# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'La-Sheng Long' _publ_contact_author_email LSLONG@XMU.EDU.CN _publ_section_title ; From 1D Zigzag Chain to 1D Tubular Structure, Weak Field Ligand-dependent Assembly of Cucurbit[6]uril-based Tubular Coordination Polymer ; loop_ _publ_author_name 'La-Sheng Long.' 'Chun-Hong Dong.' 'Rongbin Huang.' 'Jing-Xin Liu.' ; La-Sun Zheng ; # Attachment 'complex1.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 273809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(H2O)4(cucurbit[6]uril)](NO3)2(H2O)8' _chemical_formula_sum 'C36 H60 Cu N26 O30' _chemical_formula_weight 1400.64 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.559(2) _cell_length_b 15.852(3) _cell_length_c 30.320(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5555.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8898 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.23 _exptl_crystal_description block _exptl_crystal_colour sky-blue _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2908 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8174 _exptl_absorpt_correction_T_max 0.8913 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40074 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10364 _reflns_number_gt 9470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, V.5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL, V.5.0 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+0.6270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(7) _chemical_absolute_configuration rm _refine_ls_number_reflns 10364 _refine_ls_number_parameters 849 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.26044(4) 0.52806(3) 0.819059(15) 0.04063(14) Uani 1 1 d . . . N1 N 0.8996(2) 0.53347(18) 1.02128(9) 0.0284(5) Uani 1 1 d . . . N2 N 0.8349(2) 0.40260(18) 1.01985(10) 0.0305(6) Uani 1 1 d . . . N3 N 0.9592(2) 0.65902(17) 0.98190(8) 0.0262(5) Uani 1 1 d . . . N4 N 0.9845(2) 0.72617(17) 0.91856(8) 0.0255(5) Uani 1 1 d . . . N5 N 0.7709(2) 0.28489(18) 0.97523(9) 0.0319(6) Uani 1 1 d . . . N6 N 0.7360(2) 0.24408(17) 0.90657(9) 0.0295(6) Uani 1 1 d . . . N7 N 0.7290(2) 0.24940(18) 0.82675(9) 0.0315(6) Uani 1 1 d . . . N8 N 0.7494(2) 0.30671(16) 0.76107(9) 0.0280(5) Uani 1 1 d . . . N9 N 0.8085(2) 0.43188(17) 0.72156(9) 0.0264(5) Uani 1 1 d . . . N10 N 0.8775(2) 0.56160(17) 0.72822(9) 0.0265(5) Uani 1 1 d . . . N11 N 0.9802(2) 0.73420(17) 0.83850(9) 0.0262(5) Uani 1 1 d . . . N12 N 0.9440(2) 0.67673(16) 0.77365(9) 0.0251(5) Uani 1 1 d . . . N13 N 0.7031(2) 0.58603(17) 1.02688(9) 0.0285(6) Uani 1 1 d . . . N14 N 0.6363(2) 0.45547(18) 1.02399(9) 0.0290(6) Uani 1 1 d . . . N15 N 0.5722(2) 0.33930(18) 0.97861(9) 0.0286(6) Uani 1 1 d . . . N16 N 0.5345(2) 0.28837(19) 0.91236(9) 0.0299(6) Uani 1 1 d . . . N17 N 0.5316(2) 0.30115(18) 0.83229(9) 0.0277(5) Uani 1 1 d . . . N18 N 0.5568(2) 0.36833(17) 0.76876(9) 0.0260(5) Uani 1 1 d . . . N19 N 0.6824(2) 0.62173(17) 0.72597(9) 0.0271(5) Uani 1 1 d . . . N20 N 0.6135(2) 0.49153(16) 0.72762(9) 0.0258(5) Uani 1 1 d . . . N21 N 0.7821(2) 0.76883(18) 0.92079(9) 0.0269(5) Uani 1 1 d . . . N22 N 0.7596(2) 0.70980(16) 0.98595(9) 0.0275(5) Uani 1 1 d . . . N23 N 0.7771(2) 0.77778(17) 0.84119(9) 0.0269(5) Uani 1 1 d . . . N24 N 0.7493(2) 0.73633(16) 0.77202(8) 0.0263(5) Uani 1 1 d . . . N25 N 0.5060(3) 1.0206(2) 0.86889(11) 0.0385(7) Uani 1 1 d . . . N26 N 0.0199(3) 0.0088(2) 0.87651(11) 0.0416(7) Uani 1 1 d . . . O1 O 1.0149(2) 0.42948(18) 0.99115(10) 0.0451(6) Uani 1 1 d . . . O2 O 1.0989(2) 0.61182(18) 0.93398(8) 0.0402(6) Uani 1 1 d . . . O3 O 0.9240(2) 0.27608(19) 0.92703(9) 0.0414(6) Uani 1 1 d . . . O4 O 0.9129(2) 0.28656(16) 0.80332(9) 0.0384(6) Uani 1 1 d . . . O5 O 0.9940(2) 0.44943(16) 0.74717(10) 0.0402(6) Uani 1 1 d . . . O6 O 1.0845(2) 0.61601(16) 0.81792(8) 0.0373(5) Uani 1 1 d . . . O7 O 0.5185(2) 0.56419(17) 1.00016(9) 0.0382(6) Uani 1 1 d . . . O8 O 0.4316(2) 0.40389(17) 0.93728(9) 0.0394(6) Uani 1 1 d . . . O9 O 0.4262(2) 0.42272(16) 0.81906(8) 0.0356(5) Uani 1 1 d . . . O10 O 0.5048(2) 0.59998(15) 0.75734(8) 0.0314(5) Uani 1 1 d . . . O11 O 0.59018(19) 0.75185(17) 0.81783(8) 0.0354(5) Uani 1 1 d . . . O12 O 0.5993(2) 0.72769(16) 0.94230(8) 0.0342(5) Uani 1 1 d . . . O13 O 0.5747(3) 1.0535(2) 0.84208(11) 0.0605(8) Uani 1 1 d . . . O14 O 0.4274(4) 1.0644(2) 0.88282(15) 0.0754(12) Uani 1 1 d . . . O15 O 0.5068(4) 0.9442(2) 0.87604(12) 0.0655(9) Uani 1 1 d . . . O16 O -0.0656(5) -0.0269(4) 0.8883(3) 0.149(3) Uani 1 1 d . . . O17 O 0.0253(6) 0.0858(3) 0.87224(19) 0.1080(19) Uani 1 1 d . . . O18 O 0.1119(3) -0.0282(3) 0.87508(13) 0.0701(9) Uani 1 1 d . . . O1W O 0.1659(3) 0.4316(2) 0.80287(13) 0.0611(9) Uani 1 1 d . . . O2W O 0.2786(2) 0.5612(2) 0.75745(9) 0.0472(7) Uani 1 1 d . . . O3W O 0.2303(3) 0.5155(2) 0.88138(10) 0.0576(8) Uani 1 1 d . . . O4W O 0.3795(3) 0.61235(18) 0.83521(9) 0.0459(6) Uani 1 1 d . . . O5W O 0.2307(4) 0.4759(3) 0.68690(13) 0.0791(12) Uani 1 1 d . . . O6W O 0.5006(7) 0.5746(4) 0.90352(17) 0.134(3) Uani 1 1 d . . . O7W O 0.7649(5) 0.0686(4) 0.9442(2) 0.1093(18) Uani 1 1 d . . . O8W O 0.1264(6) 0.2993(4) 0.8542(2) 0.078(2) Uani 0.669(13) 1 d P A 1 O8W' O 0.1714(12) 0.2298(10) 0.8803(5) 0.082(5) Uani 0.331(13) 1 d P A 2 O9W O 0.3572(4) 0.7936(3) 0.87204(17) 0.0873(13) Uani 1 1 d . . . O10W O 0.2760(3) 0.5754(3) 0.99959(13) 0.0742(11) Uani 1 1 d . . . O11W O -0.0373(16) 0.4391(15) 0.8738(5) 0.364(15) Uani 1 1 d . . . O12W O 0.1947(3) 0.3800(3) 0.93612(14) 0.0759(11) Uani 1 1 d . . . C1 C 0.7645(3) 0.2022(2) 0.86575(10) 0.0298(6) Uani 1 1 d . . . H1A H 0.7275 0.1473 0.8653 0.036 Uiso 1 1 calc R . . H1B H 0.8475 0.1932 0.8646 0.036 Uiso 1 1 calc R . . C2 C 0.6269(3) 0.29259(19) 0.76409(10) 0.0255(6) Uani 1 1 d . . . H2A H 0.5989 0.2567 0.7400 0.031 Uiso 1 1 calc R . . C3 C 0.8361(3) 0.31294(19) 1.01301(12) 0.0305(7) Uani 1 1 d . . . H3A H 0.8052 0.2857 1.0391 0.037 Uiso 1 1 calc R . . H3B H 0.9156 0.2947 1.0096 0.037 Uiso 1 1 calc R . . C4 C 0.6138(3) 0.24878(18) 0.80946(10) 0.0259(6) Uani 1 1 d . . . H4A H 0.5848 0.1910 0.8062 0.031 Uiso 1 1 calc R . . C5 C 0.5549(3) 0.3881(2) 1.01871(11) 0.0288(6) Uani 1 1 d . . . H5A H 0.4774 0.4115 1.0184 0.035 Uiso 1 1 calc R . . H5B H 0.5607 0.3507 1.0439 0.035 Uiso 1 1 calc R . . C6 C 1.0209(3) 0.6595(2) 0.94356(10) 0.0252(6) Uani 1 1 d . . . C7 C 0.8070(3) 0.3417(2) 0.72315(11) 0.0297(7) Uani 1 1 d . . . H7A H 0.8862 0.3215 0.7228 0.036 Uiso 1 1 calc R . . H7B H 0.7692 0.3208 0.6968 0.036 Uiso 1 1 calc R . . C8 C 0.9262(3) 0.4529(2) 1.00838(11) 0.0297(7) Uani 1 1 d . . . C9 C 0.6484(3) 0.26658(19) 0.97563(10) 0.0256(6) Uani 1 1 d . . . H9A H 0.6292 0.2240 0.9979 0.031 Uiso 1 1 calc R . . C10 C 0.6870(3) 0.7116(2) 0.73308(10) 0.0253(6) Uani 1 1 d . . . H10A H 0.7231 0.7378 0.7076 0.030 Uiso 1 1 calc R . . H10B H 0.6086 0.7330 0.7351 0.030 Uiso 1 1 calc R . . C11 C 1.0428(3) 0.7529(2) 0.87855(10) 0.0283(6) Uani 1 1 d . . . H11A H 1.0558 0.8133 0.8801 0.034 Uiso 1 1 calc R . . H11B H 1.1178 0.7257 0.8772 0.034 Uiso 1 1 calc R . . C12 C 0.6260(3) 0.23352(19) 0.92835(11) 0.0276(6) Uani 1 1 d . . . H12A H 0.6016 0.1743 0.9285 0.033 Uiso 1 1 calc R . . C13 C 0.8088(3) 0.2818(2) 0.79827(12) 0.0293(7) Uani 1 1 d . . . C14 C 0.4710(3) 0.2755(2) 0.87200(10) 0.0283(6) Uani 1 1 d . . . H14A H 0.3988 0.3065 0.8738 0.034 Uiso 1 1 calc R . . H14B H 0.4519 0.2161 0.8695 0.034 Uiso 1 1 calc R . . C15 C 0.7468(3) 0.8177(2) 0.88248(10) 0.0297(6) Uani 1 1 d . . . H15A H 0.6636 0.8259 0.8834 0.036 Uiso 1 1 calc R . . H15B H 0.7830 0.8728 0.8838 0.036 Uiso 1 1 calc R . . C16 C 0.8819(3) 0.73058(19) 0.98532(10) 0.0233(6) Uani 1 1 d . . . H16A H 0.9032 0.7676 1.0099 0.028 Uiso 1 1 calc R . . C17 C 0.8722(2) 0.75189(18) 0.77385(10) 0.0223(6) Uani 1 1 d . . . H17A H 0.8965 0.7921 0.7511 0.027 Uiso 1 1 calc R . . C18 C 0.8214(3) 0.26938(19) 0.93520(12) 0.0292(7) Uani 1 1 d . . . C19 C 0.9639(2) 0.6268(2) 0.73452(10) 0.0251(6) Uani 1 1 d . . . H19A H 1.0396 0.6007 0.7365 0.030 Uiso 1 1 calc R . . H19B H 0.9640 0.6636 0.7090 0.030 Uiso 1 1 calc R . . C20 C 1.0090(3) 0.67016(19) 0.81099(10) 0.0248(6) Uani 1 1 d . . . C21 C 0.5068(3) 0.3501(2) 0.94174(10) 0.0266(6) Uani 1 1 d . . . C22 C 0.7197(2) 0.48373(19) 0.70172(10) 0.0234(6) Uani 1 1 d . . . H22A H 0.7035 0.4664 0.6713 0.028 Uiso 1 1 calc R . . C23 C 0.8900(2) 0.78813(18) 0.82075(11) 0.0240(6) Uani 1 1 d . . . H23A H 0.9139 0.8474 0.8200 0.029 Uiso 1 1 calc R . . C24 C 0.7944(3) 0.5377(2) 1.04705(10) 0.0250(6) Uani 1 1 d . . . H24A H 0.8094 0.5560 1.0774 0.030 Uiso 1 1 calc R . . C25 C 0.9819(3) 0.6029(2) 1.01798(10) 0.0254(6) Uani 1 1 d . . . H25A H 0.9803 0.6348 1.0453 0.030 Uiso 1 1 calc R . . H25B H 1.0591 0.5798 1.0146 0.030 Uiso 1 1 calc R . . C26 C 0.4984(3) 0.37048(19) 0.80809(10) 0.0232(6) Uani 1 1 d . . . C27 C 0.5938(3) 0.5731(2) 0.73911(10) 0.0243(6) Uani 1 1 d . . . C28 C 0.6946(3) 0.75481(19) 0.81133(10) 0.0251(6) Uani 1 1 d . . . C29 C 0.7724(3) 0.57334(19) 0.70356(9) 0.0238(6) Uani 1 1 d . . . H29A H 0.7879 0.5955 0.6740 0.029 Uiso 1 1 calc R . . C30 C 0.7483(3) 0.44665(19) 1.04534(9) 0.0243(6) Uani 1 1 d . . . H30A H 0.7407 0.4226 1.0750 0.029 Uiso 1 1 calc R . . C31 C 0.6103(3) 0.5379(2) 1.01519(10) 0.0272(6) Uani 1 1 d . . . C32 C 0.7007(3) 0.6762(2) 1.02407(11) 0.0277(6) Uani 1 1 d . . . H32A H 0.7360 0.6994 1.0504 0.033 Uiso 1 1 calc R . . H32B H 0.6207 0.6947 1.0234 0.033 Uiso 1 1 calc R . . C33 C 0.8951(3) 0.77587(19) 0.94001(10) 0.0231(6) Uani 1 1 d . . . H33A H 0.9185 0.8349 0.9436 0.028 Uiso 1 1 calc R . . C34 C 0.9018(3) 0.4780(2) 0.73435(10) 0.0253(6) Uani 1 1 d . . . C35 C 0.7026(3) 0.73430(19) 0.94880(10) 0.0242(6) Uani 1 1 d . . . C36 C 0.5297(3) 0.4244(2) 0.73340(10) 0.0256(6) Uani 1 1 d . . . H36A H 0.4543 0.4491 0.7388 0.031 Uiso 1 1 calc R . . H36B H 0.5248 0.3922 0.7063 0.031 Uiso 1 1 calc 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 Cu1 0.0388(2) 0.0440(2) 0.0391(2) -0.00162(18) 0.00127(19) 0.0007(2) N1 0.0204(12) 0.0294(13) 0.0354(14) -0.0037(12) 0.0035(10) -0.0034(11) N2 0.0230(13) 0.0299(13) 0.0387(15) -0.0048(12) -0.0003(11) -0.0008(11) N3 0.0212(12) 0.0318(13) 0.0256(12) 0.0012(10) 0.0009(10) 0.0034(10) N4 0.0198(12) 0.0314(13) 0.0255(12) -0.0002(10) 0.0029(10) 0.0015(10) N5 0.0247(13) 0.0335(13) 0.0374(14) -0.0046(11) -0.0051(11) -0.0004(12) N6 0.0226(13) 0.0303(13) 0.0356(14) -0.0012(11) -0.0009(11) 0.0049(11) N7 0.0245(13) 0.0347(14) 0.0354(14) 0.0020(11) -0.0027(11) 0.0057(11) N8 0.0174(12) 0.0285(12) 0.0381(13) 0.0011(10) -0.0013(11) 0.0009(10) N9 0.0205(12) 0.0260(12) 0.0327(13) -0.0038(11) -0.0015(10) -0.0007(10) N10 0.0155(12) 0.0259(12) 0.0381(14) -0.0019(11) -0.0020(10) -0.0050(10) N11 0.0167(12) 0.0350(13) 0.0268(12) 0.0007(11) -0.0034(10) 0.0036(10) N12 0.0219(12) 0.0250(12) 0.0286(12) 0.0000(10) 0.0010(10) 0.0038(10) N13 0.0196(12) 0.0276(13) 0.0384(14) 0.0026(11) 0.0002(11) -0.0002(10) N14 0.0228(13) 0.0308(13) 0.0334(14) 0.0033(11) -0.0042(11) -0.0029(11) N15 0.0248(13) 0.0312(13) 0.0297(13) -0.0013(11) -0.0062(11) 0.0003(11) N16 0.0228(13) 0.0378(15) 0.0292(13) 0.0012(11) -0.0058(11) 0.0048(11) N17 0.0204(13) 0.0344(14) 0.0284(13) 0.0023(11) 0.0003(10) 0.0030(10) N18 0.0228(13) 0.0260(12) 0.0292(13) 0.0001(10) -0.0010(10) 0.0035(10) N19 0.0169(12) 0.0300(13) 0.0345(14) -0.0028(11) 0.0005(10) 0.0006(10) N20 0.0154(12) 0.0275(13) 0.0346(13) 0.0010(10) 0.0032(10) -0.0022(10) N21 0.0179(12) 0.0344(13) 0.0285(12) 0.0013(11) -0.0004(10) 0.0014(10) N22 0.0200(12) 0.0322(13) 0.0302(12) 0.0051(10) 0.0033(11) -0.0009(11) N23 0.0214(13) 0.0320(13) 0.0275(12) -0.0025(10) 0.0041(10) 0.0047(10) N24 0.0192(12) 0.0320(12) 0.0277(12) -0.0012(10) -0.0001(11) 0.0006(10) N25 0.0363(16) 0.0365(16) 0.0428(17) -0.0027(13) 0.0015(14) -0.0042(14) N26 0.0405(17) 0.050(2) 0.0339(15) -0.0045(13) -0.0010(14) -0.0028(15) O1 0.0298(13) 0.0427(13) 0.0630(17) -0.0110(13) 0.0141(12) 0.0031(11) O2 0.0365(14) 0.0492(14) 0.0348(12) 0.0037(11) 0.0067(10) 0.0177(12) O3 0.0205(12) 0.0518(15) 0.0518(15) -0.0132(12) 0.0005(11) 0.0020(11) O4 0.0195(12) 0.0413(13) 0.0544(15) 0.0020(12) 0.0005(10) 0.0061(10) O5 0.0212(11) 0.0398(13) 0.0595(16) 0.0000(12) -0.0127(11) 0.0052(10) O6 0.0323(12) 0.0420(13) 0.0378(12) 0.0003(11) -0.0033(11) 0.0140(10) O7 0.0191(11) 0.0440(13) 0.0517(15) 0.0031(12) -0.0073(10) 0.0019(10) O8 0.0275(12) 0.0453(14) 0.0454(14) -0.0005(11) -0.0076(10) 0.0126(11) O9 0.0295(12) 0.0411(13) 0.0363(12) 0.0004(10) 0.0030(10) 0.0140(10) O10 0.0197(10) 0.0384(12) 0.0361(12) -0.0024(10) 0.0056(9) -0.0003(9) O11 0.0172(11) 0.0492(14) 0.0396(13) -0.0063(11) 0.0018(10) 0.0050(9) O12 0.0174(11) 0.0425(13) 0.0428(13) 0.0014(11) 0.0000(9) 0.0006(10) O13 0.0550(18) 0.064(2) 0.0624(19) 0.0085(16) 0.0129(15) -0.0138(16) O14 0.067(2) 0.0553(19) 0.103(3) 0.005(2) 0.040(2) 0.0080(18) O15 0.084(2) 0.0474(18) 0.065(2) 0.0120(15) 0.0151(19) 0.0074(17) O16 0.075(3) 0.108(4) 0.263(9) -0.026(5) 0.056(5) -0.039(3) O17 0.136(4) 0.075(3) 0.113(4) 0.035(3) 0.049(4) 0.035(3) O18 0.065(2) 0.082(2) 0.064(2) 0.0036(19) 0.0072(18) 0.014(2) O1W 0.0536(19) 0.0502(17) 0.079(2) -0.0004(16) -0.0228(16) -0.0100(15) O2W 0.0380(14) 0.0662(18) 0.0373(13) 0.0006(13) 0.0017(11) 0.0006(13) O3W 0.073(2) 0.0566(18) 0.0436(15) 0.0089(13) 0.0203(15) 0.0096(17) O4W 0.0474(15) 0.0441(14) 0.0464(14) -0.0043(12) 0.0007(12) -0.0053(12) O5W 0.077(3) 0.090(3) 0.070(2) -0.029(2) 0.0081(19) -0.028(2) O6W 0.212(7) 0.111(4) 0.079(3) 0.035(3) -0.077(4) -0.074(5) O7W 0.098(4) 0.099(3) 0.131(4) 0.046(3) 0.014(3) 0.031(3) O8W 0.066(4) 0.070(4) 0.100(5) 0.000(3) 0.012(3) -0.021(3) O8W' 0.067(8) 0.087(10) 0.093(10) -0.027(8) -0.009(7) 0.006(6) O9W 0.077(3) 0.092(3) 0.093(3) -0.011(2) 0.012(2) 0.020(2) O10W 0.0419(18) 0.105(3) 0.076(2) 0.018(2) -0.0108(16) -0.0050(19) O11W 0.33(2) 0.48(3) 0.278(16) 0.171(19) -0.109(15) -0.29(2) O12W 0.0465(19) 0.105(3) 0.076(2) 0.005(2) 0.0124(17) 0.003(2) C1 0.0255(15) 0.0281(15) 0.0359(16) -0.0007(12) -0.0057(13) 0.0089(13) C2 0.0235(15) 0.0225(13) 0.0306(15) -0.0057(11) 0.0021(12) -0.0010(11) C3 0.0260(15) 0.0243(14) 0.0414(17) 0.0026(13) -0.0086(13) 0.0026(12) C4 0.0275(15) 0.0183(12) 0.0319(15) -0.0045(11) -0.0004(12) -0.0029(11) C5 0.0175(14) 0.0368(16) 0.0321(15) 0.0001(13) 0.0058(12) -0.0044(12) C6 0.0197(14) 0.0285(15) 0.0274(14) -0.0023(12) -0.0012(12) 0.0019(12) C7 0.0267(16) 0.0271(15) 0.0352(16) -0.0083(13) 0.0097(13) 0.0002(12) C8 0.0212(14) 0.0311(16) 0.0368(17) -0.0047(13) -0.0070(13) -0.0002(12) C9 0.0240(15) 0.0224(13) 0.0305(15) 0.0076(12) -0.0047(12) -0.0049(12) C10 0.0232(14) 0.0268(14) 0.0259(14) 0.0056(11) -0.0047(11) 0.0030(11) C11 0.0200(14) 0.0364(17) 0.0285(15) -0.0020(13) -0.0025(12) -0.0048(12) C12 0.0256(15) 0.0214(13) 0.0358(16) 0.0024(12) -0.0045(13) -0.0052(12) C13 0.0265(16) 0.0237(14) 0.0377(17) -0.0052(13) -0.0008(13) 0.0053(12) C14 0.0161(13) 0.0421(17) 0.0267(14) 0.0069(13) -0.0044(12) -0.0049(12) C15 0.0272(15) 0.0330(15) 0.0290(15) -0.0030(12) 0.0000(13) 0.0090(13) C16 0.0200(14) 0.0262(14) 0.0237(13) -0.0022(11) 0.0006(11) -0.0030(11) C17 0.0185(14) 0.0210(13) 0.0273(14) 0.0056(11) 0.0024(11) -0.0019(11) C18 0.0206(15) 0.0218(14) 0.0451(19) -0.0031(13) -0.0062(13) 0.0012(12) C19 0.0121(13) 0.0306(15) 0.0327(15) -0.0046(12) 0.0033(11) -0.0049(11) C20 0.0157(13) 0.0264(14) 0.0322(15) 0.0044(12) 0.0041(11) -0.0003(11) C21 0.0218(14) 0.0316(15) 0.0263(14) 0.0051(12) 0.0037(12) -0.0042(13) C22 0.0176(14) 0.0290(15) 0.0235(13) -0.0024(11) 0.0020(11) -0.0005(11) C23 0.0163(13) 0.0211(12) 0.0346(15) -0.0005(12) -0.0008(12) 0.0014(10) C24 0.0210(14) 0.0318(15) 0.0221(13) 0.0002(12) -0.0021(11) -0.0015(12) C25 0.0151(13) 0.0332(15) 0.0278(14) 0.0018(12) -0.0055(11) -0.0033(12) C26 0.0168(13) 0.0259(13) 0.0270(14) -0.0024(11) 0.0013(11) -0.0007(11) C27 0.0181(14) 0.0315(15) 0.0232(13) 0.0015(12) -0.0006(11) 0.0001(12) C28 0.0209(14) 0.0243(13) 0.0301(16) 0.0037(12) 0.0009(11) 0.0014(11) C29 0.0199(14) 0.0289(14) 0.0225(13) 0.0011(11) 0.0020(11) -0.0026(12) C30 0.0195(14) 0.0289(14) 0.0245(13) 0.0028(11) 0.0001(11) -0.0031(12) C31 0.0199(14) 0.0349(16) 0.0268(14) 0.0034(13) 0.0021(11) -0.0030(13) C32 0.0217(14) 0.0295(15) 0.0320(15) -0.0032(12) 0.0103(12) 0.0025(12) C33 0.0183(13) 0.0249(14) 0.0260(14) -0.0025(11) 0.0008(11) -0.0009(11) C34 0.0193(14) 0.0297(15) 0.0267(14) 0.0003(12) 0.0001(11) -0.0025(12) C35 0.0190(15) 0.0214(13) 0.0323(15) -0.0040(12) 0.0018(12) 0.0019(10) C36 0.0179(14) 0.0275(14) 0.0314(15) 0.0007(12) -0.0010(11) -0.0045(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 O3W 1.931(3) . ? Cu1 O1W 1.943(3) . ? Cu1 O2W 1.952(3) . ? Cu1 O4W 1.979(3) . ? N1 C8 1.371(4) . ? N1 C24 1.447(4) . ? N1 C25 1.458(4) . ? N2 C8 1.367(4) . ? N2 C3 1.436(4) . ? N2 C30 1.445(4) . ? N3 C6 1.364(4) . ? N3 C25 1.435(4) . ? N3 C16 1.447(4) . ? N4 C6 1.368(4) . ? N4 C11 1.451(4) . ? N4 C33 1.453(4) . ? N5 C18 1.369(5) . ? N5 C3 1.441(4) . ? N5 C9 1.445(4) . ? N6 C18 1.374(4) . ? N6 C1 1.442(4) . ? N6 C12 1.443(4) . ? N7 C13 1.364(5) . ? N7 C4 1.431(4) . ? N7 C1 1.458(4) . ? N8 C13 1.379(4) . ? N8 C2 1.437(4) . ? N8 C7 1.440(4) . ? N9 C34 1.360(4) . ? N9 C7 1.431(4) . ? N9 C22 1.446(4) . ? N10 C34 1.367(4) . ? N10 C29 1.438(4) . ? N10 C19 1.449(4) . ? N11 C20 1.355(4) . ? N11 C11 1.445(4) . ? N11 C23 1.452(4) . ? N12 C20 1.362(4) . ? N12 C19 1.445(4) . ? N12 C17 1.452(4) . ? N13 C31 1.363(4) . ? N13 C32 1.432(4) . ? N13 C24 1.440(4) . ? N14 C31 1.367(4) . ? N14 C5 1.431(4) . ? N14 C30 1.455(4) . ? N15 C21 1.361(4) . ? N15 C9 1.453(4) . ? N15 C5 1.455(4) . ? N16 C21 1.361(5) . ? N16 C14 1.442(4) . ? N16 C12 1.452(4) . ? N17 C26 1.376(4) . ? N17 C4 1.439(4) . ? N17 C14 1.451(4) . ? N18 C26 1.371(4) . ? N18 C36 1.427(4) . ? N18 C2 1.455(4) . ? N19 C27 1.342(4) . ? N19 C10 1.441(4) . ? N19 C29 1.461(4) . ? N20 C27 1.359(4) . ? N20 C36 1.450(4) . ? N20 C22 1.463(4) . ? N21 C35 1.365(4) . ? N21 C33 1.435(4) . ? N21 C15 1.454(4) . ? N22 C35 1.361(4) . ? N22 C32 1.443(4) . ? N22 C16 1.452(4) . ? N23 C28 1.365(4) . ? N23 C15 1.446(4) . ? N23 C23 1.453(4) . ? N24 C28 1.381(4) . ? N24 C10 1.438(4) . ? N24 C17 1.443(4) . ? N25 O14 1.219(5) . ? N25 O15 1.231(5) . ? N25 O13 1.251(5) . ? N26 O16 1.195(6) . ? N26 O18 1.215(5) . ? N26 O17 1.229(6) . ? O1 C8 1.209(4) . ? O2 C6 1.212(4) . ? O3 C18 1.216(4) . ? O4 C13 1.215(4) . ? O5 C34 1.221(4) . ? O6 C20 1.242(4) . ? O7 C31 1.228(4) . ? O8 C21 1.225(4) . ? O9 C26 1.222(4) . ? O10 C27 1.243(4) . ? O11 C28 1.224(4) . ? O12 C35 1.215(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.548(4) . ? C2 H2A 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9800 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C12 1.548(4) . ? C9 H9A 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C33 1.557(4) . ? C16 H16A 0.9800 . ? C17 C23 1.547(4) . ? C17 H17A 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C22 C29 1.547(4) . ? C22 H22A 0.9800 . ? C23 H23A 0.9800 . ? C24 C30 1.539(4) . ? C24 H24A 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9800 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? 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 O3W Cu1 O1W 93.72(16) . . ? O3W Cu1 O2W 169.52(13) . . ? O1W Cu1 O2W 91.75(15) . . ? O3W Cu1 O4W 87.28(14) . . ? O1W Cu1 O4W 170.02(14) . . ? O2W Cu1 O4W 88.87(12) . . ? C8 N1 C24 112.7(3) . . ? C8 N1 C25 122.5(3) . . ? C24 N1 C25 123.4(3) . . ? C8 N2 C3 122.2(3) . . ? C8 N2 C30 112.9(3) . . ? C3 N2 C30 124.2(3) . . ? C6 N3 C25 123.9(3) . . ? C6 N3 C16 112.3(3) . . ? C25 N3 C16 123.0(2) . . ? C6 N4 C11 123.1(3) . . ? C6 N4 C33 113.0(2) . . ? C11 N4 C33 123.1(3) . . ? C18 N5 C3 122.5(3) . . ? C18 N5 C9 112.9(3) . . ? C3 N5 C9 124.6(3) . . ? C18 N6 C1 120.8(3) . . ? C18 N6 C12 112.2(3) . . ? C1 N6 C12 122.7(3) . . ? C13 N7 C4 113.6(3) . . ? C13 N7 C1 121.1(3) . . ? C4 N7 C1 123.8(3) . . ? C13 N8 C2 113.2(3) . . ? C13 N8 C7 122.2(3) . . ? C2 N8 C7 124.5(3) . . ? C34 N9 C7 122.5(3) . . ? C34 N9 C22 112.1(3) . . ? C7 N9 C22 125.0(3) . . ? C34 N10 C29 111.7(2) . . ? C34 N10 C19 122.1(3) . . ? C29 N10 C19 123.9(3) . . ? C20 N11 C11 123.2(3) . . ? C20 N11 C23 112.9(2) . . ? C11 N11 C23 123.4(3) . . ? C20 N12 C19 123.6(3) . . ? C20 N12 C17 112.0(2) . . ? C19 N12 C17 122.9(3) . . ? C31 N13 C32 121.9(3) . . ? C31 N13 C24 112.9(3) . . ? C32 N13 C24 124.8(3) . . ? C31 N14 C5 123.2(3) . . ? C31 N14 C30 112.0(3) . . ? C5 N14 C30 124.3(3) . . ? C21 N15 C9 112.7(3) . . ? C21 N15 C5 122.9(3) . . ? C9 N15 C5 123.9(3) . . ? C21 N16 C14 122.5(3) . . ? C21 N16 C12 112.6(3) . . ? C14 N16 C12 124.7(3) . . ? C26 N17 C4 112.8(2) . . ? C26 N17 C14 122.1(3) . . ? C4 N17 C14 123.8(3) . . ? C26 N18 C36 122.0(3) . . ? C26 N18 C2 112.3(2) . . ? C36 N18 C2 124.2(3) . . ? C27 N19 C10 123.5(3) . . ? C27 N19 C29 112.3(3) . . ? C10 N19 C29 124.2(3) . . ? C27 N20 C36 123.8(3) . . ? C27 N20 C22 111.0(2) . . ? C36 N20 C22 124.3(3) . . ? C35 N21 C33 113.0(3) . . ? C35 N21 C15 121.4(3) . . ? C33 N21 C15 122.6(3) . . ? C35 N22 C32 122.7(3) . . ? C35 N22 C16 113.3(2) . . ? C32 N22 C16 123.6(3) . . ? C28 N23 C15 121.4(3) . . ? C28 N23 C23 112.0(2) . . ? C15 N23 C23 122.5(3) . . ? C28 N24 C10 122.5(3) . . ? C28 N24 C17 112.4(3) . . ? C10 N24 C17 124.9(3) . . ? O14 N25 O15 120.3(4) . . ? O14 N25 O13 117.4(4) . . ? O15 N25 O13 121.4(4) . . ? O16 N26 O18 120.4(5) . . ? O16 N26 O17 123.0(5) . . ? O18 N26 O17 115.6(5) . . ? N6 C1 N7 113.3(3) . . ? N6 C1 H1A 108.9 . . ? N7 C1 H1A 108.9 . . ? N6 C1 H1B 108.9 . . ? N7 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N8 C2 N18 115.2(3) . . ? N8 C2 C4 102.9(2) . . ? N18 C2 C4 103.3(2) . . ? N8 C2 H2A 111.6 . . ? N18 C2 H2A 111.6 . . ? C4 C2 H2A 111.6 . . ? N2 C3 N5 114.5(3) . . ? N2 C3 H3A 108.6 . . ? N5 C3 H3A 108.6 . . ? N2 C3 H3B 108.6 . . ? N5 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? N7 C4 N17 115.7(3) . . ? N7 C4 C2 103.4(2) . . ? N17 C4 C2 103.5(2) . . ? N7 C4 H4A 111.2 . . ? N17 C4 H4A 111.2 . . ? C2 C4 H4A 111.2 . . ? N14 C5 N15 113.6(3) . . ? N14 C5 H5A 108.8 . . ? N15 C5 H5A 108.8 . . ? N14 C5 H5B 108.8 . . ? N15 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O2 C6 N3 126.2(3) . . ? O2 C6 N4 125.3(3) . . ? N3 C6 N4 108.4(3) . . ? N9 C7 N8 114.7(3) . . ? N9 C7 H7A 108.6 . . ? N8 C7 H7A 108.6 . . ? N9 C7 H7B 108.6 . . ? N8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O1 C8 N2 125.8(3) . . ? O1 C8 N1 126.8(3) . . ? N2 C8 N1 107.3(3) . . ? N5 C9 N15 115.8(3) . . ? N5 C9 C12 103.0(3) . . ? N15 C9 C12 103.0(2) . . ? N5 C9 H9A 111.5 . . ? N15 C9 H9A 111.5 . . ? C12 C9 H9A 111.5 . . ? N24 C10 N19 114.3(3) . . ? N24 C10 H10A 108.7 . . ? N19 C10 H10A 108.7 . . ? N24 C10 H10B 108.7 . . ? N19 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N11 C11 N4 114.2(2) . . ? N11 C11 H11A 108.7 . . ? N4 C11 H11A 108.7 . . ? N11 C11 H11B 108.7 . . ? N4 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N6 C12 N16 114.8(3) . . ? N6 C12 C9 103.7(2) . . ? N16 C12 C9 103.2(3) . . ? N6 C12 H12A 111.5 . . ? N16 C12 H12A 111.5 . . ? C9 C12 H12A 111.5 . . ? O4 C13 N7 127.8(3) . . ? O4 C13 N8 125.3(3) . . ? N7 C13 N8 106.8(3) . . ? N16 C14 N17 114.7(3) . . ? N16 C14 H14A 108.6 . . ? N17 C14 H14A 108.6 . . ? N16 C14 H14B 108.6 . . ? N17 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N23 C15 N21 113.0(3) . . ? N23 C15 H15A 109.0 . . ? N21 C15 H15A 109.0 . . ? N23 C15 H15B 109.0 . . ? N21 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N3 C16 N22 115.1(2) . . ? N3 C16 C33 103.8(2) . . ? N22 C16 C33 102.2(2) . . ? N3 C16 H16A 111.7 . . ? N22 C16 H16A 111.7 . . ? C33 C16 H16A 111.7 . . ? N24 C17 N12 115.0(2) . . ? N24 C17 C23 103.3(2) . . ? N12 C17 C23 103.4(2) . . ? N24 C17 H17A 111.5 . . ? N12 C17 H17A 111.5 . . ? C23 C17 H17A 111.5 . . ? O3 C18 N5 125.5(3) . . ? O3 C18 N6 126.6(3) . . ? N5 C18 N6 107.8(3) . . ? N12 C19 N10 112.9(2) . . ? N12 C19 H19A 109.0 . . ? N10 C19 H19A 109.0 . . ? N12 C19 H19B 109.0 . . ? N10 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? O6 C20 N11 125.9(3) . . ? O6 C20 N12 125.5(3) . . ? N11 C20 N12 108.6(2) . . ? O8 C21 N15 124.9(3) . . ? O8 C21 N16 126.5(3) . . ? N15 C21 N16 108.4(3) . . ? N9 C22 N20 114.9(3) . . ? N9 C22 C29 103.2(2) . . ? N20 C22 C29 103.5(2) . . ? N9 C22 H22A 111.6 . . ? N20 C22 H22A 111.6 . . ? C29 C22 H22A 111.6 . . ? N11 C23 N23 114.8(3) . . ? N11 C23 C17 102.6(2) . . ? N23 C23 C17 103.3(2) . . ? N11 C23 H23A 111.8 . . ? N23 C23 H23A 111.8 . . ? C17 C23 H23A 111.8 . . ? N13 C24 N1 114.3(3) . . ? N13 C24 C30 103.4(2) . . ? N1 C24 C30 103.3(3) . . ? N13 C24 H24A 111.8 . . ? N1 C24 H24A 111.8 . . ? C30 C24 H24A 111.8 . . ? N3 C25 N1 113.7(2) . . ? N3 C25 H25A 108.8 . . ? N1 C25 H25A 108.8 . . ? N3 C25 H25B 108.8 . . ? N1 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? O9 C26 N18 126.2(3) . . ? O9 C26 N17 125.9(3) . . ? N18 C26 N17 107.9(2) . . ? O10 C27 N19 124.5(3) . . ? O10 C27 N20 125.3(3) . . ? N19 C27 N20 110.1(3) . . ? O11 C28 N23 126.4(3) . . ? O11 C28 N24 125.6(3) . . ? N23 C28 N24 108.0(3) . . ? N10 C29 N19 115.3(2) . . ? N10 C29 C22 103.4(2) . . ? N19 C29 C22 102.6(2) . . ? N10 C29 H29A 111.6 . . ? N19 C29 H29A 111.6 . . ? C22 C29 H29A 111.6 . . ? N2 C30 N14 115.2(2) . . ? N2 C30 C24 103.4(2) . . ? N14 C30 C24 103.5(2) . . ? N2 C30 H30A 111.4 . . ? N14 C30 H30A 111.4 . . ? C24 C30 H30A 111.4 . . ? O7 C31 N13 125.9(3) . . ? O7 C31 N14 125.9(3) . . ? N13 C31 N14 108.2(3) . . ? N13 C32 N22 114.0(3) . . ? N13 C32 H32A 108.7 . . ? N22 C32 H32A 108.7 . . ? N13 C32 H32B 108.7 . . ? N22 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? N21 C33 N4 115.1(2) . . ? N21 C33 C16 103.5(2) . . ? N4 C33 C16 102.4(2) . . ? N21 C33 H33A 111.7 . . ? N4 C33 H33A 111.7 . . ? C16 C33 H33A 111.7 . . ? O5 C34 N9 125.7(3) . . ? O5 C34 N10 125.6(3) . . ? N9 C34 N10 108.6(3) . . ? O12 C35 N22 125.8(3) . . ? O12 C35 N21 126.5(3) . . ? N22 C35 N21 107.7(3) . . ? N18 C36 N20 113.7(2) . . ? N18 C36 H36A 108.8 . . ? N20 C36 H36A 108.8 . . ? N18 C36 H36B 108.8 . . ? N20 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? 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 C18 N6 C1 N7 -117.4(3) . . . . ? C12 N6 C1 N7 87.7(4) . . . . ? C13 N7 C1 N6 114.0(3) . . . . ? C4 N7 C1 N6 -81.4(4) . . . . ? C13 N8 C2 N18 108.7(3) . . . . ? C7 N8 C2 N18 -72.5(4) . . . . ? C13 N8 C2 C4 -2.9(3) . . . . ? C7 N8 C2 C4 175.9(3) . . . . ? C26 N18 C2 N8 -116.7(3) . . . . ? C36 N18 C2 N8 77.0(4) . . . . ? C26 N18 C2 C4 -5.3(3) . . . . ? C36 N18 C2 C4 -171.6(3) . . . . ? C8 N2 C3 N5 -102.0(4) . . . . ? C30 N2 C3 N5 88.4(4) . . . . ? C18 N5 C3 N2 96.5(4) . . . . ? C9 N5 C3 N2 -86.4(4) . . . . ? C13 N7 C4 N17 -115.9(3) . . . . ? C1 N7 C4 N17 78.5(4) . . . . ? C13 N7 C4 C2 -3.5(3) . . . . ? C1 N7 C4 C2 -169.1(3) . . . . ? C26 N17 C4 N7 109.8(3) . . . . ? C14 N17 C4 N7 -82.8(4) . . . . ? C26 N17 C4 C2 -2.6(3) . . . . ? C14 N17 C4 C2 164.9(3) . . . . ? N8 C2 C4 N7 3.6(3) . . . . ? N18 C2 C4 N7 -116.5(3) . . . . ? N8 C2 C4 N17 124.7(2) . . . . ? N18 C2 C4 N17 4.5(3) . . . . ? C31 N14 C5 N15 101.8(4) . . . . ? C30 N14 C5 N15 -88.0(4) . . . . ? C21 N15 C5 N14 -100.9(3) . . . . ? C9 N15 C5 N14 88.3(4) . . . . ? C25 N3 C6 O2 2.8(5) . . . . ? C16 N3 C6 O2 172.8(3) . . . . ? C25 N3 C6 N4 -173.7(3) . . . . ? C16 N3 C6 N4 -3.8(4) . . . . ? C11 N4 C6 O2 -5.7(5) . . . . ? C33 N4 C6 O2 -175.6(3) . . . . ? C11 N4 C6 N3 170.8(3) . . . . ? C33 N4 C6 N3 1.0(4) . . . . ? C34 N9 C7 N8 99.2(4) . . . . ? C22 N9 C7 N8 -88.7(4) . . . . ? C13 N8 C7 N9 -96.4(4) . . . . ? C2 N8 C7 N9 84.9(4) . . . . ? C3 N2 C8 O1 1.2(5) . . . . ? C30 N2 C8 O1 171.9(3) . . . . ? C3 N2 C8 N1 -177.0(3) . . . . ? C30 N2 C8 N1 -6.3(4) . . . . ? C24 N1 C8 O1 -170.8(3) . . . . ? C25 N1 C8 O1 -4.0(5) . . . . ? C24 N1 C8 N2 7.3(4) . . . . ? C25 N1 C8 N2 174.2(3) . . . . ? C18 N5 C9 N15 -110.2(3) . . . . ? C3 N5 C9 N15 72.4(4) . . . . ? C18 N5 C9 C12 1.3(3) . . . . ? C3 N5 C9 C12 -176.0(3) . . . . ? C21 N15 C9 N5 114.5(3) . . . . ? C5 N15 C9 N5 -73.9(4) . . . . ? C21 N15 C9 C12 3.0(3) . . . . ? C5 N15 C9 C12 174.6(3) . . . . ? C28 N24 C10 N19 -97.5(3) . . . . ? C17 N24 C10 N19 88.2(4) . . . . ? C27 N19 C10 N24 95.2(4) . . . . ? C29 N19 C10 N24 -85.2(4) . . . . ? C20 N11 C11 N4 -104.0(3) . . . . ? C23 N11 C11 N4 84.2(4) . . . . ? C6 N4 C11 N11 108.1(3) . . . . ? C33 N4 C11 N11 -83.1(4) . . . . ? C18 N6 C12 N16 118.4(3) . . . . ? C1 N6 C12 N16 -84.7(4) . . . . ? C18 N6 C12 C9 6.6(3) . . . . ? C1 N6 C12 C9 163.5(3) . . . . ? C21 N16 C12 N6 -108.3(3) . . . . ? C14 N16 C12 N6 77.5(4) . . . . ? C21 N16 C12 C9 3.8(3) . . . . ? C14 N16 C12 C9 -170.4(3) . . . . ? N5 C9 C12 N6 -4.6(3) . . . . ? N15 C9 C12 N6 116.1(3) . . . . ? N5 C9 C12 N16 -124.6(3) . . . . ? N15 C9 C12 N16 -3.9(3) . . . . ? C4 N7 C13 O4 -176.4(3) . . . . ? C1 N7 C13 O4 -10.4(5) . . . . ? C4 N7 C13 N8 1.8(4) . . . . ? C1 N7 C13 N8 167.9(3) . . . . ? C2 N8 C13 O4 179.2(3) . . . . ? C7 N8 C13 O4 0.3(5) . . . . ? C2 N8 C13 N7 0.9(4) . . . . ? C7 N8 C13 N7 -178.0(3) . . . . ? C21 N16 C14 N17 107.5(4) . . . . ? C12 N16 C14 N17 -78.8(4) . . . . ? C26 N17 C14 N16 -109.6(3) . . . . ? C4 N17 C14 N16 84.0(4) . . . . ? C28 N23 C15 N21 119.0(3) . . . . ? C23 N23 C15 N21 -85.5(4) . . . . ? C35 N21 C15 N23 -114.3(3) . . . . ? C33 N21 C15 N23 86.6(4) . . . . ? C6 N3 C16 N22 115.5(3) . . . . ? C25 N3 C16 N22 -74.4(4) . . . . ? C6 N3 C16 C33 4.7(3) . . . . ? C25 N3 C16 C33 174.8(3) . . . . ? C35 N22 C16 N3 -110.8(3) . . . . ? C32 N22 C16 N3 76.5(4) . . . . ? C35 N22 C16 C33 0.9(3) . . . . ? C32 N22 C16 C33 -171.8(3) . . . . ? C28 N24 C17 N12 109.4(3) . . . . ? C10 N24 C17 N12 -75.8(4) . . . . ? C28 N24 C17 C23 -2.5(3) . . . . ? C10 N24 C17 C23 172.3(3) . . . . ? C20 N12 C17 N24 -118.7(3) . . . . ? C19 N12 C17 N24 74.8(3) . . . . ? C20 N12 C17 C23 -6.8(3) . . . . ? C19 N12 C17 C23 -173.3(2) . . . . ? C3 N5 C18 O3 0.9(5) . . . . ? C9 N5 C18 O3 -176.5(3) . . . . ? C3 N5 C18 N6 -179.8(3) . . . . ? C9 N5 C18 N6 2.7(4) . . . . ? C1 N6 C18 O3 15.7(5) . . . . ? C12 N6 C18 O3 173.1(3) . . . . ? C1 N6 C18 N5 -163.5(3) . . . . ? C12 N6 C18 N5 -6.1(4) . . . . ? C20 N12 C19 N10 106.6(3) . . . . ? C17 N12 C19 N10 -88.5(3) . . . . ? C34 N10 C19 N12 -108.3(3) . . . . ? C29 N10 C19 N12 90.3(4) . . . . ? C11 N11 C20 O6 6.3(5) . . . . ? C23 N11 C20 O6 178.8(3) . . . . ? C11 N11 C20 N12 -171.6(3) . . . . ? C23 N11 C20 N12 1.0(3) . . . . ? C19 N12 C20 O6 -7.5(5) . . . . ? C17 N12 C20 O6 -173.9(3) . . . . ? C19 N12 C20 N11 170.4(3) . . . . ? C17 N12 C20 N11 4.0(3) . . . . ? C9 N15 C21 O8 175.6(3) . . . . ? C5 N15 C21 O8 4.0(5) . . . . ? C9 N15 C21 N16 -0.8(4) . . . . ? C5 N15 C21 N16 -172.4(3) . . . . ? C14 N16 C21 O8 -4.1(5) . . . . ? C12 N16 C21 O8 -178.5(3) . . . . ? C14 N16 C21 N15 172.2(3) . . . . ? C12 N16 C21 N15 -2.1(4) . . . . ? C34 N9 C22 N20 -111.6(3) . . . . ? C7 N9 C22 N20 75.6(4) . . . . ? C34 N9 C22 C29 0.3(3) . . . . ? C7 N9 C22 C29 -172.5(3) . . . . ? C27 N20 C22 N9 118.4(3) . . . . ? C36 N20 C22 N9 -72.0(4) . . . . ? C27 N20 C22 C29 6.7(3) . . . . ? C36 N20 C22 C29 176.3(3) . . . . ? C20 N11 C23 N23 106.3(3) . . . . ? C11 N11 C23 N23 -81.1(4) . . . . ? C20 N11 C23 C17 -5.0(3) . . . . ? C11 N11 C23 C17 167.5(3) . . . . ? C28 N23 C23 N11 -121.0(3) . . . . ? C15 N23 C23 N11 81.4(4) . . . . ? C28 N23 C23 C17 -10.2(3) . . . . ? C15 N23 C23 C17 -167.8(3) . . . . ? N24 C17 C23 N11 126.9(2) . . . . ? N12 C17 C23 N11 6.7(3) . . . . ? N24 C17 C23 N23 7.3(3) . . . . ? N12 C17 C23 N23 -112.9(2) . . . . ? C31 N13 C24 N1 113.5(3) . . . . ? C32 N13 C24 N1 -74.2(4) . . . . ? C31 N13 C24 C30 2.1(3) . . . . ? C32 N13 C24 C30 174.4(3) . . . . ? C8 N1 C24 N13 -116.9(3) . . . . ? C25 N1 C24 N13 76.4(4) . . . . ? C8 N1 C24 C30 -5.4(3) . . . . ? C25 N1 C24 C30 -172.1(3) . . . . ? C6 N3 C25 N1 -103.7(3) . . . . ? C16 N3 C25 N1 87.4(3) . . . . ? C8 N1 C25 N3 103.9(3) . . . . ? C24 N1 C25 N3 -90.6(4) . . . . ? C36 N18 C26 O9 -6.7(5) . . . . ? C2 N18 C26 O9 -173.4(3) . . . . ? C36 N18 C26 N17 170.6(3) . . . . ? C2 N18 C26 N17 3.9(3) . . . . ? C4 N17 C26 O9 176.7(3) . . . . ? C14 N17 C26 O9 9.0(5) . . . . ? C4 N17 C26 N18 -0.6(3) . . . . ? C14 N17 C26 N18 -168.4(3) . . . . ? C10 N19 C27 O10 2.6(5) . . . . ? C29 N19 C27 O10 -177.1(3) . . . . ? C10 N19 C27 N20 179.6(3) . . . . ? C29 N19 C27 N20 0.0(4) . . . . ? C36 N20 C27 O10 2.9(5) . . . . ? C22 N20 C27 O10 172.6(3) . . . . ? C36 N20 C27 N19 -174.1(3) . . . . ? C22 N20 C27 N19 -4.4(4) . . . . ? C15 N23 C28 O11 -12.4(5) . . . . ? C23 N23 C28 O11 -170.3(3) . . . . ? C15 N23 C28 N24 166.9(3) . . . . ? C23 N23 C28 N24 9.0(3) . . . . ? C10 N24 C28 O11 0.6(5) . . . . ? C17 N24 C28 O11 175.6(3) . . . . ? C10 N24 C28 N23 -178.6(3) . . . . ? C17 N24 C28 N23 -3.7(3) . . . . ? C34 N10 C29 N19 121.1(3) . . . . ? C19 N10 C29 N19 -75.8(4) . . . . ? C34 N10 C29 C22 9.9(3) . . . . ? C19 N10 C29 C22 173.0(3) . . . . ? C27 N19 C29 N10 -107.6(3) . . . . ? C10 N19 C29 N10 72.7(4) . . . . ? C27 N19 C29 C22 4.1(3) . . . . ? C10 N19 C29 C22 -175.6(3) . . . . ? N9 C22 C29 N10 -5.9(3) . . . . ? N20 C22 C29 N10 114.1(3) . . . . ? N9 C22 C29 N19 -126.2(2) . . . . ? N20 C22 C29 N19 -6.2(3) . . . . ? C8 N2 C30 N14 115.0(3) . . . . ? C3 N2 C30 N14 -74.5(4) . . . . ? C8 N2 C30 C24 2.9(3) . . . . ? C3 N2 C30 C24 173.4(3) . . . . ? C31 N14 C30 N2 -114.7(3) . . . . ? C5 N14 C30 N2 74.1(4) . . . . ? C31 N14 C30 C24 -2.6(3) . . . . ? C5 N14 C30 C24 -173.8(3) . . . . ? N13 C24 C30 N2 120.8(3) . . . . ? N1 C24 C30 N2 1.4(3) . . . . ? N13 C24 C30 N14 0.3(3) . . . . ? N1 C24 C30 N14 -119.0(3) . . . . ? C32 N13 C31 O7 2.4(5) . . . . ? C24 N13 C31 O7 174.9(3) . . . . ? C32 N13 C31 N14 -176.3(3) . . . . ? C24 N13 C31 N14 -3.8(4) . . . . ? C5 N14 C31 O7 -3.4(5) . . . . ? C30 N14 C31 O7 -174.7(3) . . . . ? C5 N14 C31 N13 175.3(3) . . . . ? C30 N14 C31 N13 4.0(4) . . . . ? C31 N13 C32 N22 -101.5(3) . . . . ? C24 N13 C32 N22 86.8(4) . . . . ? C35 N22 C32 N13 99.3(3) . . . . ? C16 N22 C32 N13 -88.7(4) . . . . ? C35 N21 C33 N4 116.6(3) . . . . ? C15 N21 C33 N4 -82.7(4) . . . . ? C35 N21 C33 C16 5.8(3) . . . . ? C15 N21 C33 C16 166.5(3) . . . . ? C6 N4 C33 N21 -109.6(3) . . . . ? C11 N4 C33 N21 80.5(4) . . . . ? C6 N4 C33 C16 1.9(3) . . . . ? C11 N4 C33 C16 -168.0(3) . . . . ? N3 C16 C33 N21 116.1(2) . . . . ? N22 C16 C33 N21 -3.8(3) . . . . ? N3 C16 C33 N4 -3.8(3) . . . . ? N22 C16 C33 N4 -123.7(2) . . . . ? C7 N9 C34 O5 2.1(5) . . . . ? C22 N9 C34 O5 -170.9(3) . . . . ? C7 N9 C34 N10 178.9(3) . . . . ? C22 N9 C34 N10 5.9(4) . . . . ? C29 N10 C34 O5 166.6(3) . . . . ? C19 N10 C34 O5 3.2(5) . . . . ? C29 N10 C34 N9 -10.2(4) . . . . ? C19 N10 C34 N9 -173.6(3) . . . . ? C32 N22 C35 O12 -3.5(5) . . . . ? C16 N22 C35 O12 -176.3(3) . . . . ? C32 N22 C35 N21 175.4(3) . . . . ? C16 N22 C35 N21 2.6(3) . . . . ? C33 N21 C35 O12 173.4(3) . . . . ? C15 N21 C35 O12 12.5(5) . . . . ? C33 N21 C35 N22 -5.4(3) . . . . ? C15 N21 C35 N22 -166.4(3) . . . . ? C26 N18 C36 N20 105.2(3) . . . . ? C2 N18 C36 N20 -89.8(4) . . . . ? C27 N20 C36 N18 -106.3(3) . . . . ? C22 N20 C36 N18 85.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.726 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.102 # Attachment 'complex2.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 273810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu(H2O)2(Cl)2(cucurbit[6]uril)1/3](H2O)3' _chemical_formula_sum 'C12 H22.67 Cl2 Cu N8 O9' _chemical_formula_weight 557.49 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' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 19.5216(17) _cell_length_b 19.5216(17) _cell_length_c 10.5282(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3474.7(7) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6575 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1714 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6384 _exptl_absorpt_correction_T_max 0.8867 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15666 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2051 _reflns_number_gt 1852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, V.5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL, V.5.0 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+12.8962P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2051 _refine_ls_number_parameters 176 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1951 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.23321(5) 0.79332(5) 0.7500 0.0276(4) Uani 1 2 d SU . . Cl1 Cl 0.09882(10) 0.73491(12) 0.7500 0.0363(5) Uani 1 2 d SU . . Cl2 Cl 0.24776(14) 0.91573(14) 0.7500 0.0456(10) Uani 0.794(8) 2 d SPU . 1 Cl2' Cl 0.1719(6) 0.8809(7) 0.7500 0.046(4) Uani 0.206(8) 2 d SPU . 2 O1 O 0.1269(2) 0.5774(2) 0.9585(3) 0.0251(8) Uani 1 1 d U . . O2 O 0.25239(19) 0.78203(19) 0.9668(3) 0.0248(8) Uani 1 1 d U . . C1 C 0.0986(2) 0.5657(3) 1.0656(4) 0.0176(9) Uani 1 1 d U . . C2 C 0.0319(3) 0.4987(3) 1.2500 0.0126(11) Uani 1 2 d SU . . H2A H -0.0252 0.4569 1.2500 0.015 Uiso 1 2 calc SR . . C3 C 0.0419(3) 0.5824(3) 1.2500 0.0133(12) Uani 1 2 d SU . . H3A H -0.0105 0.5800 1.2500 0.016 Uiso 1 2 calc SR . . C4 C 0.0992(2) 0.6915(2) 1.0827(4) 0.0192(9) Uani 1 1 d U . . H4A H 0.0523 0.6970 1.0995 0.023 Uiso 1 1 calc R . . H4B H 0.1056 0.6912 0.9895 0.023 Uiso 1 1 calc R . . C5 C 0.2365(3) 0.8012(3) 1.0692(4) 0.0191(10) Uani 1 1 d U . . C6 C 0.1667(4) 0.7989(4) 1.2500 0.0191(13) Uani 1 2 d SU . . H6A H 0.1223 0.8106 1.2500 0.023 Uiso 1 2 calc SR . . C7 C 0.2487(4) 0.8754(4) 1.2500 0.0198(13) Uani 1 2 d SU . . H7A H 0.2439 0.9241 1.2500 0.024 Uiso 1 2 calc SR . . C8 C 0.3580(2) 0.9302(2) 1.0853(4) 0.0184(9) Uani 1 1 d U . . H8A H 0.3574 0.9257 0.9916 0.022 Uiso 1 1 calc R . . H8B H 0.3626 0.9817 1.1062 0.022 Uiso 1 1 calc R . . N1 N 0.0706(2) 0.4973(2) 1.1335(3) 0.0182(8) Uani 1 1 d U . . N2 N 0.0852(2) 0.6172(2) 1.1334(3) 0.0184(8) Uani 1 1 d U . . N3 N 0.1683(2) 0.7593(2) 1.1353(3) 0.0213(8) Uani 1 1 d U . . N4 N 0.2841(2) 0.8679(2) 1.1345(3) 0.0216(8) Uani 1 1 d U . . O1W O 0.3510(3) 0.8425(3) 0.7500 0.0363(12) Uani 1 2 d SU . . O2W O 0.2239(4) 0.6872(4) 0.7500 0.0504(16) Uani 1 2 d SU . . O3W O 0.3333 0.6667 0.5815(10) 0.072(2) Uani 1 3 d SU . . O4W O 0.2029(7) 0.9417(7) 0.5335(12) 0.068(5) Uani 0.49(2) 1 d PU A 1 O4W' O 0.1215(10) 0.8718(9) 0.5160(15) 0.091(5) Uani 0.51(2) 1 d PU A 2 O5W O 0.3333 0.6667 0.2500 0.318(7) Uani 1 6 d SU . . 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 Cu1 0.0281(5) 0.0267(5) 0.0211(6) 0.000 0.000 0.0086(4) Cl1 0.0270(9) 0.0397(10) 0.0190(8) 0.000 0.000 -0.0007(7) Cl2 0.0297(14) 0.0245(13) 0.076(2) 0.000 0.000 0.0088(10) Cl2' 0.036(5) 0.061(5) 0.043(5) 0.000 0.000 0.025(4) O1 0.0279(16) 0.0306(17) 0.0120(15) -0.0011(13) 0.0075(13) 0.0111(13) O2 0.0239(16) 0.0301(16) 0.0084(15) -0.0010(12) 0.0000(12) 0.0045(13) C1 0.0111(17) 0.026(2) 0.0107(19) -0.0010(16) 0.0009(15) 0.0059(16) C2 0.006(2) 0.020(3) 0.011(2) 0.000 0.000 0.0057(19) C3 0.009(2) 0.020(3) 0.006(2) 0.000 0.000 0.003(2) C4 0.0165(19) 0.0187(19) 0.0121(19) 0.0006(15) -0.0047(15) 0.0010(16) C5 0.018(2) 0.022(2) 0.011(2) 0.0044(16) -0.0022(15) 0.0054(16) C6 0.015(3) 0.024(3) 0.014(3) 0.000 0.000 0.007(2) C7 0.023(3) 0.020(3) 0.014(3) 0.000 0.000 0.010(2) C8 0.020(2) 0.0164(19) 0.0122(19) 0.0054(15) -0.0025(15) 0.0043(16) N1 0.0166(16) 0.0265(18) 0.0128(17) -0.0006(14) 0.0024(13) 0.0118(14) N2 0.0191(16) 0.0230(17) 0.0086(17) 0.0016(13) 0.0029(14) 0.0073(14) N3 0.0178(17) 0.0235(18) 0.0116(18) -0.0014(14) 0.0003(14) 0.0021(14) N4 0.0215(18) 0.0222(18) 0.0109(18) 0.0007(14) -0.0002(14) 0.0034(14) O1W 0.029(2) 0.046(3) 0.026(2) 0.000 0.000 0.013(2) O2W 0.051(3) 0.035(3) 0.066(3) 0.000 0.000 0.022(2) O3W 0.076(3) 0.076(3) 0.064(4) 0.000 0.000 0.0381(14) O4W 0.070(6) 0.060(6) 0.066(6) -0.005(4) 0.027(4) 0.027(4) O4W' 0.096(7) 0.097(7) 0.095(7) -0.003(4) -0.011(4) 0.058(5) O5W 0.319(6) 0.319(6) 0.316(9) 0.000 0.000 0.160(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 O2W 1.987(6) . ? Cu1 O1W 2.001(5) . ? Cu1 Cl2 2.261(3) . ? Cu1 Cl1 2.278(2) . ? Cu1 O2 2.341(3) . ? Cu1 O2 2.341(3) 10_557 ? Cu1 Cl2' 2.530(11) . ? Cl1 Cl2' 2.468(12) . ? Cl1 H8B 2.7311 8_457 ? Cl1 H4A 3.7734 . ? Cl2 H3A 2.7376 6_664 ? O1 C1 1.226(6) . ? O2 C5 1.230(6) . ? C1 N2 1.360(6) . ? C1 N1 1.366(6) . ? C2 N1 1.449(4) . ? C2 N1 1.449(4) 10_558 ? C2 C3 1.545(8) . ? C2 H2A 1.0000 . ? C3 N2 1.452(5) 10_558 ? C3 N2 1.452(5) . ? C3 H3A 1.0000 . ? C4 N2 1.438(6) . ? C4 N3 1.447(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N4 1.350(6) . ? C5 N3 1.356(6) . ? C6 N3 1.442(5) . ? C6 N3 1.442(5) 10_558 ? C6 C7 1.550(8) . ? C6 H6A 1.0000 . ? C7 N4 1.442(5) 10_558 ? C7 N4 1.442(5) . ? C7 H7A 1.0000 . ? C8 N1 1.441(6) 3_565 ? C8 N4 1.441(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C8 1.441(6) 2_665 ? 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 O2W Cu1 O1W 89.1(3) . . ? O2W Cu1 Cl2 178.3(2) . . ? O1W Cu1 Cl2 89.22(19) . . ? O2W Cu1 Cl1 89.8(2) . . ? O1W Cu1 Cl1 178.84(18) . . ? Cl2 Cu1 Cl1 91.93(9) . . ? O2W Cu1 O2 80.65(9) . . ? O1W Cu1 O2 81.11(9) . . ? Cl2 Cu1 O2 99.09(9) . . ? Cl1 Cu1 O2 98.70(8) . . ? O2W Cu1 O2 80.65(9) . 10_557 ? O1W Cu1 O2 81.11(9) . 10_557 ? Cl2 Cu1 O2 99.09(9) . 10_557 ? Cl1 Cu1 O2 98.70(8) . 10_557 ? O2 Cu1 O2 154.29(19) . 10_557 ? O2W Cu1 Cl2' 151.2(3) . . ? O1W Cu1 Cl2' 119.7(3) . . ? Cl2 Cu1 Cl2' 30.4(3) . . ? Cl1 Cu1 Cl2' 61.5(3) . . ? O2 Cu1 Cl2' 102.45(10) . . ? O2 Cu1 Cl2' 102.45(10) 10_557 . ? Cu1 Cl1 Cl2' 64.3(2) . . ? Cu1 Cl1 H8B 133.8 . 8_457 ? Cl2' Cl1 H8B 135.8 . 8_457 ? Cu1 Cl1 H4A 101.7 . . ? Cl2' Cl1 H4A 99.8 . . ? H8B Cl1 H4A 43.7 8_457 . ? Cu1 Cl2 H3A 93.3 . 6_664 ? Cl1 Cl2' Cu1 54.2(3) . . ? C5 O2 Cu1 138.6(3) . . ? O1 C1 N2 125.6(4) . . ? O1 C1 N1 125.8(4) . . ? N2 C1 N1 108.5(4) . . ? N1 C2 N1 115.7(4) . 10_558 ? N1 C2 C3 103.3(3) . . ? N1 C2 C3 103.3(3) 10_558 . ? N1 C2 H2A 111.3 . . ? N1 C2 H2A 111.3 10_558 . ? C3 C2 H2A 111.3 . . ? N2 C3 N2 115.4(5) 10_558 . ? N2 C3 C2 103.3(3) 10_558 . ? N2 C3 C2 103.3(3) . . ? N2 C3 H3A 111.4 10_558 . ? N2 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? N2 C4 N3 113.7(4) . . ? N2 C4 H4A 108.8 . . ? N3 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? N3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? O2 C5 N4 125.7(4) . . ? O2 C5 N3 126.0(4) . . ? N4 C5 N3 108.3(4) . . ? N3 C6 N3 113.7(5) . 10_558 ? N3 C6 C7 103.1(3) . . ? N3 C6 C7 103.1(3) 10_558 . ? N3 C6 H6A 112.1 . . ? N3 C6 H6A 112.1 10_558 . ? C7 C6 H6A 112.1 . . ? N4 C7 N4 115.0(5) 10_558 . ? N4 C7 C6 102.6(3) 10_558 . ? N4 C7 C6 102.6(3) . . ? N4 C7 H7A 111.9 10_558 . ? N4 C7 H7A 111.9 . . ? C6 C7 H7A 111.9 . . ? N1 C8 N4 114.1(3) 3_565 . ? N1 C8 H8A 108.7 3_565 . ? N4 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 3_565 . ? N4 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 N1 C8 123.2(4) . 2_665 ? C1 N1 C2 112.4(4) . . ? C8 N1 C2 123.8(4) 2_665 . ? C1 N2 C4 122.7(4) . . ? C1 N2 C3 112.4(4) . . ? C4 N2 C3 124.0(4) . . ? C5 N3 C6 112.7(4) . . ? C5 N3 C4 122.7(4) . . ? C6 N3 C4 123.4(4) . . ? C5 N4 C8 123.1(4) . . ? C5 N4 C7 113.2(4) . . ? C8 N4 C7 123.1(4) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.319 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.153 # Complex2 RESULTS (APPEND TO CIF) _vrf_PLAT601_complex2 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 431.00 A**3 RESPONSE: The solvent accessible voids were filled by solvent molecular, which couldn't be located because of crystallographic disorder. ; # end Validation Reply Form