#------------------------------------------------------------------------------ #$Date: 2017-06-23 06:26:08 +0300 (Fri, 23 Jun 2017) $ #$Revision: 198108 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/63/7056352.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_7056352 loop_ _publ_author_name 'Gu, Xiaoxia' 'Wang, Shaowu' 'Wei, Yun' 'Zhu, Xiancui' 'Zhou, Shuangliu' 'Huang, Zeming' 'Mu, Xiaolong' _publ_section_title ; Rare earth metal bisamido complexes with a NNO tridentate ligand and catalytic activity for selective polymerization of isoprene ; _journal_name_full 'New J. Chem.' _journal_paper_doi 10.1039/C7NJ01454F _journal_year 2017 _chemical_formula_moiety 'C24 H51 N4 Nd O Si4' _chemical_formula_sum 'C24 H51 N4 Nd O Si4' _chemical_formula_weight 668.28 _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 _atom_sites_solution_primary direct _audit_creation_date 2017-06-15 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2017-06-17 deposited with the CCDC. 2017-06-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.8170(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7474(13) _cell_length_b 16.9894(18) _cell_length_c 16.8809(18) _cell_measurement_reflns_used 9957 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.559 _cell_measurement_theta_min 2.397 _cell_volume 3564.8(6) _computing_cell_refinement 'SAINT v7.34A (Bruker, 200?)' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'SAINT v7.34A (Bruker, 200?)' _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 30310 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.584 _diffrn_reflns_theta_min 1.723 _exptl_absorpt_coefficient_mu 1.611 _exptl_absorpt_correction_T_max 0.7941 _exptl_absorpt_correction_T_min 0.7602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.245 _exptl_crystal_description block _exptl_crystal_F_000 1388 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.404 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 321 _refine_ls_number_reflns 8219 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0418 _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^)+(0.0551P)^2^+5.2304P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.1158 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6815 _reflns_number_total 8219 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7nj01454f2.cif _cod_data_source_block 2_0m _cod_database_code 7056352 _shelx_shelxl_version_number 2014/8 _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 0.794 _shelx_estimated_absorpt_t_min 0.760 _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 Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C7(H7A,H7B) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C10(H10) 2.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B, H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A, H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C) ; _shelx_res_file ; 150310c_0m.res created by SHELXL-2014/8 TITL 150310c_0m in P2(1)/n CELL 0.71073 12.7474 16.9894 16.8809 90 102.817 90 ZERR 4 0.0013 0.0018 0.0018 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Nd O Si UNIT 96 204 16 4 4 16 L.S. 10 PLAN 2 SIZE 0.15 0.16 0.18 TEMP 20 FREE Nd1 C11 FREE Nd1 Si2 FREE Nd1 Si3 BOND $H fmap 2 acta REM REM REM WGHT 0.055100 5.230400 FVAR 0.29731 C1 1 1.137549 0.685402 0.934957 11.00000 0.07402 0.08754 = 0.07300 -0.01095 0.01171 -0.01383 AFIX 43 H1 2 1.162878 0.736871 0.941216 11.00000 -1.20000 AFIX 0 C2 1 1.189637 0.630674 0.987818 11.00000 0.08028 0.12900 = 0.06517 0.00305 -0.00043 -0.00615 AFIX 43 H2 2 1.248090 0.644207 1.029188 11.00000 -1.20000 AFIX 0 C3 1 1.152933 0.554611 0.978024 11.00000 0.11819 0.10028 = 0.08533 0.02430 0.00431 0.01264 AFIX 43 H3 2 1.187779 0.514843 1.011697 11.00000 -1.20000 AFIX 0 C4 1 1.064457 0.538072 0.918106 11.00000 0.10459 0.06832 = 0.07622 0.01038 0.01327 -0.00006 AFIX 43 H4 2 1.037638 0.487004 0.911731 11.00000 -1.20000 AFIX 0 C5 1 1.014952 0.596929 0.867147 11.00000 0.06747 0.05525 = 0.06381 0.00285 0.02037 -0.00109 C6 1 0.919909 0.580887 0.800217 11.00000 0.07632 0.04382 = 0.08114 0.00226 0.00866 -0.01044 AFIX 23 H6A 2 0.868757 0.623607 0.797533 11.00000 -1.20000 H6B 2 0.885273 0.532978 0.812484 11.00000 -1.20000 AFIX 0 C7 1 0.947987 0.572132 0.718322 11.00000 0.08786 0.04581 = 0.08241 -0.01650 0.00214 0.00091 AFIX 23 H7A 2 1.009054 0.536963 0.723338 11.00000 -1.20000 H7B 2 0.887666 0.548638 0.680469 11.00000 -1.20000 AFIX 0 C8 1 1.024772 0.569853 0.578240 11.00000 0.15085 0.09767 = 0.09721 -0.04026 0.04226 0.02468 AFIX 137 H8A 2 1.080371 0.541135 0.614437 11.00000 -1.50000 H8B 2 1.046266 0.579511 0.528090 11.00000 -1.50000 H8C 2 0.959500 0.539650 0.567713 11.00000 -1.50000 AFIX 0 C9 1 1.006029 0.647970 0.617056 11.00000 0.06498 0.07504 = 0.06612 -0.02601 0.01169 0.00769 C10 1 1.020193 0.716532 0.573769 11.00000 0.07863 0.08908 = 0.07204 -0.01267 0.03444 0.00137 AFIX 43 H10 2 1.066916 0.712158 0.538792 11.00000 -1.20000 AFIX 0 C11 1 0.974612 0.787577 0.576662 11.00000 0.06407 0.09501 = 0.05458 0.00132 0.01350 -0.00645 C12 1 0.986917 0.850692 0.516167 11.00000 0.12310 0.12667 = 0.08936 0.02881 0.04163 0.00267 AFIX 137 H12A 2 0.919069 0.859068 0.478971 11.00000 -1.50000 H12B 2 1.039359 0.834275 0.486612 11.00000 -1.50000 H12C 2 1.010131 0.898788 0.544528 11.00000 -1.50000 AFIX 0 C13 1 1.242656 0.731203 0.762627 11.00000 0.05609 0.08549 = 0.13085 -0.01486 0.02542 0.00643 AFIX 137 H13A 2 1.215978 0.702571 0.803078 11.00000 -1.50000 H13B 2 1.316099 0.716647 0.765181 11.00000 -1.50000 H13C 2 1.199853 0.718939 0.709757 11.00000 -1.50000 AFIX 0 C14 1 1.293556 0.886109 0.702141 11.00000 0.10938 0.16703 = 0.22964 0.08280 0.09127 0.01152 AFIX 137 H14A 2 1.243006 0.883383 0.650764 11.00000 -1.50000 H14B 2 1.358736 0.859604 0.698257 11.00000 -1.50000 H14C 2 1.309073 0.940222 0.716471 11.00000 -1.50000 AFIX 0 C15 1 1.330646 0.857682 0.880325 11.00000 0.11941 0.11537 = 0.16807 -0.01184 -0.04623 -0.03200 AFIX 137 H15A 2 1.397727 0.876123 0.870349 11.00000 -1.50000 H15B 2 1.342586 0.810110 0.911728 11.00000 -1.50000 H15C 2 1.300855 0.897045 0.909736 11.00000 -1.50000 AFIX 0 C16 1 1.098448 1.021008 0.684944 11.00000 0.20614 0.06858 = 0.29541 0.03116 0.14723 0.00817 AFIX 137 H16A 2 1.170458 1.040882 0.701764 11.00000 -1.50000 H16B 2 1.049271 1.064198 0.670922 11.00000 -1.50000 H16C 2 1.093701 0.987442 0.638535 11.00000 -1.50000 AFIX 0 C17 1 1.118256 1.023260 0.858786 11.00000 0.14327 0.12955 = 0.24034 -0.11607 0.01014 -0.01664 AFIX 137 H17A 2 1.131852 0.990611 0.906386 11.00000 -1.50000 H17B 2 1.067658 1.063651 0.864225 11.00000 -1.50000 H17C 2 1.184317 1.047047 0.852679 11.00000 -1.50000 AFIX 0 C18 1 0.913665 0.967161 0.754747 11.00000 0.10196 0.05686 = 0.24732 -0.00067 0.06064 0.00921 AFIX 137 H18A 2 0.881609 0.931932 0.711696 11.00000 -1.50000 H18B 2 0.888976 1.019799 0.740759 11.00000 -1.50000 H18C 2 0.893527 0.951610 0.803997 11.00000 -1.50000 AFIX 0 C19 1 0.953100 0.844747 0.949560 11.00000 0.09838 0.21911 = 0.08762 -0.07629 -0.00227 0.02776 AFIX 137 H19A 2 0.994795 0.845883 0.908689 11.00000 -1.50000 H19B 2 0.989446 0.813300 0.994588 11.00000 -1.50000 H19C 2 0.944482 0.897370 0.967838 11.00000 -1.50000 AFIX 0 C20 1 0.716835 0.876167 0.922141 11.00000 0.10560 0.20255 = 0.11982 -0.05839 0.04325 0.04739 AFIX 137 H20A 2 0.728199 0.924225 0.895326 11.00000 -1.50000 H20B 2 0.725970 0.885695 0.979320 11.00000 -1.50000 H20C 2 0.645224 0.857342 0.900411 11.00000 -1.50000 AFIX 0 C21 1 0.804018 0.714183 0.969510 11.00000 0.18587 0.23082 = 0.10292 0.06767 0.07179 0.05167 AFIX 137 H21A 2 0.733281 0.692044 0.952685 11.00000 -1.50000 H21B 2 0.815772 0.730210 1.025321 11.00000 -1.50000 H21C 2 0.856661 0.675456 0.963752 11.00000 -1.50000 AFIX 0 C22 1 0.622672 0.855429 0.696698 11.00000 0.09273 0.07904 = 0.12660 0.00511 0.00882 0.02608 AFIX 137 H22A 2 0.603662 0.886845 0.738662 11.00000 -1.50000 H22B 2 0.559218 0.844013 0.655751 11.00000 -1.50000 H22C 2 0.673000 0.883769 0.672767 11.00000 -1.50000 AFIX 0 C23 1 0.583226 0.711608 0.788561 11.00000 0.07271 0.11155 = 0.18285 -0.00246 0.06098 -0.02802 AFIX 137 H23A 2 0.610420 0.661335 0.809645 11.00000 -1.50000 H23B 2 0.517740 0.704324 0.748344 11.00000 -1.50000 H23C 2 0.569262 0.743584 0.831967 11.00000 -1.50000 AFIX 0 C24 1 0.698084 0.696670 0.654116 11.00000 0.06651 0.08654 = 0.08872 -0.01635 -0.00974 -0.00280 AFIX 137 H24A 2 0.749731 0.718923 0.626904 11.00000 -1.50000 H24B 2 0.629596 0.692607 0.616676 11.00000 -1.50000 H24C 2 0.721564 0.645266 0.674134 11.00000 -1.50000 AFIX 0 N1 3 1.052456 0.670846 0.874490 11.00000 0.06484 0.06110 = 0.06197 -0.00442 0.00989 -0.00816 N2 3 0.974316 0.648384 0.685856 11.00000 0.05656 0.04841 = 0.05862 -0.01416 0.00711 0.00227 N3 3 1.107205 0.866413 0.780247 11.00000 0.05775 0.05171 = 0.10654 -0.01560 0.02612 -0.01408 N4 3 0.806553 0.776652 0.806438 11.00000 0.04712 0.06193 = 0.05720 -0.00121 0.02027 0.00068 ND1 4 0.966677 0.774389 0.760291 11.00000 0.04482 0.03751 = 0.05791 -0.00909 0.02015 -0.00379 O1 5 0.916106 0.806658 0.626988 11.00000 0.08005 0.07029 = 0.06839 0.00762 0.02464 0.01070 SI1 6 1.235038 0.837812 0.781591 11.00000 0.04704 0.07242 = 0.10192 0.00624 0.01274 -0.01426 SI2 6 1.063218 0.963547 0.769897 11.00000 0.10112 0.05322 = 0.15092 -0.02458 0.05323 -0.01804 SI3 6 0.816262 0.800767 0.905342 11.00000 0.07730 0.14576 = 0.06132 -0.00830 0.03004 0.02815 SI4 6 0.685123 0.761488 0.741225 11.00000 0.04329 0.05810 = 0.08529 0.00410 0.01413 -0.00051 HKLF 4 REM 150310c_0m in P2(1)/n REM R1 = 0.0418 for 6815 Fo > 4sig(Fo) and 0.0522 for all 8219 data REM 321 parameters refined using 0 restraints END WGHT 0.0551 5.2302 REM Highest difference peak 2.404, deepest hole -1.364, 1-sigma level 0.101 Q1 1 1.0898 0.9477 0.8444 11.00000 0.05 2.40 Q2 1 1.0005 0.7663 0.8032 11.00000 0.05 1.02 ; _shelx_res_checksum 96124 _olex2_submission_special_instructions 'No special instructions were received' 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 C1 C 1.1375(4) 0.6854(4) 0.9350(3) 0.0789(14) Uani 1 1 d . H1 H 1.1629 0.7369 0.9412 0.095 Uiso 1 1 calc R C2 C 1.1896(5) 0.6307(5) 0.9878(3) 0.0941(19) Uani 1 1 d . H2 H 1.2481 0.6442 1.0292 0.113 Uiso 1 1 calc R C3 C 1.1529(6) 0.5546(4) 0.9780(4) 0.104(2) Uani 1 1 d . H3 H 1.1878 0.5148 1.0117 0.125 Uiso 1 1 calc R C4 C 1.0645(5) 0.5381(3) 0.9181(3) 0.0841(16) Uani 1 1 d . H4 H 1.0376 0.4870 0.9117 0.101 Uiso 1 1 calc R C5 C 1.0150(4) 0.5969(3) 0.8671(3) 0.0613(10) Uani 1 1 d . C6 C 0.9199(4) 0.5809(3) 0.8002(3) 0.0685(12) Uani 1 1 d . H6A H 0.8688 0.6236 0.7975 0.082 Uiso 1 1 calc R H6B H 0.8853 0.5330 0.8125 0.082 Uiso 1 1 calc R C7 C 0.9480(5) 0.5721(3) 0.7183(3) 0.0746(14) Uani 1 1 d . H7A H 1.0091 0.5370 0.7233 0.090 Uiso 1 1 calc R H7B H 0.8877 0.5486 0.6805 0.090 Uiso 1 1 calc R C8 C 1.0248(7) 0.5699(4) 0.5782(4) 0.113(2) Uani 1 1 d . H8A H 1.0804 0.5411 0.6144 0.169 Uiso 1 1 calc GR H8B H 1.0463 0.5795 0.5281 0.169 Uiso 1 1 calc GR H8C H 0.9595 0.5396 0.5677 0.169 Uiso 1 1 calc GR C9 C 1.0060(4) 0.6480(3) 0.6171(3) 0.0692(13) Uani 1 1 d . C10 C 1.0202(5) 0.7165(3) 0.5738(3) 0.0772(14) Uani 1 1 d . H10 H 1.0669 0.7122 0.5388 0.093 Uiso 1 1 calc R C11 C 0.9746(4) 0.7876(3) 0.5767(3) 0.0712(13) Uani 1 1 d . C12 C 0.9869(6) 0.8507(5) 0.5162(4) 0.110(2) Uani 1 1 d . H12A H 0.9191 0.8591 0.4790 0.165 Uiso 1 1 calc GR H12B H 1.0394 0.8343 0.4866 0.165 Uiso 1 1 calc GR H12C H 1.0101 0.8988 0.5445 0.165 Uiso 1 1 calc GR C13 C 1.2427(5) 0.7312(3) 0.7626(5) 0.0901(18) Uani 1 1 d . H13A H 1.2160 0.7026 0.8031 0.135 Uiso 1 1 calc GR H13B H 1.3161 0.7166 0.7652 0.135 Uiso 1 1 calc GR H13C H 1.1999 0.7189 0.7098 0.135 Uiso 1 1 calc GR C14 C 1.2936(7) 0.8861(6) 0.7021(7) 0.160(4) Uani 1 1 d . H14A H 1.2430 0.8834 0.6508 0.241 Uiso 1 1 calc GR H14B H 1.3587 0.8596 0.6983 0.241 Uiso 1 1 calc GR H14C H 1.3091 0.9402 0.7165 0.241 Uiso 1 1 calc GR C15 C 1.3306(7) 0.8577(5) 0.8803(6) 0.146(4) Uani 1 1 d . H15A H 1.3977 0.8761 0.8703 0.220 Uiso 1 1 calc GR H15B H 1.3426 0.8101 0.9117 0.220 Uiso 1 1 calc GR H15C H 1.3009 0.8970 0.9097 0.220 Uiso 1 1 calc GR C16 C 1.0984(9) 1.0210(5) 0.6849(7) 0.176(5) Uani 1 1 d . H16A H 1.1705 1.0409 0.7018 0.264 Uiso 1 1 calc GR H16B H 1.0493 1.0642 0.6709 0.264 Uiso 1 1 calc GR H16C H 1.0937 0.9874 0.6385 0.264 Uiso 1 1 calc GR C17 C 1.1183(8) 1.0233(5) 0.8588(7) 0.176(5) Uani 1 1 d . H17A H 1.1319 0.9906 0.9064 0.264 Uiso 1 1 calc GR H17B H 1.0677 1.0637 0.8642 0.264 Uiso 1 1 calc GR H17C H 1.1843 1.0470 0.8527 0.264 Uiso 1 1 calc GR C18 C 0.9137(6) 0.9672(4) 0.7547(6) 0.132(3) Uani 1 1 d . H18A H 0.8816 0.9319 0.7117 0.198 Uiso 1 1 calc GR H18B H 0.8890 1.0198 0.7408 0.198 Uiso 1 1 calc GR H18C H 0.8935 0.9516 0.8040 0.198 Uiso 1 1 calc GR C19 C 0.9531(6) 0.8447(6) 0.9496(4) 0.139(4) Uani 1 1 d . H19A H 0.9948 0.8459 0.9087 0.208 Uiso 1 1 calc GR H19B H 0.9894 0.8133 0.9946 0.208 Uiso 1 1 calc GR H19C H 0.9445 0.8974 0.9678 0.208 Uiso 1 1 calc GR C20 C 0.7168(6) 0.8762(6) 0.9221(5) 0.140(3) Uani 1 1 d . H20A H 0.7282 0.9242 0.8953 0.210 Uiso 1 1 calc GR H20B H 0.7260 0.8857 0.9793 0.210 Uiso 1 1 calc GR H20C H 0.6452 0.8573 0.9004 0.210 Uiso 1 1 calc GR C21 C 0.8040(9) 0.7142(7) 0.9695(5) 0.167(5) Uani 1 1 d . H21A H 0.7333 0.6920 0.9527 0.251 Uiso 1 1 calc GR H21B H 0.8158 0.7302 1.0253 0.251 Uiso 1 1 calc GR H21C H 0.8567 0.6755 0.9638 0.251 Uiso 1 1 calc GR C22 C 0.6227(5) 0.8554(4) 0.6967(5) 0.102(2) Uani 1 1 d . H22A H 0.6037 0.8868 0.7387 0.153 Uiso 1 1 calc GR H22B H 0.5592 0.8440 0.6558 0.153 Uiso 1 1 calc GR H22C H 0.6730 0.8838 0.6728 0.153 Uiso 1 1 calc GR C23 C 0.5832(5) 0.7116(4) 0.7886(6) 0.117(3) Uani 1 1 d . H23A H 0.6104 0.6613 0.8096 0.176 Uiso 1 1 calc GR H23B H 0.5177 0.7043 0.7483 0.176 Uiso 1 1 calc GR H23C H 0.5693 0.7436 0.8320 0.176 Uiso 1 1 calc GR C24 C 0.6981(4) 0.6967(4) 0.6541(3) 0.0848(16) Uani 1 1 d . H24A H 0.7497 0.7189 0.6269 0.127 Uiso 1 1 calc GR H24B H 0.6296 0.6926 0.6167 0.127 Uiso 1 1 calc GR H24C H 0.7216 0.6453 0.6741 0.127 Uiso 1 1 calc GR N1 N 1.0525(3) 0.6708(2) 0.8745(2) 0.0633(9) Uani 1 1 d . N2 N 0.9743(3) 0.6484(2) 0.6859(2) 0.0554(8) Uani 1 1 d . N3 N 1.1072(3) 0.8664(2) 0.7802(3) 0.0708(11) Uani 1 1 d . N4 N 0.8066(3) 0.7767(2) 0.8064(2) 0.0541(8) Uani 1 1 d . Nd1 Nd 0.96668(2) 0.77439(2) 0.76029(2) 0.04539(8) Uani 1 1 d . O1 O 0.9161(3) 0.8067(2) 0.6270(2) 0.0716(8) Uani 1 1 d . Si1 Si 1.23504(11) 0.83781(9) 0.78159(10) 0.0744(4) Uani 1 1 d . Si2 Si 1.06322(16) 0.96355(10) 0.76990(15) 0.0978(6) Uani 1 1 d . Si3 Si 0.81626(14) 0.80077(14) 0.90534(9) 0.0925(5) Uani 1 1 d . Si4 Si 0.68512(10) 0.76149(8) 0.74122(9) 0.0622(3) 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 C1 0.074(3) 0.088(4) 0.073(3) -0.011(3) 0.012(3) -0.014(3) C2 0.080(4) 0.129(6) 0.065(3) 0.003(3) 0.000(3) -0.006(4) C3 0.118(5) 0.100(5) 0.085(4) 0.024(4) 0.004(4) 0.013(4) C4 0.105(4) 0.068(3) 0.076(3) 0.010(3) 0.013(3) 0.000(3) C5 0.067(3) 0.055(2) 0.064(2) 0.0029(19) 0.020(2) -0.001(2) C6 0.076(3) 0.044(2) 0.081(3) 0.002(2) 0.009(2) -0.010(2) C7 0.088(4) 0.046(2) 0.082(3) -0.017(2) 0.002(3) 0.001(2) C8 0.151(7) 0.098(5) 0.097(4) -0.040(4) 0.042(4) 0.025(4) C9 0.065(3) 0.075(3) 0.066(3) -0.026(2) 0.012(2) 0.008(2) C10 0.079(3) 0.089(4) 0.072(3) -0.013(3) 0.034(3) 0.001(3) C11 0.064(3) 0.095(4) 0.055(2) 0.001(2) 0.014(2) -0.006(3) C12 0.123(6) 0.127(6) 0.089(4) 0.029(4) 0.042(4) 0.003(5) C13 0.056(3) 0.085(4) 0.131(5) -0.015(3) 0.025(3) 0.006(3) C14 0.109(6) 0.167(9) 0.230(11) 0.083(8) 0.091(7) 0.012(6) C15 0.119(6) 0.115(6) 0.168(8) -0.012(6) -0.046(6) -0.032(5) C16 0.206(11) 0.069(5) 0.295(14) 0.031(6) 0.147(10) 0.008(6) C17 0.143(8) 0.130(7) 0.240(12) -0.116(8) 0.010(7) -0.017(6) C18 0.102(5) 0.057(4) 0.247(11) -0.001(5) 0.061(6) 0.009(3) C19 0.098(5) 0.219(10) 0.088(4) -0.076(6) -0.002(4) 0.028(6) C20 0.106(5) 0.203(9) 0.120(6) -0.058(6) 0.043(4) 0.047(6) C21 0.186(10) 0.231(12) 0.103(6) 0.068(7) 0.072(6) 0.052(8) C22 0.093(4) 0.079(4) 0.127(5) 0.005(4) 0.009(4) 0.026(3) C23 0.073(4) 0.112(5) 0.183(8) -0.002(5) 0.061(5) -0.028(4) C24 0.067(3) 0.087(4) 0.089(4) -0.016(3) -0.010(3) -0.003(3) N1 0.065(2) 0.061(2) 0.062(2) -0.0044(17) 0.0099(17) -0.0082(18) N2 0.057(2) 0.0484(18) 0.0586(19) -0.0142(15) 0.0071(15) 0.0023(15) N3 0.058(2) 0.052(2) 0.107(3) -0.016(2) 0.026(2) -0.0141(17) N4 0.0471(18) 0.062(2) 0.0572(19) -0.0012(15) 0.0203(15) 0.0007(15) Nd1 0.04482(12) 0.03751(12) 0.05791(13) -0.00909(8) 0.02015(9) -0.00379(8) O1 0.080(2) 0.070(2) 0.0684(19) 0.0076(16) 0.0246(17) 0.0107(18) Si1 0.0470(7) 0.0724(9) 0.1019(10) 0.0062(7) 0.0127(7) -0.0143(6) Si2 0.1011(12) 0.0532(8) 0.1509(16) -0.0246(9) 0.0532(12) -0.0180(8) Si3 0.0773(10) 0.1458(16) 0.0613(8) -0.0083(9) 0.0300(7) 0.0282(10) Si4 0.0433(6) 0.0581(7) 0.0853(9) 0.0041(6) 0.0141(6) -0.0005(5) 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' Nd Nd -0.1943 3.0179 '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' Si Si 0.0817 0.0704 '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 C2 C1 H1 117.6 N1 C1 H1 117.6 N1 C1 C2 124.8(6) C1 C2 H2 121.2 C1 C2 C3 117.5(6) C3 C2 H2 121.2 C2 C3 H3 120.5 C4 C3 C2 119.1(6) C4 C3 H3 120.5 C3 C4 H4 120.0 C3 C4 C5 120.1(6) C5 C4 H4 120.0 C4 C5 C6 121.6(5) N1 C5 C4 121.2(5) N1 C5 C6 117.1(4) C5 C6 H6A 108.9 C5 C6 H6B 108.9 C5 C6 C7 113.3(4) H6A C6 H6B 107.7 C7 C6 H6A 108.9 C7 C6 H6B 108.9 C6 C7 H7A 109.2 C6 C7 H7B 109.2 H7A C7 H7B 107.9 N2 C7 C6 111.9(4) N2 C7 H7A 109.2 N2 C7 H7B 109.2 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C9 C8 H8A 109.5 C9 C8 H8B 109.5 C9 C8 H8C 109.5 C10 C9 C8 116.6(5) N2 C9 C8 119.6(5) N2 C9 C10 123.7(4) C9 C10 H10 115.9 C11 C10 C9 128.1(5) C11 C10 H10 115.9 C10 C11 C12 120.1(5) O1 C11 C10 124.5(5) O1 C11 C12 115.3(5) C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 Si1 C13 H13A 109.5 Si1 C13 H13B 109.5 Si1 C13 H13C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 Si1 C14 H14A 109.5 Si1 C14 H14B 109.5 Si1 C14 H14C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 Si1 C15 H15A 109.5 Si1 C15 H15B 109.5 Si1 C15 H15C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 Si2 C16 H16A 109.5 Si2 C16 H16B 109.5 Si2 C16 H16C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 Si2 C17 H17A 109.5 Si2 C17 H17B 109.5 Si2 C17 H17C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 Si2 C18 H18A 109.5 Si2 C18 H18B 109.5 Si2 C18 H18C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 Si3 C19 H19A 109.5 Si3 C19 H19B 109.5 Si3 C19 H19C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 Si3 C20 H20A 109.5 Si3 C20 H20B 109.5 Si3 C20 H20C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 Si3 C21 H21A 109.5 Si3 C21 H21B 109.5 Si3 C21 H21C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 Si4 C22 H22A 109.5 Si4 C22 H22B 109.5 Si4 C22 H22C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 Si4 C23 H23A 109.5 Si4 C23 H23B 109.5 Si4 C23 H23C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 Si4 C24 H24A 109.5 Si4 C24 H24B 109.5 Si4 C24 H24C 109.5 C1 N1 C5 117.2(5) C1 N1 Nd1 124.4(4) C5 N1 Nd1 118.2(3) C7 N2 Nd1 122.0(3) C9 N2 C7 117.7(4) C9 N2 Nd1 120.3(3) Si1 N3 Nd1 120.8(2) Si1 N3 Si2 124.1(2) Si2 N3 Nd1 113.5(2) Si3 N4 Nd1 116.92(19) Si3 N4 Si4 121.9(2) Si4 N4 Nd1 121.02(18) N2 Nd1 N1 75.04(12) N3 Nd1 N1 99.13(14) N3 Nd1 N2 122.04(13) N4 Nd1 N1 91.05(12) N4 Nd1 N2 108.42(12) N4 Nd1 N3 129.49(13) O1 Nd1 N1 149.37(12) O1 Nd1 N2 75.04(12) O1 Nd1 N3 91.22(15) O1 Nd1 N4 104.45(13) C11 O1 Nd1 121.0(3) C13 Si1 C14 105.2(4) C13 Si1 C15 106.5(4) C14 Si1 C15 106.1(5) N3 Si1 C13 111.5(2) N3 Si1 C14 113.6(3) N3 Si1 C15 113.3(4) C17 Si2 C16 103.1(5) C17 Si2 C18 106.9(4) C18 Si2 C16 106.8(5) N3 Si2 C16 116.5(3) N3 Si2 C17 112.9(4) N3 Si2 C18 110.0(3) C20 Si3 C19 105.5(4) C21 Si3 C19 105.8(5) C21 Si3 C20 107.9(4) N4 Si3 C19 110.1(3) N4 Si3 C20 114.3(3) N4 Si3 C21 112.7(4) C22 Si4 C23 106.5(4) C22 Si4 C24 106.9(3) C23 Si4 C24 105.0(3) N4 Si4 C22 112.0(3) N4 Si4 C23 114.1(3) N4 Si4 C24 111.7(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 H1 0.9300 C1 C2 1.356(8) C1 N1 1.337(6) C2 H2 0.9300 C2 C3 1.372(10) C3 H3 0.9300 C3 C4 1.367(9) C4 H4 0.9300 C4 C5 1.377(7) C5 C6 1.487(7) C5 N1 1.340(6) C6 H6A 0.9700 C6 H6B 0.9700 C6 C7 1.510(7) C7 H7A 0.9700 C7 H7B 0.9700 C7 N2 1.474(6) C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C8 C9 1.522(7) C9 C10 1.408(8) C9 N2 1.312(6) C10 H10 0.9300 C10 C11 1.345(8) C11 C12 1.513(8) C11 O1 1.290(6) C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 C13 Si1 1.846(6) C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C14 Si1 1.863(8) C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C15 Si1 1.864(7) C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C16 Si2 1.870(9) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C17 Si2 1.818(8) C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C18 Si2 1.867(7) C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C19 Si3 1.892(8) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C20 Si3 1.867(7) C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C21 Si3 1.854(9) C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C22 Si4 1.866(6) C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 C23 Si4 1.872(6) C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C24 Si4 1.874(6) N1 Nd1 2.659(4) N2 Nd1 2.495(3) N3 Nd1 2.345(4) N3 Si1 1.696(4) N3 Si2 1.739(4) N4 Nd1 2.341(3) N4 Si3 1.697(4) N4 Si4 1.708(4) Nd1 O1 2.266(3)