#------------------------------------------------------------------------------ #$Date: 2023-01-27 11:12:43 +0200 (Fri, 27 Jan 2023) $ #$Revision: 280631 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/65/8106598.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_8106598 loop_ _publ_author_name 'Li, Ya-Xue' 'Wen, Dong-Xiao' 'An, Meng-Jin' 'Yang, Huai-Xia' _publ_section_title ; Crystal structure of diaqua-(2,2′-(butane-1,4-diyl)-bis(5-carboxy-1H-imidazole-4-carboxylato)-\k4 O,O′,N,N′)cadmium(II) monohydrate, C14H18O11N4Cd ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 545 _journal_page_last 547 _journal_paper_doi 10.1515/ncrs-2016-0311 _journal_volume 232 _journal_year 2017 _chemical_formula_sum 'C14 H18 Cd N4 O11' _chemical_formula_weight 530.72 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 83.2390(10) _cell_angle_beta 82.0000(10) _cell_angle_gamma 61.4610(10) _cell_formula_units_Z 2 _cell_length_a 9.5135(3) _cell_length_b 9.8632(3) _cell_length_c 11.1419(4) _cell_measurement_reflns_used 9997 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.64 _cell_measurement_theta_min 2.86 _cell_volume 907.93(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker D8 VENTURE' _computing_data_reduction "'Bruker SAINT" _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON' _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 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 32290 _diffrn_reflns_theta_full 27.68 _diffrn_reflns_theta_max 27.68 _diffrn_reflns_theta_min 2.35 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 532 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 2.416 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 4230 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0288 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+1.0964P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.0781 _reflns_number_gt 3973 _reflns_number_total 4230 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL a_a.res in P-1 CELL 0.71073 9.5135 9.8632 11.1419 83.239 82.000 61.461 ZERR 2.00 0.0003 0.0003 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N O Cd UNIT 28 36 8 22 2 L.S. 20 ACTA BOND $H FMAP 2 PLAN 20 conf HTAB OMIT 2 1 0 OMIT 0 1 3 OMIT -1 0 2 OMIT 4 3 0 TEMP 20 EQIV $1 -x+2, -y, -z EQIV $2 x-1, y, z EQIV $3 -x+1, -y, -z+1 EQIV $4 x+1, y, z EQIV $5 -x, -y+1, -z+1 EQIV $6 x, y+1, z HTAB O2 O4 HTAB O7 O6 HTAB O11 O5 HTAB O11 O9_$1 HTAB O9 O6_$1 HTAB O9 O8_$2 HTAB O10 O4_$3 HTAB O10 O3_$4 HTAB N2 O3_$5 HTAB N4 O11_$6 WGHT 0.045500 1.096400 FVAR 0.24563 CD1 5 0.744196 0.217249 0.235907 11.00000 0.02119 0.02366 = 0.04056 -0.00980 0.00795 -0.01265 O1 4 0.683124 0.012543 0.280075 11.00000 0.02634 0.02090 = 0.06993 -0.01236 0.01105 -0.01031 O2 4 0.493740 -0.052013 0.349679 11.00000 0.03626 0.02222 = 0.08744 -0.01093 0.01759 -0.01667 AFIX 147 H2 2 0.399746 -0.009378 0.378548 11.00000 -1.50000 AFIX 0 O3 4 0.021455 0.311285 0.482566 11.00000 0.02662 0.04104 = 0.06241 -0.01104 0.01246 -0.01926 O4 4 0.208429 0.077736 0.430959 11.00000 0.04005 0.03292 = 0.05911 -0.00469 0.01027 -0.02553 O5 4 0.992492 0.039902 0.150370 11.00000 0.02584 0.02179 = 0.05947 -0.01534 0.01071 -0.01265 O6 4 1.233303 0.008379 0.071193 11.00000 0.02495 0.02773 = 0.06755 -0.02223 0.01344 -0.01137 O7 4 1.382965 0.162755 0.027280 11.00000 0.02697 0.03435 = 0.08385 -0.02485 0.02231 -0.01706 AFIX 147 H7 2 1.338509 0.108610 0.045898 11.00000 -1.50000 AFIX 0 O8 4 1.330427 0.401669 0.052405 11.00000 0.02737 0.03196 = 0.05733 -0.00743 0.00803 -0.01826 O9 4 0.665930 0.258015 0.041376 11.00000 0.02688 0.03039 = 0.04076 -0.01237 0.00295 -0.01435 AFIX 3 H1W 2 0.694520 0.180075 0.000326 11.00000 -1.20000 H2W 2 0.566350 0.307135 0.031416 11.00000 -1.20000 AFIX 0 O10 4 0.831334 0.156758 0.430656 11.00000 0.04576 0.04399 = 0.04911 0.00923 -0.01002 -0.03214 AFIX 3 H3W 2 0.833144 0.078488 0.472976 11.00000 -1.20000 H4W 2 0.900984 0.178558 0.450566 11.00000 -1.20000 AFIX 0 N1 3 0.480385 0.323084 0.313528 11.00000 0.02001 0.01878 = 0.03083 -0.00494 0.00315 -0.00984 N2 3 0.229173 0.435953 0.391635 11.00000 0.01766 0.02142 = 0.03479 -0.00620 0.00243 -0.00824 AFIX 43 H2A 2 0.136636 0.507392 0.417602 11.00000 -1.20000 AFIX 0 N3 3 0.894659 0.341605 0.200463 11.00000 0.02066 0.01913 = 0.03138 -0.00709 0.00508 -0.01029 N4 3 1.022514 0.479278 0.159267 11.00000 0.02242 0.01944 = 0.03136 -0.00419 0.00134 -0.01189 AFIX 43 H4A 2 1.041990 0.556513 0.154140 11.00000 -1.20000 AFIX 0 C1 1 0.430276 0.212469 0.345571 11.00000 0.02186 0.01978 = 0.02962 -0.00408 0.00112 -0.01103 C2 1 0.273005 0.281875 0.394501 11.00000 0.02310 0.02292 = 0.02835 -0.00284 0.00048 -0.01271 C3 1 0.157726 0.221317 0.441207 11.00000 0.02710 0.03270 = 0.03404 -0.00134 0.00118 -0.01944 C4 1 0.355320 0.457375 0.341251 11.00000 0.01815 0.02134 = 0.03078 -0.00472 0.00074 -0.00942 C5 1 0.342094 0.614733 0.317862 11.00000 0.02438 0.01924 = 0.06604 -0.00381 0.00068 -0.00956 AFIX 23 H5B 2 0.317645 0.661388 0.395059 11.00000 -1.20000 H5C 2 0.252035 0.677275 0.270215 11.00000 -1.20000 AFIX 0 C6 1 0.490614 0.621213 0.252108 11.00000 0.03322 0.02335 = 0.03896 -0.00044 -0.00173 -0.01602 AFIX 23 H6B 2 0.538007 0.546110 0.190295 11.00000 -1.20000 H6C 2 0.458759 0.722927 0.211847 11.00000 -1.20000 AFIX 0 C7 1 0.615852 0.588126 0.338182 11.00000 0.02614 0.02109 = 0.03301 -0.00759 0.00470 -0.00967 AFIX 23 H7A 2 0.656593 0.482167 0.371349 11.00000 -1.20000 H7B 2 0.565096 0.655376 0.405199 11.00000 -1.20000 AFIX 0 C8 1 0.756196 0.612340 0.275956 11.00000 0.02718 0.02391 = 0.05080 -0.01623 0.00898 -0.01360 AFIX 23 H8A 2 0.714616 0.701201 0.218550 11.00000 -1.20000 H8B 2 0.802939 0.636809 0.336820 11.00000 -1.20000 AFIX 0 C9 1 0.886611 0.477942 0.210111 11.00000 0.02024 0.02022 = 0.02987 -0.00496 0.00153 -0.01067 C10 1 1.124955 0.335890 0.116894 11.00000 0.01875 0.02155 = 0.02780 -0.00456 0.00100 -0.00867 C11 1 1.287816 0.301773 0.061805 11.00000 0.02283 0.02953 = 0.03560 -0.00596 0.00359 -0.01319 C12 1 1.043339 0.251521 0.143218 11.00000 0.01880 0.01962 = 0.02854 -0.00688 0.00278 -0.00842 C13 1 1.092912 0.088103 0.119896 11.00000 0.02210 0.01985 = 0.03919 -0.00961 0.00337 -0.00895 C14 1 0.544039 0.049160 0.323168 11.00000 0.02822 0.01995 = 0.04400 -0.00656 0.00513 -0.01197 O11 4 1.066528 -0.267280 0.121649 11.00000 0.10241 0.04456 = 0.09976 0.00227 -0.01995 -0.04805 AFIX 3 H5W 2 1.033718 -0.171990 0.130259 11.00000 -1.20000 H6W 2 1.149578 -0.283330 0.073209 11.00000 -1.20000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM a_a.res in P-1 REM R1 = 0.0288 for 3973 Fo > 4sig(Fo) and 0.0311 for all 4230 data REM 273 parameters refined using 0 restraints END WGHT 0.0455 1.0947 REM Highest difference peak 2.416, deepest hole -1.308, 1-sigma level 0.087 Q1 1 0.9766 -0.2321 0.1878 11.00000 0.05 2.42 Q2 1 1.0629 0.1822 0.1297 11.00000 0.05 0.31 Q3 1 1.0952 0.2823 0.1357 11.00000 0.05 0.29 Q4 1 0.3511 0.2381 0.3740 11.00000 0.05 0.28 Q5 1 0.5031 0.6051 0.3562 11.00000 0.05 0.28 Q6 1 0.5836 0.6408 0.2347 11.00000 0.05 0.28 Q7 1 0.2254 0.2545 0.4201 11.00000 0.05 0.27 Q8 1 0.4783 0.1383 0.3395 11.00000 0.05 0.27 Q9 1 1.1985 0.3144 0.0929 11.00000 0.05 0.25 Q10 1 0.0412 0.3172 0.5493 11.00000 0.05 0.24 Q11 1 0.2439 0.3632 0.3868 11.00000 0.05 0.24 Q12 1 0.4540 0.2584 0.3311 11.00000 0.05 0.24 Q13 1 0.9046 0.0784 0.3938 11.00000 0.05 0.22 Q14 1 0.5423 0.6293 0.3022 11.00000 0.05 0.22 Q15 1 0.8938 0.3955 0.2173 11.00000 0.05 0.21 Q16 1 1.0852 0.4041 0.1336 11.00000 0.05 0.21 Q17 1 0.5677 0.3075 0.2814 11.00000 0.05 0.21 Q18 1 0.8760 0.3125 0.2398 11.00000 0.05 0.21 Q19 1 0.3246 0.0271 0.3794 11.00000 0.05 0.21 Q20 1 0.5337 -0.2004 0.3563 11.00000 0.05 0.20 ; _cod_data_source_file suppl_ncrs-2016-0311_suppl.cif _cod_data_source_block a _cod_original_sg_symbol_H-M P-1 _cod_database_code 8106598 loop_ _symmetry_equiv_pos_as_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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.744196(19) 0.217249(19) 0.235907(16) 0.02804(7) Uani 1 1 d . . . O1 O 0.6831(2) 0.0125(2) 0.2801(2) 0.0402(5) Uani 1 1 d . . . O2 O 0.4937(3) -0.0520(2) 0.3497(3) 0.0492(6) Uani 1 1 d . . . H2 H 0.3997 -0.0094 0.3785 0.074 Uiso 1 1 calc R . . O3 O 0.0215(2) 0.3113(2) 0.4826(2) 0.0430(5) Uani 1 1 d . . . O4 O 0.2084(3) 0.0777(2) 0.4310(2) 0.0420(5) Uani 1 1 d . . . O5 O 0.9925(2) 0.0399(2) 0.15037(19) 0.0355(4) Uani 1 1 d . . . O6 O 1.2333(2) 0.0084(2) 0.0712(2) 0.0406(5) Uani 1 1 d . . . O7 O 1.3830(2) 0.1628(2) 0.0273(2) 0.0483(6) Uani 1 1 d . . . H7 H 1.3385 0.1086 0.0459 0.072 Uiso 1 1 calc R . . O8 O 1.3304(2) 0.4017(2) 0.0524(2) 0.0379(4) Uani 1 1 d . . . O9 O 0.6659(2) 0.2580(2) 0.04138(17) 0.0320(4) Uani 1 1 d . . . H1W H 0.6945 0.1801 0.0003 0.038 Uiso 1 1 d R . . H2W H 0.5663 0.3071 0.0314 0.038 Uiso 1 1 d R . . O10 O 0.8313(3) 0.1568(3) 0.4307(2) 0.0422(5) Uani 1 1 d . . . H3W H 0.8331 0.0785 0.4730 0.051 Uiso 1 1 d R . . H4W H 0.9010 0.1786 0.4506 0.051 Uiso 1 1 d R . . N1 N 0.4804(2) 0.3231(2) 0.31353(18) 0.0232(4) Uani 1 1 d . . . N2 N 0.2292(2) 0.4360(2) 0.39164(19) 0.0251(4) Uani 1 1 d . . . H2A H 0.1366 0.5074 0.4176 0.030 Uiso 1 1 calc R . . N3 N 0.8947(2) 0.3416(2) 0.20046(18) 0.0236(4) Uani 1 1 d . . . N4 N 1.0225(2) 0.4793(2) 0.15927(18) 0.0237(4) Uani 1 1 d . . . H4A H 1.0420 0.5565 0.1541 0.028 Uiso 1 1 calc R . . C1 C 0.4303(3) 0.2125(3) 0.3456(2) 0.0234(4) Uani 1 1 d . . . C2 C 0.2730(3) 0.2819(3) 0.3945(2) 0.0242(4) Uani 1 1 d . . . C3 C 0.1577(3) 0.2213(3) 0.4412(2) 0.0295(5) Uani 1 1 d . . . C4 C 0.3553(3) 0.4574(3) 0.3413(2) 0.0234(4) Uani 1 1 d . . . C5 C 0.3421(3) 0.6147(3) 0.3179(3) 0.0373(6) Uani 1 1 d . . . H5B H 0.3176 0.6614 0.3951 0.045 Uiso 1 1 calc R . . H5C H 0.2520 0.6773 0.2702 0.045 Uiso 1 1 calc R . . C6 C 0.4906(3) 0.6212(3) 0.2521(2) 0.0310(5) Uani 1 1 d . . . H6B H 0.5380 0.5461 0.1903 0.037 Uiso 1 1 calc R . . H6C H 0.4588 0.7229 0.2118 0.037 Uiso 1 1 calc R . . C7 C 0.6159(3) 0.5881(3) 0.3382(2) 0.0276(5) Uani 1 1 d . . . H7A H 0.6566 0.4822 0.3713 0.033 Uiso 1 1 calc R . . H7B H 0.5651 0.6554 0.4052 0.033 Uiso 1 1 calc R . . C8 C 0.7562(3) 0.6123(3) 0.2760(3) 0.0334(6) Uani 1 1 d . . . H8A H 0.7146 0.7012 0.2186 0.040 Uiso 1 1 calc R . . H8B H 0.8029 0.6368 0.3368 0.040 Uiso 1 1 calc R . . C9 C 0.8866(3) 0.4779(3) 0.2101(2) 0.0231(4) Uani 1 1 d . . . C10 C 1.1250(3) 0.3359(3) 0.1169(2) 0.0231(4) Uani 1 1 d . . . C11 C 1.2878(3) 0.3018(3) 0.0618(2) 0.0293(5) Uani 1 1 d . . . C12 C 1.0433(3) 0.2515(3) 0.1432(2) 0.0226(4) Uani 1 1 d . . . C13 C 1.0929(3) 0.0881(3) 0.1199(2) 0.0274(5) Uani 1 1 d . . . C14 C 0.5440(3) 0.0492(3) 0.3232(3) 0.0309(5) Uani 1 1 d . . . O11 O 1.0665(4) -0.2673(3) 0.1216(3) 0.0761(9) Uani 1 1 d . . . H5W H 1.0337 -0.1720 0.1303 0.091 Uiso 1 1 d R . . H6W H 1.1496 -0.2833 0.0732 0.091 Uiso 1 1 d R . . 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 0.02119(10) 0.02366(10) 0.04056(12) -0.00980(7) 0.00795(7) -0.01265(8) O1 0.0263(9) 0.0209(8) 0.0699(14) -0.0124(9) 0.0111(9) -0.0103(7) O2 0.0363(11) 0.0222(9) 0.0874(17) -0.0109(10) 0.0176(11) -0.0167(8) O3 0.0266(9) 0.0410(11) 0.0624(13) -0.0110(10) 0.0125(9) -0.0193(9) O4 0.0400(11) 0.0329(10) 0.0591(13) -0.0047(9) 0.0103(9) -0.0255(9) O5 0.0258(9) 0.0218(8) 0.0595(12) -0.0153(8) 0.0107(8) -0.0126(7) O6 0.0250(9) 0.0277(9) 0.0676(14) -0.0222(9) 0.0134(9) -0.0114(8) O7 0.0270(10) 0.0344(11) 0.0838(16) -0.0249(11) 0.0223(10) -0.0171(9) O8 0.0274(9) 0.0320(9) 0.0573(12) -0.0074(8) 0.0080(8) -0.0183(8) O9 0.0269(9) 0.0304(9) 0.0408(10) -0.0124(7) 0.0029(7) -0.0144(7) O10 0.0458(12) 0.0440(11) 0.0491(12) 0.0092(9) -0.0100(9) -0.0321(10) N1 0.0200(9) 0.0188(9) 0.0308(10) -0.0049(7) 0.0032(7) -0.0098(7) N2 0.0177(9) 0.0214(9) 0.0348(10) -0.0062(8) 0.0024(7) -0.0082(7) N3 0.0207(9) 0.0191(9) 0.0314(10) -0.0071(7) 0.0051(7) -0.0103(7) N4 0.0224(9) 0.0194(9) 0.0314(10) -0.0042(7) 0.0013(7) -0.0119(8) C1 0.0219(10) 0.0198(10) 0.0296(11) -0.0041(8) 0.0011(8) -0.0110(9) C2 0.0231(11) 0.0229(11) 0.0283(11) -0.0028(8) 0.0005(9) -0.0127(9) C3 0.0271(12) 0.0327(12) 0.0340(12) -0.0013(10) 0.0012(9) -0.0194(10) C4 0.0182(10) 0.0213(10) 0.0308(11) -0.0047(8) 0.0007(8) -0.0094(8) C5 0.0244(12) 0.0192(11) 0.0660(18) -0.0038(11) 0.0007(12) -0.0096(10) C6 0.0332(13) 0.0234(11) 0.0390(13) -0.0004(10) -0.0017(10) -0.0160(10) C7 0.0261(11) 0.0211(10) 0.0330(12) -0.0076(9) 0.0047(9) -0.0097(9) C8 0.0272(12) 0.0239(11) 0.0508(15) -0.0162(11) 0.0090(11) -0.0136(10) C9 0.0202(10) 0.0202(10) 0.0299(11) -0.0050(8) 0.0015(8) -0.0107(9) C10 0.0188(10) 0.0215(10) 0.0278(11) -0.0046(8) 0.0010(8) -0.0087(9) C11 0.0228(11) 0.0295(12) 0.0356(12) -0.0060(10) 0.0036(9) -0.0132(10) C12 0.0188(10) 0.0196(10) 0.0285(11) -0.0069(8) 0.0028(8) -0.0084(8) C13 0.0221(11) 0.0199(10) 0.0392(13) -0.0096(9) 0.0034(9) -0.0089(9) C14 0.0282(12) 0.0200(11) 0.0440(14) -0.0066(10) 0.0051(10) -0.0120(10) O11 0.102(2) 0.0446(14) 0.100(2) 0.0023(15) -0.0199(19) -0.0481(16) 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' Cd Cd -0.8075 1.2024 '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 N3 Cd1 N1 125.73(7) . . N3 Cd1 O5 74.23(7) . . N1 Cd1 O5 159.93(7) . . N3 Cd1 O9 96.58(7) . . N1 Cd1 O9 89.97(7) . . O5 Cd1 O9 85.01(7) . . N3 Cd1 O1 158.80(7) . . N1 Cd1 O1 73.49(7) . . O5 Cd1 O1 87.23(6) . . O9 Cd1 O1 91.87(8) . . N3 Cd1 O10 85.63(7) . . N1 Cd1 O10 91.61(7) . . O5 Cd1 O10 92.21(8) . . O9 Cd1 O10 175.83(7) . . O1 Cd1 O10 84.88(8) . . C14 O1 Cd1 115.26(16) . . C14 O2 H2 109.5 . . C13 O5 Cd1 115.93(15) . . C11 O7 H7 109.5 . . Cd1 O9 H1W 118.7 . . Cd1 O9 H2W 119.0 . . H1W O9 H2W 100.2 . . Cd1 O10 H3W 120.7 . . Cd1 O10 H4W 122.3 . . H3W O10 H4W 110.8 . . C4 N1 C1 106.30(19) . . C4 N1 Cd1 141.60(16) . . C1 N1 Cd1 112.09(14) . . C4 N2 C2 108.73(19) . . C4 N2 H2A 125.6 . . C2 N2 H2A 125.6 . . C9 N3 C12 106.45(19) . . C9 N3 Cd1 141.59(16) . . C12 N3 Cd1 111.82(14) . . C9 N4 C10 108.11(19) . . C9 N4 H4A 125.9 . . C10 N4 H4A 125.9 . . C2 C1 N1 109.5(2) . . C2 C1 C14 131.4(2) . . N1 C1 C14 119.1(2) . . N2 C2 C1 105.25(19) . . N2 C2 C3 121.8(2) . . C1 C2 C3 133.0(2) . . O3 C3 O4 124.7(2) . . O3 C3 C2 119.2(2) . . O4 C3 C2 116.1(2) . . N1 C4 N2 110.2(2) . . N1 C4 C5 128.1(2) . . N2 C4 C5 121.7(2) . . C4 C5 C6 115.6(2) . . C4 C5 H5B 108.4 . . C6 C5 H5B 108.4 . . C4 C5 H5C 108.4 . . C6 C5 H5C 108.4 . . H5B C5 H5C 107.4 . . C7 C6 C5 112.2(2) . . C7 C6 H6B 109.2 . . C5 C6 H6B 109.2 . . C7 C6 H6C 109.2 . . C5 C6 H6C 109.2 . . H6B C6 H6C 107.9 . . C6 C7 C8 112.6(2) . . C6 C7 H7A 109.1 . . C8 C7 H7A 109.1 . . C6 C7 H7B 109.1 . . C8 C7 H7B 109.1 . . H7A C7 H7B 107.8 . . C9 C8 C7 115.3(2) . . C9 C8 H8A 108.4 . . C7 C8 H8A 108.4 . . C9 C8 H8B 108.4 . . C7 C8 H8B 108.4 . . H8A C8 H8B 107.5 . . N3 C9 N4 110.5(2) . . N3 C9 C8 127.8(2) . . N4 C9 C8 121.5(2) . . C12 C10 N4 105.64(19) . . C12 C10 C11 134.5(2) . . N4 C10 C11 119.8(2) . . O8 C11 O7 122.2(2) . . O8 C11 C10 120.0(2) . . O7 C11 C10 117.8(2) . . C10 C12 N3 109.28(19) . . C10 C12 C13 130.4(2) . . N3 C12 C13 120.3(2) . . O5 C13 O6 124.7(2) . . O5 C13 C12 117.6(2) . . O6 C13 C12 117.7(2) . . O1 C14 O2 121.6(2) . . O1 C14 C1 120.1(2) . . O2 C14 C1 118.3(2) . . H5W O11 H6W 97.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 N3 2.2618(19) . Cd1 N1 2.2895(19) . Cd1 O5 2.3164(18) . Cd1 O9 2.3177(19) . Cd1 O1 2.3375(19) . Cd1 O10 2.340(2) . O1 C14 1.233(3) . O2 C14 1.288(3) . O2 H2 0.8200 . O3 C3 1.229(3) . O4 C3 1.273(3) . O5 C13 1.249(3) . O6 C13 1.262(3) . O7 C11 1.300(3) . O7 H7 0.8200 . O8 C11 1.221(3) . O9 H1W 0.8500 . O9 H2W 0.8500 . O10 H3W 0.8500 . O10 H4W 0.8502 . N1 C4 1.324(3) . N1 C1 1.379(3) . N2 C4 1.352(3) . N2 C2 1.368(3) . N2 H2A 0.8600 . N3 C9 1.326(3) . N3 C12 1.371(3) . N4 C9 1.343(3) . N4 C10 1.373(3) . N4 H4A 0.8600 . C1 C2 1.374(3) . C1 C14 1.477(3) . C2 C3 1.491(3) . C4 C5 1.490(3) . C5 C6 1.525(4) . C5 H5B 0.9700 . C5 H5C 0.9700 . C6 C7 1.523(4) . C6 H6B 0.9700 . C6 H6C 0.9700 . C7 C8 1.526(3) . C7 H7A 0.9700 . C7 H7B 0.9700 . C8 C9 1.496(3) . C8 H8A 0.9700 . C8 H8B 0.9700 . C10 C12 1.370(3) . C10 C11 1.475(3) . C12 C13 1.492(3) . O11 H5W 0.8500 . O11 H6W 0.8500 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O4 0.82 1.65 2.469(3) 177.7 . O7 H7 O6 0.82 1.69 2.507(3) 173.4 . O11 H5W O5 0.85 1.97 2.812(3) 171.3 . O11 H6W O9 0.85 2.12 2.947(4) 164.2 2_755 O9 H1W O6 0.85 1.88 2.726(3) 172.4 2_755 O9 H2W O8 0.85 1.97 2.797(3) 165.1 1_455 O10 H3W O4 0.85 1.94 2.776(3) 168.7 2_656 O10 H4W O3 0.85 2.19 3.010(3) 161.0 1_655 N2 H2A O3 0.86 2.03 2.842(3) 156.6 2_566 N4 H4A O11 0.86 1.85 2.703(3) 171.0 1_565 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 N3 Cd1 O1 C14 157.0(2) . . . . N1 Cd1 O1 C14 0.0(2) . . . . O5 Cd1 O1 C14 -174.3(2) . . . . O9 Cd1 O1 C14 -89.4(2) . . . . O10 Cd1 O1 C14 93.2(2) . . . . N3 Cd1 O5 C13 -2.30(19) . . . . N1 Cd1 O5 C13 172.08(19) . . . . O9 Cd1 O5 C13 96.0(2) . . . . O1 Cd1 O5 C13 -171.9(2) . . . . O10 Cd1 O5 C13 -87.1(2) . . . . N3 Cd1 N1 C4 9.6(3) . . . . O5 Cd1 N1 C4 -163.7(2) . . . . O9 Cd1 N1 C4 -88.4(3) . . . . O1 Cd1 N1 C4 179.6(3) . . . . O10 Cd1 N1 C4 95.4(3) . . . . N3 Cd1 N1 C1 -168.82(14) . . . . O5 Cd1 N1 C1 17.8(3) . . . . O9 Cd1 N1 C1 93.09(16) . . . . O1 Cd1 N1 C1 1.13(15) . . . . O10 Cd1 N1 C1 -83.05(16) . . . . N1 Cd1 N3 C9 0.7(3) . . . . O5 Cd1 N3 C9 178.3(3) . . . . O9 Cd1 N3 C9 95.4(3) . . . . O1 Cd1 N3 C9 -151.8(3) . . . . O10 Cd1 N3 C9 -88.2(3) . . . . N1 Cd1 N3 C12 -174.28(14) . . . . O5 Cd1 N3 C12 3.35(15) . . . . O9 Cd1 N3 C12 -79.56(16) . . . . O1 Cd1 N3 C12 33.3(3) . . . . O10 Cd1 N3 C12 96.89(16) . . . . C4 N1 C1 C2 -0.7(3) . . . . Cd1 N1 C1 C2 178.35(15) . . . . C4 N1 C1 C14 178.9(2) . . . . Cd1 N1 C1 C14 -2.1(3) . . . . C4 N2 C2 C1 0.8(3) . . . . C4 N2 C2 C3 -177.8(2) . . . . N1 C1 C2 N2 -0.1(3) . . . . C14 C1 C2 N2 -179.5(3) . . . . N1 C1 C2 C3 178.3(2) . . . . C14 C1 C2 C3 -1.1(5) . . . . N2 C2 C3 O3 -2.8(4) . . . . C1 C2 C3 O3 178.9(3) . . . . N2 C2 C3 O4 174.9(2) . . . . C1 C2 C3 O4 -3.3(4) . . . . C1 N1 C4 N2 1.2(3) . . . . Cd1 N1 C4 N2 -177.34(18) . . . . C1 N1 C4 C5 -175.8(3) . . . . Cd1 N1 C4 C5 5.7(4) . . . . C2 N2 C4 N1 -1.3(3) . . . . C2 N2 C4 C5 175.9(2) . . . . N1 C4 C5 C6 1.0(4) . . . . N2 C4 C5 C6 -175.6(2) . . . . C4 C5 C6 C7 -82.4(3) . . . . C5 C6 C7 C8 -173.5(2) . . . . C6 C7 C8 C9 -84.2(3) . . . . C12 N3 C9 N4 1.2(3) . . . . Cd1 N3 C9 N4 -173.87(18) . . . . C12 N3 C9 C8 -173.6(2) . . . . Cd1 N3 C9 C8 11.3(4) . . . . C10 N4 C9 N3 -1.3(3) . . . . C10 N4 C9 C8 173.9(2) . . . . C7 C8 C9 N3 -0.5(4) . . . . C7 C8 C9 N4 -174.9(2) . . . . C9 N4 C10 C12 0.8(3) . . . . C9 N4 C10 C11 -176.9(2) . . . . C12 C10 C11 O8 -178.0(3) . . . . N4 C10 C11 O8 -1.0(4) . . . . C12 C10 C11 O7 0.4(4) . . . . N4 C10 C11 O7 177.3(2) . . . . N4 C10 C12 N3 -0.1(3) . . . . C11 C10 C12 N3 177.1(3) . . . . N4 C10 C12 C13 -179.6(2) . . . . C11 C10 C12 C13 -2.4(5) . . . . C9 N3 C12 C10 -0.7(3) . . . . Cd1 N3 C12 C10 176.03(15) . . . . C9 N3 C12 C13 178.9(2) . . . . Cd1 N3 C12 C13 -4.4(3) . . . . Cd1 O5 C13 O6 -179.4(2) . . . . Cd1 O5 C13 C12 0.8(3) . . . . C10 C12 C13 O5 -178.0(2) . . . . N3 C12 C13 O5 2.5(4) . . . . C10 C12 C13 O6 2.2(4) . . . . N3 C12 C13 O6 -177.3(2) . . . . Cd1 O1 C14 O2 178.8(2) . . . . Cd1 O1 C14 C1 -1.2(3) . . . . C2 C1 C14 O1 -178.3(3) . . . . N1 C1 C14 O1 2.3(4) . . . . C2 C1 C14 O2 1.8(4) . . . . N1 C1 C14 O2 -177.6(2) . . . .