#------------------------------------------------------------------------------ #$Date: 2022-07-06 11:19:06 +0300 (Wed, 06 Jul 2022) $ #$Revision: 276637 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/15/7061534.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_7061534 loop_ _publ_author_name 'Xu, Xiao' 'Xia, Ting' 'Chen, Xu-Lang' 'Hao, Xiang' 'Liang, Tongling' 'Li, Huan-Rong' 'Gong, Han-Yuan' _publ_section_title ; Tetrabenzo[b,de,gh,j][1,10]phenanthroline: a nitrogen-doped nanographene as a selective metal cation and proton fluorophore ; _journal_issue 24 _journal_name_full 'New Journal of Chemistry' _journal_page_first 11835 _journal_page_last 11839 _journal_paper_doi 10.1039/D2NJ01861F _journal_volume 46 _journal_year 2022 _chemical_formula_sum 'C27 H18 Cd N4 O7' _chemical_formula_weight 622.85 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-12-10 deposited with the CCDC. 2022-05-19 downloaded from the CCDC. ; _cell_angle_alpha 72.454(3) _cell_angle_beta 71.768(3) _cell_angle_gamma 86.420(3) _cell_formula_units_Z 2 _cell_length_a 8.5338(3) _cell_length_b 11.7951(4) _cell_length_c 12.6718(4) _cell_measurement_reflns_used 3697 _cell_measurement_temperature 170.00(12) _cell_measurement_theta_max 62.498 _cell_measurement_theta_min 3.847 _cell_volume 1154.39(7) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 170.00(12) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 11366 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 62.498 _diffrn_reflns_theta_max 62.498 _diffrn_reflns_theta_min 3.847 _exptl_absorpt_coefficient_mu 8.101 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74470 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'dark orange' _exptl_crystal_density_diffrn 1.792 _exptl_crystal_description plate _exptl_crystal_F_000 624 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.300 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 3697 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0220 _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^)+(0.0156P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0494 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3474 _reflns_number_total 3697 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2nj01861f2.cif _cod_data_source_block A_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7061532--7061536.cif.' _cod_database_code 7061534 _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_res_file ; TITL tx9668_xx_cd_a.res in P-1 A.res created by SHELXL-2018/3 at 08:15:38 on 10-Nov-2021 CELL 1.54184 8.5338 11.7951 12.6718 72.454 71.768 86.42 ZERR 2 0.0003 0.0004 0.0004 0.003 0.003 0.003 LATT 1 SFAC C H Cd N O UNIT 54 36 2 8 14 DFIX 0.85 0.01 O7 H7 DANG 1.899044 0.02 C27 H7 DANG 2.890962 0.02 Cd1 H7 L.S. 24 PLAN 5 CONF BOND $H HTAB LIST 6 fmap 2 ACTA MORE -1 MERG 2 OMIT -4 125 WGHT 0.015600 0.800000 FVAR 0.37960 CD1 3 0.502419 0.784814 0.179348 11.00000 0.02667 0.01953 = 0.01848 -0.00196 -0.00784 -0.00357 O1 5 0.758203 0.868852 0.038256 11.00000 0.04062 0.03675 = 0.04068 -0.01645 -0.00568 -0.00849 O2 5 0.715379 0.680582 0.077022 11.00000 0.03305 0.02913 = 0.03218 -0.00784 -0.00807 -0.00150 O3 5 0.950744 0.763534 -0.041354 11.00000 0.02447 0.07547 = 0.04434 -0.02832 -0.00622 -0.00169 O4 5 0.445595 0.985391 0.157431 11.00000 0.02554 0.02675 = 0.03034 0.00110 -0.00536 -0.00223 O5 5 0.229056 0.878212 0.273526 11.00000 0.03095 0.02537 = 0.03994 -0.00226 -0.00784 -0.00710 O6 5 0.228382 1.070612 0.238245 11.00000 0.04163 0.03148 = 0.04750 -0.02004 -0.01679 0.00811 O7 5 0.415551 0.817452 0.016921 11.00000 0.02974 0.03195 = 0.02207 0.00360 -0.01139 -0.00749 H7 2 0.472434 0.872408 -0.044053 11.00000 -1.50000 N1 4 0.531442 0.770247 0.359610 11.00000 0.02011 0.01865 = 0.02192 -0.00585 -0.00735 0.00209 N2 4 0.373723 0.609234 0.309277 11.00000 0.02216 0.01830 = 0.02053 -0.00508 -0.00941 0.00105 N3 4 0.812107 0.771111 0.022706 11.00000 0.02583 0.04321 = 0.02547 -0.01213 -0.01161 -0.00341 N4 4 0.296451 0.979663 0.224593 11.00000 0.02860 0.02545 = 0.02289 -0.00617 -0.01245 -0.00159 C1 1 0.620002 0.850164 0.381035 11.00000 0.02185 0.01785 = 0.02842 -0.00725 -0.01387 0.00359 C2 1 0.733515 0.929993 0.284835 11.00000 0.02698 0.02413 = 0.02857 -0.00279 -0.01249 -0.00092 AFIX 43 H2A 2 0.742301 0.930486 0.209669 11.00000 -1.20000 AFIX 0 C3 1 0.830698 1.006678 0.301812 11.00000 0.03018 0.02427 = 0.03971 -0.00413 -0.01532 -0.00549 AFIX 43 H3A 2 0.906063 1.058668 0.238329 11.00000 -1.20000 AFIX 0 C4 1 0.816385 1.006651 0.414801 11.00000 0.03830 0.02647 = 0.05000 -0.01189 -0.02345 -0.00439 AFIX 43 H4A 2 0.883080 1.058553 0.425968 11.00000 -1.20000 AFIX 0 C5 1 0.704969 0.930870 0.509585 11.00000 0.03836 0.02801 = 0.03614 -0.01383 -0.01952 0.00252 AFIX 43 H5A 2 0.696448 0.932768 0.584013 11.00000 -1.20000 AFIX 0 C6 1 0.603585 0.850421 0.495483 11.00000 0.02484 0.01901 = 0.03056 -0.00942 -0.01412 0.00582 C7 1 0.488916 0.765553 0.591214 11.00000 0.02344 0.02100 = 0.02703 -0.01070 -0.01138 0.00737 C8 1 0.458709 0.761771 0.708197 11.00000 0.03799 0.02648 = 0.02944 -0.01505 -0.01605 0.00598 AFIX 43 H8A 2 0.512427 0.816302 0.726079 11.00000 -1.20000 AFIX 0 C9 1 0.350387 0.677878 0.795323 11.00000 0.04849 0.03244 = 0.02231 -0.01286 -0.01164 0.00540 AFIX 43 H9A 2 0.330560 0.676566 0.872154 11.00000 -1.20000 AFIX 0 C10 1 0.269517 0.594760 0.771562 11.00000 0.03897 0.02711 = 0.02057 -0.00701 -0.00692 0.00270 AFIX 43 H10A 2 0.196064 0.539140 0.832736 11.00000 -1.20000 AFIX 0 C11 1 0.295867 0.592811 0.658421 11.00000 0.02236 0.02026 = 0.02150 -0.00638 -0.00800 0.00524 C12 1 0.405377 0.682143 0.566572 11.00000 0.02250 0.01841 = 0.02279 -0.00694 -0.00953 0.00621 C13 1 0.432276 0.688819 0.447486 11.00000 0.01899 0.01652 = 0.02181 -0.00495 -0.01017 0.00541 C14 1 0.348758 0.599742 0.419286 11.00000 0.01756 0.01494 = 0.02040 -0.00517 -0.00765 0.00382 C15 1 0.247604 0.505856 0.513059 11.00000 0.01864 0.01493 = 0.02192 -0.00363 -0.00676 0.00455 C16 1 0.218033 0.502548 0.630831 11.00000 0.02125 0.01939 = 0.02303 -0.00494 -0.00823 0.00450 C17 1 0.115087 0.411302 0.717200 11.00000 0.02514 0.02538 = 0.02021 -0.00158 -0.00522 0.00273 AFIX 43 H17A 2 0.092999 0.407544 0.794872 11.00000 -1.20000 AFIX 0 C18 1 0.044716 0.325663 0.689260 11.00000 0.02473 0.02121 = 0.02731 0.00122 -0.00433 -0.00071 AFIX 43 H18A 2 -0.023007 0.265348 0.748873 11.00000 -1.20000 AFIX 0 C19 1 0.072495 0.327770 0.576231 11.00000 0.02243 0.01743 = 0.03044 -0.00425 -0.00787 0.00105 AFIX 43 H19A 2 0.024464 0.269289 0.559624 11.00000 -1.20000 AFIX 0 C20 1 0.174494 0.419260 0.485054 11.00000 0.01873 0.01510 = 0.02566 -0.00331 -0.00872 0.00359 C21 1 0.208104 0.427192 0.364059 11.00000 0.02089 0.01745 = 0.02509 -0.00525 -0.00981 0.00240 C22 1 0.144141 0.345079 0.325741 11.00000 0.02997 0.01681 = 0.03260 -0.00451 -0.01243 -0.00061 AFIX 43 H22A 2 0.078175 0.280718 0.380344 11.00000 -1.20000 AFIX 0 C23 1 0.177196 0.358235 0.209944 11.00000 0.03841 0.02256 = 0.03939 -0.01420 -0.01967 0.00076 AFIX 43 H23A 2 0.133109 0.303236 0.186653 11.00000 -1.20000 AFIX 0 C24 1 0.277330 0.454280 0.125827 11.00000 0.04204 0.02572 = 0.02686 -0.01084 -0.01469 0.00202 AFIX 43 H24A 2 0.299675 0.462598 0.047127 11.00000 -1.20000 AFIX 0 C25 1 0.342063 0.535701 0.159780 11.00000 0.03275 0.02151 = 0.02318 -0.00596 -0.01127 -0.00207 AFIX 43 H25A 2 0.408781 0.599030 0.103974 11.00000 -1.20000 AFIX 0 C26 1 0.308103 0.523964 0.278586 11.00000 0.02141 0.01749 = 0.02533 -0.00681 -0.00991 0.00178 C27 1 0.249200 0.835705 0.014593 11.00000 0.03365 0.03411 = 0.02879 -0.00553 -0.01374 -0.00401 AFIX 33 H27A 2 0.245872 0.847178 -0.062957 11.00000 -1.50000 H27B 2 0.181063 0.767370 0.066776 11.00000 -1.50000 H27C 2 0.209038 0.904815 0.038396 11.00000 -1.50000 AFIX 0 HKLF 4 REM tx9668_xx_cd_a.res in P-1 REM wR2 = 0.0494, GooF = S = 1.003, Restrained GooF = 1.008 for all data REM R1 = 0.0220 for 3474 Fo > 4sig(Fo) and 0.0247 for all 3697 data REM 355 parameters refined using 3 restraints END WGHT 0.0151 0.6291 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+2, -z HTAB O7 O4_$1 HTAB C2 O1 HTAB C25 O7 HTAB C27 O1_$1 REM Highest difference peak 0.300, deepest hole -0.358, 1-sigma level 0.058 Q1 1 0.6140 0.8197 0.1323 11.00000 0.05 0.30 Q2 1 0.4524 0.8033 0.1015 11.00000 0.05 0.25 Q3 1 0.4079 0.6363 0.4245 11.00000 0.05 0.24 Q4 1 0.4256 0.6619 0.2654 11.00000 0.05 0.24 Q5 1 0.6000 0.6774 0.1543 11.00000 0.05 0.23 ; _shelx_res_checksum 25650 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Cd1 Cd 0.50242(2) 0.78481(2) 0.17935(2) 0.02201(7) Uani 1 1 d D . . . . O1 O 0.7582(3) 0.86885(17) 0.03826(16) 0.0394(5) Uani 1 1 d . . . . . O2 O 0.7154(2) 0.68058(16) 0.07702(15) 0.0321(4) Uani 1 1 d . . . . . O3 O 0.9507(2) 0.7635(2) -0.04135(18) 0.0466(5) Uani 1 1 d . . . . . O4 O 0.4456(2) 0.98539(15) 0.15743(15) 0.0304(4) Uani 1 1 d . . . . . O5 O 0.2291(2) 0.87821(16) 0.27353(16) 0.0342(4) Uani 1 1 d . . . . . O6 O 0.2284(2) 1.07061(16) 0.23824(17) 0.0379(5) Uani 1 1 d . . . . . O7 O 0.4156(2) 0.81745(15) 0.01692(14) 0.0294(4) Uani 1 1 d D . . . . H7 H 0.472(2) 0.872(2) -0.0441(14) 0.044 Uiso 1 1 d D U . . . N1 N 0.5314(2) 0.77025(17) 0.35961(16) 0.0201(4) Uani 1 1 d . . . . . N2 N 0.3737(2) 0.60923(16) 0.30928(16) 0.0198(4) Uani 1 1 d . . . . . N3 N 0.8121(3) 0.7711(2) 0.02271(18) 0.0299(5) Uani 1 1 d . . . . . N4 N 0.2965(3) 0.97966(18) 0.22459(17) 0.0247(5) Uani 1 1 d . . . . . C1 C 0.6200(3) 0.8502(2) 0.3810(2) 0.0213(5) Uani 1 1 d . . . . . C2 C 0.7335(3) 0.9300(2) 0.2848(2) 0.0267(5) Uani 1 1 d . . . . . H2A H 0.742301 0.930486 0.209669 0.032 Uiso 1 1 calc R U . . . C3 C 0.8307(3) 1.0067(2) 0.3018(2) 0.0312(6) Uani 1 1 d . . . . . H3A H 0.906063 1.058668 0.238329 0.037 Uiso 1 1 calc R U . . . C4 C 0.8164(4) 1.0067(2) 0.4148(3) 0.0355(6) Uani 1 1 d . . . . . H4A H 0.883080 1.058553 0.425968 0.043 Uiso 1 1 calc R U . . . C5 C 0.7050(3) 0.9309(2) 0.5096(2) 0.0313(6) Uani 1 1 d . . . . . H5A H 0.696448 0.932768 0.584013 0.038 Uiso 1 1 calc R U . . . C6 C 0.6036(3) 0.8504(2) 0.4955(2) 0.0232(5) Uani 1 1 d . . . . . C7 C 0.4889(3) 0.7656(2) 0.5912(2) 0.0224(5) Uani 1 1 d . . . . . C8 C 0.4587(3) 0.7618(2) 0.7082(2) 0.0286(6) Uani 1 1 d . . . . . H8A H 0.512427 0.816302 0.726079 0.034 Uiso 1 1 calc R U . . . C9 C 0.3504(4) 0.6779(2) 0.7953(2) 0.0333(6) Uani 1 1 d . . . . . H9A H 0.330560 0.676566 0.872154 0.040 Uiso 1 1 calc R U . . . C10 C 0.2695(3) 0.5948(2) 0.7716(2) 0.0295(6) Uani 1 1 d . . . . . H10A H 0.196064 0.539140 0.832736 0.035 Uiso 1 1 calc R U . . . C11 C 0.2959(3) 0.5928(2) 0.6584(2) 0.0212(5) Uani 1 1 d . . . . . C12 C 0.4054(3) 0.6821(2) 0.5666(2) 0.0207(5) Uani 1 1 d . . . . . C13 C 0.4323(3) 0.68882(19) 0.44749(19) 0.0186(5) Uani 1 1 d . . . . . C14 C 0.3488(3) 0.59974(19) 0.41929(19) 0.0174(5) Uani 1 1 d . . . . . C15 C 0.2476(3) 0.50586(19) 0.51306(19) 0.0190(5) Uani 1 1 d . . . . . C16 C 0.2180(3) 0.5025(2) 0.6308(2) 0.0214(5) Uani 1 1 d . . . . . C17 C 0.1151(3) 0.4113(2) 0.7172(2) 0.0253(5) Uani 1 1 d . . . . . H17A H 0.092999 0.407544 0.794872 0.030 Uiso 1 1 calc R U . . . C18 C 0.0447(3) 0.3257(2) 0.6893(2) 0.0272(6) Uani 1 1 d . . . . . H18A H -0.023007 0.265348 0.748873 0.033 Uiso 1 1 calc R U . . . C19 C 0.0725(3) 0.3278(2) 0.5762(2) 0.0242(5) Uani 1 1 d . . . . . H19A H 0.024464 0.269289 0.559624 0.029 Uiso 1 1 calc R U . . . C20 C 0.1745(3) 0.41926(19) 0.4851(2) 0.0202(5) Uani 1 1 d . . . . . C21 C 0.2081(3) 0.4272(2) 0.3641(2) 0.0208(5) Uani 1 1 d . . . . . C22 C 0.1441(3) 0.3451(2) 0.3257(2) 0.0264(5) Uani 1 1 d . . . . . H22A H 0.078175 0.280718 0.380344 0.032 Uiso 1 1 calc R U . . . C23 C 0.1772(3) 0.3582(2) 0.2099(2) 0.0304(6) Uani 1 1 d . . . . . H23A H 0.133109 0.303236 0.186653 0.037 Uiso 1 1 calc R U . . . C24 C 0.2773(3) 0.4543(2) 0.1258(2) 0.0299(6) Uani 1 1 d . . . . . H24A H 0.299675 0.462598 0.047127 0.036 Uiso 1 1 calc R U . . . C25 C 0.3421(3) 0.5357(2) 0.1598(2) 0.0252(5) Uani 1 1 d . . . . . H25A H 0.408781 0.599030 0.103974 0.030 Uiso 1 1 calc R U . . . C26 C 0.3081(3) 0.5240(2) 0.2786(2) 0.0207(5) Uani 1 1 d . . . . . C27 C 0.2492(3) 0.8357(2) 0.0146(2) 0.0318(6) Uani 1 1 d D . . . . H27A H 0.245872 0.847178 -0.062957 0.048 Uiso 1 1 calc R U . . . H27B H 0.181063 0.767370 0.066776 0.048 Uiso 1 1 calc R U . . . H27C H 0.209038 0.904815 0.038396 0.048 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 Cd1 0.02667(10) 0.01953(9) 0.01848(9) -0.00196(6) -0.00784(7) -0.00357(6) O1 0.0406(11) 0.0368(11) 0.0407(11) -0.0164(9) -0.0057(9) -0.0085(9) O2 0.0331(10) 0.0291(10) 0.0322(9) -0.0078(8) -0.0081(8) -0.0015(8) O3 0.0245(11) 0.0755(15) 0.0443(11) -0.0283(11) -0.0062(9) -0.0017(10) O4 0.0255(10) 0.0268(9) 0.0303(9) 0.0011(7) -0.0054(8) -0.0022(7) O5 0.0309(10) 0.0254(9) 0.0399(10) -0.0023(8) -0.0078(8) -0.0071(8) O6 0.0416(11) 0.0315(10) 0.0475(11) -0.0200(9) -0.0168(9) 0.0081(9) O7 0.0297(10) 0.0320(10) 0.0221(8) 0.0036(7) -0.0114(7) -0.0075(8) N1 0.0201(10) 0.0187(10) 0.0219(10) -0.0059(8) -0.0074(8) 0.0021(8) N2 0.0222(10) 0.0183(10) 0.0205(10) -0.0051(8) -0.0094(8) 0.0010(8) N3 0.0258(12) 0.0432(14) 0.0255(11) -0.0121(10) -0.0116(10) -0.0034(10) N4 0.0286(12) 0.0254(11) 0.0229(10) -0.0062(9) -0.0125(9) -0.0016(9) C1 0.0219(12) 0.0179(11) 0.0284(12) -0.0072(9) -0.0139(10) 0.0036(9) C2 0.0270(13) 0.0241(13) 0.0286(13) -0.0028(10) -0.0125(11) -0.0009(10) C3 0.0302(14) 0.0243(13) 0.0397(15) -0.0041(11) -0.0153(12) -0.0055(11) C4 0.0383(16) 0.0265(14) 0.0500(17) -0.0119(12) -0.0234(14) -0.0044(12) C5 0.0384(15) 0.0280(14) 0.0361(14) -0.0138(11) -0.0195(12) 0.0025(12) C6 0.0248(13) 0.0190(11) 0.0306(13) -0.0094(10) -0.0141(11) 0.0058(10) C7 0.0234(13) 0.0210(12) 0.0270(12) -0.0107(10) -0.0114(10) 0.0074(10) C8 0.0380(15) 0.0265(13) 0.0294(13) -0.0150(11) -0.0161(11) 0.0060(11) C9 0.0485(17) 0.0324(14) 0.0223(12) -0.0129(11) -0.0116(12) 0.0054(13) C10 0.0390(15) 0.0271(13) 0.0206(12) -0.0070(10) -0.0069(11) 0.0027(11) C11 0.0224(12) 0.0203(12) 0.0215(12) -0.0064(9) -0.0080(10) 0.0052(10) C12 0.0225(12) 0.0184(11) 0.0228(11) -0.0069(9) -0.0095(10) 0.0062(9) C13 0.0190(12) 0.0165(11) 0.0218(11) -0.0050(9) -0.0102(10) 0.0054(9) C14 0.0176(11) 0.0149(11) 0.0204(11) -0.0052(9) -0.0076(9) 0.0038(9) C15 0.0186(12) 0.0149(11) 0.0219(11) -0.0036(9) -0.0068(9) 0.0046(9) C16 0.0213(12) 0.0194(12) 0.0230(12) -0.0049(9) -0.0082(10) 0.0045(10) C17 0.0251(13) 0.0254(13) 0.0202(12) -0.0016(10) -0.0052(10) 0.0027(10) C18 0.0247(13) 0.0212(12) 0.0273(13) 0.0012(10) -0.0043(10) -0.0007(10) C19 0.0224(13) 0.0174(12) 0.0304(13) -0.0042(10) -0.0079(10) 0.0011(10) C20 0.0187(12) 0.0151(11) 0.0257(12) -0.0033(9) -0.0087(10) 0.0036(9) C21 0.0209(12) 0.0174(11) 0.0251(12) -0.0053(9) -0.0098(10) 0.0024(9) C22 0.0300(14) 0.0168(12) 0.0326(13) -0.0045(10) -0.0124(11) -0.0006(10) C23 0.0384(15) 0.0226(13) 0.0394(15) -0.0142(11) -0.0197(12) 0.0008(11) C24 0.0420(16) 0.0257(13) 0.0269(13) -0.0108(10) -0.0147(12) 0.0020(11) C25 0.0328(14) 0.0215(12) 0.0232(12) -0.0060(10) -0.0113(11) -0.0021(10) C26 0.0214(12) 0.0175(11) 0.0253(12) -0.0068(9) -0.0099(10) 0.0018(9) C27 0.0337(15) 0.0341(14) 0.0288(13) -0.0055(11) -0.0137(11) -0.0040(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 N2 Cd1 O7 106.33(6) . . ? N2 Cd1 N1 72.01(7) . . ? O7 Cd1 N1 166.78(6) . . ? N2 Cd1 O4 133.92(6) . . ? O7 Cd1 O4 83.67(6) . . ? N1 Cd1 O4 88.35(6) . . ? N2 Cd1 O2 91.61(6) . . ? O7 Cd1 O2 82.82(6) . . ? N1 Cd1 O2 110.20(6) . . ? O4 Cd1 O2 134.47(6) . . ? N2 Cd1 O1 143.09(7) . . ? O7 Cd1 O1 83.40(6) . . ? N1 Cd1 O1 105.92(7) . . ? O4 Cd1 O1 81.76(6) . . ? O2 Cd1 O1 53.60(6) . . ? N2 Cd1 O5 83.68(6) . . ? O7 Cd1 O5 87.44(6) . . ? N1 Cd1 O5 79.35(6) . . ? O4 Cd1 O5 51.32(6) . . ? O2 Cd1 O5 167.55(6) . . ? O1 Cd1 O5 132.94(6) . . ? N3 O1 Cd1 94.86(14) . . ? N3 O2 Cd1 94.72(14) . . ? N4 O4 Cd1 102.12(13) . . ? N4 O5 Cd1 89.89(14) . . ? C27 O7 Cd1 125.71(15) . . ? C27 O7 H7 103.7(13) . . ? Cd1 O7 H7 114.5(13) . . ? C13 N1 C1 119.9(2) . . ? C13 N1 Cd1 114.09(15) . . ? C1 N1 Cd1 125.11(14) . . ? C14 N2 C26 120.41(19) . . ? C14 N2 Cd1 115.08(15) . . ? C26 N2 Cd1 124.09(14) . . ? O3 N3 O1 122.0(2) . . ? O3 N3 O2 121.4(2) . . ? O1 N3 O2 116.7(2) . . ? O6 N4 O5 123.6(2) . . ? O6 N4 O4 119.8(2) . . ? O5 N4 O4 116.6(2) . . ? N1 C1 C2 118.0(2) . . ? N1 C1 C6 121.7(2) . . ? C2 C1 C6 120.2(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 117.9(2) . . ? C5 C6 C7 123.7(2) . . ? C1 C6 C7 118.4(2) . . ? C12 C7 C8 118.8(2) . . ? C12 C7 C6 118.4(2) . . ? C8 C7 C6 122.7(2) . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.4(2) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C11 121.4(2) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C12 117.6(2) . . ? C10 C11 C16 122.6(2) . . ? C12 C11 C16 119.7(2) . . ? C7 C12 C11 120.8(2) . . ? C7 C12 C13 118.6(2) . . ? C11 C12 C13 120.6(2) . . ? N1 C13 C12 122.8(2) . . ? N1 C13 C14 117.5(2) . . ? C12 C13 C14 119.64(19) . . ? N2 C14 C15 122.8(2) . . ? N2 C14 C13 118.26(19) . . ? C15 C14 C13 118.9(2) . . ? C20 C15 C16 121.0(2) . . ? C20 C15 C14 118.3(2) . . ? C16 C15 C14 120.7(2) . . ? C17 C16 C15 117.8(2) . . ? C17 C16 C11 122.0(2) . . ? C15 C16 C11 120.2(2) . . ? C18 C17 C16 121.0(2) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C19 C18 C17 121.7(2) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 119.6(2) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C19 C20 C15 118.9(2) . . ? C19 C20 C21 122.5(2) . . ? C15 C20 C21 118.6(2) . . ? C22 C21 C26 117.8(2) . . ? C22 C21 C20 123.7(2) . . ? C26 C21 C20 118.4(2) . . ? C23 C22 C21 121.3(2) . . ? C23 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? C22 C23 C24 120.4(2) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? N2 C26 C25 118.5(2) . . ? N2 C26 C21 121.3(2) . . ? C25 C26 C21 120.2(2) . . ? O7 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.3027(18) . ? Cd1 O7 2.3185(16) . ? Cd1 N1 2.3282(19) . ? Cd1 O4 2.3354(18) . ? Cd1 O2 2.3881(19) . ? Cd1 O1 2.3882(19) . ? Cd1 O5 2.6095(19) . ? O1 N3 1.262(3) . ? O2 N3 1.268(3) . ? O3 N3 1.223(3) . ? O4 N4 1.283(3) . ? O5 N4 1.250(3) . ? O6 N4 1.220(3) . ? O7 C27 1.431(3) . ? O7 H7 0.869(9) . ? N1 C13 1.321(3) . ? N1 C1 1.380(3) . ? N2 C14 1.313(3) . ? N2 C26 1.385(3) . ? C1 C2 1.412(4) . ? C1 C6 1.414(3) . ? C2 C3 1.369(4) . ? C2 H2A 0.9300 . ? C3 C4 1.398(4) . ? C3 H3A 0.9300 . ? C4 C5 1.375(4) . ? C4 H4A 0.9300 . ? C5 C6 1.408(4) . ? C5 H5A 0.9300 . ? C6 C7 1.442(4) . ? C7 C12 1.409(3) . ? C7 C8 1.410(3) . ? C8 C9 1.367(4) . ? C8 H8A 0.9300 . ? C9 C10 1.386(4) . ? C9 H9A 0.9300 . ? C10 C11 1.387(3) . ? C10 H10A 0.9300 . ? C11 C12 1.429(3) . ? C11 C16 1.468(3) . ? C12 C13 1.432(3) . ? C13 C14 1.490(3) . ? C14 C15 1.438(3) . ? C15 C20 1.412(3) . ? C15 C16 1.422(3) . ? C16 C17 1.391(3) . ? C17 C18 1.390(4) . ? C17 H17A 0.9300 . ? C18 C19 1.369(4) . ? C18 H18A 0.9300 . ? C19 C20 1.412(3) . ? C19 H19A 0.9300 . ? C20 C21 1.443(3) . ? C21 C22 1.410(4) . ? C21 C26 1.415(3) . ? C22 C23 1.366(4) . ? C22 H22A 0.9300 . ? C23 C24 1.404(4) . ? C23 H23A 0.9300 . ? C24 C25 1.370(4) . ? C24 H24A 0.9300 . ? C25 C26 1.406(3) . ? C25 H25A 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd1 O1 N3 O3 -176.31(19) . . . . ? Cd1 O1 N3 O2 3.6(2) . . . . ? Cd1 O2 N3 O3 176.31(19) . . . . ? Cd1 O2 N3 O1 -3.6(2) . . . . ? Cd1 O5 N4 O6 -177.2(2) . . . . ? Cd1 O5 N4 O4 2.45(19) . . . . ? Cd1 O4 N4 O6 176.83(17) . . . . ? Cd1 O4 N4 O5 -2.8(2) . . . . ? C13 N1 C1 C2 175.4(2) . . . . ? Cd1 N1 C1 C2 -16.2(3) . . . . ? C13 N1 C1 C6 -2.3(3) . . . . ? Cd1 N1 C1 C6 166.08(17) . . . . ? N1 C1 C2 C3 -176.5(2) . . . . ? C6 C1 C2 C3 1.2(4) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? C4 C5 C6 C7 177.5(2) . . . . ? N1 C1 C6 C5 176.7(2) . . . . ? C2 C1 C6 C5 -0.9(3) . . . . ? N1 C1 C6 C7 -1.0(3) . . . . ? C2 C1 C6 C7 -178.6(2) . . . . ? C5 C6 C7 C12 -174.1(2) . . . . ? C1 C6 C7 C12 3.4(3) . . . . ? C5 C6 C7 C8 5.1(4) . . . . ? C1 C6 C7 C8 -177.4(2) . . . . ? C12 C7 C8 C9 0.2(4) . . . . ? C6 C7 C8 C9 -179.0(2) . . . . ? C7 C8 C9 C10 0.6(4) . . . . ? C8 C9 C10 C11 0.4(4) . . . . ? C9 C10 C11 C12 -2.0(4) . . . . ? C9 C10 C11 C16 177.1(2) . . . . ? C8 C7 C12 C11 -2.0(3) . . . . ? C6 C7 C12 C11 177.3(2) . . . . ? C8 C7 C12 C13 178.0(2) . . . . ? C6 C7 C12 C13 -2.8(3) . . . . ? C10 C11 C12 C7 2.8(3) . . . . ? C16 C11 C12 C7 -176.3(2) . . . . ? C10 C11 C12 C13 -177.1(2) . . . . ? C16 C11 C12 C13 3.8(3) . . . . ? C1 N1 C13 C12 2.9(3) . . . . ? Cd1 N1 C13 C12 -166.62(17) . . . . ? C1 N1 C13 C14 -175.88(19) . . . . ? Cd1 N1 C13 C14 14.6(2) . . . . ? C7 C12 C13 N1 -0.4(3) . . . . ? C11 C12 C13 N1 179.5(2) . . . . ? C7 C12 C13 C14 178.4(2) . . . . ? C11 C12 C13 C14 -1.7(3) . . . . ? C26 N2 C14 C15 -3.1(3) . . . . ? Cd1 N2 C14 C15 169.79(16) . . . . ? C26 N2 C14 C13 175.53(19) . . . . ? Cd1 N2 C14 C13 -11.6(3) . . . . ? N1 C13 C14 N2 -2.2(3) . . . . ? C12 C13 C14 N2 178.9(2) . . . . ? N1 C13 C14 C15 176.4(2) . . . . ? C12 C13 C14 C15 -2.4(3) . . . . ? N2 C14 C15 C20 1.1(3) . . . . ? C13 C14 C15 C20 -177.50(19) . . . . ? N2 C14 C15 C16 -177.0(2) . . . . ? C13 C14 C15 C16 4.4(3) . . . . ? C20 C15 C16 C17 0.1(3) . . . . ? C14 C15 C16 C17 178.1(2) . . . . ? C20 C15 C16 C11 179.6(2) . . . . ? C14 C15 C16 C11 -2.3(3) . . . . ? C10 C11 C16 C17 -1.4(4) . . . . ? C12 C11 C16 C17 177.7(2) . . . . ? C10 C11 C16 C15 179.1(2) . . . . ? C12 C11 C16 C15 -1.8(3) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C11 C16 C17 C18 -179.0(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C15 0.9(3) . . . . ? C18 C19 C20 C21 -179.6(2) . . . . ? C16 C15 C20 C19 -0.8(3) . . . . ? C14 C15 C20 C19 -178.9(2) . . . . ? C16 C15 C20 C21 179.7(2) . . . . ? C14 C15 C20 C21 1.6(3) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C15 C20 C21 C22 179.1(2) . . . . ? C19 C20 C21 C26 178.2(2) . . . . ? C15 C20 C21 C26 -2.3(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? C20 C21 C22 C23 178.6(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 C26 -0.3(4) . . . . ? C14 N2 C26 C25 -178.1(2) . . . . ? Cd1 N2 C26 C25 9.7(3) . . . . ? C14 N2 C26 C21 2.3(3) . . . . ? Cd1 N2 C26 C21 -169.88(16) . . . . ? C24 C25 C26 N2 -179.0(2) . . . . ? C24 C25 C26 C21 0.7(4) . . . . ? C22 C21 C26 N2 179.1(2) . . . . ? C20 C21 C26 N2 0.4(3) . . . . ? C22 C21 C26 C25 -0.5(3) . . . . ? C20 C21 C26 C25 -179.2(2) . . . . ?