.265423 11.00000 -1.50000 AFIX 0 C30 1 0.150462 0.643671 0.619807 11.00000 0.05344 0.04336 = 0.03292 -0.00071 0.01292 0.00495 AFIX 23 H30A 2 0.107462 0.698391 0.626598 11.00000 -1.20000 H30B 2 0.118605 0.589975 0.642493 11.00000 -1.20000 AFIX 0 C29 1 0.254692 0.659894 0.648068 11.00000 0.06853 0.05446 = 0.02641 -0.01107 -0.00056 0.01192 AFIX 23 H29A 2 0.274751 0.725018 0.642585 11.00000 -1.20000 H29B 2 0.258972 0.642838 0.697972 11.00000 -1.20000 AFIX 0 C7 1 0.242694 0.360174 0.441420 11.00000 0.01487 0.01840 = 0.01509 0.00045 0.00280 -0.00288 N2 5 0.322243 0.592971 0.293964 11.00000 0.01202 0.02269 = 0.01590 0.00224 -0.00013 -0.00019 C5 1 -0.064632 0.570068 0.368004 11.00000 0.01471 0.06489 = 0.03462 0.01162 0.00670 0.00722 AFIX 137 H5A 2 -0.057873 0.506134 0.383429 11.00000 -1.50000 H5B 2 -0.133771 0.581340 0.353126 11.00000 -1.50000 H5C 2 -0.047789 0.611418 0.406621 11.00000 -1.50000 AFIX 0 C35 1 0.346359 0.809877 0.469183 11.00000 0.03254 0.02179 = 0.02947 -0.00790 -0.00684 0.00450 AFIX 23 H35A 2 0.406160 0.790612 0.495988 11.00000 -1.20000 H35B 2 0.288633 0.814772 0.501381 11.00000 -1.20000 AFIX 0 C26 1 0.550780 0.392786 0.399278 11.00000 0.02910 0.03494 = 0.03491 -0.00106 -0.01112 0.01447 AFIX 23 H26A 2 0.537534 0.336828 0.427190 11.00000 -1.20000 H26B 2 0.591682 0.435789 0.427397 11.00000 -1.20000 AFIX 0 C27 1 0.317812 0.598822 0.604624 11.00000 0.05290 0.05577 = 0.02293 -0.00124 -0.00350 0.00411 AFIX 23 H27A 2 0.388291 0.619962 0.604335 11.00000 -1.20000 H27B 2 0.315412 0.534740 0.621942 11.00000 -1.20000 AFIX 0 C15 1 0.399990 0.604439 0.246960 11.00000 0.01533 0.01300 = 0.01729 0.00087 0.00187 0.00023 HKLF 4 REM 2ndintlai_a.res in P2(1)2(1)2(1) REM wR2 = 0.0619, GooF = S = 1.060, Restrained GooF = 1.060 for all data REM R1 = 0.0262 for 9194 Fo > 4sig(Fo) and 0.0264 for all 9274 data REM 387 parameters refined using 0 restraints END WGHT 0.0165 8.9705 REM Highest difference peak 3.471, deepest hole -2.008, 1-sigma level 0.090 Q1 1 0.5202 0.6194 0.5270 11.00000 0.05 3.47 Q2 1 0.3176 0.5887 0.4452 11.00000 0.05 0.82 Q3 1 0.9794 0.7641 0.0255 11.00000 0.05 0.78 Q4 1 0.2815 0.8797 0.4737 11.00000 0.05 0.76 Q5 1 0.5208 0.5206 0.5283 11.00000 0.05 0.67 Q6 1 0.9792 0.3816 0.1410 11.00000 0.05 0.65 Q7 1 0.5204 0.6241 0.3076 11.00000 0.05 0.56 Q8 1 0.5778 0.6662 0.4390 11.00000 0.05 0.49 Q9 1 0.5623 0.5732 0.4882 11.00000 0.05 0.44 Q10 1 0.2022 0.6278 0.6543 11.00000 0.05 0.44 Q11 1 0.3772 0.5712 0.4473 11.00000 0.05 0.40 Q12 1 0.3822 0.6708 0.6041 11.00000 0.05 0.38 Q13 1 0.3743 0.6133 0.4167 11.00000 0.05 0.38 Q14 1 0.9682 0.8634 0.0343 11.00000 0.05 0.37 Q15 1 0.3481 0.5229 0.4163 11.00000 0.05 0.36 Q16 1 0.3766 0.6196 0.5254 11.00000 0.05 0.35 Q17 1 0.3920 0.1760 0.5725 11.00000 0.05 0.34 Q18 1 0.2168 0.9370 0.4388 11.00000 0.05 0.33 Q19 1 0.3324 0.6776 0.5591 11.00000 0.05 0.33 Q20 1 0.1765 0.5200 0.3018 11.00000 0.05 0.32 Q21 1 0.5791 0.5934 0.4346 11.00000 0.05 0.32 Q22 1 0.5167 0.6186 0.4591 11.00000 0.05 0.31 Q23 1 0.1817 0.4106 0.2277 11.00000 0.05 0.31 Q24 1 0.3214 0.1923 0.6044 11.00000 0.05 0.30 ; _shelx_res_checksum 1524 _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 La1 La 0.35021(2) 0.57023(2) 0.41653(2) 0.01442(5) Uani 1 1 d . . . . . I1 I 0.55756(3) 0.62500(2) 0.49228(2) 0.03586(9) Uani 1 1 d . . . . . P1 P 0.13708(8) 0.57972(8) 0.34147(5) 0.01696(19) Uani 1 1 d . . . . . O2 O 0.2739(3) 0.6057(3) 0.53559(17) 0.0277(7) Uani 1 1 d . . . . . O1 O 0.4576(2) 0.4358(2) 0.37762(16) 0.0210(6) Uani 1 1 d . . . . . O3 O 0.3253(2) 0.7454(2) 0.41312(18) 0.0224(6) Uani 1 1 d . . . . . C13 C 0.3854(4) 0.2566(4) 0.5960(3) 0.0287(10) Uani 1 1 d . . . . . H13A H 0.351212 0.220184 0.631855 0.043 Uiso 1 1 calc GR . . . . H13B H 0.400271 0.317925 0.614495 0.043 Uiso 1 1 calc GR . . . . H13C H 0.447971 0.226048 0.582790 0.043 Uiso 1 1 calc GR . . . . C3 C 0.0065(3) 0.5877(4) 0.3068(2) 0.0258(10) Uani 1 1 d . . . . . C10 C 0.2688(3) 0.1879(3) 0.5070(2) 0.0206(8) Uani 1 1 d . . . . . H10 H 0.276987 0.129974 0.529186 0.025 Uiso 1 1 calc R . . . . C17 C 0.4713(3) 0.6197(3) 0.1300(2) 0.0202(8) Uani 1 1 d . . . . . C24 C 0.5189(4) 0.3597(3) 0.2781(3) 0.0286(10) Uani 1 1 d . . . . . H24A H 0.527743 0.404271 0.239546 0.034 Uiso 1 1 calc R . . . . H24B H 0.516693 0.296808 0.258452 0.034 Uiso 1 1 calc R . . . . C11 C 0.3185(3) 0.2653(3) 0.5327(2) 0.0205(9) Uani 1 1 d . . . . . N1 N 0.2302(2) 0.4470(2) 0.4140(2) 0.0170(6) Uani 1 1 d . . . . . C6 C -0.0097(4) 0.6862(4) 0.2809(3) 0.0355(13) Uani 1 1 d . . . . . H6A H 0.007202 0.729620 0.318229 0.053 Uiso 1 1 calc GR . . . . H6B H -0.080007 0.694397 0.267581 0.053 Uiso 1 1 calc GR . . . . H6C H 0.033280 0.697708 0.240433 0.053 Uiso 1 1 calc GR . . . . C19 C 0.5813(3) 0.6192(3) 0.2301(2) 0.0183(8) Uani 1 1 d . . . . . C25 C 0.6033(4) 0.3688(4) 0.3318(3) 0.0344(12) Uani 1 1 d . . . . . H25A H 0.640557 0.310309 0.336423 0.041 Uiso 1 1 calc R . . . . H25B H 0.650660 0.418010 0.318216 0.041 Uiso 1 1 calc R . . . . C8 C 0.1948(3) 0.2807(3) 0.4162(2) 0.0179(7) Uani 1 1 d . . . . . H8 H 0.153236 0.284962 0.376132 0.022 Uiso 1 1 calc R . . . . C22 C 0.4571(4) 0.6274(4) 0.0525(2) 0.0279(10) Uani 1 1 d . . . . . H22A H 0.404570 0.672601 0.042476 0.042 Uiso 1 1 calc GR . . . . H22B H 0.437372 0.567430 0.033586 0.042 Uiso 1 1 calc GR . . . . H22C H 0.519939 0.647094 0.030734 0.042 Uiso 1 1 calc GR . . . . C14 C 0.1531(4) 0.1134(3) 0.4199(3) 0.0281(9) Uani 1 1 d . . . . . H14A H 0.177891 0.057739 0.442949 0.042 Uiso 1 1 calc GR . . . . H14B H 0.165371 0.109017 0.369609 0.042 Uiso 1 1 calc GR . . . . H14C H 0.081062 0.119681 0.428390 0.042 Uiso 1 1 calc GR . . . . C23 C 0.4241(3) 0.3805(3) 0.3193(2) 0.0236(9) Uani 1 1 d . . . . . H23A H 0.375466 0.414888 0.290355 0.028 Uiso 1 1 calc R . . . . H23B H 0.392276 0.323037 0.335790 0.028 Uiso 1 1 calc R . . . . C18 C 0.5671(3) 0.6238(3) 0.1578(2) 0.0189(8) Uani 1 1 d . . . . . H18 H 0.623278 0.629830 0.127686 0.023 Uiso 1 1 calc R . . . . C12 C 0.3058(3) 0.3493(3) 0.5002(2) 0.0194(8) Uani 1 1 d . . . . . H12 H 0.340449 0.401331 0.517831 0.023 Uiso 1 1 calc R . . . . C33 C 0.2918(4) 0.8966(3) 0.3716(3) 0.0304(11) Uani 1 1 d . . . . . H33A H 0.225685 0.921443 0.385374 0.036 Uiso 1 1 calc R . . . . H33B H 0.317271 0.932242 0.331286 0.036 Uiso 1 1 calc R . . . . C21 C 0.6853(3) 0.6251(4) 0.2603(3) 0.0267(10) Uani 1 1 d . . . . . H21A H 0.721830 0.568278 0.250032 0.040 Uiso 1 1 calc GR . . . . H21B H 0.681000 0.633611 0.310880 0.040 Uiso 1 1 calc GR . . . . H21C H 0.720728 0.677411 0.239476 0.040 Uiso 1 1 calc GR . . . . C1 C 0.1532(3) 0.4554(3) 0.3608(2) 0.0195(8) Uani 1 1 d . . . . . H1A H 0.089429 0.428914 0.377795 0.023 Uiso 1 1 calc R . . . . H1B H 0.173570 0.421991 0.318116 0.023 Uiso 1 1 calc R . . . . C9 C 0.2070(3) 0.1961(3) 0.4487(2) 0.0204(9) Uani 1 1 d . . . . . C34 C 0.3650(4) 0.9005(3) 0.4321(3) 0.0379(13) Uani 1 1 d . . . . . H34A H 0.350558 0.953355 0.463015 0.046 Uiso 1 1 calc R . . . . H34B H 0.434936 0.904844 0.415332 0.046 Uiso 1 1 calc R . . . . C2 C 0.2209(3) 0.5932(3) 0.2654(2) 0.0178(8) Uani 1 1 d . . . . . H2A H 0.211758 0.541788 0.232184 0.021 Uiso 1 1 calc R . . . . H2B H 0.207026 0.651774 0.240895 0.021 Uiso 1 1 calc R . . . . C16 C 0.3886(3) 0.6104(3) 0.1738(2) 0.0176(8) Uani 1 1 d . . . . . H16 H 0.323333 0.607898 0.154158 0.021 Uiso 1 1 calc R . . . . C31 C 0.1695(4) 0.6253(4) 0.5413(3) 0.0319(11) Uani 1 1 d . . . . . H31A H 0.129113 0.572447 0.524928 0.038 Uiso 1 1 calc R . . . . H31B H 0.151766 0.680003 0.513117 0.038 Uiso 1 1 calc R . . . . C20 C 0.4991(3) 0.6106(3) 0.2730(2) 0.0186(8) Uani 1 1 d . . . . . H20 H 0.509247 0.608834 0.322000 0.022 Uiso 1 1 calc R . . . . C32 C 0.2844(4) 0.7960(3) 0.3539(3) 0.0284(10) Uani 1 1 d . . . . . H32A H 0.213677 0.778489 0.345939 0.034 Uiso 1 1 calc R . . . . H32B H 0.323139 0.782307 0.311120 0.034 Uiso 1 1 calc R . . . . C4 C -0.0143(4) 0.5189(4) 0.2482(3) 0.0353(12) Uani 1 1 d . . . . . H4A H 0.031157 0.530867 0.209062 0.053 Uiso 1 1 calc GR . . . . H4B H -0.083771 0.525552 0.232416 0.053 Uiso 1 1 calc GR . . . . H4C H -0.003637 0.456257 0.265423 0.053 Uiso 1 1 calc GR . . . . C30 C 0.1505(6) 0.6437(4) 0.6198(3) 0.0432(13) Uani 1 1 d . . . . . H30A H 0.107462 0.698391 0.626598 0.052 Uiso 1 1 calc R . . . . H30B H 0.118605 0.589975 0.642493 0.052 Uiso 1 1 calc R . . . . C29 C 0.2547(6) 0.6599(5) 0.6481(3) 0.0498(17) Uani 1 1 d . . . . . H29A H 0.274751 0.725018 0.642585 0.060 Uiso 1 1 calc R . . . . H29B H 0.258972 0.642838 0.697972 0.060 Uiso 1 1 calc R . . . . C7 C 0.2427(3) 0.3602(3) 0.4414(2) 0.0161(8) Uani 1 1 d . . . . . N2 N 0.3222(3) 0.5930(3) 0.29396(19) 0.0169(7) Uani 1 1 d . . . . . C5 C -0.0646(4) 0.5701(5) 0.3680(3) 0.0381(12) Uani 1 1 d . . . . . H5A H -0.057873 0.506134 0.383429 0.057 Uiso 1 1 calc GR . . . . H5B H -0.133771 0.581340 0.353126 0.057 Uiso 1 1 calc GR . . . . H5C H -0.047789 0.611418 0.406621 0.057 Uiso 1 1 calc GR . . . . C35 C 0.3464(4) 0.8099(3) 0.4692(3) 0.0279(9) Uani 1 1 d . . . . . H35A H 0.406160 0.790612 0.495988 0.034 Uiso 1 1 calc R . . . . H35B H 0.288633 0.814772 0.501381 0.034 Uiso 1 1 calc R . . . . C26 C 0.5508(4) 0.3928(4) 0.3993(3) 0.0330(11) Uani 1 1 d . . . . . H26A H 0.537534 0.336828 0.427190 0.040 Uiso 1 1 calc R . . . . H26B H 0.591682 0.435789 0.427397 0.040 Uiso 1 1 calc R . . . . C27 C 0.3178(5) 0.5988(5) 0.6046(3) 0.0439(15) Uani 1 1 d . . . . . H27A H 0.388291 0.619962 0.604335 0.053 Uiso 1 1 calc R . . . . H27B H 0.315412 0.534740 0.621942 0.053 Uiso 1 1 calc R . . . . C15 C 0.4000(3) 0.6044(3) 0.2470(2) 0.0152(7) Uani 1 1 d . . . . . 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 La1 0.01405(9) 0.01432(9) 0.01489(9) 0.00175(8) -0.00347(8) -0.00061(8) I1 0.02864(16) 0.02717(15) 0.0518(2) -0.00035(15) -0.02388(15) -0.00107(13) P1 0.0135(4) 0.0232(5) 0.0142(4) 0.0015(4) -0.0005(4) 0.0023(4) O2 0.0362(19) 0.0308(18) 0.0160(15) -0.0017(13) 0.0031(14) -0.0054(15) O1 0.0202(14) 0.0198(14) 0.0231(14) -0.0003(13) -0.0038(12) 0.0041(13) O3 0.0290(16) 0.0160(13) 0.0222(14) -0.0004(13) -0.0048(13) 0.0024(11) C13 0.028(2) 0.033(3) 0.024(2) 0.0050(19) -0.0002(18) 0.0013(19) C3 0.0127(18) 0.042(3) 0.023(2) 0.0024(19) -0.0010(16) 0.0066(18) C10 0.020(2) 0.021(2) 0.020(2) 0.0035(17) 0.0043(17) 0.0013(16) C17 0.021(2) 0.022(2) 0.0182(19) 0.0040(17) -0.0005(16) 0.0013(17) C24 0.027(2) 0.023(2) 0.036(3) -0.005(2) 0.006(2) 0.0009(18) C11 0.019(2) 0.026(2) 0.0165(18) 0.0039(16) 0.0027(15) 0.0021(16) N1 0.0153(15) 0.0195(17) 0.0163(15) 0.0020(14) -0.0023(14) -0.0034(12) C6 0.023(2) 0.050(3) 0.034(3) 0.009(2) 0.005(2) 0.016(2) C19 0.0152(19) 0.0153(18) 0.024(2) -0.0006(16) -0.0005(15) -0.0004(15) C25 0.023(2) 0.029(3) 0.050(3) -0.008(2) 0.003(2) 0.005(2) C8 0.0157(17) 0.0225(19) 0.0156(17) -0.0022(17) 0.0050(16) -0.0017(15) C22 0.020(2) 0.044(3) 0.020(2) 0.007(2) 0.0005(17) -0.001(2) C14 0.030(2) 0.0199(19) 0.034(2) -0.0034(19) 0.004(2) -0.0065(19) C23 0.022(2) 0.020(2) 0.029(2) -0.0039(18) 0.0005(17) 0.0006(17) C18 0.0156(18) 0.0206(19) 0.0203(19) 0.0033(16) 0.0023(15) 0.0007(16) C12 0.0158(18) 0.022(2) 0.021(2) 0.0009(17) -0.0008(16) -0.0028(15) C33 0.037(3) 0.018(2) 0.036(3) 0.0055(19) 0.011(2) 0.0059(19) C21 0.0153(19) 0.035(3) 0.030(2) -0.003(2) -0.0013(17) -0.0015(19) C1 0.0164(18) 0.0227(19) 0.0193(18) 0.0018(14) -0.0028(17) -0.0022(17) C9 0.018(2) 0.020(2) 0.023(2) -0.0022(16) 0.0077(17) -0.0033(16) C34 0.035(3) 0.020(2) 0.059(4) -0.004(2) -0.007(3) -0.005(2) C2 0.0127(18) 0.025(2) 0.0161(18) 0.0021(15) -0.0012(14) 0.0024(15) C16 0.0137(17) 0.020(2) 0.0187(19) 0.0006(16) -0.0023(15) 0.0015(15) C31 0.035(3) 0.036(3) 0.025(2) -0.002(2) 0.000(2) -0.002(2) C20 0.0182(19) 0.018(2) 0.0198(19) 0.0018(16) -0.0002(16) 0.0004(16) C32 0.036(3) 0.019(2) 0.030(2) 0.0088(19) -0.004(2) 0.0008(19) C4 0.018(2) 0.059(4) 0.029(3) -0.003(2) -0.0069(19) 0.002(2) C30 0.053(4) 0.043(3) 0.033(3) -0.001(2) 0.013(3) 0.005(3) C29 0.069(5) 0.054(4) 0.026(3) -0.011(3) -0.001(3) 0.012(3) C7 0.0149(18) 0.018(2) 0.0151(17) 0.0005(15) 0.0028(14) -0.0029(15) N2 0.0120(15) 0.0227(18) 0.0159(16) 0.0022(13) -0.0001(12) -0.0002(12) C5 0.015(2) 0.065(4) 0.035(3) 0.012(3) 0.0067(19) 0.007(3) C35 0.033(2) 0.022(2) 0.029(2) -0.0079(17) -0.007(2) 0.004(2) C26 0.029(2) 0.035(3) 0.035(3) -0.001(2) -0.011(2) 0.014(2) C27 0.053(4) 0.056(4) 0.023(2) -0.001(2) -0.004(2) 0.004(3) C15 0.0153(18) 0.0130(17) 0.0173(18) 0.0009(14) 0.0019(15) 0.0002(14) 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' La La -0.2871 2.4523 '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 P1 La1 I1 163.20(2) . . ? O2 La1 I1 83.70(9) . . ? O2 La1 P1 92.20(9) . . ? O2 La1 O3 76.74(11) . . ? O1 La1 I1 80.65(7) . . ? O1 La1 P1 113.88(7) . . ? O1 La1 O2 130.13(11) . . ? O1 La1 O3 146.05(11) . . ? O3 La1 I1 82.96(7) . . ? O3 La1 P1 80.24(7) . . ? N1 La1 I1 139.91(8) . . ? N1 La1 P1 55.18(9) . . ? N1 La1 O2 84.41(12) . . ? N1 La1 O1 78.26(11) . . ? N1 La1 O3 130.71(11) . . ? N2 La1 I1 122.66(8) . . ? N2 La1 P1 54.16(9) . . ? N2 La1 O2 141.70(13) . . ? N2 La1 O1 84.63(11) . . ? N2 La1 O3 79.55(12) . . ? N2 La1 N1 88.82(12) . . ? C3 P1 La1 173.93(15) . . ? C1 P1 La1 76.38(14) . . ? C1 P1 C3 103.9(2) . . ? C2 P1 La1 79.67(13) . . ? C2 P1 C3 106.1(2) . . ? C2 P1 C1 101.0(2) . . ? C31 O2 La1 119.9(3) . . ? C31 O2 C27 109.8(4) . . ? C27 O2 La1 129.8(3) . . ? C23 O1 La1 118.7(2) . . ? C23 O1 C26 104.2(3) . . ? C26 O1 La1 137.0(3) . . ? C32 O3 La1 124.6(3) . . ? C35 O3 La1 126.6(3) . . ? C35 O3 C32 108.8(3) . . ? C6 C3 P1 107.8(4) . . ? C4 C3 P1 112.9(3) . . ? C4 C3 C6 110.4(4) . . ? C5 C3 P1 107.2(3) . . ? C5 C3 C6 108.5(4) . . ? C5 C3 C4 109.9(5) . . ? C9 C10 C11 119.6(4) . . ? C18 C17 C22 119.6(4) . . ? C18 C17 C16 120.2(4) . . ? C16 C17 C22 120.2(4) . . ? C23 C24 C25 104.2(4) . . ? C10 C11 C13 119.7(4) . . ? C12 C11 C13 120.6(4) . . ? C12 C11 C10 119.7(4) . . ? C1 N1 La1 115.0(2) . . ? C7 N1 La1 126.5(3) . . ? C7 N1 C1 115.5(3) . . ? C18 C19 C21 120.1(4) . . ? C20 C19 C18 119.2(4) . . ? C20 C19 C21 120.7(4) . . ? C26 C25 C24 104.7(4) . . ? C9 C8 C7 121.4(4) . . ? O1 C23 C24 104.7(4) . . ? C17 C18 C19 120.2(4) . . ? C11 C12 C7 122.1(4) . . ? C32 C33 C34 104.5(4) . . ? N1 C1 P1 107.7(3) . . ? C10 C9 C14 120.5(4) . . ? C8 C9 C10 120.3(4) . . ? C8 C9 C14 119.1(4) . . ? C33 C34 C35 102.8(4) . . ? N2 C2 P1 105.4(3) . . ? C17 C16 C15 121.2(4) . . ? O2 C31 C30 105.6(5) . . ? C19 C20 C15 122.7(4) . . ? O3 C32 C33 106.9(4) . . ? C29 C30 C31 103.0(5) . . ? C27 C29 C30 103.2(5) . . ? N1 C7 C8 124.5(4) . . ? N1 C7 C12 118.6(4) . . ? C8 C7 C12 116.8(4) . . ? C2 N2 La1 120.7(3) . . ? C15 N2 La1 122.5(3) . . ? C15 N2 C2 116.8(3) . . ? O3 C35 C34 104.2(4) . . ? O1 C26 C25 104.6(4) . . ? O2 C27 C29 104.0(5) . . ? C16 C15 C20 116.5(4) . . ? N2 C15 C16 124.9(4) . . ? N2 C15 C20 118.6(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 La1 I1 3.2263(6) . ? La1 P1 3.1918(11) . ? La1 O2 2.552(3) . ? La1 O1 2.537(3) . ? La1 O3 2.571(3) . ? La1 N1 2.405(3) . ? La1 N2 2.402(4) . ? P1 C3 1.869(5) . ? P1 C1 1.858(4) . ? P1 C2 1.848(4) . ? O2 C31 1.427(7) . ? O2 C27 1.451(6) . ? O1 C23 1.448(5) . ? O1 C26 1.453(5) . ? O3 C32 1.459(6) . ? O3 C35 1.453(5) . ? C13 C11 1.513(6) . ? C3 C6 1.532(8) . ? C3 C4 1.531(8) . ? C3 C5 1.531(7) . ? C10 C11 1.397(6) . ? C10 C9 1.394(6) . ? C17 C22 1.503(6) . ? C17 C18 1.387(6) . ? C17 C16 1.395(6) . ? C24 C25 1.533(8) . ? C24 C23 1.521(6) . ? C11 C12 1.381(6) . ? N1 C1 1.453(5) . ? N1 C7 1.378(5) . ? C19 C18 1.401(6) . ? C19 C21 1.507(6) . ? C19 C20 1.377(6) . ? C25 C26 1.512(8) . ? C8 C9 1.389(6) . ? C8 C7 1.407(6) . ? C14 C9 1.506(6) . ? C12 C7 1.415(6) . ? C33 C34 1.517(8) . ? C33 C32 1.505(7) . ? C34 C35 1.518(7) . ? C2 N2 1.460(5) . ? C16 C15 1.413(6) . ? C31 C30 1.550(7) . ? C20 C15 1.417(6) . ? C30 C29 1.512(10) . ? C29 C27 1.481(9) . ? N2 C15 1.385(5) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.980(16) 2 0.020(16)