#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239046.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_2239046 loop_ _publ_author_name '\,Celik, Fatih' 'Dilek, Nefise' '\,Caylak Deliba\,s, Nagihan' 'Necefo\(glu, Hacali' 'H\"okelek, Tuncer' _publ_section_title ; catena-Poly[[aquabis(4-formylbenzoato-\k^2^O^1^,O^1'^)cadmium]-\m-pyrazine-\k^2^N:N'] ; _journal_coeditor_code SU2679 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m37 _journal_page_last m38 _journal_paper_doi 10.1107/S1600536813035010 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac '[Cd (C8 H5 O3)2 (C4 H4 N2) (H2 O)]' _chemical_formula_moiety 'C20 H16 Cd N2 O7' _chemical_formula_sum 'C20 H16 Cd N2 O7' _chemical_formula_weight 508.76 _chemical_name_systematic catena-Poly[[aquabis(4-formylbenzoato-\k^2^O^1^,O^1'^)cadmium]-\m-pyrazine-\k^2^N:N'] _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.673(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 22.6016(5) _cell_length_b 7.4947(2) _cell_length_c 11.9196(3) _cell_measurement_reflns_used 9816 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 28.42 _cell_measurement_theta_min 2.72 _cell_volume 1990.38(9) _computing_cell_refinement 'SAINT (Bruker, 2012)' _computing_data_collection 'APEX2 (Bruker, 2012)' _computing_data_reduction 'SAINT (Bruker, 2012)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012) and PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART BREEZE CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 40178 _diffrn_reflns_theta_full 25.25 _diffrn_reflns_theta_max 25.25 _diffrn_reflns_theta_min 1.83 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2012)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.770 _refine_diff_density_min -1.847 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.345 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 3587 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.344 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0585 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+14.8406P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1439 _refine_ls_wR_factor_ref 0.1443 _reflns_number_gt 3497 _reflns_number_total 3587 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL I P 21/C R 0.07 CELL 0.71073 22.6016 7.4947 11.9196 90.000 99.673 90.000 ZERR 4.00 0.0005 0.0002 0.0003 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CD N O UNIT 80 64 4 8 27 MERG 2 OMIT 0.00 50.50 OMIT 2 2 2 DFIX 0.82 .02 O7 H71 O7 H72 DFIX 1.35 .02 H71 H72 HTAB O7 N1 EQIV $1 X, -Y+1/2, Z-1/2 HTAB O7 O5_$1 EQIV $2 -X, -Y+1, -Z HTAB C18 O6A_$2 EQIV $3 -X+1, -Y+1, -Z+1 HTAB C19 O3_$3 HTAB C20 O1 EADP C10B C11B C12B C14B C15B EADP C10A C11A C12A C14A C15A HTAB O7 N1 HTAB O7 O5_$1 HTAB C18 O6A_$2 HTAB C19 O3_$3 HTAB C20 O1 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP 21.00 WGHT 0.031600 14.840600 FVAR 0.28652 0.78784 CD1 3 0.252291 0.176413 0.129176 11.00000 0.03345 0.02044 = 0.02677 -0.00010 0.00312 -0.00118 O1 5 0.323748 0.191371 0.298300 11.00000 0.03087 0.06010 = 0.04462 -0.00998 0.00709 0.00676 O2 5 0.360111 0.150430 0.142992 11.00000 0.04202 0.09175 = 0.03481 -0.00051 0.00195 -0.00797 O3 5 0.625688 0.268530 0.577711 11.00000 0.06791 0.14740 = 0.08372 0.00310 -0.02985 -0.01715 O4 5 0.144670 0.168732 0.079767 11.00000 0.03644 0.08667 = 0.04259 0.00910 0.00801 0.00180 O5 5 0.182928 0.159690 0.259446 11.00000 0.03358 0.07057 = 0.04475 -0.02052 0.00076 -0.00585 PART 1 O6A 5 -0.144927 0.133785 0.227995 21.00000 0.03637 0.23268 = 0.10210 0.02559 0.01307 0.00811 PART 2 O6B 5 -0.111129 0.138842 0.378111 -21.00000 0.09799 0.21203 = 0.20014 0.04129 0.10235 -0.00492 PART 0 O7 5 0.252100 0.171315 -0.062500 11.00000 0.04359 0.03689 = 0.02720 0.00207 0.00351 -0.00014 N1 4 0.251934 0.479715 0.124247 11.00000 0.01037 0.06782 = 0.01073 -0.00542 -0.00079 -0.00005 N2 4 0.250303 0.864455 0.121613 11.00000 0.03458 0.00551 = 0.03770 -0.00111 0.00284 0.00181 C1 1 0.367803 0.170025 0.247191 11.00000 0.03476 0.02268 = 0.04086 0.00173 0.00401 -0.00127 C2 1 0.429736 0.171165 0.314283 11.00000 0.03505 0.02355 = 0.03287 0.00355 0.00681 -0.00280 C3 1 0.442118 0.252232 0.420058 11.00000 0.03923 0.04786 = 0.03652 -0.00839 0.01194 0.00336 AFIX 43 H3 2 0.411224 0.302484 0.452099 11.00000 -1.20000 AFIX 0 C4 1 0.500496 0.258351 0.477975 11.00000 0.04724 0.06034 = 0.03111 -0.00614 0.00031 -0.00717 AFIX 43 H4 2 0.508859 0.315777 0.548015 11.00000 -1.20000 AFIX 0 C5 1 0.546021 0.180552 0.432989 11.00000 0.03354 0.05664 = 0.04966 0.01040 0.00054 -0.00053 C6 1 0.533596 0.095004 0.329352 11.00000 0.03786 0.07767 = 0.06361 -0.00610 0.01362 0.00832 AFIX 43 H6 2 0.564491 0.040222 0.299621 11.00000 -1.20000 AFIX 0 C7 1 0.476041 0.089670 0.269350 11.00000 0.03956 0.05420 = 0.04345 -0.00832 0.01195 0.00265 AFIX 43 H7 2 0.468079 0.032110 0.199314 11.00000 -1.20000 AFIX 0 C8 1 0.608208 0.188927 0.495982 11.00000 0.04242 0.12289 = 0.07453 0.00231 -0.01056 -0.00433 AFIX 43 H8 2 0.636584 0.122106 0.466177 11.00000 -1.20000 AFIX 0 C9 1 0.138692 0.161307 0.181333 11.00000 0.03719 0.02091 = 0.04215 -0.00439 0.00592 0.00100 C10 1 0.076741 0.147487 0.211088 11.00000 0.03410 0.03540 = 0.03434 -0.00316 0.00190 -0.00231 C13 1 -0.038635 0.129598 0.261959 11.00000 0.04082 0.06757 = 0.05663 -0.00609 0.01332 0.00228 PART 1 C11A 1 0.065315 0.171133 0.320196 10.50000 0.03887 0.07028 = 0.04161 0.00162 0.00617 0.00899 AFIX 43 H11A 2 0.097161 0.187951 0.379660 10.50000 -1.20000 AFIX 0 C12A 1 0.007434 0.170211 0.342413 10.50000 0.03887 0.07028 = 0.04161 0.00162 0.00617 0.00899 AFIX 43 H12A 2 0.000527 0.198549 0.415068 10.50000 -1.20000 AFIX 0 C14A 1 -0.027833 0.089200 0.152750 10.50000 0.03887 0.07028 = 0.04161 0.00162 0.00617 0.00899 AFIX 43 H14A 2 -0.059182 0.052887 0.096583 10.50000 -1.20000 AFIX 0 C15A 1 0.030126 0.103615 0.128492 10.50000 0.03887 0.07028 = 0.04161 0.00162 0.00617 0.00899 AFIX 43 H15A 2 0.036948 0.082917 0.054800 10.50000 -1.20000 AFIX 0 PART 2 C11B 1 0.070196 0.105606 0.319495 10.50000 0.03864 0.08930 = 0.04035 0.00366 0.00199 0.01192 AFIX 43 H11B 2 0.103832 0.085641 0.374674 10.50000 -1.20000 AFIX 0 C12B 1 0.012578 0.092707 0.347586 10.50000 0.03864 0.08930 = 0.04035 0.00366 0.00199 0.01192 AFIX 43 H12B 2 0.007579 0.060649 0.420786 10.50000 -1.20000 AFIX 0 C14B 1 -0.030457 0.170889 0.153110 10.50000 0.03864 0.08930 = 0.04035 0.00366 0.00199 0.01192 AFIX 43 H14B 2 -0.063462 0.196552 0.097636 10.50000 -1.20000 AFIX 0 C15B 1 0.025498 0.174298 0.126449 10.50000 0.03864 0.08930 = 0.04035 0.00366 0.00199 0.01192 AFIX 43 H15B 2 0.030329 0.194521 0.051540 10.50000 -1.20000 AFIX 0 PART 0 C16 1 -0.099593 0.125865 0.290818 11.00000 0.05485 0.11720 = 0.07474 0.00183 0.02302 -0.00517 PART 1 AFIX 43 H16A 2 -0.102093 0.116109 0.367662 10.80000 -1.20000 PART 2 H16B 2 -0.131333 0.110390 0.230977 10.20000 -1.20000 AFIX 0 PART 0 C17 1 0.226414 0.586117 0.030980 11.00000 0.04518 0.03644 = 0.04679 -0.01289 -0.00347 -0.00432 AFIX 43 H17 2 0.208693 0.528269 -0.035225 11.00000 -1.20000 AFIX 0 C18 1 0.225950 0.770534 0.031286 11.00000 0.04873 0.02242 = 0.04101 0.00500 -0.00728 -0.00475 AFIX 43 H18 2 0.208001 0.830620 -0.033884 11.00000 -1.20000 AFIX 0 C19 1 0.275526 0.772763 0.211341 11.00000 0.05582 0.02557 = 0.02960 0.00250 -0.00246 -0.01117 AFIX 43 H19 2 0.293274 0.834042 0.276177 11.00000 -1.20000 AFIX 0 C20 1 0.276437 0.587697 0.212131 11.00000 0.05101 0.02342 = 0.03683 0.00552 0.00385 -0.00082 AFIX 43 H20 2 0.295401 0.532322 0.278328 11.00000 -1.20000 AFIX 0 H71 2 0.262643 0.277569 -0.053646 11.00000 -1.50000 H72 2 0.221009 0.167651 -0.109377 11.00000 -1.50000 HKLF 4 REM I P 21/C R 0.07 REM R1 = 0.0585 for 3497 Fo > 4sig(Fo) and 0.0595 for all 3587 data REM 287 parameters refined using 3 restraints END WGHT 0.0316 14.8416 REM Highest difference peak 1.770, deepest hole -1.847, 1-sigma level 0.129 Q1 1 0.2434 0.4168 0.1156 11.00000 0.05 1.77 Q2 1 0.2470 0.5270 0.1038 11.00000 0.05 1.44 Q3 1 0.2367 0.2523 0.0849 11.00000 0.05 1.30 Q4 1 0.2669 0.4857 0.1545 11.00000 0.05 1.28 Q5 1 0.2682 0.3172 0.1593 11.00000 0.05 1.10 Q6 1 0.2363 0.1096 0.0815 11.00000 0.05 1.03 Q7 1 0.2648 1.0042 0.1443 11.00000 0.05 0.63 Q8 1 0.2781 0.1708 0.1945 11.00000 0.05 0.56 Q9 1 0.5403 0.3159 0.4274 11.00000 0.05 0.54 Q10 1 0.2471 0.4656 -0.0588 11.00000 0.05 0.49 Q11 1 0.5219 -0.0795 0.2376 11.00000 0.05 0.47 Q12 1 0.3288 0.3279 0.3059 11.00000 0.05 0.46 Q13 1 -0.1786 -0.0238 0.2510 11.00000 0.05 0.44 Q14 1 0.2842 0.1445 0.0993 11.00000 0.05 0.43 Q15 1 -0.0128 0.1027 0.3135 11.00000 0.05 0.42 Q16 1 -0.0680 -0.0378 0.1853 11.00000 0.05 0.42 Q17 1 0.2588 0.6941 0.1541 11.00000 0.05 0.40 Q18 1 0.3587 0.2437 0.0566 11.00000 0.05 0.40 Q19 1 0.2227 0.8345 0.0126 11.00000 0.05 0.38 Q20 1 0.2790 0.2394 -0.1165 11.00000 0.05 0.38 ; _cod_data_source_file su2679sup1.cf _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2239046 _cod_database_fobs_code 2239046 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.25229(2) 0.17641(6) 0.12918(4) 0.02711(18) Uani d . 1 1 . . O O1 0.3237(2) 0.1914(8) 0.2983(4) 0.0451(13) Uani d . 1 1 . . O O2 0.3601(2) 0.1504(9) 0.1430(5) 0.0567(16) Uani d . 1 1 . . O O3 0.6257(4) 0.2685(15) 0.5777(8) 0.105(3) Uani d . 1 1 . . O O4 0.1447(2) 0.1687(9) 0.0798(5) 0.0551(16) Uani d . 1 1 . . O O5 0.1829(2) 0.1597(8) 0.2594(5) 0.0503(15) Uani d . 1 1 . . O O6A -0.1449(4) 0.134(2) 0.2280(11) 0.124(6) Uani d P 0.79(2) 1 A 1 O O6B -0.111(2) 0.139(9) 0.378(6) 0.16(3) Uani d P 0.21(2) 1 A 2 O O7 0.2521(2) 0.1713(7) -0.0625(4) 0.0362(11) Uani d D 1 1 . . H H71 0.263(3) 0.278(4) -0.054(7) 0.056 Uiso d D 1 1 . . H H72 0.221(2) 0.168(9) -0.109(6) 0.056 Uiso d D 1 1 . . N N1 0.2519(2) 0.4797(9) 0.1242(4) 0.0299(13) Uani d . 1 1 . . N N2 0.2503(2) 0.8645(6) 0.1216(5) 0.0263(11) Uani d . 1 1 . . C C1 0.3678(3) 0.1700(9) 0.2472(6) 0.0330(15) Uani d . 1 1 . . C C2 0.4297(3) 0.1712(9) 0.3143(6) 0.0304(14) Uani d . 1 1 . . C C3 0.4421(3) 0.2522(11) 0.4201(6) 0.0406(17) Uani d . 1 1 . . H H3 0.4112 0.3025 0.4521 0.049 Uiso calc R 1 1 . . C C4 0.5005(4) 0.2584(12) 0.4780(6) 0.047(2) Uani d . 1 1 . . H H4 0.5089 0.3158 0.5480 0.056 Uiso calc R 1 1 . . C C5 0.5460(3) 0.1806(12) 0.4330(7) 0.047(2) Uani d . 1 1 . . C C6 0.5336(4) 0.0950(14) 0.3294(8) 0.059(2) Uani d . 1 1 . . H H6 0.5645 0.0402 0.2996 0.071 Uiso calc R 1 1 . . C C7 0.4760(3) 0.0897(12) 0.2694(7) 0.0452(19) Uani d . 1 1 . . H H7 0.4681 0.0321 0.1993 0.054 Uiso calc R 1 1 . . C C8 0.6082(4) 0.1889(19) 0.4960(10) 0.082(4) Uani d . 1 1 . . H H8 0.6366 0.1221 0.4662 0.099 Uiso calc R 1 1 . . C C9 0.1387(3) 0.1613(9) 0.1813(6) 0.0335(15) Uani d . 1 1 B . C C10 0.0767(3) 0.1475(10) 0.2111(6) 0.0351(16) Uani d . 1 1 . . C C13 -0.0386(4) 0.1296(14) 0.2620(8) 0.054(2) Uani d . 1 1 . . C C11A 0.0653(14) 0.171(3) 0.320(3) 0.050(4) Uani d P 0.50 1 B 1 H H11A 0.0972 0.1880 0.3797 0.060 Uiso calc PR 0.50 1 B 1 C C12A 0.0074(12) 0.170(3) 0.342(2) 0.050(4) Uani d P 0.50 1 B 1 H H12A 0.0005 0.1985 0.4151 0.060 Uiso calc PR 0.50 1 B 1 C C14A -0.0278(12) 0.089(3) 0.153(2) 0.050(4) Uani d P 0.50 1 B 1 H H14A -0.0592 0.0529 0.0966 0.060 Uiso calc PR 0.50 1 B 1 C C15A 0.0301(13) 0.104(3) 0.128(3) 0.050(4) Uani d P 0.50 1 B 1 H H15A 0.0369 0.0829 0.0548 0.060 Uiso calc PR 0.50 1 B 1 C C11B 0.0702(14) 0.106(4) 0.319(3) 0.057(5) Uani d P 0.50 1 B 2 H H11B 0.1038 0.0856 0.3747 0.068 Uiso calc PR 0.50 1 B 2 C C12B 0.0126(12) 0.093(3) 0.348(2) 0.057(5) Uani d P 0.50 1 B 2 H H12B 0.0076 0.0606 0.4208 0.068 Uiso calc PR 0.50 1 B 2 C C14B -0.0305(12) 0.171(3) 0.153(2) 0.057(5) Uani d P 0.50 1 B 2 H H14B -0.0635 0.1966 0.0976 0.068 Uiso calc PR 0.50 1 B 2 C C15B 0.0255(13) 0.174(3) 0.126(3) 0.057(5) Uani d P 0.50 1 B 2 H H15B 0.0303 0.1945 0.0515 0.068 Uiso calc PR 0.50 1 B 2 C C16 -0.0996(5) 0.1259(19) 0.2908(12) 0.081(3) Uani d . 1 1 A . H H16A -0.1021 0.1161 0.3677 0.097 Uiso calc PR 0.80 1 C 1 H H16B -0.1313 0.1104 0.2310 0.097 Uiso d PR 0.20 1 C 2 C C17 0.2264(3) 0.5861(11) 0.0310(7) 0.0441(18) Uani d . 1 1 . . H H17 0.2087 0.5283 -0.0352 0.053 Uiso calc R 1 1 . . C C18 0.2260(3) 0.7705(9) 0.0313(6) 0.0391(17) Uani d . 1 1 . . H H18 0.2080 0.8306 -0.0339 0.047 Uiso calc R 1 1 . . C C19 0.2755(3) 0.7728(10) 0.2113(6) 0.0381(17) Uani d . 1 1 . . H H19 0.2933 0.8340 0.2762 0.046 Uiso calc R 1 1 . . C C20 0.2764(3) 0.5877(9) 0.2121(6) 0.0375(16) Uani d . 1 1 . . H H20 0.2954 0.5323 0.2783 0.045 Uiso calc R 1 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.0334(3) 0.0204(3) 0.0268(3) -0.00118(19) 0.00312(19) -0.00010(18) O1 0.031(3) 0.060(4) 0.045(3) 0.007(2) 0.007(2) -0.010(3) O2 0.042(3) 0.092(5) 0.035(3) -0.008(3) 0.002(2) -0.001(3) O3 0.068(5) 0.147(9) 0.084(6) -0.017(5) -0.030(4) 0.003(6) O4 0.036(3) 0.087(5) 0.043(3) 0.002(3) 0.008(2) 0.009(3) O5 0.034(3) 0.071(4) 0.045(3) -0.006(3) 0.001(2) -0.021(3) O6A 0.036(6) 0.233(17) 0.102(10) 0.008(7) 0.013(5) 0.026(10) O6B 0.10(4) 0.21(7) 0.20(7) 0.00(4) 0.10(4) 0.04(5) O7 0.044(3) 0.037(3) 0.027(2) 0.000(2) 0.004(2) 0.002(2) N1 0.010(2) 0.068(4) 0.011(2) 0.000(2) -0.0008(17) -0.005(3) N2 0.035(3) 0.006(2) 0.038(3) 0.002(2) 0.003(2) -0.001(2) C1 0.035(4) 0.023(4) 0.041(4) -0.001(3) 0.004(3) 0.002(3) C2 0.035(3) 0.024(3) 0.033(3) -0.003(3) 0.007(3) 0.004(3) C3 0.039(4) 0.048(5) 0.037(4) 0.003(3) 0.012(3) -0.008(3) C4 0.047(4) 0.060(6) 0.031(4) -0.007(4) 0.000(3) -0.006(4) C5 0.034(4) 0.057(5) 0.050(5) -0.001(4) 0.001(3) 0.010(4) C6 0.038(4) 0.078(7) 0.064(6) 0.008(4) 0.014(4) -0.006(5) C7 0.040(4) 0.054(5) 0.043(4) 0.003(4) 0.012(3) -0.008(4) C8 0.042(5) 0.123(11) 0.075(7) -0.004(6) -0.011(5) 0.002(7) C9 0.037(4) 0.021(3) 0.042(4) 0.001(3) 0.006(3) -0.004(3) C10 0.034(4) 0.035(4) 0.034(4) -0.002(3) 0.002(3) -0.003(3) C13 0.041(4) 0.068(6) 0.057(5) 0.002(4) 0.013(4) -0.006(5) C11A 0.039(6) 0.070(11) 0.042(6) 0.009(8) 0.006(4) 0.002(8) C12A 0.039(6) 0.070(11) 0.042(6) 0.009(8) 0.006(4) 0.002(8) C14A 0.039(6) 0.070(11) 0.042(6) 0.009(8) 0.006(4) 0.002(8) C15A 0.039(6) 0.070(11) 0.042(6) 0.009(8) 0.006(4) 0.002(8) C11B 0.039(6) 0.089(14) 0.040(6) 0.012(10) 0.002(4) 0.004(10) C12B 0.039(6) 0.089(14) 0.040(6) 0.012(10) 0.002(4) 0.004(10) C14B 0.039(6) 0.089(14) 0.040(6) 0.012(10) 0.002(4) 0.004(10) C15B 0.039(6) 0.089(14) 0.040(6) 0.012(10) 0.002(4) 0.004(10) C16 0.055(7) 0.117(10) 0.075(7) -0.005(6) 0.023(6) 0.002(7) C17 0.045(4) 0.036(4) 0.047(4) -0.004(3) -0.003(3) -0.013(3) C18 0.049(4) 0.022(4) 0.041(4) -0.005(3) -0.007(3) 0.005(3) C19 0.056(5) 0.026(4) 0.030(4) -0.011(3) -0.002(3) 0.002(3) C20 0.051(4) 0.023(4) 0.037(4) -0.001(3) 0.004(3) 0.006(3) 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' Cd Cd -0.8075 1.2024 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N1 Cd1 O7 . . 89.51(17) N1 Cd1 N2 . 1_545 176.30(17) O7 Cd1 N2 . 1_545 87.02(18) N1 Cd1 O1 . . 88.49(18) O7 Cd1 O1 . . 137.71(18) N2 Cd1 O1 1_545 . 94.94(19) N1 Cd1 O5 . . 93.98(19) O7 Cd1 O5 . . 139.32(18) N2 Cd1 O5 1_545 . 87.8(2) O1 Cd1 O5 . . 82.94(17) N1 Cd1 O4 . . 91.1(2) O7 Cd1 O4 . . 85.57(18) N2 Cd1 O4 1_545 . 87.4(2) O1 Cd1 O4 . . 136.69(18) O5 Cd1 O4 . . 53.88(18) N1 Cd1 O2 . . 94.7(2) O7 Cd1 O2 . . 84.23(18) N2 Cd1 O2 1_545 . 86.3(2) O1 Cd1 O2 . . 53.89(17) O5 Cd1 O2 . . 135.59(18) O4 Cd1 O2 . . 168.3(2) N1 Cd1 C9 . . 92.74(18) O7 Cd1 C9 . . 112.4(2) N2 Cd1 C9 1_545 . 87.41(19) O1 Cd1 C9 . . 109.87(19) O5 Cd1 C9 . . 26.99(19) O4 Cd1 C9 . . 26.9(2) O2 Cd1 C9 . . 161.8(2) N1 Cd1 C1 . . 91.69(18) O7 Cd1 C1 . . 110.7(2) N2 Cd1 C1 1_545 . 90.73(19) O1 Cd1 C1 . . 27.25(19) O5 Cd1 C1 . . 109.70(19) O4 Cd1 C1 . . 163.5(2) O2 Cd1 C1 . . 26.64(19) C9 Cd1 C1 . . 136.7(2) C1 O1 Cd1 . . 93.7(4) C1 O2 Cd1 . . 91.7(4) C9 O4 Cd1 . . 91.9(4) C9 O5 Cd1 . . 92.6(4) Cd1 O7 H71 . . 85(6) Cd1 O7 H72 . . 123(6) H71 O7 H72 . . 108(3) C20 N1 C17 . . 109.2(6) C20 N1 Cd1 . . 125.0(4) C17 N1 Cd1 . . 125.8(4) C19 N2 C18 . . 116.5(5) C19 N2 Cd1 . 1_565 119.1(4) C18 N2 Cd1 . 1_565 124.4(4) O2 C1 O1 . . 120.8(7) O2 C1 C2 . . 120.1(6) O1 C1 C2 . . 119.1(6) O2 C1 Cd1 . . 61.7(4) O1 C1 Cd1 . . 59.1(4) C2 C1 Cd1 . . 177.9(5) C3 C2 C7 . . 119.5(7) C3 C2 C1 . . 121.2(6) C7 C2 C1 . . 119.3(6) C4 C3 C2 . . 119.9(7) C4 C3 H3 . . 120.0 C2 C3 H3 . . 120.0 C5 C4 C3 . . 120.5(7) C5 C4 H4 . . 119.8 C3 C4 H4 . . 119.8 C4 C5 C6 . . 119.7(7) C4 C5 C8 . . 119.7(9) C6 C5 C8 . . 120.5(9) C7 C6 C5 . . 120.8(8) C7 C6 H6 . . 119.6 C5 C6 H6 . . 119.6 C6 C7 C2 . . 119.5(7) C6 C7 H7 . . 120.2 C2 C7 H7 . . 120.2 O3 C8 C5 . . 127.7(12) O3 C8 H8 . . 116.1 C5 C8 H8 . . 116.1 O4 C9 O5 . . 121.6(7) O4 C9 C10 . . 119.4(6) O5 C9 C10 . . 119.0(6) O4 C9 Cd1 . . 61.2(4) O5 C9 Cd1 . . 60.4(4) C10 C9 Cd1 . . 178.3(5) C15A C10 C11B . . 116(2) C15A C10 C11A . . 118.0(17) C11B C10 C15B . . 120.2(17) C11A C10 C15B . . 113.1(19) C15A C10 C9 . . 119.1(14) C11B C10 C9 . . 119.6(14) C11A C10 C9 . . 122.9(15) C15B C10 C9 . . 120.3(14) C12A C13 C14B . . 114.6(19) C12A C13 C14A . . 119.0(16) C14B C13 C12B . . 119.6(15) C14A C13 C12B . . 112.0(17) C12A C13 C16 . . 119.1(14) C14B C13 C16 . . 120.2(14) C14A C13 C16 . . 122.0(14) C12B C13 C16 . . 120.2(14) C12A C11A C10 . . 121(2) C12A C11A H11A . . 119.5 C10 C11A H11A . . 119.5 C13 C12A C11A . . 121.2(19) C13 C12A H12A . . 119.4 C11A C12A H12A . . 119.4 C15A C14A C13 . . 119.6(18) C15A C14A H14A . . 120.2 C13 C14A H14A . . 120.2 C10 C15A C14A . . 121(2) C10 C15A H15A . . 119.6 C14A C15A H15A . . 119.6 C10 C11B C12B . . 120(2) C10 C11B H11B . . 120.1 C12B C11B H11B . . 120.1 C11B C12B C13 . . 119.2(19) C11B C12B H12B . . 120.4 C13 C12B H12B . . 120.4 C15B C14B C13 . . 120.3(18) C15B C14B H14B . . 119.9 C13 C14B H14B . . 119.9 C14B C15B C10 . . 121(2) C14B C15B H15B . . 119.5 C10 C15B H15B . . 119.5 O6B C16 O6A . . 106(3) O6B C16 C13 . . 126(3) O6A C16 C13 . . 127.2(13) O6A C16 H16A . . 116.4 C13 C16 H16A . . 116.4 O6B C16 H16B . . 117.0 C13 C16 H16B . . 117.0 H16A C16 H16B . . 125.4 C18 C17 N1 . . 124.4(7) C18 C17 H17 . . 117.8 N1 C17 H17 . . 117.8 N2 C18 C17 . . 122.0(7) N2 C18 H18 . . 119.0 C17 C18 H18 . . 119.0 N2 C19 C20 . . 122.1(7) N2 C19 H19 . . 119.0 C20 C19 H19 . . 119.0 N1 C20 C19 . . 125.7(7) N1 C20 H20 . . 117.1 C19 C20 H20 . . 117.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cd1 N1 . 2.274(6) Cd1 O7 . 2.284(5) Cd1 N2 1_545 2.340(5) Cd1 O1 . 2.364(5) Cd1 O5 . 2.388(5) Cd1 O4 . 2.405(5) Cd1 O2 . 2.423(6) Cd1 C9 . 2.744(7) Cd1 C1 . 2.750(7) O1 C1 . 1.262(9) O2 C1 . 1.234(9) O3 C8 . 1.154(14) O4 C9 . 1.242(9) O5 C9 . 1.247(9) O6A C16 . 1.165(15) O6A H16B . 0.3504 O6B C16 . 1.12(6) O7 H71 . 0.83(2) O7 H72 . 0.82(2) N1 C20 . 1.365(9) N1 C17 . 1.410(10) N2 C19 . 1.318(9) N2 C18 . 1.326(9) N2 Cd1 1_565 2.340(5) C1 C2 . 1.491(9) C2 C3 . 1.385(10) C2 C7 . 1.394(10) C3 C4 . 1.383(11) C3 H3 . 0.9300 C4 C5 . 1.368(12) C4 H4 . 0.9300 C5 C6 . 1.378(12) C5 C8 . 1.479(12) C6 C7 . 1.376(11) C6 H6 . 0.9300 C7 H7 . 0.9300 C8 H8 . 0.9300 C9 C10 . 1.505(10) C10 C15A . 1.36(3) C10 C11B . 1.36(3) C10 C11A . 1.38(3) C10 C15B . 1.42(3) C13 C12A . 1.33(3) C13 C14B . 1.38(3) C13 C14A . 1.40(3) C13 C12B . 1.44(3) C13 C16 . 1.475(13) C11A C12A . 1.38(3) C11A H11A . 0.9300 C12A H12A . 0.9300 C14A C15A . 1.39(3) C14A H14A . 0.9300 C15A H15A . 0.9300 C11B C12B . 1.40(3) C11B H11B . 0.9300 C12B H12B . 0.9300 C14B C15B . 1.36(3) C14B H14B . 0.9300 C15B H15B . 0.9300 C16 H16A . 0.9300 C16 H16B . 0.9300 C17 C18 . 1.382(11) C17 H17 . 0.9300 C18 H18 . 0.9300 C19 C20 . 1.387(10) C19 H19 . 0.9300 C20 H20 . 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O7 H72 O5 4_565 0.82(2) 2.10(6) 2.727(7) 133(7) yes C18 H18 O6A 3_565 0.93 2.52 3.394(14) 157 yes C19 H19 O3 3_666 0.93 2.43 3.085(10) 127 yes C8 H8 Cg1 2_645 0.93 2.93 3.691(10) 147 yes 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_site_symmetry_1 _geom_torsion N1 Cd1 O1 C1 . -96.7(4) O7 Cd1 O1 C1 . -9.0(6) N2 Cd1 O1 C1 1_545 82.0(4) O5 Cd1 O1 C1 . 169.1(5) O4 Cd1 O1 C1 . 173.4(4) O2 Cd1 O1 C1 . 0.2(4) C9 Cd1 O1 C1 . 171.0(4) N1 Cd1 O2 C1 . 84.5(5) O7 Cd1 O2 C1 . 173.5(5) N2 Cd1 O2 C1 1_545 -99.1(5) O1 Cd1 O2 C1 . -0.2(4) O5 Cd1 O2 C1 . -16.1(6) O4 Cd1 O2 C1 . -156.6(9) C9 Cd1 O2 C1 . -29.3(10) N1 Cd1 O4 C9 . -94.0(5) O7 Cd1 O4 C9 . 176.6(5) N2 Cd1 O4 C9 1_545 89.4(5) O1 Cd1 O4 C9 . -5.0(6) O5 Cd1 O4 C9 . 0.2(4) O2 Cd1 O4 C9 . 146.8(9) C1 Cd1 O4 C9 . 5.7(10) N1 Cd1 O5 C9 . 88.2(4) O7 Cd1 O5 C9 . -5.7(6) N2 Cd1 O5 C9 1_545 -88.6(4) O1 Cd1 O5 C9 . 176.2(5) O4 Cd1 O5 C9 . -0.2(4) O2 Cd1 O5 C9 . -171.0(4) C1 Cd1 O5 C9 . -178.6(4) O7 Cd1 N1 C20 . -150.7(5) O1 Cd1 N1 C20 . -13.0(5) O5 Cd1 N1 C20 . 69.8(5) O4 Cd1 N1 C20 . 123.7(5) O2 Cd1 N1 C20 . -66.6(5) C9 Cd1 N1 C20 . 96.9(5) C1 Cd1 N1 C20 . -40.0(5) O7 Cd1 N1 C17 . 29.5(5) O1 Cd1 N1 C17 . 167.3(5) O5 Cd1 N1 C17 . -109.9(5) O4 Cd1 N1 C17 . -56.0(5) O2 Cd1 N1 C17 . 113.7(5) C9 Cd1 N1 C17 . -82.9(5) C1 Cd1 N1 C17 . 140.2(5) Cd1 O2 C1 O1 . 0.4(7) Cd1 O2 C1 C2 . -178.8(5) Cd1 O1 C1 O2 . -0.4(8) Cd1 O1 C1 C2 . 178.8(5) N1 Cd1 C1 O2 . -97.0(5) O7 Cd1 C1 O2 . -6.9(5) N2 Cd1 C1 O2 1_545 80.2(5) O1 Cd1 C1 O2 . 179.6(7) O5 Cd1 C1 O2 . 168.1(5) O4 Cd1 C1 O2 . 163.5(7) C9 Cd1 C1 O2 . 167.2(4) N1 Cd1 C1 O1 . 83.4(4) O7 Cd1 C1 O1 . 173.5(4) N2 Cd1 C1 O1 1_545 -99.4(4) O5 Cd1 C1 O1 . -11.5(5) O4 Cd1 C1 O1 . -16.1(10) O2 Cd1 C1 O1 . -179.6(7) C9 Cd1 C1 O1 . -12.4(6) O2 C1 C2 C3 . 157.1(7) O1 C1 C2 C3 . -22.1(10) O2 C1 C2 C7 . -22.7(10) O1 C1 C2 C7 . 158.2(7) C7 C2 C3 C4 . 2.7(11) C1 C2 C3 C4 . -177.0(7) C2 C3 C4 C5 . -1.8(13) C3 C4 C5 C6 . -0.2(14) C3 C4 C5 C8 . 179.8(9) C4 C5 C6 C7 . 1.2(15) C8 C5 C6 C7 . -178.8(10) C5 C6 C7 C2 . -0.3(14) C3 C2 C7 C6 . -1.7(12) C1 C2 C7 C6 . 178.0(8) C4 C5 C8 O3 . -7.4(19) C6 C5 C8 O3 . 172.6(13) Cd1 O4 C9 O5 . -0.4(7) Cd1 O4 C9 C10 . -178.2(6) Cd1 O5 C9 O4 . 0.4(7) Cd1 O5 C9 C10 . 178.2(5) N1 Cd1 C9 O4 . 87.0(5) O7 Cd1 C9 O4 . -3.6(5) N2 Cd1 C9 O4 1_545 -89.3(5) O1 Cd1 C9 O4 . 176.3(4) O5 Cd1 C9 O4 . -179.6(7) O2 Cd1 C9 O4 . -159.0(7) C1 Cd1 C9 O4 . -177.7(4) N1 Cd1 C9 O5 . -93.4(4) O7 Cd1 C9 O5 . 176.0(4) N2 Cd1 C9 O5 1_545 90.3(4) O1 Cd1 C9 O5 . -4.0(5) O4 Cd1 C9 O5 . 179.6(7) O2 Cd1 C9 O5 . 20.6(9) C1 Cd1 C9 O5 . 2.0(6) O4 C9 C10 C15A . 14.6(15) O5 C9 C10 C15A . -163.3(13) O4 C9 C10 C11B . 167.6(15) O5 C9 C10 C11B . -10.3(16) O4 C9 C10 C11A . -167.9(13) O5 C9 C10 C11A . 14.2(15) O4 C9 C10 C15B . -11.1(16) O5 C9 C10 C15B . 171.0(13) C15A C10 C11A C12A . -7(2) C11B C10 C11A C12A . -97(8) C15B C10 C11A C12A . 17(3) C9 C10 C11A C12A . 175.2(14) C14B C13 C12A C11A . -29(2) C14A C13 C12A C11A . -1(3) C12B C13 C12A C11A . 79(5) C16 C13 C12A C11A . 178.4(16) C10 C11A C12A C13 . 7(3) C12A C13 C14A C15A . -4(2) C14B C13 C14A C15A . 83(5) C12B C13 C14A C15A . -30(2) C16 C13 C14A C15A . 176.7(15) C11B C10 C15A C14A . 26(3) C11A C10 C15A C14A . 2(2) C15B C10 C15A C14A . -81(6) C9 C10 C15A C14A . 179.9(14) C13 C14A C15A C10 . 3(3) C15A C10 C11B C12B . -26(3) C11A C10 C11B C12B . 75(7) C15B C10 C11B C12B . -1(3) C9 C10 C11B C12B . 180.0(16) C10 C11B C12B C13 . -2(3) C12A C13 C12B C11B . -83(5) C14B C13 C12B C11B . 2(3) C14A C13 C12B C11B . 29(3) C16 C13 C12B C11B . -176.9(17) C12A C13 C14B C15B . 28(3) C14A C13 C14B C15B . -78(5) C12B C13 C14B C15B . 1(3) C16 C13 C14B C15B . -180.0(17) C13 C14B C15B C10 . -4(3) C15A C10 C15B C14B . 90(7) C11B C10 C15B C14B . 5(3) C11A C10 C15B C14B . -18(3) C9 C10 C15B C14B . -176.8(16) C12A C13 C16 O6B . -8(5) C14B C13 C16 O6B . -159(5) C14A C13 C16 O6B . 171(5) C12B C13 C16 O6B . 21(5) C12A C13 C16 O6A . 160.9(19) C14B C13 C16 O6A . 10(3) C14A C13 C16 O6A . -20(3) C12B C13 C16 O6A . -171(2) C20 N1 C17 C18 . -1.0(10) Cd1 N1 C17 C18 . 178.8(6) C19 N2 C18 C17 . 0.5(11) Cd1 N2 C18 C17 1_565 179.5(6) N1 C17 C18 N2 . 0.2(13) C18 N2 C19 C20 . -0.3(11) Cd1 N2 C19 C20 1_565 -179.4(6) C17 N1 C20 C19 . 1.2(10) Cd1 N1 C20 C19 . -178.6(6) N2 C19 C20 N1 . -0.6(13)