#------------------------------------------------------------------------------ #$Date: 2019-07-13 03:45:55 +0300 (Sat, 13 Jul 2019) $ #$Revision: 216989 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/30/7233084.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_7233084 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 Nd O9' _chemical_formula_sum 'C20 H15 N10 Nd O9' _chemical_formula_weight 683.66 _chemical_melting_point ? _chemical_name_common NdTPTZ _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 103.2810(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6200(7) _cell_length_b 10.5736(5) _cell_length_c 16.4263(7) _cell_measurement_reflns_used 39956 _cell_measurement_temperature 302(2) _cell_measurement_theta_max 27.506 _cell_measurement_theta_min 2.558 _cell_volume 2471.4(2) _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 0.996 _diffrn_measured_fraction_theta_max 0.996 _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 0.0388 _diffrn_reflns_av_unetI/netI 0.0243 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 39956 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.506 _diffrn_reflns_theta_min 2.558 _diffrn_source 'Turbo X-ray Source' _exptl_absorpt_coefficient_mu 2.173 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SHELTXPREP _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1348 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.606 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.108 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 314 _refine_ls_number_reflns 5672 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0410 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+11.1716P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.0974 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4916 _reflns_number_total 5672 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce00867e2.cif _cod_data_source_block NdTPTZ-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 7233084 _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 0.087, Rweak 0.003, Alpha 0.062, Orientation as input REM Formula found by SHELXT: C23 N7 O9 Nd CELL 0.71073 14.62 10.5736 16.4263 90 103.281 90 ZERR 4 0.0007 0.0005 0.0007 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Nd 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 0.026900 11.171600 FVAR 0.38993 ND01 5 0.915319 0.571693 0.701497 11.00000 0.02129 0.03699 = 0.03196 0.00085 0.00457 0.00048 O1 4 0.852667 0.767928 0.761454 11.00000 0.03678 0.04454 = 0.04404 -0.00279 -0.00041 0.00232 O2 4 1.096804 0.579336 0.731421 11.00000 0.02918 0.06229 = 0.05778 0.01100 0.00763 0.00033 O3 4 0.861549 0.353401 0.646508 11.00000 0.03928 0.05238 = 0.06105 -0.00720 0.01901 -0.00531 O4 4 0.985459 0.696366 0.831600 11.00000 0.03450 0.04902 = 0.04899 -0.00593 -0.00295 0.00306 O5 4 0.977007 0.432484 0.602015 11.00000 0.04244 0.05329 = 0.06066 -0.00556 0.02269 -0.00049 O6 4 1.035631 0.431345 0.791290 11.00000 0.03871 0.05762 = 0.06167 0.01937 0.01480 0.01080 O7 4 0.919843 0.853872 0.879685 11.00000 0.08206 0.05118 = 0.04158 -0.01139 0.00502 0.00698 O8 4 0.926397 0.244806 0.562115 11.00000 0.07453 0.06081 = 0.07980 -0.02790 0.02389 0.00364 O9 4 1.186229 0.459350 0.821533 11.00000 0.03352 0.14294 = 0.08746 0.04176 -0.00042 0.02463 N7 3 0.919569 0.775201 0.826228 11.00000 0.04037 0.03791 = 0.03477 0.00070 0.00702 -0.00533 N9 3 0.921823 0.339930 0.602826 11.00000 0.03828 0.05230 = 0.04599 -0.00799 0.00729 0.00651 N8 3 1.108639 0.489525 0.782293 11.00000 0.03219 0.06887 = 0.04641 0.00611 0.00679 0.01324 AFIX 66 N5 3 0.815819 0.623267 0.549497 11.00000 0.02703 0.05196 = 0.03093 0.00411 0.00932 0.00291 C13 1 0.861443 0.642560 0.485040 11.00000 0.03702 0.06940 = 0.03893 0.00338 0.01221 -0.00081 AFIX 43 H13 2 0.926565 0.636565 0.495456 11.00000 -1.20000 AFIX 65 C12 1 0.809737 0.670815 0.405015 11.00000 0.04584 0.07416 = 0.03339 0.00645 0.01575 0.00560 AFIX 43 H12 2 0.840263 0.683723 0.361889 11.00000 -1.20000 AFIX 65 C11 1 0.712405 0.679776 0.389447 11.00000 0.04823 0.06478 = 0.03282 0.00750 0.00592 0.00752 AFIX 43 H11 2 0.677810 0.698680 0.335905 11.00000 -1.20000 AFIX 65 C10 1 0.666779 0.660484 0.453904 11.00000 0.03344 0.04844 = 0.03889 0.00300 0.00466 0.00638 AFIX 43 H10 2 0.601658 0.666480 0.443488 11.00000 -1.20000 AFIX 65 C9 1 0.718485 0.632229 0.533929 11.00000 0.02860 0.03606 = 0.03289 0.00120 0.00423 0.00321 AFIX 66 C14 1 0.745294 0.526062 0.820389 11.00000 0.03056 0.03793 = 0.03426 -0.00319 0.00791 -0.00319 C15 1 0.709625 0.516512 0.891633 11.00000 0.03615 0.06733 = 0.03620 0.00274 0.01028 0.00072 AFIX 43 H15 2 0.647073 0.536501 0.889034 11.00000 -1.20000 AFIX 65 C16 1 0.767448 0.477084 0.966762 11.00000 0.04843 0.07963 = 0.03211 0.00470 0.01362 0.00097 AFIX 43 H16 2 0.743583 0.470694 1.014429 11.00000 -1.20000 AFIX 65 C17 1 0.860940 0.447208 0.970647 11.00000 0.04184 0.05896 = 0.03296 0.00706 0.00110 -0.00442 AFIX 43 H17 2 0.899627 0.420828 1.020913 11.00000 -1.20000 AFIX 65 C18 1 0.896610 0.456758 0.899403 11.00000 0.03549 0.05048 = 0.04038 0.00774 0.00294 -0.00021 AFIX 43 H18 2 0.959163 0.436768 0.902003 11.00000 -1.20000 AFIX 65 N6 3 0.838788 0.496185 0.824274 11.00000 0.02599 0.04299 = 0.03304 0.00445 0.00223 -0.00081 AFIX 66 C5 1 0.449154 0.637522 0.643511 11.00000 0.02640 0.04192 = 0.04367 -0.00159 0.00726 -0.00101 C4 1 0.395958 0.673805 0.565614 11.00000 0.02921 0.06564 = 0.04232 0.00080 0.00511 0.00629 AFIX 43 H4 2 0.425169 0.689392 0.521944 11.00000 -1.20000 AFIX 65 C3 1 0.299102 0.686791 0.552989 11.00000 0.03070 0.06735 = 0.05550 0.00083 -0.00065 0.00862 AFIX 43 H3 2 0.263510 0.711067 0.500870 11.00000 -1.20000 AFIX 65 C2 1 0.255442 0.663494 0.618259 11.00000 0.02523 0.06427 = 0.07399 0.00199 0.00896 0.00507 AFIX 43 H2 2 0.190638 0.672183 0.609812 11.00000 -1.20000 AFIX 65 C1 1 0.308637 0.627211 0.696157 11.00000 0.03647 0.07698 = 0.07076 0.00752 0.02177 0.00560 AFIX 43 H1 2 0.279425 0.611624 0.739827 11.00000 -1.20000 AFIX 65 N1 3 0.405493 0.614224 0.708784 11.00000 0.02984 0.06868 = 0.05148 0.00727 0.01501 0.00447 AFIX 66 C8 1 0.680400 0.616038 0.600738 11.00000 0.02589 0.03336 = 0.03987 -0.00028 0.00121 -0.00031 N3 3 0.584777 0.637886 0.591270 11.00000 0.02622 0.04253 = 0.03826 0.00371 0.00692 0.00040 C6 1 0.543402 0.620933 0.658685 11.00000 0.03647 0.03665 = 0.03532 -0.00061 0.00833 -0.00161 N2 3 0.597650 0.582131 0.735568 11.00000 0.02307 0.04680 = 0.03397 0.00045 0.00494 0.00130 C7 1 0.693273 0.560282 0.745037 11.00000 0.02922 0.03451 = 0.03788 -0.00823 0.01105 -0.00683 N4 3 0.734649 0.577235 0.677623 11.00000 0.02393 0.03843 = 0.02705 0.00144 0.00365 -0.00198 AFIX 0 N10 3 0.985165 0.773235 0.644223 11.00000 0.04554 0.05599 = 0.06095 0.01168 0.01278 -0.00560 C19 1 1.025489 0.858798 0.631346 11.00000 0.03485 0.05740 = 0.04584 0.00377 0.00537 -0.00201 C20 1 1.077045 0.967648 0.613056 11.00000 0.06442 0.08072 = 0.06818 0.00848 0.00993 -0.02674 AFIX 137 H20A 2 1.058575 0.986383 0.554378 11.00000 -1.20000 H20B 2 1.143185 0.949884 0.628109 11.00000 -1.20000 H20C 2 1.063633 1.039010 0.644527 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1_a.res in P2(1)/n REM R1 = 0.0410 for 4916 Fo > 4sig(Fo) and 0.0501 for all 5672 data REM 314 parameters refined using 0 restraints END WGHT 0.0269 11.1711 REM Highest difference peak 1.606, deepest hole -1.392, 1-sigma level 0.108 Q1 1 0.5629 0.6057 0.6585 11.00000 0.05 1.40 Q2 1 0.6599 0.6040 0.6105 11.00000 0.05 1.35 Q3 1 0.8763 0.4575 0.8842 11.00000 0.05 0.99 Q4 1 0.7392 0.6355 0.5285 11.00000 0.05 0.97 Q5 1 0.8418 0.6375 0.4953 11.00000 0.05 0.97 Q6 1 0.7641 0.5095 0.8274 11.00000 0.05 0.93 Q7 1 0.3246 0.6337 0.6846 11.00000 0.05 0.92 Q8 1 0.4332 0.6335 0.6582 11.00000 0.05 0.92 Q9 1 0.6020 0.6268 0.6100 11.00000 0.05 0.64 Q10 1 0.7137 0.5798 0.6792 11.00000 0.05 0.42 Q11 1 0.7812 0.6731 0.4107 11.00000 0.05 0.39 Q12 1 0.8603 0.5409 0.8398 11.00000 0.05 0.39 Q13 1 0.3987 0.6724 0.5948 11.00000 0.05 0.38 Q14 1 0.4377 0.6602 0.7149 11.00000 0.05 0.36 Q15 1 0.8223 0.4494 0.9618 11.00000 0.05 0.36 Q16 1 0.6069 0.5811 0.7143 11.00000 0.05 0.34 Q17 1 0.7244 0.4849 0.9060 11.00000 0.05 0.33 Q18 1 0.8403 0.6217 0.5999 11.00000 0.05 0.33 Q19 1 0.3655 0.6949 0.5637 11.00000 0.05 0.30 Q20 1 0.9205 0.3634 0.8717 11.00000 0.05 0.30 ; _shelx_res_checksum 60903 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 Nd01 Nd 0.91532(2) 0.57169(2) 0.70150(2) 0.03033(8) Uani 1 1 d . . O1 O 0.8527(2) 0.7679(3) 0.7615(2) 0.0434(8) Uani 1 1 d . . O2 O 1.0968(2) 0.5793(4) 0.7314(2) 0.0501(9) Uani 1 1 d . . O3 O 0.8615(2) 0.3534(4) 0.6465(2) 0.0497(9) Uani 1 1 d . . O4 O 0.9855(2) 0.6964(3) 0.8316(2) 0.0462(8) Uani 1 1 d . . O5 O 0.9770(3) 0.4325(4) 0.6020(2) 0.0504(9) Uani 1 1 d . . O6 O 1.0356(3) 0.4313(4) 0.7913(3) 0.0521(9) Uani 1 1 d . . O7 O 0.9198(3) 0.8539(4) 0.8797(2) 0.0598(11) Uani 1 1 d . . O8 O 0.9264(3) 0.2448(4) 0.5621(3) 0.0707(13) Uani 1 1 d . . O9 O 1.1862(3) 0.4593(6) 0.8215(3) 0.0903(18) Uani 1 1 d . . N7 N 0.9196(3) 0.7752(4) 0.8262(2) 0.0379(9) Uani 1 1 d . . N9 N 0.9218(3) 0.3399(4) 0.6028(3) 0.0459(10) Uani 1 1 d . . N8 N 1.1086(3) 0.4895(5) 0.7823(3) 0.0495(11) Uani 1 1 d . . N5 N 0.81582(16) 0.6233(3) 0.54950(13) 0.0362(8) Uani 1 1 d G . C13 C 0.86144(14) 0.6426(4) 0.48504(17) 0.0479(13) Uani 1 1 d G . H13 H 0.9266 0.6366 0.4955 0.057 Uiso 1 1 calc R U C12 C 0.8097(2) 0.6708(4) 0.40502(15) 0.0501(13) Uani 1 1 d G . H12 H 0.8403 0.6837 0.3619 0.060 Uiso 1 1 calc R U C11 C 0.7124(2) 0.6798(4) 0.38945(13) 0.0492(13) Uani 1 1 d G . H11 H 0.6778 0.6987 0.3359 0.059 Uiso 1 1 calc R U C10 C 0.66678(14) 0.6605(3) 0.45390(17) 0.0408(11) Uani 1 1 d G . H10 H 0.6017 0.6665 0.4435 0.049 Uiso 1 1 calc R U C9 C 0.71848(16) 0.6322(3) 0.53393(15) 0.0330(9) Uani 1 1 d G . C14 C 0.74529(16) 0.5261(3) 0.82039(14) 0.0342(9) Uani 1 1 d G . C15 C 0.70963(16) 0.5165(4) 0.89163(18) 0.0462(12) Uani 1 1 d G . H15 H 0.6471 0.5365 0.8890 0.055 Uiso 1 1 calc R U C16 C 0.7674(2) 0.4771(4) 0.96676(15) 0.0527(14) Uani 1 1 d G . H16 H 0.7436 0.4707 1.0144 0.063 Uiso 1 1 calc R U C17 C 0.8609(2) 0.4472(4) 0.97065(14) 0.0458(12) Uani 1 1 d G . H17 H 0.8996 0.4208 1.0209 0.055 Uiso 1 1 calc R U C18 C 0.89661(15) 0.4568(3) 0.89940(17) 0.0431(11) Uani 1 1 d G . H18 H 0.9592 0.4368 0.9020 0.052 Uiso 1 1 calc R U N6 N 0.83879(17) 0.4962(3) 0.82427(14) 0.0347(8) Uani 1 1 d G . C5 C 0.44915(14) 0.6375(3) 0.64351(18) 0.0375(10) Uani 1 1 d G . C4 C 0.3960(2) 0.6738(4) 0.56561(16) 0.0462(12) Uani 1 1 d G . H4 H 0.4252 0.6894 0.5219 0.055 Uiso 1 1 calc R U C3 C 0.29910(19) 0.6868(4) 0.55299(17) 0.0529(14) Uani 1 1 d G . H3 H 0.2635 0.7111 0.5009 0.063 Uiso 1 1 calc R U C2 C 0.25544(14) 0.6635(4) 0.6183(2) 0.0549(14) Uani 1 1 d G . H2 H 0.1906 0.6722 0.6098 0.066 Uiso 1 1 calc R U C1 C 0.30864(19) 0.6272(4) 0.69616(19) 0.0599(16) Uani 1 1 d G . H1 H 0.2794 0.6116 0.7398 0.072 Uiso 1 1 calc R U N1 N 0.40549(19) 0.6142(4) 0.70878(15) 0.0491(11) Uani 1 1 d G . C8 C 0.68040(15) 0.6160(3) 0.60074(12) 0.0341(9) Uani 1 1 d G . N3 N 0.58478(15) 0.6379(3) 0.59127(12) 0.0358(8) Uani 1 1 d G . C6 C 0.54340(12) 0.6209(3) 0.65868(15) 0.0361(10) Uani 1 1 d G . N2 N 0.59765(16) 0.5821(3) 0.73557(13) 0.0349(8) Uani 1 1 d G . C7 C 0.69327(15) 0.5603(3) 0.74504(12) 0.0333(9) Uani 1 1 d G . N4 N 0.73465(12) 0.5772(3) 0.67762(14) 0.0302(7) Uani 1 1 d G . N10 N 0.9852(3) 0.7732(5) 0.6442(3) 0.0541(12) Uani 1 1 d . . C19 C 1.0255(4) 0.8588(6) 0.6313(3) 0.0467(12) Uani 1 1 d . . C20 C 1.0770(5) 0.9676(7) 0.6131(4) 0.0720(19) Uani 1 1 d . . H20A H 1.0586 0.9864 0.5544 0.086 Uiso 1 1 calc R U H20B H 1.1432 0.9499 0.6281 0.086 Uiso 1 1 calc R U H20C H 1.0636 1.0390 0.6445 0.086 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 Nd01 0.02129(12) 0.03699(14) 0.03196(13) 0.00085(10) 0.00457(8) 0.00048(9) O1 0.0368(17) 0.0445(19) 0.0440(19) -0.0028(16) -0.0004(14) 0.0023(15) O2 0.0292(17) 0.062(2) 0.058(2) 0.0110(19) 0.0076(15) 0.0003(16) O3 0.0393(19) 0.052(2) 0.061(2) -0.0072(18) 0.0190(17) -0.0053(17) O4 0.0345(17) 0.049(2) 0.049(2) -0.0059(17) -0.0029(15) 0.0031(16) O5 0.042(2) 0.053(2) 0.061(2) -0.0056(19) 0.0227(17) -0.0005(17) O6 0.0387(19) 0.058(2) 0.062(2) 0.0194(19) 0.0148(17) 0.0108(17) O7 0.082(3) 0.051(2) 0.042(2) -0.0114(18) 0.0050(19) 0.007(2) O8 0.075(3) 0.061(3) 0.080(3) -0.028(2) 0.024(2) 0.004(2) O9 0.034(2) 0.143(5) 0.087(3) 0.042(3) 0.000(2) 0.025(3) N7 0.040(2) 0.038(2) 0.035(2) 0.0007(17) 0.0070(16) -0.0053(18) N9 0.038(2) 0.052(3) 0.046(2) -0.008(2) 0.0073(19) 0.007(2) N8 0.032(2) 0.069(3) 0.046(2) 0.006(2) 0.0068(18) 0.013(2) N5 0.0270(18) 0.052(2) 0.0309(18) 0.0041(17) 0.0093(15) 0.0029(17) C13 0.037(3) 0.069(4) 0.039(3) 0.003(3) 0.012(2) -0.001(2) C12 0.046(3) 0.074(4) 0.033(2) 0.006(2) 0.016(2) 0.006(3) C11 0.048(3) 0.065(4) 0.033(2) 0.008(2) 0.006(2) 0.008(3) C10 0.033(2) 0.048(3) 0.039(2) 0.003(2) 0.0047(19) 0.006(2) C9 0.029(2) 0.036(2) 0.033(2) 0.0012(18) 0.0042(17) 0.0032(18) C14 0.031(2) 0.038(2) 0.034(2) -0.0032(19) 0.0079(18) -0.0032(18) C15 0.036(3) 0.067(3) 0.036(2) 0.003(2) 0.010(2) 0.001(2) C16 0.048(3) 0.080(4) 0.032(2) 0.005(3) 0.014(2) 0.001(3) C17 0.042(3) 0.059(3) 0.033(2) 0.007(2) 0.001(2) -0.004(2) C18 0.035(2) 0.050(3) 0.040(3) 0.008(2) 0.003(2) 0.000(2) N6 0.0260(18) 0.043(2) 0.0330(19) 0.0044(17) 0.0022(14) -0.0008(16) C5 0.026(2) 0.042(3) 0.044(3) -0.002(2) 0.0073(19) -0.0010(19) C4 0.029(2) 0.066(3) 0.042(3) 0.001(2) 0.005(2) 0.006(2) C3 0.031(2) 0.067(4) 0.056(3) 0.001(3) -0.001(2) 0.009(2) C2 0.025(2) 0.064(4) 0.074(4) 0.002(3) 0.009(2) 0.005(2) C1 0.036(3) 0.077(4) 0.071(4) 0.008(3) 0.022(3) 0.006(3) N1 0.030(2) 0.069(3) 0.051(3) 0.007(2) 0.0150(19) 0.004(2) C8 0.026(2) 0.033(2) 0.040(2) -0.0003(19) 0.0012(18) -0.0003(17) N3 0.0262(18) 0.043(2) 0.038(2) 0.0037(17) 0.0069(15) 0.0004(16) C6 0.036(2) 0.037(2) 0.035(2) -0.0006(19) 0.0083(19) -0.0016(19) N2 0.0231(17) 0.047(2) 0.0340(19) 0.0005(17) 0.0049(14) 0.0013(16) C7 0.029(2) 0.035(2) 0.038(2) -0.0082(19) 0.0110(17) -0.0068(18) N4 0.0239(16) 0.0384(19) 0.0271(17) 0.0014(15) 0.0037(13) -0.0020(15) N10 0.046(3) 0.056(3) 0.061(3) 0.012(2) 0.013(2) -0.006(2) C19 0.035(2) 0.057(3) 0.046(3) 0.004(2) 0.005(2) -0.002(2) C20 0.064(4) 0.081(5) 0.068(4) 0.008(4) 0.010(3) -0.027(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 '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 Nd01 O5 74.21(13) O6 Nd01 O4 73.55(13) O5 Nd01 O4 136.08(12) O6 Nd01 O3 77.82(13) O5 Nd01 O3 50.53(12) O4 Nd01 O3 144.14(13) O6 Nd01 O1 121.29(12) O5 Nd01 O1 159.94(12) O4 Nd01 O1 50.23(11) O3 Nd01 O1 140.08(11) O6 Nd01 O2 49.90(12) O5 Nd01 O2 68.68(13) O4 Nd01 O2 67.83(12) O3 Nd01 O2 108.46(12) O1 Nd01 O2 110.14(12) O6 Nd01 N4 131.19(10) O5 Nd01 N4 114.95(11) O4 Nd01 N4 108.66(10) O3 Nd01 N4 75.16(10) O1 Nd01 N4 66.11(10) O2 Nd01 N4 176.23(11) O6 Nd01 N10 114.38(14) O5 Nd01 N10 90.87(14) O4 Nd01 N10 76.33(14) O3 Nd01 N10 136.41(14) O1 Nd01 N10 71.50(14) O2 Nd01 N10 64.96(14) N4 Nd01 N10 113.29(12) O6 Nd01 N5 146.95(12) O5 Nd01 N5 73.06(11) O4 Nd01 N5 136.22(11) O3 Nd01 N5 78.05(12) O1 Nd01 N5 91.62(10) O2 Nd01 N5 119.43(10) N4 Nd01 N5 61.93(7) N10 Nd01 N5 70.69(13) O6 Nd01 N6 74.64(10) O5 Nd01 N6 126.61(11) O4 Nd01 N6 70.86(11) O3 Nd01 N6 81.14(11) O1 Nd01 N6 72.50(11) O2 Nd01 N6 117.38(10) N4 Nd01 N6 61.65(7) N10 Nd01 N6 141.71(13) N5 Nd01 N6 123.06(8) O6 Nd01 N9 74.02(13) O5 Nd01 N9 25.29(12) O4 Nd01 N9 147.34(12) O3 Nd01 N9 25.24(12) O1 Nd01 N9 160.99(11) O2 Nd01 N9 88.24(12) N4 Nd01 N9 95.53(10) N10 Nd01 N9 114.35(15) N5 Nd01 N9 74.49(11) N6 Nd01 N9 103.93(12) O6 Nd01 N8 25.10(13) O5 Nd01 N8 70.85(13) O4 Nd01 N8 67.24(12) O3 Nd01 N8 94.50(13) O1 Nd01 N8 117.06(12) O2 Nd01 N8 24.87(12) N4 Nd01 N8 155.85(11) N10 Nd01 N8 89.37(15) N5 Nd01 N8 138.18(11) N6 Nd01 N8 95.57(11) N9 Nd01 N8 81.65(13) N7 O1 Nd01 95.5(3) N8 O2 Nd01 94.7(3) N9 O3 Nd01 96.0(3) N7 O4 Nd01 97.5(3) N9 O5 Nd01 96.9(3) N8 O6 Nd01 98.0(3) O7 N7 O4 121.9(4) O7 N7 O1 121.5(4) O4 N7 O1 116.5(4) O7 N7 Nd01 176.7(3) O4 N7 Nd01 57.5(2) O1 N7 Nd01 59.2(2) O8 N9 O3 122.5(5) O8 N9 O5 121.0(5) O3 N9 O5 116.5(4) O8 N9 Nd01 178.7(4) O3 N9 Nd01 58.7(2) O5 N9 Nd01 57.8(2) O9 N8 O2 121.6(5) O9 N8 O6 121.3(5) O2 N8 O6 117.0(4) O9 N8 Nd01 174.6(4) O2 N8 Nd01 60.4(2) O6 N8 Nd01 56.9(2) C13 N5 C9 120.0 C13 N5 Nd01 119.59(12) C9 N5 Nd01 120.41(12) N5 C13 C12 120.0 N5 C13 H13 120.0 C12 C13 H13 120.0 C13 C12 C11 120.0 C13 C12 H12 120.0 C11 C12 H12 120.0 C10 C11 C12 120.0 C10 C11 H11 120.0 C12 C11 H11 120.0 C11 C10 C9 120.0 C11 C10 H10 120.0 C9 C10 H10 120.0 C8 C9 C10 124.0(2) C8 C9 N5 115.9(2) C10 C9 N5 120.0 C7 C14 C15 123.5(2) C7 C14 N6 116.5(2) 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 C17 C18 N6 120.0 C17 C18 H18 120.0 N6 C18 H18 120.0 C18 N6 C14 120.0 C18 N6 Nd01 119.34(13) C14 N6 Nd01 118.70(13) C6 C5 C4 122.4(2) C6 C5 N1 117.6(2) C4 C5 N1 120.0 C5 C4 C3 120.0 C5 C4 H4 120.0 C3 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 118.67(19) C9 C8 N4 121.33(19) N3 C8 N4 120.0 C6 N3 C8 120.0 C5 C6 N2 123.3(2) C5 C6 N3 116.6(2) N2 C6 N3 120.0 C7 N2 C6 120.0 C14 C7 N2 119.29(19) C14 C7 N4 120.68(19) N2 C7 N4 120.0 C7 N4 C8 120.0 C7 N4 Nd01 119.58(11) C8 N4 Nd01 119.69(11) C19 N10 Nd01 169.0(5) N10 C19 C20 178.8(7) 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 Nd01 O6 2.506(4) Nd01 O5 2.515(4) Nd01 O4 2.520(3) Nd01 O3 2.537(4) Nd01 O1 2.555(4) Nd01 O2 2.586(3) Nd01 N4 2.5804(17) Nd01 N10 2.629(5) Nd01 N5 2.6417(19) Nd01 N6 2.645(2) Nd01 N9 2.952(4) Nd01 N8 2.963(4) O1 N7 1.271(5) O2 N8 1.250(6) O3 N9 1.266(5) O4 N7 1.262(5) O5 N9 1.270(6) O6 N8 1.270(6) O7 N7 1.209(5) O8 N9 1.218(6) O9 N8 1.212(6) 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 1.351(3) C14 C7 1.345(3) 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 1.354(3) 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 1.126(7) C19 C20 1.445(8) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600