#------------------------------------------------------------------------------ #$Date: 2019-07-13 03:45:55 +0300 (Sat, 13 Jul 2019) $ #$Revision: 216989 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/30/7233083.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_7233083 loop_ _publ_author_name 'Yue, Zenghui' 'Lu, Huangjie' 'Li, Zijian' 'Guo, Shangyao' 'Song, Junze' 'Ren, Yi Ming' 'Huang, Yuying' 'Lin, Jian' 'Wang, Jian-Qiang' _publ_section_title ; Structural Evolution and Tuneable Photoluminescence of f-Element Bearing Coordination Polymers of the 2,4,6-tri-\a-pyridyl-1,3,5-triazine Ligand ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE00867E _journal_year 2019 _chemical_formula_moiety 'C20 H15 N10 O9 Pr' _chemical_formula_sum 'C20 H15 N10 O9 Pr' _chemical_formula_weight 680.33 _chemical_melting_point ? _chemical_name_common PrTPTZ _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-07-05 deposited with the CCDC. 2019-07-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.302(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6447(10) _cell_length_b 10.5774(8) _cell_length_c 16.4505(12) _cell_measurement_reflns_used 47228 _cell_measurement_temperature 302(2) _cell_measurement_theta_max 27.613 _cell_measurement_theta_min 2.308 _cell_volume 2479.9(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 302(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method '0.5 wide w/ exposures' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 47228 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.613 _diffrn_reflns_theta_min 2.308 _diffrn_source 'Turbo X-ray Source' _exptl_absorpt_coefficient_mu 2.037 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.530 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 314 _refine_ls_number_reflns 5727 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0551 _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^)+(0.1056P)^2^+14.7144P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1580 _refine_ls_wR_factor_ref 0.1988 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4198 _reflns_number_total 5727 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce00867e2.cif _cod_data_source_block PrTPTZ-1 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'N/A' was changed to '?' - the value is undefined or not given. '_exptl_crystal_density_meas' value 'Not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7233083 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in P2(1)/n REM Old TITL 1 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.121, Rweak 0.003, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C24 N7 O9 Pr CELL 0.71073 14.6447 10.5774 16.4505 90 103.302 90 ZERR 4 0.001 0.0008 0.0012 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Pr UNIT 80 60 40 36 4 L.S. 20 PLAN 20 TEMP 28.85 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.105600 14.714399 FVAR 0.27735 PR01 5 0.916056 0.572295 0.701558 11.00000 0.02523 0.04531 = 0.03894 0.00052 0.00438 0.00083 O1 4 0.852948 0.768311 0.762111 11.00000 0.03532 0.05234 = 0.05391 -0.00213 -0.00244 0.00474 O2 4 1.097706 0.579724 0.731724 11.00000 0.02668 0.06689 = 0.06080 0.01081 0.00945 0.00063 O3 4 0.862630 0.352359 0.646041 11.00000 0.04395 0.06273 = 0.06828 -0.00882 0.01756 -0.00433 O4 4 0.985347 0.698201 0.832951 11.00000 0.03306 0.05569 = 0.05507 -0.00670 -0.00662 0.00318 O5 4 0.977908 0.432296 0.602333 11.00000 0.05019 0.06565 = 0.06121 -0.00616 0.02477 0.00260 O6 4 1.037539 0.433620 0.792671 11.00000 0.04598 0.06163 = 0.06818 0.02196 0.01530 0.01150 O7 4 0.919582 0.854142 0.880322 11.00000 0.08621 0.05804 = 0.04988 -0.01181 0.00789 0.00450 O8 4 0.926350 0.245395 0.561572 11.00000 0.08231 0.06836 = 0.09156 -0.02870 0.02734 0.00029 O9 4 1.187577 0.461018 0.822262 11.00000 0.03927 0.15999 = 0.09385 0.03890 0.00013 0.02416 N7 3 0.918695 0.776524 0.826860 11.00000 0.04228 0.04138 = 0.04252 0.00145 0.00673 -0.00514 N9 3 0.922518 0.339533 0.602434 11.00000 0.04665 0.04779 = 0.05597 -0.00575 0.01026 0.00619 N8 3 1.109934 0.490684 0.783342 11.00000 0.02721 0.08248 = 0.05140 0.00179 0.00434 0.01035 AFIX 66 N5 3 0.814902 0.623535 0.549066 11.00000 0.02601 0.05797 = 0.03705 0.00519 0.00911 0.00205 C13 1 0.860016 0.642674 0.484411 11.00000 0.03865 0.06958 = 0.04555 0.00682 0.01271 0.00300 AFIX 43 H13 2 0.925021 0.636770 0.494559 11.00000 -1.20000 AFIX 65 C12 1 0.807973 0.670637 0.404590 11.00000 0.05061 0.08720 = 0.03435 0.00536 0.01786 0.00695 AFIX 43 H12 2 0.838158 0.683442 0.361332 11.00000 -1.20000 AFIX 65 C11 1 0.710816 0.679461 0.389422 11.00000 0.04517 0.07977 = 0.03753 0.00505 0.00576 0.00458 AFIX 43 H11 2 0.675995 0.698170 0.336015 11.00000 -1.20000 AFIX 65 C10 1 0.665701 0.660323 0.454075 11.00000 0.03899 0.05380 = 0.04432 0.00255 0.00342 0.00495 AFIX 43 H10 2 0.600696 0.666227 0.443927 11.00000 -1.20000 AFIX 65 C9 1 0.717743 0.632360 0.533898 11.00000 0.03971 0.04277 = 0.03709 -0.00029 0.00315 0.00089 AFIX 66 C14 1 0.744898 0.526726 0.820231 11.00000 0.03452 0.03905 = 0.04289 -0.00312 0.01023 -0.00695 C15 1 0.709170 0.517475 0.891309 11.00000 0.04123 0.07625 = 0.03892 0.00508 0.00824 0.00067 AFIX 43 H15 2 0.646759 0.537774 0.888634 11.00000 -1.20000 AFIX 65 C16 1 0.766722 0.477885 0.966386 11.00000 0.05376 0.09270 = 0.03318 0.00536 0.01110 0.00439 AFIX 43 H16 2 0.742817 0.471695 1.013942 11.00000 -1.20000 AFIX 65 C17 1 0.860002 0.447546 0.970386 11.00000 0.04260 0.06779 = 0.04227 0.00673 0.00072 -0.00203 AFIX 43 H17 2 0.898508 0.421057 1.020618 11.00000 -1.20000 AFIX 65 C18 1 0.895732 0.456796 0.899308 11.00000 0.04001 0.06487 = 0.04331 0.00881 0.00025 -0.00196 AFIX 43 H18 2 0.958143 0.436497 0.901984 11.00000 -1.20000 AFIX 65 N6 3 0.838181 0.496386 0.824230 11.00000 0.03155 0.04963 = 0.03814 0.00541 0.00566 -0.00557 AFIX 66 C5 1 0.449349 0.638200 0.643898 11.00000 0.03414 0.04992 = 0.04541 0.00046 0.00777 0.00060 C4 1 0.395877 0.673844 0.566100 11.00000 0.03384 0.07025 = 0.04466 0.00146 0.00478 0.00785 AFIX 43 H4 2 0.424796 0.689211 0.522318 11.00000 -1.20000 AFIX 65 C3 1 0.299182 0.686519 0.553741 11.00000 0.03235 0.07479 = 0.06741 0.00552 0.00025 0.00627 AFIX 43 H3 2 0.263406 0.710367 0.501689 11.00000 -1.20000 AFIX 65 C2 1 0.255958 0.663551 0.619178 11.00000 0.03056 0.07508 = 0.08350 -0.00316 0.01677 0.00632 AFIX 43 H2 2 0.191263 0.672032 0.610908 11.00000 -1.20000 AFIX 65 C1 1 0.309429 0.627908 0.696976 11.00000 0.03392 0.08660 = 0.08154 0.01003 0.02069 0.00820 AFIX 43 H1 2 0.280509 0.612540 0.740758 11.00000 -1.20000 AFIX 65 N1 3 0.406125 0.615232 0.709337 11.00000 0.03233 0.08233 = 0.05534 0.00984 0.01567 0.00968 AFIX 66 C8 1 0.679958 0.617112 0.600964 11.00000 0.02929 0.03951 = 0.04400 -0.00021 0.00564 0.00002 N3 3 0.584476 0.638655 0.591654 11.00000 0.02773 0.05303 = 0.03856 0.00241 0.00853 -0.00114 C6 1 0.543294 0.620958 0.658962 11.00000 0.04695 0.03877 = 0.04131 -0.00234 0.01103 -0.00354 N2 3 0.597594 0.581718 0.735582 11.00000 0.02438 0.05839 = 0.03633 0.00033 0.00355 0.00144 C7 1 0.693076 0.560174 0.744894 11.00000 0.03515 0.03842 = 0.04496 -0.00678 0.01509 -0.00716 N4 3 0.734259 0.577871 0.677586 11.00000 0.02536 0.03860 = 0.03036 0.00208 0.00317 -0.00173 AFIX 0 N10 3 0.985201 0.772688 0.643559 11.00000 0.05082 0.06501 = 0.06844 0.01264 0.01375 -0.01082 C19 1 1.025224 0.860850 0.631567 11.00000 0.03468 0.06278 = 0.05092 -0.00052 0.00537 -0.00297 C20 1 1.076196 0.969307 0.611251 11.00000 0.06741 0.09233 = 0.08150 0.02202 0.00173 -0.03218 AFIX 137 H20A 2 1.050312 0.994336 0.554532 11.00000 -1.20000 H20B 2 1.141096 0.947456 0.617703 11.00000 -1.20000 H20C 2 1.070948 1.037982 0.648058 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1_a.res in P2(1)/n REM R1 = 0.0551 for 4198 Fo > 4sig(Fo) and 0.0875 for all 5727 data REM 314 parameters refined using 0 restraints END WGHT 0.0609 14.8902 REM Highest difference peak 1.530, deepest hole -1.424, 1-sigma level 0.162 Q1 1 0.7475 0.4289 1.1018 11.00000 0.05 1.53 Q2 1 0.5653 0.6129 0.6584 11.00000 0.05 1.51 Q3 1 0.9186 0.4655 0.7193 11.00000 0.05 1.48 Q4 1 0.9197 0.5795 0.7616 11.00000 0.05 1.48 Q5 1 0.9187 0.6709 0.7109 11.00000 0.05 1.47 Q6 1 0.9144 0.5741 0.6403 11.00000 0.05 1.26 Q7 1 0.9058 0.4654 0.6608 11.00000 0.05 1.25 Q8 1 0.6709 0.6052 0.6212 11.00000 0.05 1.14 Q9 1 0.9159 0.2852 0.7024 11.00000 0.05 0.99 Q10 1 0.9353 0.5714 0.8007 11.00000 0.05 0.90 Q11 1 0.8369 0.6387 0.4896 11.00000 0.05 0.82 Q12 1 0.4344 0.6256 0.6588 11.00000 0.05 0.80 Q13 1 0.9248 0.3409 0.7467 11.00000 0.05 0.80 Q14 1 0.9150 0.3428 0.6649 11.00000 0.05 0.79 Q15 1 0.3262 0.6181 0.6824 11.00000 0.05 0.77 Q16 1 0.5766 0.7186 0.7587 11.00000 0.05 0.74 Q17 1 0.8732 0.4624 0.8870 11.00000 0.05 0.74 Q18 1 0.9344 0.6861 0.7729 11.00000 0.05 0.74 Q19 1 0.7643 0.5138 0.8332 11.00000 0.05 0.68 Q20 1 0.6038 0.5666 0.7199 11.00000 0.05 0.63 ; _shelx_res_checksum 71831 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Pr01 Pr 0.91606(2) 0.57230(4) 0.70156(2) 0.03698(17) Uani 1 1 d . . O1 O 0.8529(4) 0.7683(6) 0.7621(4) 0.0492(13) Uani 1 1 d . . O2 O 1.0977(4) 0.5797(6) 0.7317(4) 0.0516(14) Uani 1 1 d . . O3 O 0.8626(4) 0.3524(6) 0.6460(4) 0.0576(15) Uani 1 1 d . . O4 O 0.9853(4) 0.6982(6) 0.8330(4) 0.0507(14) Uani 1 1 d . . O5 O 0.9779(5) 0.4323(6) 0.6023(4) 0.0571(16) Uani 1 1 d . . O6 O 1.0375(5) 0.4336(6) 0.7927(4) 0.0582(16) Uani 1 1 d . . O7 O 0.9196(5) 0.8541(7) 0.8803(4) 0.0660(18) Uani 1 1 d . . O8 O 0.9263(6) 0.2454(7) 0.5616(5) 0.080(2) Uani 1 1 d . . O9 O 1.1876(5) 0.4610(11) 0.8223(6) 0.100(3) Uani 1 1 d . . N7 N 0.9187(5) 0.7765(6) 0.8269(4) 0.0426(14) Uani 1 1 d . . N9 N 0.9225(5) 0.3395(7) 0.6024(5) 0.0504(16) Uani 1 1 d . . N8 N 1.1099(5) 0.4907(9) 0.7833(5) 0.0545(18) Uani 1 1 d . . N5 N 0.8149(3) 0.6235(5) 0.5491(2) 0.0400(14) Uani 1 1 d G . C13 C 0.8600(2) 0.6427(6) 0.4844(3) 0.051(2) Uani 1 1 d G . H13 H 0.9250 0.6368 0.4946 0.061 Uiso 1 1 calc R U C12 C 0.8080(3) 0.6706(7) 0.4046(2) 0.056(2) Uani 1 1 d G . H12 H 0.8382 0.6834 0.3613 0.067 Uiso 1 1 calc R U C11 C 0.7108(3) 0.6795(6) 0.3894(2) 0.055(2) Uani 1 1 d G . H11 H 0.6760 0.6982 0.3360 0.066 Uiso 1 1 calc R U C10 C 0.6657(2) 0.6603(6) 0.4541(3) 0.0467(18) Uani 1 1 d G . H10 H 0.6007 0.6662 0.4439 0.056 Uiso 1 1 calc R U C9 C 0.7177(3) 0.6324(5) 0.5339(2) 0.0408(16) Uani 1 1 d G . C14 C 0.7449(3) 0.5267(5) 0.8202(2) 0.0386(15) Uani 1 1 d G . C15 C 0.7092(3) 0.5175(6) 0.8913(3) 0.052(2) Uani 1 1 d G . H15 H 0.6468 0.5378 0.8886 0.063 Uiso 1 1 calc R U C16 C 0.7667(4) 0.4779(7) 0.9664(2) 0.060(2) Uani 1 1 d G . H16 H 0.7428 0.4717 1.0139 0.072 Uiso 1 1 calc R U C17 C 0.8600(3) 0.4475(6) 0.9704(2) 0.052(2) Uani 1 1 d G . H17 H 0.8985 0.4211 1.0206 0.063 Uiso 1 1 calc R U C18 C 0.8957(2) 0.4568(6) 0.8993(3) 0.051(2) Uani 1 1 d G . H18 H 0.9581 0.4365 0.9020 0.061 Uiso 1 1 calc R U N6 N 0.8382(3) 0.4964(5) 0.8242(2) 0.0402(14) Uani 1 1 d G . C5 C 0.4493(2) 0.6382(6) 0.6439(3) 0.0434(17) Uani 1 1 d G . C4 C 0.3959(3) 0.6738(6) 0.5661(3) 0.050(2) Uani 1 1 d G . H4 H 0.4248 0.6892 0.5223 0.060 Uiso 1 1 calc R U C3 C 0.2992(3) 0.6865(6) 0.5537(3) 0.060(2) Uani 1 1 d G . H3 H 0.2634 0.7104 0.5017 0.072 Uiso 1 1 calc R U C2 C 0.2560(2) 0.6636(7) 0.6192(4) 0.062(2) Uani 1 1 d G . H2 H 0.1913 0.6720 0.6109 0.075 Uiso 1 1 calc R U C1 C 0.3094(3) 0.6279(7) 0.6970(3) 0.066(3) Uani 1 1 d G . H1 H 0.2805 0.6125 0.7408 0.079 Uiso 1 1 calc R U N1 N 0.4061(3) 0.6152(6) 0.7093(3) 0.0558(19) Uani 1 1 d G . C8 C 0.6800(3) 0.6171(4) 0.6010(2) 0.0381(15) Uani 1 1 d G . N3 N 0.5845(2) 0.6387(5) 0.5917(2) 0.0396(14) Uani 1 1 d G . C6 C 0.5433(2) 0.6210(5) 0.6590(2) 0.0422(16) Uani 1 1 d G . N2 N 0.5976(3) 0.5817(5) 0.7356(2) 0.0403(14) Uani 1 1 d G . C7 C 0.6931(3) 0.5602(4) 0.74489(19) 0.0386(16) Uani 1 1 d G . N4 N 0.73426(19) 0.5779(4) 0.6776(2) 0.0320(12) Uani 1 1 d G . N10 N 0.9852(6) 0.7727(8) 0.6436(5) 0.061(2) Uani 1 1 d . . C19 C 1.0252(6) 0.8608(9) 0.6316(5) 0.0502(19) Uani 1 1 d . . C20 C 1.0762(8) 0.9693(13) 0.6113(8) 0.083(4) Uani 1 1 d . . H20A H 1.0503 0.9943 0.5545 0.099 Uiso 1 1 calc R U H20B H 1.1411 0.9475 0.6177 0.099 Uiso 1 1 calc R U H20C H 1.0709 1.0380 0.6481 0.099 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr01 0.0252(2) 0.0453(3) 0.0389(2) 0.00052(17) 0.00438(15) 0.00083(16) O1 0.035(3) 0.052(3) 0.054(3) -0.002(3) -0.002(2) 0.005(2) O2 0.027(3) 0.067(4) 0.061(4) 0.011(3) 0.009(2) 0.001(2) O3 0.044(3) 0.063(4) 0.068(4) -0.009(3) 0.018(3) -0.004(3) O4 0.033(3) 0.056(3) 0.055(3) -0.007(3) -0.007(2) 0.003(2) O5 0.050(4) 0.066(4) 0.061(4) -0.006(3) 0.025(3) 0.003(3) O6 0.046(4) 0.062(4) 0.068(4) 0.022(3) 0.015(3) 0.012(3) O7 0.086(5) 0.058(4) 0.050(3) -0.012(3) 0.008(3) 0.004(4) O8 0.082(5) 0.068(5) 0.092(5) -0.029(4) 0.027(4) 0.000(4) O9 0.039(4) 0.160(9) 0.094(6) 0.039(6) 0.000(4) 0.024(5) N7 0.042(3) 0.041(3) 0.043(3) 0.001(3) 0.007(3) -0.005(3) N9 0.047(4) 0.048(4) 0.056(4) -0.006(3) 0.010(3) 0.006(3) N8 0.027(3) 0.082(6) 0.051(4) 0.002(4) 0.004(3) 0.010(3) N5 0.026(3) 0.058(4) 0.037(3) 0.005(3) 0.009(2) 0.002(3) C13 0.039(4) 0.070(6) 0.046(4) 0.007(4) 0.013(3) 0.003(4) C12 0.051(5) 0.087(7) 0.034(4) 0.005(4) 0.018(3) 0.007(4) C11 0.045(4) 0.080(6) 0.038(4) 0.005(4) 0.006(3) 0.005(4) C10 0.039(4) 0.054(5) 0.044(4) 0.003(4) 0.003(3) 0.005(3) C9 0.040(4) 0.043(4) 0.037(4) 0.000(3) 0.003(3) 0.001(3) C14 0.035(4) 0.039(4) 0.043(4) -0.003(3) 0.010(3) -0.007(3) C15 0.041(4) 0.076(6) 0.039(4) 0.005(4) 0.008(3) 0.001(4) C16 0.054(5) 0.093(7) 0.033(4) 0.005(4) 0.011(4) 0.004(5) C17 0.043(4) 0.068(6) 0.042(4) 0.007(4) 0.001(3) -0.002(4) C18 0.040(4) 0.065(6) 0.043(4) 0.009(4) 0.000(3) -0.002(4) N6 0.032(3) 0.050(4) 0.038(3) 0.005(3) 0.006(2) -0.006(3) C5 0.034(4) 0.050(4) 0.045(4) 0.000(3) 0.008(3) 0.001(3) C4 0.034(4) 0.070(6) 0.045(4) 0.001(4) 0.005(3) 0.008(4) C3 0.032(4) 0.075(6) 0.067(6) 0.006(5) 0.000(4) 0.006(4) C2 0.031(4) 0.075(6) 0.084(7) -0.003(5) 0.017(4) 0.006(4) C1 0.034(4) 0.087(7) 0.082(7) 0.010(6) 0.021(4) 0.008(5) N1 0.032(4) 0.082(6) 0.055(4) 0.010(4) 0.016(3) 0.010(3) C8 0.029(3) 0.040(4) 0.044(4) 0.000(3) 0.006(3) 0.000(3) N3 0.028(3) 0.053(4) 0.039(3) 0.002(3) 0.009(2) -0.001(3) C6 0.047(4) 0.039(4) 0.041(4) -0.002(3) 0.011(3) -0.004(3) N2 0.024(3) 0.058(4) 0.036(3) 0.000(3) 0.004(2) 0.001(3) C7 0.035(4) 0.038(4) 0.045(4) -0.007(3) 0.015(3) -0.007(3) N4 0.025(3) 0.039(3) 0.030(3) 0.002(2) 0.003(2) -0.002(2) N10 0.051(4) 0.065(5) 0.068(5) 0.013(4) 0.014(4) -0.011(4) C19 0.035(4) 0.063(5) 0.051(5) -0.001(4) 0.005(3) -0.003(4) C20 0.067(7) 0.092(8) 0.081(8) 0.022(7) 0.002(6) -0.032(6) 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' 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' Pr Pr -0.2180 2.8214 '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 O6 Pr01 O5 74.5(2) O6 Pr01 O4 73.1(2) O5 Pr01 O4 136.5(2) O6 Pr01 O3 78.4(2) O5 Pr01 O3 50.2(2) O4 Pr01 O3 144.1(2) O6 Pr01 O1 120.6(2) O5 Pr01 O1 160.4(2) O4 Pr01 O1 49.84(17) O3 Pr01 O1 140.11(19) O6 Pr01 O2 49.5(2) O5 Pr01 O2 68.7(2) O4 Pr01 O2 68.3(2) O3 Pr01 O2 108.2(2) O1 Pr01 O2 110.30(19) O6 Pr01 N4 131.46(18) O5 Pr01 N4 115.01(18) O4 Pr01 N4 108.14(16) O3 Pr01 N4 75.40(17) O1 Pr01 N4 65.95(16) O2 Pr01 N4 176.22(18) O6 Pr01 N10 114.1(2) O5 Pr01 N10 90.7(2) O4 Pr01 N10 76.9(2) O3 Pr01 N10 135.9(2) O1 Pr01 N10 72.0(3) O2 Pr01 N10 65.2(2) N4 Pr01 N10 113.2(2) O6 Pr01 N5 147.6(2) O5 Pr01 N5 73.39(19) O4 Pr01 N5 136.21(18) O3 Pr01 N5 77.88(19) O1 Pr01 N5 91.68(17) O2 Pr01 N5 119.92(16) N4 Pr01 N5 61.56(12) N10 Pr01 N5 70.7(2) O6 Pr01 N6 74.93(18) O5 Pr01 N6 126.47(18) O4 Pr01 N6 70.74(18) O3 Pr01 N6 81.19(18) O1 Pr01 N6 72.15(18) O2 Pr01 N6 117.65(17) N4 Pr01 N6 61.27(12) N10 Pr01 N6 142.1(2) N5 Pr01 N6 122.29(13) O6 Pr01 N9 74.7(2) O5 Pr01 N9 25.2(2) O4 Pr01 N9 147.66(19) O3 Pr01 N9 25.02(19) O1 Pr01 N9 160.90(18) O2 Pr01 N9 88.2(2) N4 Pr01 N9 95.54(17) N10 Pr01 N9 114.0(3) N5 Pr01 N9 74.45(19) N6 Pr01 N9 103.88(19) O6 Pr01 N7 96.6(2) O5 Pr01 N7 157.5(2) O4 Pr01 N7 24.94(17) O3 Pr01 N7 149.47(19) O1 Pr01 N7 24.93(17) O2 Pr01 N7 89.78(19) N4 Pr01 N7 86.47(16) N10 Pr01 N7 73.8(2) N5 Pr01 N7 114.87(17) N6 Pr01 N7 68.51(16) N9 Pr01 N7 170.02(19) N7 O1 Pr01 96.3(4) N8 O2 Pr01 95.0(4) N9 O3 Pr01 96.0(5) N7 O4 Pr01 97.2(4) N9 O5 Pr01 97.3(5) N8 O6 Pr01 98.5(5) O7 N7 O4 120.7(7) O7 N7 O1 122.8(7) O4 N7 O1 116.5(6) O7 N7 Pr01 176.7(6) O4 N7 Pr01 57.8(4) O1 N7 Pr01 58.7(4) O8 N9 O3 122.1(8) O8 N9 O5 121.5(8) O3 N9 O5 116.4(7) O8 N9 Pr01 179.0(7) O3 N9 Pr01 58.9(4) O5 N9 Pr01 57.5(4) O9 N8 O2 121.6(8) O9 N8 O6 121.7(9) O2 N8 O6 116.7(6) O9 N8 Pr01 175.0(7) O2 N8 Pr01 60.2(4) O6 N8 Pr01 56.8(4) C13 N5 C9 120.0 C13 N5 Pr01 119.5(2) C9 N5 Pr01 120.5(2) C12 C13 N5 120.0 C12 C13 H13 120.0 N5 C13 H13 120.0 C13 C12 C11 120.0 C13 C12 H12 120.0 C11 C12 H12 120.0 C12 C11 C10 120.0 C12 C11 H11 120.0 C10 C11 H11 120.0 C9 C10 C11 120.0 C9 C10 H10 120.0 C11 C10 H10 120.0 C8 C9 C10 123.9(3) C8 C9 N5 116.1(3) C10 C9 N5 120.0 C7 C14 C15 123.5(3) C7 C14 N6 116.4(3) C15 C14 N6 120.0 C16 C15 C14 120.0 C16 C15 H15 120.0 C14 C15 H15 120.0 C17 C16 C15 120.0 C17 C16 H16 120.0 C15 C16 H16 120.0 C16 C17 C18 120.0 C16 C17 H17 120.0 C18 C17 H17 120.0 N6 C18 C17 120.0 N6 C18 H18 120.0 C17 C18 H18 120.0 C18 N6 C14 120.0 C18 N6 Pr01 119.1(2) C14 N6 Pr01 118.9(2) C6 C5 C4 122.6(4) C6 C5 N1 117.4(4) C4 C5 N1 120.0 C3 C4 C5 120.0 C3 C4 H4 120.0 C5 C4 H4 120.0 C4 C3 C2 120.0 C4 C3 H3 120.0 C2 C3 H3 120.0 C1 C2 C3 120.0 C1 C2 H2 120.0 C3 C2 H2 120.0 C2 C1 N1 120.0 C2 C1 H1 120.0 N1 C1 H1 120.0 C1 N1 C5 120.0 C9 C8 N3 118.7(3) C9 C8 N4 121.3(3) N3 C8 N4 120.0 C8 N3 C6 120.0 C5 C6 N2 123.5(3) C5 C6 N3 116.4(3) N2 C6 N3 120.0 C7 N2 C6 120.0 C14 C7 N2 119.0(3) C14 C7 N4 120.9(3) N2 C7 N4 120.0 C7 N4 C8 120.0 C7 N4 Pr01 119.53(18) C8 N4 Pr01 119.76(18) C19 N10 Pr01 168.3(7) N10 C19 C20 176.4(11) C19 C20 H20A 109.5 C19 C20 H20B 109.5 H20A C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pr01 O6 2.517(6) Pr01 O5 2.522(6) Pr01 O4 2.543(6) Pr01 O3 2.555(7) Pr01 O1 2.563(6) Pr01 O2 2.593(5) Pr01 N4 2.601(3) Pr01 N10 2.622(8) Pr01 N5 2.659(3) Pr01 N6 2.660(3) Pr01 N9 2.967(7) Pr01 N7 2.980(7) O1 N7 1.264(8) O2 N8 1.253(10) O3 N9 1.262(9) O4 N7 1.267(9) O5 N9 1.273(9) O6 N8 1.260(10) O7 N7 1.201(9) O8 N9 1.210(9) O9 N8 1.211(9) N5 C13 1.3900 N5 C9 1.3900 C13 C12 1.3900 C13 H13 0.9300 C12 C11 1.3900 C12 H12 0.9300 C11 C10 1.3900 C11 H11 0.9300 C10 C9 1.3900 C10 H10 0.9300 C9 C8 1.353(4) C14 C7 1.343(4) C14 C15 1.3900 C14 N6 1.3900 C15 C16 1.3900 C15 H15 0.9300 C16 C17 1.3900 C16 H16 0.9300 C17 C18 1.3900 C17 H17 0.9300 C18 N6 1.3900 C18 H18 0.9300 C5 C6 1.353(4) C5 C4 1.3900 C5 N1 1.3900 C4 C3 1.3900 C4 H4 0.9300 C3 C2 1.3900 C3 H3 0.9300 C2 C1 1.3900 C2 H2 0.9300 C1 N1 1.3900 C1 H1 0.9300 C8 N3 1.3900 C8 N4 1.3900 N3 C6 1.3900 C6 N2 1.3900 N2 C7 1.3900 C7 N4 1.3900 N10 C19 1.142(12) C19 C20 1.449(14) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600