#------------------------------------------------------------------------------ #$Date: 2025-05-03 02:47:55 +0100 (Sat, 03 May 2025) $ #$Revision: 299503 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023490.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023490 loop_ _publ_author_name 'Tsymbal, Liudmyla V.' 'Andriichuk, Irina L.' 'Stoica, Alexandru-Constantin' 'Lampeka, Yaroslaw D.' _publ_section_title ; Synthesis and structural characterization of the dichloride complex formed by carboxy-functionalized Cu(diazacyclam)2+ cation and its heterometallic coordination polymer with CdCl2 ; _journal_coeditor_code HB8137 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025003792 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Cu Cd (C16 H32 N6 O4) Cl2 (H2 O)], 1.25H2 O' _chemical_formula_moiety 'C16 H34 Cd Cl2 Cu N6 O5, 1.25(H2 O)' _chemical_formula_sum 'C16 H36.5 Cd Cl2 Cu N6 O6.25' _chemical_formula_weight 659.85 _chemical_name_systematic 'Poly[[aqua[\m~3~-3,10-bis(3-carboxypropyl)-1,3,5,8,10,12-hexaazacyclotetradecane-\k^4^N^1^,N^5^,N^8^,N^12^:\k^2^O,O':\k^2^O'',O''']-\m-chloridocopper(II)cadmium(II]] 1.25-hydrate]' _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 _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 80.305(3) _cell_angle_beta 80.117(3) _cell_angle_gamma 64.149(3) _cell_formula_units_Z 2 _cell_length_a 10.1565(4) _cell_length_b 10.4249(5) _cell_length_c 14.6531(7) _cell_measurement_reflns_used 2340 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 25.05 _cell_measurement_theta_min 2.53 _cell_volume 1367.82(11) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2022) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12964 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.517 _exptl_absorpt_coefficient_mu 1.790 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2022) ; _exptl_crystal_colour 'clear light violet' _exptl_crystal_density_diffrn 1.602 _exptl_crystal_description prism _exptl_crystal_F_000 671 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.311 _refine_diff_density_min -0.687 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 297 _refine_ls_number_reflns 4762 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0496 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+2.6254P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1298 _refine_ls_wR_factor_ref 0.1487 _reflns_number_gt 3446 _reflns_number_total 4762 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8137.cif _cod_data_source_block II _cod_original_formula_sum 'C16 H36.50 Cd Cl2 Cu N6 O6.25' _cod_database_code 2023490 _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_min 0.775 _shelx_estimated_absorpt_t_max 0.916 _shelx_hkl_file ; -2 0 0 37025 890 -2 2 0 0 37025 890 1 -3 0 0 154055 2167 -2 3 0 0 154055 2167 1 -4 0 0 705578 10625 -2 4 0 0 705578 10625 1 5 0 0 102181 2199 1 6 0 0 8160 1048 1 7 0 0 8608 1366 1 8 0 0 5200 2127 1 9 0 0 -1853 1853 1 10 0 0 9374 3181 1 -10 1 0 2876 3234 1 -9 1 0 12845 2306 1 -8 1 0 101112 3124 1 -7 1 0 214753 4395 1 -6 1 0 -1256 1256 1 -5 1 0 452916 5627 1 -4 1 0 705737 8031 1 -3 1 0 603491 6625 1 -2 1 0 2732795 25694 1 2 1 0 573964 13015 1 3 1 0 175422 4777 1 4 1 0 482538 8082 1 5 1 0 86463 1893 1 6 1 0 87945 2009 1 7 1 0 167389 3604 1 8 1 0 116320 4621 1 9 1 0 -1514 1778 1 10 1 0 16215 3323 1 11 1 0 10140 3232 1 -9 2 0 13943 3875 1 -8 2 0 17137 2213 1 -7 2 0 14559 2546 1 -6 2 0 10332 1594 1 -5 2 0 43821 1630 1 -4 2 0 399954 4987 1 -3 2 0 623675 6808 1 -2 2 0 111829 1810 1 -1 2 0 543600 5692 1 0 2 0 4631153 46600 1 1 2 0 389047 3691 1 2 2 0 145462 2000 1 3 2 0 359031 5244 1 4 2 0 20934 1308 1 5 2 0 8280 1380 1 6 2 0 5686 875 1 7 2 0 33733 1807 1 8 2 0 -550 1696 1 9 2 0 11875 1782 1 10 2 0 23878 2316 1 11 2 0 71381 3828 1 -9 3 0 9312 3209 1 -8 3 0 44450 4058 1 -7 3 0 70108 3413 1 -6 3 0 -1597 1597 1 -5 3 0 92998 2544 1 -4 3 0 144483 2673 1 -3 3 0 36702 1392 1 -2 3 0 35550 1251 1 -1 3 0 -244 727 1 0 3 0 154020 2448 1 1 3 0 16854 905 1 2 3 0 359294 3874 1 3 3 0 219498 2810 1 4 3 0 1650127 20215 1 5 3 0 217247 4767 1 6 3 0 526685 9698 1 7 3 0 287807 5802 1 8 3 0 202335 6072 1 9 3 0 17894 2887 1 10 3 0 4870 2242 1 11 3 0 13502 2220 1 -8 4 0 5443 3005 1 -7 4 0 -148 3566 1 -6 4 0 -759 2121 1 -5 4 0 129895 4856 1 -4 4 0 199302 3805 1 -3 4 0 113088 2545 1 -2 4 0 62343 1906 1 -1 4 0 1399036 15628 1 0 4 0 1133600 12240 1 1 4 0 17508 1128 1 2 4 0 55217 1296 1 3 4 0 528302 6254 1 4 4 0 616215 7267 1 5 4 0 45038 1274 1 6 4 0 94848 2270 1 7 4 0 1099 1842 1 8 4 0 1469 2030 1 9 4 0 8815 2448 1 10 4 0 34851 2369 1 11 4 0 38215 3846 1 -7 5 0 22225 3688 1 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163131 4069 1 8 7 0 30405 2316 1 9 7 0 13820 2116 1 10 7 0 27949 2436 1 11 7 0 12028 3033 1 -4 8 0 7835 4400 1 -3 8 0 6509 3435 1 -2 8 0 6370 2934 1 -1 8 0 152311 5143 1 0 8 0 50469 3617 1 1 8 0 4993 1952 1 2 8 0 45698 3211 1 3 8 0 149232 4255 1 4 8 0 43724 2340 1 5 8 0 79106 3836 1 6 8 0 1026 1791 1 7 8 0 15103 2088 1 8 8 0 19978 2505 1 9 8 0 56636 2944 1 10 8 0 110489 4171 1 11 8 0 16374 2708 1 -3 9 0 -3439 3439 1 -2 9 0 -2913 2913 1 -1 9 0 4544 2776 1 0 9 0 1796 2347 1 1 9 0 27133 2993 1 2 9 0 17255 2794 1 3 9 0 67738 4274 1 4 9 0 12801 2965 1 5 9 0 106808 6504 1 6 9 0 186613 7449 1 7 9 0 102768 3979 1 8 9 0 -2043 2043 1 9 9 0 22282 2278 1 10 9 0 12071 3163 1 -2 10 0 7896 3768 1 -1 10 0 14876 4119 1 0 10 0 2226 3330 1 1 10 0 35382 3763 1 2 10 0 36900 4258 1 3 10 0 39787 4143 1 4 10 0 -1234 2998 1 5 10 0 -1530 4014 1 6 10 0 7956 4084 1 7 10 0 -2709 2709 1 8 10 0 -2625 2625 1 9 10 0 3324 3064 1 10 10 0 17276 4722 1 0 11 0 -3412 3412 1 1 11 0 15276 3540 1 2 11 0 -215 2886 1 3 11 0 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0 15 8873 3971 1 -1 0 15 316 3222 1 0 0 15 -1571 3582 1 1 0 15 30684 5285 1 2 0 15 144341 8951 1 3 0 15 110279 11305 1 4 0 15 9700 5422 1 5 0 15 103143 6777 1 -6 0 -15 111597 7046 -2 6 0 15 111597 7046 1 -4 1 15 4429 5965 1 -3 1 15 15565 4888 1 -2 1 15 76198 5903 1 -1 1 15 52262 4678 1 0 1 15 -3041 3041 1 1 1 15 66346 4910 1 2 1 15 98002 5509 1 3 1 15 45222 5310 1 4 1 15 2721 5170 1 5 1 15 1131 3604 1 6 1 15 4402 3802 1 -3 2 15 9107 4745 1 -2 2 15 2171 3807 1 -1 2 15 5 3771 1 0 2 15 19640 3874 1 1 2 15 75847 5145 1 2 2 15 47745 4444 1 3 2 15 30373 4383 1 4 2 15 44506 5217 1 5 2 15 101691 6571 1 6 2 15 40525 6545 1 7 2 15 304 3632 1 -3 3 15 16922 5268 1 -2 3 15 58603 5149 1 -1 3 15 14625 3999 1 0 3 15 3921 3369 1 1 3 15 41779 5268 1 2 3 15 17077 3752 1 3 3 15 -916 3273 1 4 3 15 2840 3417 1 5 3 15 3974 5184 1 6 3 15 393 3512 1 7 3 15 -779 3572 1 -2 4 15 -491 4232 1 -1 4 15 2928 4344 1 0 4 15 -2327 3393 1 1 4 15 40112 4632 1 2 4 15 20575 4212 1 3 4 15 -1531 3487 1 4 4 15 67652 6357 1 5 4 15 206966 8765 1 6 4 15 67354 5723 1 7 4 15 -2505 2999 1 -1 5 15 -227 4273 1 0 5 15 16027 4232 1 1 5 15 30224 5329 1 2 5 15 37268 5353 1 3 5 15 25617 4633 1 4 5 15 222 3747 1 5 5 15 4522 3965 1 6 5 15 6481 4001 1 7 5 15 42052 4486 1 0 6 15 9781 4107 1 1 6 15 23400 4401 1 2 6 15 4221 4105 1 3 6 15 18617 4524 1 4 6 15 99213 6541 1 5 6 15 156605 8956 1 6 6 15 34942 5079 1 7 6 15 1535 3652 1 1 7 15 20556 5374 1 2 7 15 7604 4468 1 3 7 15 14998 4631 1 4 7 15 624 4279 1 5 7 15 3835 4099 1 6 7 15 -2595 3782 1 4 8 15 45366 6026 1 -2 -2 16 -1741 7935 1 -1 -2 16 10482 5383 1 0 -2 16 29913 6321 1 1 -2 16 12414 5512 1 2 -2 16 -2552 4342 1 -2 -1 16 2386 4768 1 -1 -1 16 11995 5874 1 0 -1 16 42027 5864 1 1 -1 16 17696 4874 1 2 -1 16 496 4219 1 3 -1 16 4564 4329 1 4 -1 16 2598 4262 1 -2 0 16 -1291 5921 1 -1 0 16 -1753 5438 1 0 0 16 6706 6495 1 1 0 16 2267 3774 1 2 0 16 5406 4502 1 3 0 16 143273 8130 1 4 0 16 68148 6214 1 5 0 16 6147 4259 1 -2 1 16 6970 4489 1 -1 1 16 27333 5112 1 0 1 16 36711 4872 1 1 1 16 596 3353 1 2 1 16 10442 5432 1 3 1 16 9772 4521 1 4 1 16 5211 4210 1 5 1 16 1915 3997 1 -2 2 16 -1565 4333 1 -1 2 16 3458 5450 1 0 2 16 10773 4251 1 1 2 16 -2610 3273 1 2 2 16 13638 3817 1 3 2 16 187047 8183 1 4 2 16 136634 9418 1 5 2 16 14131 4469 1 6 2 16 17390 4353 1 -1 3 16 61369 5926 1 0 3 16 70830 6221 1 1 3 16 13441 3864 1 2 3 16 -171 3931 1 3 3 16 5463 3958 1 4 3 16 -3026 3626 1 5 3 16 6685 4086 1 6 3 16 6544 4123 1 -1 4 16 9775 6796 1 0 4 16 9456 4320 1 1 4 16 -726 3566 1 2 4 16 22450 4786 1 3 4 16 49213 5350 1 4 4 16 24233 5279 1 5 4 16 12042 4246 1 6 4 16 77908 6337 1 0 5 16 1034 4945 1 1 5 16 -3778 3778 1 2 5 16 12315 4657 1 3 5 16 5084 4266 1 4 5 16 5123 4817 1 5 5 16 9327 5287 1 6 5 16 12856 4544 1 2 6 16 45647 5705 1 3 6 16 25217 5197 1 4 6 16 5843 4386 1 5 6 16 5182 4421 1 0 0 17 7104 5004 1 1 0 17 22658 6320 1 2 0 17 36858 5696 1 0 1 17 1266 4045 1 1 1 17 35840 5947 1 2 1 17 17985 5368 1 3 1 17 17666 5066 1 0 2 17 46195 5545 1 1 2 17 56628 5848 1 2 2 17 26533 4834 1 3 2 17 936 4573 1 4 2 17 59368 6535 1 1 3 17 53216 5850 1 2 3 17 2360 4304 1 3 3 17 -3126 3852 1 4 3 17 125 4231 1 2 4 17 11760 4662 1 3 4 17 6132 4337 1 4 4 17 62194 5852 1 ; _shelx_hkl_checksum 8552 _shelx_res_file ; TITL II_p_1_a.res in P-1 II.res created by SHELXL-2018/3 at 07:09:10 on 01-Nov-2022 REM Old TITL II_p_1_b.res in P1 REM SHELXT solution in P-1: R1 0.196, Rweak 0.032, Alpha 0.044 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C17 Cl2 N7 Ni2 O5 CELL 0.71073 10.1565 10.4249 14.6531 80.305 80.117 64.149 ZERR 2 0.0004 0.0005 0.0007 0.003 0.003 0.003 LATT 1 SFAC C H Cd Cl Cu N O UNIT 32 73 2 4 2 12 12.5 EQIV $1 -X,-Y,-Z EQIV $2 1-X,1-Y,1-Z EQIV $3 +X,+Y,-1+Z EQIV $4 1-X,-Y,1-Z EQIV $5 -X,1-Y,-Z EQIV $6 -X,1-Y,1-Z DFIX 0.86 0.01 O4W H4Wa O4W H4Wb DFIX 1.44 0.01 H4Wb H4Wa L.S. 10 PLAN 10 SIZE 0.05 0.05 0.15 TEMP 0 CONF HTAB N4 O4_$1 HTAB N1 Cl2_$2 HTAB N6 Cl1_$3 HTAB N6 Cl1_$4 HTAB N3 O2W HTAB O1W O2W HTAB O1W O3_$5 HTAB C9 O1 HTAB C6 Cl2_$3 HTAB C2 O1_$4 HTAB C1 Cl1_$4 HTAB C13 Cl1_$3 HTAB C3 O1_$4 HTAB O2W O2_$2 HTAB O2W O5W_$6 HTAB O2W O4W_$6 HTAB O3W Cl2_$6 FREE Cd1 C12 BIND Cu1 O1W htab LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 999 0.84 OMIT 1 1 2 OMIT 3 6 6 OMIT 0 -2 1 OMIT 5 -6 2 OMIT 5 6 1 OMIT -5 -6 2 OMIT 0 -6 10 OMIT -1 -1 1 OMIT 6 -6 4 OMIT -1 -6 9 OMIT 0 -6 7 OMIT 0 6 8 OMIT -3 0 2 OMIT 1 -6 10 OMIT -3 6 0 REM REM REM WGHT 0.075700 2.625400 BASF 0.36050 FVAR 12.22026 PART 1 CD1 3 0.596701 0.268532 0.762208 11.00000 0.05450 0.04863 = 0.03674 -0.00472 -0.01186 -0.02891 PART 0 CU1 5 0.330397 0.224346 0.196073 11.00000 0.03788 0.04422 = 0.03401 0.00062 -0.00874 -0.02231 CL1 4 0.518032 0.082870 0.854615 11.00000 0.05885 0.03977 = 0.04981 -0.00451 -0.00139 -0.02511 CL2 4 0.379537 0.503754 0.787499 11.00000 0.07046 0.04801 = 0.06414 -0.00144 -0.00270 -0.02225 O3 7 -0.242663 0.275738 -0.151027 11.00000 0.05340 0.05396 = 0.05964 -0.00257 -0.02219 -0.02655 N4 6 0.140249 0.212457 0.194232 11.00000 0.03386 0.04040 = 0.04460 -0.01124 -0.00338 -0.01610 AFIX 13 H4 2 0.163812 0.116420 0.178712 11.00000 -1.20000 AFIX 0 O1 7 0.607934 0.230811 0.612022 11.00000 0.09343 0.07248 = 0.04039 -0.00446 -0.00879 -0.05419 N1 6 0.527978 0.226400 0.198559 11.00000 0.04173 0.04871 = 0.03777 -0.00590 -0.00426 -0.02868 AFIX 13 H1 2 0.509753 0.317288 0.220179 11.00000 -1.20000 AFIX 0 O4 7 -0.135159 0.072702 -0.213431 11.00000 0.07563 0.06212 = 0.07464 -0.01721 -0.01695 -0.04047 N6 6 0.361647 0.265060 0.057274 11.00000 0.04362 0.03302 = 0.03840 -0.00341 -0.01104 -0.01888 AFIX 13 H6 2 0.402797 0.173055 0.031144 11.00000 -1.20000 AFIX 0 N3 6 0.301876 0.180213 0.335773 11.00000 0.04636 0.04555 = 0.03205 -0.00215 -0.00799 -0.02543 AFIX 13 H3 2 0.268598 0.269992 0.363502 11.00000 -1.20000 AFIX 0 O1W 7 0.200788 0.477688 0.221683 11.00000 0.09988 0.04743 = 0.06672 -0.00360 -0.01473 -0.03188 AFIX 3 H1WA 2 0.209328 0.487228 0.276563 11.00000 -1.50000 H1WB 2 0.244848 0.523768 0.186423 11.00000 -1.50000 AFIX 0 N2 6 0.559319 0.110202 0.357998 11.00000 0.04584 0.05205 = 0.03823 -0.00250 -0.01431 -0.02354 N5 6 0.114970 0.312253 0.031727 11.00000 0.04713 0.04380 = 0.04675 -0.00797 -0.01539 -0.01543 O2 7 0.704948 0.374954 0.621225 11.00000 0.09772 0.09606 = 0.05566 -0.02473 -0.00298 -0.06050 C16 1 -0.134066 0.157341 -0.164673 11.00000 0.04987 0.04167 = 0.04234 -0.00062 -0.01051 -0.02257 C12 1 0.670087 0.307546 0.574778 11.00000 0.05697 0.05040 = 0.04740 -0.01226 -0.00985 -0.02512 C8 1 0.596145 0.226219 0.101600 11.00000 0.04433 0.06394 = 0.04860 -0.01313 -0.00148 -0.03091 AFIX 23 H8A 2 0.642826 0.129227 0.084057 11.00000 -1.20000 H8B 2 0.670876 0.262438 0.095161 11.00000 -1.20000 AFIX 0 C9 1 0.551728 0.225380 0.407369 11.00000 0.05193 0.05173 = 0.03755 -0.00770 -0.00848 -0.02629 AFIX 23 H9A 2 0.496317 0.223751 0.468128 11.00000 -1.20000 H9B 2 0.499763 0.317219 0.372695 11.00000 -1.20000 AFIX 0 C6 1 0.227844 0.361121 0.010996 11.00000 0.05338 0.03831 = 0.04467 -0.00100 -0.01606 -0.01911 AFIX 23 H6A 2 0.190725 0.456242 0.030616 11.00000 -1.20000 H6B 2 0.254370 0.368360 -0.055885 11.00000 -1.20000 AFIX 0 C2 1 0.435617 0.074397 0.378162 11.00000 0.06326 0.05087 = 0.04711 0.00307 -0.02298 -0.03362 AFIX 23 H2A 2 0.411541 0.064332 0.445198 11.00000 -1.20000 H2B 2 0.463691 -0.017891 0.356448 11.00000 -1.20000 AFIX 0 C1 1 0.621807 0.109083 0.262412 11.00000 0.04310 0.05377 = 0.04930 -0.01297 -0.01564 -0.01783 AFIX 23 H1A 2 0.641518 0.018262 0.241569 11.00000 -1.20000 H1B 2 0.715277 0.115140 0.258505 11.00000 -1.20000 AFIX 0 C7 1 0.478189 0.320202 0.038949 11.00000 0.06156 0.05863 = 0.03975 -0.00997 0.00304 -0.04029 AFIX 23 H7A 2 0.437003 0.419018 0.052579 11.00000 -1.20000 H7B 2 0.519349 0.315835 -0.025881 11.00000 -1.20000 AFIX 0 C5 1 0.044045 0.317750 0.124898 11.00000 0.04264 0.05004 = 0.04861 -0.01152 -0.01167 -0.01529 AFIX 23 H5A 2 -0.042463 0.299751 0.126945 11.00000 -1.20000 H5B 2 0.011290 0.413532 0.142412 11.00000 -1.20000 AFIX 0 C4 1 0.066185 0.223479 0.291102 11.00000 0.04399 0.06514 = 0.04477 -0.01565 0.00237 -0.02577 AFIX 23 H4A 2 -0.009896 0.188734 0.299020 11.00000 -1.20000 H4B 2 0.020861 0.322564 0.304598 11.00000 -1.20000 AFIX 0 C13 1 0.132417 0.193809 -0.018180 11.00000 0.04547 0.05026 = 0.04992 -0.00733 -0.01664 -0.01107 AFIX 23 H13A 2 0.156987 0.106670 0.024350 11.00000 -1.20000 H13B 2 0.212635 0.178056 -0.067872 11.00000 -1.20000 AFIX 0 C3 1 0.181297 0.133872 0.355704 11.00000 0.05783 0.06458 = 0.03830 -0.00456 0.00347 -0.03932 AFIX 23 H3A 2 0.138471 0.145448 0.419911 11.00000 -1.20000 H3B 2 0.218770 0.033436 0.346619 11.00000 -1.20000 AFIX 0 C14 1 -0.007419 0.227001 -0.058686 11.00000 0.04986 0.05404 = 0.06967 -0.01674 -0.02150 -0.01800 AFIX 23 H14A 2 -0.083924 0.232508 -0.007732 11.00000 -1.20000 H14B 2 -0.037838 0.320795 -0.094049 11.00000 -1.20000 AFIX 0 C15 1 0.002663 0.122942 -0.119804 11.00000 0.05334 0.05131 = 0.06018 -0.00932 -0.01503 -0.02129 AFIX 23 H15A 2 0.028909 0.030147 -0.083454 11.00000 -1.20000 H15B 2 0.082553 0.114088 -0.168889 11.00000 -1.20000 AFIX 0 C10 1 0.701504 0.210367 0.419393 11.00000 0.06341 0.08938 = 0.04350 -0.02066 -0.00079 -0.04755 AFIX 23 H10A 2 0.756318 0.210913 0.358318 11.00000 -1.20000 H10B 2 0.752778 0.117877 0.453587 11.00000 -1.20000 AFIX 0 C11 1 0.702584 0.324451 0.469192 11.00000 0.09307 0.10643 = 0.03821 -0.01424 -0.00241 -0.07333 AFIX 23 H11A 2 0.630509 0.416470 0.445325 11.00000 -1.20000 H11B 2 0.798489 0.326495 0.453979 11.00000 -1.20000 AFIX 0 PART 3 O5W 7 -0.129008 0.756063 0.372687 10.25000 0.07503 AFIX 3 H5WA 2 -0.133178 0.717443 0.327227 10.25000 -1.50000 H5WB 2 -0.043408 0.754503 0.363557 10.25000 -1.50000 AFIX 0 PART 2 O4W 7 -0.215377 0.686038 0.340509 10.25000 0.08469 AFIX 3 H4WA 2 -0.178747 0.593968 0.349859 10.25000 -1.50000 H4WB 2 -0.210637 0.725748 0.386049 10.25000 -1.50000 AFIX 0 PART 0 O2W 7 0.156684 0.447953 0.433217 10.50000 0.07385 AFIX 3 H2WA 2 0.212914 0.489423 0.431887 10.50000 -1.50000 H2WB 2 0.144304 0.419643 0.491597 10.50000 -1.50000 AFIX 0 PART 1 O3W 7 -0.142153 0.609766 0.273345 10.25000 0.08818 AFIX 3 H3WA 2 -0.167073 0.670086 0.312565 10.25000 -1.50000 H3WB 2 -0.167283 0.544546 0.302075 10.25000 -1.50000 AFIX 0 HKLF 5 REM II_a.res in P-1 REM wR2 = 0.1487, GooF = S = 1.037, Restrained GooF = 1.037 for all data REM R1 = 0.0496 for 3446 Fo > 4sig(Fo) and 0.0783 for all 4762 data REM 297 parameters refined using 3 restraints END WGHT 0.0755 2.6329 REM Instructions for potential hydrogen bonds HTAB N4 O4_$1 HTAB N1 Cl2_$2 HTAB N6 Cl1_$3 HTAB N6 Cl1_$4 HTAB N3 O2W HTAB O1W O2W HTAB O1W O3_$5 HTAB C9 O1 HTAB C6 Cl2_$3 HTAB C2 O1_$4 HTAB C1 Cl1_$4 HTAB C13 Cl1_$3 HTAB C3 O1_$4 HTAB O2W O2_$2 HTAB O2W O5W_$6 HTAB O2W O4W_$6 HTAB O3W Cl2_$6 REM Highest difference peak 1.311, deepest hole -0.687, 1-sigma level 0.127 Q1 1 0.1099 0.5054 0.4003 11.00000 0.05 0.97 Q2 1 0.3978 0.2352 0.2402 11.00000 0.05 0.84 Q3 1 0.5975 0.0857 0.7625 11.00000 0.05 0.82 Q4 1 0.5959 0.3899 0.7583 11.00000 0.05 0.78 Q5 1 0.3259 0.3559 0.1899 11.00000 0.05 0.72 Q6 1 0.4025 0.3877 0.2315 11.00000 0.05 0.67 Q7 1 0.4827 0.4907 0.7922 11.00000 0.05 0.63 Q8 1 0.4016 0.0749 0.2401 11.00000 0.05 0.62 Q9 1 0.2584 0.6364 0.7811 11.00000 0.05 0.58 Q10 1 -0.2077 0.6133 0.4276 11.00000 0.05 0.58 ; _shelx_res_checksum 9188 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.59670(6) 0.26853(5) 0.76221(3) 0.04306(19) Uani d 1 A 1 Cu Cu1 0.33040(8) 0.22435(8) 0.19607(5) 0.0368(2) Uani d 1 . . Cl Cl1 0.51803(19) 0.08287(18) 0.85462(13) 0.0485(4) Uani d 1 . . Cl Cl2 0.3795(2) 0.5038(2) 0.78750(15) 0.0630(5) Uani d 1 . . O O3 -0.2427(5) 0.2757(5) -0.1510(4) 0.0526(13) Uani d 1 . . N N4 0.1402(5) 0.2125(6) 0.1942(4) 0.0387(13) Uani d 1 . . H H4 0.163812 0.116420 0.178712 0.046 Uiso calc 1 . . O O1 0.6079(6) 0.2308(6) 0.6120(3) 0.0617(14) Uani d 1 . . N N1 0.5280(6) 0.2264(6) 0.1986(4) 0.0391(13) Uani d 1 . . H H1 0.509753 0.317288 0.220179 0.047 Uiso calc 1 . . O O4 -0.1352(6) 0.0727(6) -0.2134(4) 0.0642(15) Uani d 1 . . N N6 0.3616(5) 0.2651(5) 0.0573(4) 0.0365(12) Uani d 1 . . H H6 0.402797 0.173055 0.031144 0.044 Uiso calc 1 . . N N3 0.3019(6) 0.1802(6) 0.3358(4) 0.0389(12) Uani d 1 . . H H3 0.268598 0.269992 0.363502 0.047 Uiso calc 1 . . O O1W 0.2008(7) 0.4777(6) 0.2217(4) 0.0706(16) Uani d 1 . . H H1WA 0.209328 0.487228 0.276563 0.106 Uiso d 1 . . H H1WB 0.244848 0.523768 0.186423 0.106 Uiso d 1 . . N N2 0.5593(6) 0.1102(6) 0.3580(4) 0.0433(14) Uani d 1 . . N N5 0.1150(6) 0.3123(6) 0.0317(4) 0.0455(14) Uani d 1 . . O O2 0.7049(7) 0.3750(7) 0.6212(4) 0.0745(17) Uani d 1 . . C C16 -0.1341(8) 0.1573(8) -0.1647(5) 0.0432(16) Uani d 1 . . C C12 0.6701(8) 0.3075(8) 0.5748(5) 0.0492(18) Uani d 1 . . C C8 0.5961(7) 0.2262(8) 0.1016(5) 0.0489(18) Uani d 1 . . H H8A 0.642826 0.129227 0.084057 0.059 Uiso calc 1 . . H H8B 0.670876 0.262438 0.095161 0.059 Uiso calc 1 . . C C9 0.5517(7) 0.2254(8) 0.4074(5) 0.0446(16) Uani d 1 . . H H9A 0.496317 0.223751 0.468128 0.053 Uiso calc 1 . . H H9B 0.499763 0.317219 0.372695 0.053 Uiso calc 1 . . C C6 0.2278(7) 0.3611(7) 0.0110(5) 0.0445(16) Uani d 1 . . H H6A 0.190725 0.456242 0.030616 0.053 Uiso calc 1 . . H H6B 0.254370 0.368360 -0.055885 0.053 Uiso calc 1 . . C C2 0.4356(8) 0.0744(8) 0.3782(5) 0.0491(18) Uani d 1 . . H H2A 0.411541 0.064332 0.445198 0.059 Uiso calc 1 . . H H2B 0.463691 -0.017891 0.356448 0.059 Uiso calc 1 . . C C1 0.6218(7) 0.1091(8) 0.2624(5) 0.0473(18) Uani d 1 . . H H1A 0.641518 0.018262 0.241569 0.057 Uiso calc 1 . . H H1B 0.715277 0.115140 0.258505 0.057 Uiso calc 1 . . C C7 0.4782(8) 0.3202(8) 0.0389(5) 0.0483(17) Uani d 1 . . H H7A 0.437003 0.419018 0.052579 0.058 Uiso calc 1 . . H H7B 0.519349 0.315835 -0.025881 0.058 Uiso calc 1 . . C C5 0.0440(7) 0.3178(8) 0.1249(5) 0.0469(17) Uani d 1 . . H H5A -0.042463 0.299751 0.126945 0.056 Uiso calc 1 . . H H5B 0.011290 0.413532 0.142412 0.056 Uiso calc 1 . . C C4 0.0662(7) 0.2235(9) 0.2911(5) 0.0499(18) Uani d 1 . . H H4A -0.009896 0.188734 0.299020 0.060 Uiso calc 1 . . H H4B 0.020861 0.322564 0.304598 0.060 Uiso calc 1 . . C C13 0.1324(8) 0.1938(8) -0.0182(5) 0.0501(18) Uani d 1 . . H H13A 0.156987 0.106670 0.024350 0.060 Uiso calc 1 . . H H13B 0.212635 0.178056 -0.067872 0.060 Uiso calc 1 . . C C3 0.1813(8) 0.1339(8) 0.3557(5) 0.0499(18) Uani d 1 . . H H3A 0.138471 0.145448 0.419911 0.060 Uiso calc 1 . . H H3B 0.218770 0.033436 0.346619 0.060 Uiso calc 1 . . C C14 -0.0074(8) 0.2270(8) -0.0587(6) 0.056(2) Uani d 1 . . H H14A -0.083924 0.232508 -0.007732 0.067 Uiso calc 1 . . H H14B -0.037838 0.320795 -0.094049 0.067 Uiso calc 1 . . C C15 0.0027(8) 0.1229(8) -0.1198(6) 0.0536(19) Uani d 1 . . H H15A 0.028909 0.030147 -0.083454 0.064 Uiso calc 1 . . H H15B 0.082553 0.114088 -0.168889 0.064 Uiso calc 1 . . C C10 0.7015(8) 0.2104(10) 0.4194(5) 0.059(2) Uani d 1 . . H H10A 0.756318 0.210913 0.358318 0.070 Uiso calc 1 . . H H10B 0.752778 0.117877 0.453587 0.070 Uiso calc 1 . . C C11 0.7026(10) 0.3245(11) 0.4692(5) 0.068(2) Uani d 1 . . H H11A 0.630509 0.416470 0.445325 0.081 Uiso calc 1 . . H H11B 0.798489 0.326495 0.453979 0.081 Uiso calc 1 . . O O5W -0.129(3) 0.756(3) 0.3727(17) 0.075(7) Uiso d 0.25 B 3 H H5WA -0.133178 0.717443 0.327227 0.113 Uiso d 0.25 B 3 H H5WB -0.043408 0.754503 0.363557 0.113 Uiso d 0.25 B 3 O O4W -0.215(3) 0.686(3) 0.3405(19) 0.085(7) Uiso d 0.25 C 2 H H4WA -0.178747 0.593968 0.349859 0.127 Uiso d 0.25 C 2 H H4WB -0.210637 0.725748 0.386049 0.127 Uiso d 0.25 C 2 O O2W 0.1567(12) 0.4480(13) 0.4332(8) 0.074(3) Uiso d 0.5 . . H H2WA 0.212914 0.489423 0.431887 0.111 Uiso d 0.5 . . H H2WB 0.144304 0.419643 0.491597 0.111 Uiso d 0.5 . . O O3W -0.142(3) 0.610(3) 0.2733(19) 0.088(8) Uiso d 0.25 D 1 H H3WA -0.167073 0.670086 0.312565 0.132 Uiso d 0.25 D 1 H H3WB -0.167283 0.544546 0.302075 0.132 Uiso d 0.25 D 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 0.0545(3) 0.0486(3) 0.0367(3) -0.0289(3) -0.0119(2) -0.0047(2) Cu1 0.0379(4) 0.0442(5) 0.0340(5) -0.0223(4) -0.0087(3) 0.0006(4) Cl1 0.0588(10) 0.0398(9) 0.0498(11) -0.0251(8) -0.0014(8) -0.0045(8) Cl2 0.0705(13) 0.0480(11) 0.0641(13) -0.0222(10) -0.0027(10) -0.0014(10) O3 0.053(3) 0.054(3) 0.060(3) -0.027(3) -0.022(2) -0.003(3) N4 0.034(3) 0.040(3) 0.045(3) -0.016(2) -0.003(2) -0.011(3) O1 0.093(4) 0.072(4) 0.040(3) -0.054(3) -0.009(3) -0.004(3) N1 0.042(3) 0.049(3) 0.038(3) -0.029(3) -0.004(2) -0.006(3) O4 0.076(4) 0.062(3) 0.075(4) -0.040(3) -0.017(3) -0.017(3) N6 0.044(3) 0.033(3) 0.038(3) -0.019(2) -0.011(2) -0.003(2) N3 0.046(3) 0.046(3) 0.032(3) -0.025(3) -0.008(2) -0.002(2) O1W 0.100(4) 0.047(3) 0.067(4) -0.032(3) -0.015(3) -0.004(3) N2 0.046(3) 0.052(3) 0.038(3) -0.024(3) -0.014(3) -0.003(3) N5 0.047(3) 0.044(3) 0.047(4) -0.015(3) -0.015(3) -0.008(3) O2 0.098(4) 0.096(5) 0.056(4) -0.061(4) -0.003(3) -0.025(3) C16 0.050(4) 0.042(4) 0.042(4) -0.023(4) -0.011(3) -0.001(3) C12 0.057(4) 0.050(4) 0.047(4) -0.025(4) -0.010(4) -0.012(4) C8 0.044(4) 0.064(5) 0.049(4) -0.031(4) -0.001(3) -0.013(4) C9 0.052(4) 0.052(4) 0.038(4) -0.026(3) -0.008(3) -0.008(3) C6 0.053(4) 0.038(4) 0.045(4) -0.019(3) -0.016(3) -0.001(3) C2 0.063(5) 0.051(4) 0.047(4) -0.034(4) -0.023(4) 0.003(3) C1 0.043(4) 0.054(4) 0.049(4) -0.018(3) -0.016(3) -0.013(4) C7 0.062(4) 0.059(5) 0.040(4) -0.040(4) 0.003(3) -0.010(3) C5 0.043(4) 0.050(4) 0.049(4) -0.015(3) -0.012(3) -0.012(3) C4 0.044(4) 0.065(5) 0.045(4) -0.026(4) 0.002(3) -0.016(4) C13 0.045(4) 0.050(4) 0.050(4) -0.011(3) -0.017(3) -0.007(4) C3 0.058(4) 0.065(5) 0.038(4) -0.039(4) 0.003(3) -0.005(4) C14 0.050(4) 0.054(5) 0.070(5) -0.018(4) -0.022(4) -0.017(4) C15 0.053(4) 0.051(4) 0.060(5) -0.021(4) -0.015(4) -0.009(4) C10 0.063(5) 0.089(6) 0.043(4) -0.048(5) -0.001(4) -0.021(4) C11 0.093(6) 0.106(7) 0.038(4) -0.073(6) -0.002(4) -0.014(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 _geom_angle_publ_flag Cl1 Cd1 Cl2 . . 104.67(7) y Cl1 Cd1 O4 . 1_656 84.16(13) ? Cl2 Cd1 O4 . 1_656 153.76(12) ? O3 Cd1 Cl1 1_656 . 103.44(14) ? O3 Cd1 Cl2 1_656 . 101.32(14) ? O3 Cd1 O1 1_656 . 134.6(2) ? O3 Cd1 O4 1_656 1_656 52.44(17) y O3 Cd1 O2 1_656 . 90.52(19) ? O1 Cd1 Cl1 . . 103.28(14) ? O1 Cd1 Cl2 . . 106.49(16) ? O1 Cd1 O4 . 1_656 95.06(19) ? O1 Cd1 O2 . . 53.54(19) y O2 Cd1 Cl1 . . 154.86(14) ? O2 Cd1 Cl2 . . 92.68(16) ? O2 Cd1 O4 . 1_656 88.2(2) ? N4 Cu1 N1 . . 177.4(2) ? N4 Cu1 N6 . . 93.9(2) y N4 Cu1 N3 . . 86.5(2) y N4 Cu1 O1W . . 91.0(2) ? N1 Cu1 O1W . . 91.6(2) ? N6 Cu1 N1 . . 86.6(2) y N6 Cu1 N3 . . 179.1(2) ? N6 Cu1 O1W . . 93.9(2) ? N3 Cu1 N1 . . 93.0(2) y N3 Cu1 O1W . . 86.9(2) ? C16 O3 Cd1 . 1_454 100.6(4) ? Cu1 N4 H4 . . 107.3 ? C5 N4 Cu1 . . 115.2(4) ? C5 N4 H4 . . 107.3 ? C4 N4 Cu1 . . 106.6(4) ? C4 N4 H4 . . 107.3 ? C4 N4 C5 . . 112.7(5) ? C12 O1 Cd1 . . 97.8(4) ? Cu1 N1 H1 . . 107.7 ? C8 N1 Cu1 . . 106.7(4) ? C8 N1 H1 . . 107.7 ? C8 N1 C1 . . 113.5(5) ? C1 N1 Cu1 . . 113.3(4) ? C1 N1 H1 . . 107.7 ? C16 O4 Cd1 . 1_454 84.1(4) ? Cu1 N6 H6 . . 107.3 ? C6 N6 Cu1 . . 116.0(4) ? C6 N6 H6 . . 107.3 ? C6 N6 C7 . . 112.8(5) ? C7 N6 Cu1 . . 105.9(4) ? C7 N6 H6 . . 107.3 ? Cu1 N3 H3 . . 107.7 ? C2 N3 Cu1 . . 115.1(4) ? C2 N3 H3 . . 107.7 ? C3 N3 Cu1 . . 106.6(4) ? C3 N3 H3 . . 107.7 ? C3 N3 C2 . . 111.9(5) ? Cu1 O1W H1WA . . 109.1 ? Cu1 O1W H1WB . . 108.8 ? H1WA O1W H1WB . . 104.5 ? C2 N2 C9 . . 116.2(6) ? C2 N2 C1 . . 115.4(5) ? C1 N2 C9 . . 116.2(6) ? C6 N5 C5 . . 117.2(5) ? C6 N5 C13 . . 116.7(6) ? C5 N5 C13 . . 117.3(6) ? C12 O2 Cd1 . . 87.1(5) ? O3 C16 C15 . . 117.2(6) ? O4 C16 O3 . . 122.9(6) ? O4 C16 C15 . . 119.9(7) ? O1 C12 O2 . . 121.5(7) ? O1 C12 C11 . . 119.9(6) ? O2 C12 C11 . . 118.5(7) ? N1 C8 H8A . . 109.9 ? N1 C8 H8B . . 109.9 ? N1 C8 C7 . . 108.9(6) ? H8A C8 H8B . . 108.3 ? C7 C8 H8A . . 109.9 ? C7 C8 H8B . . 109.9 ? N2 C9 H9A . . 109.2 ? N2 C9 H9B . . 109.2 ? N2 C9 C10 . . 112.0(6) ? H9A C9 H9B . . 107.9 ? C10 C9 H9A . . 109.2 ? C10 C9 H9B . . 109.2 ? N6 C6 H6A . . 109.0 ? N6 C6 H6B . . 109.0 ? N5 C6 N6 . . 112.8(5) ? N5 C6 H6A . . 109.0 ? N5 C6 H6B . . 109.0 ? H6A C6 H6B . . 107.8 ? N3 C2 H2A . . 108.6 ? N3 C2 H2B . . 108.6 ? N2 C2 N3 . . 114.7(6) ? N2 C2 H2A . . 108.6 ? N2 C2 H2B . . 108.6 ? H2A C2 H2B . . 107.6 ? N1 C1 H1A . . 108.7 ? N1 C1 H1B . . 108.7 ? N2 C1 N1 . . 114.4(5) ? N2 C1 H1A . . 108.7 ? N2 C1 H1B . . 108.7 ? H1A C1 H1B . . 107.6 ? N6 C7 C8 . . 107.2(6) ? N6 C7 H7A . . 110.3 ? N6 C7 H7B . . 110.3 ? C8 C7 H7A . . 110.3 ? C8 C7 H7B . . 110.3 ? H7A C7 H7B . . 108.5 ? N4 C5 H5A . . 108.9 ? N4 C5 H5B . . 108.9 ? N5 C5 N4 . . 113.5(5) ? N5 C5 H5A . . 108.9 ? N5 C5 H5B . . 108.9 ? H5A C5 H5B . . 107.7 ? N4 C4 H4A . . 110.2 ? N4 C4 H4B . . 110.2 ? N4 C4 C3 . . 107.7(5) ? H4A C4 H4B . . 108.5 ? C3 C4 H4A . . 110.2 ? C3 C4 H4B . . 110.2 ? N5 C13 H13A . . 109.5 ? N5 C13 H13B . . 109.5 ? N5 C13 C14 . . 110.8(6) ? H13A C13 H13B . . 108.1 ? C14 C13 H13A . . 109.5 ? C14 C13 H13B . . 109.5 ? N3 C3 C4 . . 108.8(6) ? N3 C3 H3A . . 109.9 ? N3 C3 H3B . . 109.9 ? C4 C3 H3A . . 109.9 ? C4 C3 H3B . . 109.9 ? H3A C3 H3B . . 108.3 ? C13 C14 H14A . . 108.4 ? C13 C14 H14B . . 108.4 ? H14A C14 H14B . . 107.5 ? C15 C14 C13 . . 115.5(6) ? C15 C14 H14A . . 108.4 ? C15 C14 H14B . . 108.4 ? C16 C15 H15A . . 108.2 ? C16 C15 H15B . . 108.2 ? C14 C15 C16 . . 116.5(6) ? C14 C15 H15A . . 108.2 ? C14 C15 H15B . . 108.2 ? H15A C15 H15B . . 107.3 ? C9 C10 H10A . . 108.5 ? C9 C10 H10B . . 108.5 ? C9 C10 C11 . . 115.1(7) ? H10A C10 H10B . . 107.5 ? C11 C10 H10A . . 108.5 ? C11 C10 H10B . . 108.5 ? C12 C11 H11A . . 108.3 ? C12 C11 H11B . . 108.3 ? C10 C11 C12 . . 115.8(7) ? C10 C11 H11A . . 108.3 ? C10 C11 H11B . . 108.3 ? H11A C11 H11B . . 107.4 ? H5WA O5W H5WB . . 104.5 ? H4WA O4W H4WB . . 113.5 ? H2WA O2W H2WB . . 103.1 ? H3WA O3W H3WB . . 104.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 Cl1 . 2.5125(18) y Cd1 Cl2 . 2.515(2) y Cd1 O3 1_656 2.266(4) y Cd1 O1 . 2.275(5) y Cd1 O4 1_656 2.637(6) y Cd1 O2 . 2.494(6) y Cu1 N4 . 1.993(5) y Cu1 N1 . 2.023(5) y Cu1 N6 . 2.006(5) y Cu1 N3 . 2.020(5) y Cu1 O1W . 2.446(5) y Cu1 Cl1 2_656 3.048(2) y O3 C16 . 1.265(8) ? N4 H4 . 0.9800 ? N4 C5 . 1.491(8) ? N4 C4 . 1.486(8) ? O1 C12 . 1.229(9) ? N1 H1 . 0.9800 ? N1 C8 . 1.470(8) ? N1 C1 . 1.478(8) ? O4 C16 . 1.230(8) ? N6 H6 . 0.9800 ? N6 C6 . 1.487(8) ? N6 C7 . 1.495(8) ? N3 H3 . 0.9800 ? N3 C2 . 1.483(8) ? N3 C3 . 1.471(8) ? O1W H1WA . 0.8500 ? O1W H1WB . 0.8500 ? N2 C9 . 1.471(8) ? N2 C2 . 1.432(8) ? N2 C1 . 1.435(9) ? N5 C6 . 1.416(9) ? N5 C5 . 1.428(9) ? N5 C13 . 1.470(9) ? O2 C12 . 1.242(8) ? C16 C15 . 1.513(9) ? C12 C11 . 1.522(10) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C8 C7 . 1.513(10) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C9 C10 . 1.498(9) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C4 C3 . 1.505(10) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C13 C14 . 1.510(9) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C14 C15 . 1.479(10) ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C10 C11 . 1.501(10) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? O5W H5WA . 0.8500 ? O5W H5WB . 0.8500 ? O4W H4WA . 0.8604 ? O4W H4WB . 0.8605 ? O2W H2WA . 0.8498 ? O2W H2WB . 0.8632 ? O3W H3WA . 0.8501 ? O3W H3WB . 0.8501 ? 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 O1W H1WB O3 2_565 0.85 2.06 2.787(7) 143 yes N4 H4 O4 2 0.98 2.08 2.961(8) 148 yes N1 H1 Cl2 2_666 0.98 2.54 3.377(5) 143 yes N6 H6 Cl1 2_656 0.98 2.77 3.379(5) 121 yes N3 H3 O2W . 0.98 2.04 3.006(13) 167 yes O1W H1WA O2W . 0.85 2.28 3.037(14) 149 yes O2W H2WA O2 2_666 0.85 1.93 2.721(14) 154 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cd1 O3 C16 O4 1_454 . . . -0.8(8) ? Cd1 O3 C16 C15 1_454 . . . 177.9(5) ? Cd1 O1 C12 O2 . . . . 0.0(8) ? Cd1 O1 C12 C11 . . . . -178.5(6) ? Cd1 O4 C16 O3 1_454 . . . 0.7(7) ? Cd1 O4 C16 C15 1_454 . . . -177.9(7) ? Cd1 O2 C12 O1 . . . . 0.0(8) ? Cd1 O2 C12 C11 . . . . 178.5(7) ? Cu1 N4 C5 N5 . . . . 55.3(7) ? Cu1 N4 C4 C3 . . . . -41.9(6) ? Cu1 N1 C8 C7 . . . . 38.4(6) ? Cu1 N1 C1 N2 . . . . -60.1(6) ? Cu1 N6 C6 N5 . . . . -55.0(6) ? Cu1 N6 C7 C8 . . . . 43.3(6) ? Cu1 N3 C2 N2 . . . . 55.6(7) ? Cu1 N3 C3 C4 . . . . -38.4(6) ? O3 C16 C15 C14 . . . . 4.1(11) ? N4 C4 C3 N3 . . . . 54.4(7) ? O1 C12 C11 C10 . . . . -19.3(12) ? N1 C8 C7 N6 . . . . -55.6(7) ? O4 C16 C15 C14 . . . . -177.2(7) ? N2 C9 C10 C11 . . . . 179.9(6) ? N5 C13 C14 C15 . . . . 173.1(7) ? O2 C12 C11 C10 . . . . 162.1(7) ? C8 N1 C1 N2 . . . . 178.0(5) ? C9 N2 C2 N3 . . . . 74.3(7) ? C9 N2 C1 N1 . . . . -71.1(7) ? C9 C10 C11 C12 . . . . 78.6(10) ? C6 N6 C7 C8 . . . . 171.2(5) ? C6 N5 C5 N4 . . . . -69.7(8) ? C6 N5 C13 C14 . . . . -131.6(7) ? C2 N3 C3 C4 . . . . -165.0(6) ? C2 N2 C9 C10 . . . . 152.8(6) ? C2 N2 C1 N1 . . . . 69.9(8) ? C1 N1 C8 C7 . . . . 163.9(5) ? C1 N2 C9 C10 . . . . -66.4(8) ? C1 N2 C2 N3 . . . . -66.8(8) ? C7 N6 C6 N5 . . . . -177.3(5) ? C5 N4 C4 C3 . . . . -169.2(6) ? C5 N5 C6 N6 . . . . 69.0(8) ? C5 N5 C13 C14 . . . . 81.8(8) ? C4 N4 C5 N5 . . . . 177.9(6) ? C13 N5 C6 N6 . . . . -77.7(7) ? C13 N5 C5 N4 . . . . 76.8(7) ? C13 C14 C15 C16 . . . . -177.4(7) ? C3 N3 C2 N2 . . . . 177.4(6) ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.640(4) 2 0.360(4)