# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- Cif_data.cif' # 1. SUBMISSION DETAILS _publ_contact_autor ; Konstantin V. Domasevitch Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@univ.kiev.ua _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Self-assembly hexanuclear metallacontainer hosting halogenated guest species and sustaining structure of 3D coordination framework ; loop_ _publ_author_name _publ_author_address 'Govor, Evgen V.' ; Inorganic Chemistry Department National Taras Shevchenko University of Kyiv Volodimirska Str. 64 01033 Kyiv Ukraine ; 'Lysenko, Andrey B.' ; Inorganic Chemistry Department National Taras Shevchenko University of Kyiv Volodimirska Str. 64 01033 Kyiv Ukraine ; 'Quinonero, David' ; Departament de Quimica, Universitat de les Illes Balears, 07122 Palma de Mallorca, Spain ; 'Rusanov, Eduard B.' ; Institute of Organic Chemistry, Murmanskaya Str.4, Kyiv 253660, Ukraine ; 'Chernega, Alexander N.' ; Institute of Organic Chemistry, Murmanskaya Str.4, Kyiv 253660, Ukraine ; 'Moellmer, Jens' ; Institut fur Nichtklassische Chemie e.V., Permoserstrasse 15, D-04318 Leipzig, Deutschland ; 'Staudt, Reiner' ; Institut fur Nichtklassische Chemie e.V., Permoserstrasse 15, D-04318 Leipzig, Deutschland ; 'Krautscheid, Harald' ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Deutschland ; 'Frontera, Antonio' ; Departament de Quimica, Universitat de les Illes Balears, 07122 Palma de Mallorca, Spain ; 'Domasevitch, Konstantin V.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; The authors acknowledge support from Deutsche Forschungsgemeinschaft, grant UKR 17/1/06 (HK and KVD) and SPP1362-MOF (STA428/17-1) and Leonard-Euler Fellowship from DAAD. ; #============================================================================== data_(1) _database_code_depnum_ccdc_archive 'CCDC 796878' #TrackingRef '- Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(1,4-dioxane)-(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium \m6-chlorido-hexakis-[\m-(4-(1,2,4-triazol-4-yl)-3,5-dimethylpyrazolato]- hexa-\m-hydroxido-hexacopper(II) Solvate with 4 Chloroform and 2 1,4-Dioxane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 Cl Cu6 N30 O6, C20 H40 K O10, 2(C4 H8 O2), 4(C H Cl3)' _chemical_formula_sum 'C74 H114 Cl13 Cu6 K N30 O20' _chemical_formula_weight 2625.14 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' K K 0.2009 0.2494 '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 triclinic _symmetry_space_group_name_H-M P-1 _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9372(5) _cell_length_b 14.5888(5) _cell_length_c 15.0259(6) _cell_angle_alpha 87.674(2) _cell_angle_beta 70.698(2) _cell_angle_gamma 74.380(2) _cell_volume 2773.01(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22499 _cell_measurement_theta_min 5.52 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1342 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6444 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 22499 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.52 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10284 _reflns_number_gt 5576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _refine_special_details ; The complex cations [K(18c6)(Diox)2]+ are situated across a center of inversion. The coordinated dioxane molecule is equally disordered over two positions. The disorder was resolved with restraints in geometry and thermal parameters (DFIX/SIMU). It possible to refine the disordered atoms anisotropically and the hydrogen atoms were at calculated positions. Two unique solvate dioxane molecules are ordered, both are situated across i nversion center. Solvate CHCl3 molecule exhibits typical rotational disorder of chlorine atoms. The unequal partial occupancies (85/15) were established by refinement of thermal parameters and only atoms of the major contribution were refined anisotropically. The uncoordinated triazole group of the organic ligand is also equally disordered over two positions (similarly to the disorder model for complex 3). This group was refined anisotropically with set of restraints in geometry (DFIX) and thermal parameters (SIMU). CH hydrogen atoms were placed in calculated positions and refined within a riding model, with Uiso = 1.2Ueq of the carrier atom (1.5Ueq for methyl groups). OH hydrogen atoms were located and then fixed with Uiso = 1.5Ueq(O). 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^)+(0.0926P)^2^+0.0000P] 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_number_reflns 10284 _refine_ls_number_parameters 796 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 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 0.78238(5) 0.07034(4) 0.16434(5) 0.0283(2) Uani 1 1 d . . . Cu2 Cu 0.90897(5) 0.21069(5) 0.06482(5) 0.0287(2) Uani 1 1 d . . . Cu3 Cu 1.12251(5) 0.14191(5) -0.09785(5) 0.0293(2) Uani 1 1 d . . . K1 K 0.5000 0.5000 0.5000 0.0514(6) Uani 1 2 d S . . Cl1 Cl 1.0000 0.0000 0.0000 0.0474(6) Uani 1 2 d S . . O1 O 0.7523(3) -0.0361(3) 0.1164(3) 0.0328(9) Uani 1 1 d . . . H1W H 0.7412 -0.0235 0.0643 0.049 Uiso 1 1 d . . . O2 O 0.8470(3) 0.1643(3) 0.1874(2) 0.0311(9) Uani 1 1 d . . . H2W H 0.8945 0.1393 0.2120 0.047 Uiso 1 1 d . . . O3 O 0.9818(3) 0.2255(2) -0.0664(3) 0.0309(9) Uani 1 1 d . . . H3W H 0.9495 0.2105 -0.1008 0.046 Uiso 1 1 d . . . N1 N 0.7152(3) 0.1661(3) 0.0927(3) 0.0296(11) Uani 1 1 d . . . N2 N 0.7720(3) 0.2287(3) 0.0481(3) 0.0289(11) Uani 1 1 d . . . N3 N 0.4112(5) 0.4128(4) -0.0514(6) 0.073(2) Uani 1 1 d . . . N4 N 0.4655(5) 0.3547(5) -0.1288(5) 0.0696(18) Uani 1 1 d . . . N5 N 0.5453(4) 0.3119(4) -0.0251(4) 0.0424(13) Uani 1 1 d . . . N6 N 1.0330(4) 0.2282(3) 0.0888(3) 0.0307(11) Uani 1 1 d . . . N7 N 1.1275(3) 0.1974(3) 0.0168(3) 0.0318(11) Uani 1 1 d . . . N8 N 1.2697(7) 0.4087(8) 0.2298(6) 0.101(3) Uani 1 1 d . . . N9 N 1.3011(5) 0.3239(8) 0.2644(6) 0.087(3) Uani 1 1 d . . . N10 N 1.2047(4) 0.3094(4) 0.1789(4) 0.0480(15) Uani 1 1 d . . . N11 N 1.1333(4) 0.1110(3) -0.2266(3) 0.0340(11) Uani 1 1 d . . . N12 N 1.1775(4) 0.0167(3) -0.2574(3) 0.0352(12) Uani 1 1 d . . . C1 C 0.5407(5) 0.1367(5) 0.1118(5) 0.0443(16) Uani 1 1 d . . . H1A H 0.5218 0.1354 0.1806 0.067 Uiso 1 1 calc R . . H1B H 0.5679 0.0712 0.0841 0.067 Uiso 1 1 calc R . . H1C H 0.4780 0.1694 0.0954 0.067 Uiso 1 1 calc R . . C2 C 0.6240(4) 0.1886(4) 0.0739(4) 0.0302(13) Uani 1 1 d . . . C3 C 0.6237(4) 0.2645(4) 0.0157(4) 0.0363(14) Uani 1 1 d . . . C4 C 0.7181(4) 0.2888(4) 0.0009(4) 0.0313(13) Uani 1 1 d . . . C5 C 0.7551(5) 0.3666(4) -0.0536(5) 0.0504(18) Uani 1 1 d . . . H5A H 0.8291 0.3588 -0.0597 0.076 Uiso 1 1 calc R . . H5B H 0.7119 0.4281 -0.0207 0.076 Uiso 1 1 calc R . . H5C H 0.7489 0.3645 -0.1165 0.076 Uiso 1 1 calc R . . C6 C 0.4602(6) 0.3858(5) 0.0096(6) 0.065(2) Uani 1 1 d . . . H6 H 0.4382 0.4149 0.0711 0.078 Uiso 1 1 calc R . . C7 C 0.5446(6) 0.2941(6) -0.1118(5) 0.064(2) Uani 1 1 d . . . H7 H 0.5947 0.2442 -0.1549 0.077 Uiso 1 1 calc R . . C8 C 0.9611(5) 0.3134(5) 0.2471(5) 0.0511(19) Uani 1 1 d . . . H8A H 0.8942 0.3052 0.2453 0.077 Uiso 1 1 calc R . . H8B H 0.9551 0.3815 0.2534 0.077 Uiso 1 1 calc R . . H8C H 0.9772 0.2814 0.3011 0.077 Uiso 1 1 calc R . . C9 C 1.0474(4) 0.2711(4) 0.1582(4) 0.0334(14) Uani 1 1 d . . . C10 C 1.1542(5) 0.2686(4) 0.1285(4) 0.0381(15) Uani 1 1 d . . . C11 C 1.2026(4) 0.2220(4) 0.0397(4) 0.0361(14) Uani 1 1 d . . . C12 C 1.3140(5) 0.2005(5) -0.0216(5) 0.0525(19) Uani 1 1 d . . . H12A H 1.3448 0.1313 -0.0295 0.079 Uiso 1 1 calc R . . H12B H 1.3532 0.2294 0.0073 0.079 Uiso 1 1 calc R . . H12C H 1.3180 0.2267 -0.0835 0.079 Uiso 1 1 calc R . . C13 C 1.2126(7) 0.3985(7) 0.1792(6) 0.082(3) Uani 1 1 d . . . H13 H 1.1809 0.4483 0.1467 0.098 Uiso 1 1 calc R . . C14 C 1.2595(6) 0.2645(7) 0.2329(6) 0.075(3) Uani 1 1 d . . . H14 H 1.2679 0.1994 0.2472 0.090 Uiso 1 1 calc R . . C15 C 1.0551(6) 0.2640(4) -0.2889(5) 0.0521(18) Uani 1 1 d . . . H15A H 0.9848 0.2757 -0.2946 0.078 Uiso 1 1 calc R . . H15B H 1.0987 0.2945 -0.3396 0.078 Uiso 1 1 calc R . . H15C H 1.0485 0.2906 -0.2276 0.078 Uiso 1 1 calc R . . C16 C 1.1054(5) 0.1600(4) -0.2961(4) 0.0410(15) Uani 1 1 d . . . C17 C 1.1311(6) 0.0959(5) -0.3711(4) 0.0474(17) Uani 1 1 d . . . C18 C 1.1766(5) 0.0067(4) -0.3456(4) 0.0393(15) Uani 1 1 d . . . C19 C 1.2193(7) -0.0873(5) -0.4008(5) 0.063(2) Uani 1 1 d . . . H19A H 1.2427 -0.1376 -0.3614 0.094 Uiso 1 1 calc R . . H19B H 1.2791 -0.0845 -0.4570 0.094 Uiso 1 1 calc R . . H19C H 1.1638 -0.1012 -0.4201 0.094 Uiso 1 1 calc R . . N15 N 1.1111(6) 0.1167(5) -0.4573(4) 0.074(2) Uani 1 1 d D . . N13 N 1.1623(19) 0.1236(16) -0.6146(13) 0.126(6) Uani 0.50 1 d PDU A -1 N14 N 1.054(2) 0.164(2) -0.5704(15) 0.115(5) Uani 0.50 1 d PDU A -1 C20 C 1.1943(13) 0.1050(16) -0.5418(9) 0.106(6) Uani 0.50 1 d PDU A -1 H20 H 1.2666 0.0856 -0.5462 0.127 Uiso 0.50 1 calc PR A -1 C21 C 1.0225(14) 0.1547(16) -0.4793(16) 0.106(6) Uani 0.50 1 d PDU A -1 H21 H 0.9517 0.1709 -0.4372 0.127 Uiso 0.50 1 calc PR A -1 C20A C 1.1497(19) 0.1643(16) -0.5340(11) 0.102(5) Uani 0.50 1 d PDU A -2 H20A H 1.2090 0.1884 -0.5431 0.123 Uiso 0.50 1 calc PR A -2 C21A C 1.0205(14) 0.1080(19) -0.4692(15) 0.114(6) Uani 0.50 1 d PDU A -2 H21A H 0.9670 0.0868 -0.4227 0.137 Uiso 0.50 1 calc PR A -2 N13A N 1.099(2) 0.1747(19) -0.5947(16) 0.114(6) Uani 0.50 1 d PDU A -2 N14A N 1.0172(18) 0.1327(16) -0.5537(15) 0.110(5) Uani 0.50 1 d PDU A -2 O4 O 0.6231(5) 0.6282(5) 0.4345(6) 0.094(2) Uani 1 1 d . H . O5 O 0.4974(5) 0.6340(4) 0.6270(5) 0.089(2) Uani 1 1 d . H . O6 O 0.3468(5) 0.5370(5) 0.6784(4) 0.093(2) Uani 1 1 d . H . C22 C 0.7154(9) 0.5840(10) 0.3583(11) 0.129(4) Uani 1 1 d . . . H22A H 0.7617 0.5320 0.3817 0.155 Uiso 1 1 calc R H . H22B H 0.7550 0.6313 0.3310 0.155 Uiso 1 1 calc R . . C23 C 0.6424(13) 0.6707(9) 0.5116(13) 0.150(6) Uani 1 1 d . . . H23A H 0.6769 0.7221 0.4882 0.179 Uiso 1 1 calc R H . H23B H 0.6894 0.6217 0.5373 0.179 Uiso 1 1 calc R . . C24 C 0.5381(14) 0.7100(9) 0.5870(12) 0.144(6) Uani 1 1 d . H . H24A H 0.5472 0.7467 0.6362 0.173 Uiso 1 1 calc R . . H24B H 0.4885 0.7534 0.5595 0.173 Uiso 1 1 calc R . . C25 C 0.4019(11) 0.6629(10) 0.7093(9) 0.139(6) Uani 1 1 d . . . H25A H 0.4153 0.6981 0.7569 0.167 Uiso 1 1 calc R H . H25B H 0.3443 0.7057 0.6904 0.167 Uiso 1 1 calc R . . C26 C 0.3712(10) 0.5801(10) 0.7490(8) 0.124(5) Uani 1 1 d . H . H26A H 0.4296 0.5354 0.7653 0.148 Uiso 1 1 calc R . . H26B H 0.3087 0.5982 0.8069 0.148 Uiso 1 1 calc R . . C27 C 0.3128(9) 0.4540(13) 0.7131(9) 0.136(5) Uani 1 1 d . . . H27A H 0.3703 0.4059 0.7274 0.164 Uiso 1 1 calc R H . H27B H 0.2511 0.4711 0.7719 0.164 Uiso 1 1 calc R . . C28 C 0.8499(11) 0.0306(9) -0.1632(10) 0.057(4) Uani 1 1 d . . . H28 H 0.8872 0.0222 -0.1156 0.069 Uiso 1 1 calc R . . Cl2 Cl 0.8365(3) 0.1463(2) -0.2009(3) 0.0788(10) Uani 1 1 d . . . Cl3 Cl 0.9230(3) -0.0519(2) -0.2563(2) 0.0754(9) Uani 1 1 d . . . Cl4 Cl 0.7220(3) 0.0130(3) -0.1081(3) 0.0685(10) Uani 1 1 d . . . C29 C 0.5595(7) -0.0674(5) 0.2908(6) 0.122(4) Uani 1 1 d D B -3 H29 H 0.6203 -0.0624 0.2342 0.147 Uiso 1 1 calc R B -3 Cl5 Cl 0.4505(3) -0.0581(3) 0.2532(3) 0.1491(15) Uani 0.85 1 d PD B -3 Cl6 Cl 0.5316(4) 0.0268(4) 0.3678(3) 0.170(2) Uani 0.85 1 d PD B -3 Cl7 Cl 0.5924(4) -0.1778(3) 0.3325(5) 0.215(3) Uani 0.85 1 d PD B -3 Cl5A Cl 0.4442(16) 0.0293(15) 0.3345(19) 0.196(12) Uiso 0.15 1 d PD C -4 Cl6A Cl 0.614(2) -0.0939(19) 0.3839(15) 0.175(10) Uiso 0.15 1 d PD D -4 Cl7A Cl 0.516(3) -0.1675(15) 0.274(3) 0.27(2) Uiso 0.15 1 d PD E -4 O7 O 1.0475(6) 0.5074(4) 0.0678(5) 0.094(2) Uani 1 1 d . . . C30 C 1.1084(8) 0.4865(7) -0.0360(6) 0.100(4) Uani 1 1 d . . . H30A H 1.1162 0.5466 -0.0669 0.120 Uiso 1 1 calc R . . H30B H 1.1799 0.4442 -0.0446 0.120 Uiso 1 1 calc R . . C31 C 0.9461(8) 0.5582(7) 0.0779(7) 0.091(3) Uani 1 1 d . . . H31A H 0.9476 0.6206 0.0499 0.109 Uiso 1 1 calc R . . H31B H 0.9057 0.5706 0.1461 0.109 Uiso 1 1 calc R . . O8 O 0.9246(8) 0.5531(9) 0.4668(8) 0.172(4) Uani 1 1 d . . . C32 C 1.0009(12) 0.4948(10) 0.4088(7) 0.107(4) Uani 1 1 d . . . H32A H 1.0491 0.5302 0.3681 0.128 Uiso 1 1 calc R . . H32B H 0.9738 0.4648 0.3678 0.128 Uiso 1 1 calc R . . C33 C 0.9389(9) 0.5801(8) 0.5481(9) 0.108(4) Uani 1 1 d . . . H33A H 0.8685 0.6073 0.5956 0.129 Uiso 1 1 calc R . . H33B H 0.9749 0.6315 0.5329 0.129 Uiso 1 1 calc R . . O9 O 0.6315(17) 0.3950(17) 0.5847(14) 0.111(5) Uani 0.50 1 d PDU F -5 O10 O 0.8269(11) 0.3054(11) 0.6020(11) 0.101(4) Uani 0.50 1 d PDU F -5 C34 C 0.6963(15) 0.3129(19) 0.5227(18) 0.121(5) Uani 0.50 1 d PDU F -5 H34A H 0.6885 0.3227 0.4595 0.145 Uiso 0.50 1 calc PR G -5 H34B H 0.6726 0.2560 0.5477 0.145 Uiso 0.50 1 calc PR G -5 C35 C 0.8101(15) 0.297(2) 0.5140(13) 0.128(6) Uani 0.50 1 d PDU G -5 H35A H 0.8499 0.2322 0.4847 0.153 Uiso 0.50 1 calc PR G -5 H35B H 0.8391 0.3433 0.4711 0.153 Uiso 0.50 1 calc PR G -5 C36 C 0.7712(13) 0.3934(13) 0.6543(17) 0.097(5) Uani 0.50 1 d PDU G -5 H36A H 0.8061 0.4429 0.6242 0.116 Uiso 0.50 1 calc PR G -5 H36B H 0.7753 0.3872 0.7189 0.116 Uiso 0.50 1 calc PR G -5 C37 C 0.6586(15) 0.4249(16) 0.6608(17) 0.101(5) Uani 0.50 1 d PDU G -5 H37A H 0.6167 0.4020 0.7200 0.121 Uiso 0.50 1 calc PR G -5 H37B H 0.6360 0.4954 0.6665 0.121 Uiso 0.50 1 calc PR H -5 O9A O 0.6639(17) 0.4097(16) 0.5545(13) 0.105(5) Uani 0.50 1 d PDU G -6 O10A O 0.7675(13) 0.2835(9) 0.6667(11) 0.096(4) Uani 0.50 1 d PDU G -6 C34A C 0.736(2) 0.3170(17) 0.5216(19) 0.143(6) Uani 0.50 1 d PDU G -6 H34C H 0.8099 0.3215 0.4981 0.172 Uiso 0.50 1 calc PR G -6 H34D H 0.7213 0.2903 0.4696 0.172 Uiso 0.50 1 calc PR G -6 C35A C 0.720(2) 0.2548(14) 0.6042(16) 0.118(5) Uani 0.50 1 d PDU G -6 H35C H 0.6440 0.2627 0.6373 0.142 Uiso 0.50 1 calc PR G -6 H35D H 0.7544 0.1870 0.5827 0.142 Uiso 0.50 1 calc PR H -6 C36A C 0.7220(17) 0.3839(9) 0.6803(15) 0.086(5) Uani 0.50 1 d PDU G -6 H36C H 0.7590 0.4077 0.7165 0.103 Uiso 0.50 1 calc PR G -6 H36D H 0.6482 0.3935 0.7227 0.103 Uiso 0.50 1 calc PR H -6 C37A C 0.718(2) 0.4494(14) 0.6033(16) 0.108(5) Uani 0.50 1 d PDU G -6 H37C H 0.6772 0.5152 0.6285 0.130 Uiso 0.50 1 calc PR G -6 H37D H 0.7892 0.4495 0.5614 0.130 Uiso 0.50 1 calc PR G -6 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 0.0292(4) 0.0265(4) 0.0316(4) -0.0029(3) -0.0145(3) -0.0053(3) Cu2 0.0249(4) 0.0278(4) 0.0360(4) -0.0040(3) -0.0140(3) -0.0059(3) Cu3 0.0281(4) 0.0279(4) 0.0337(4) -0.0041(3) -0.0131(3) -0.0059(3) K1 0.0580(14) 0.0520(13) 0.0436(12) -0.0109(10) -0.0254(11) -0.0016(11) Cl1 0.0627(15) 0.0257(11) 0.0415(13) -0.0045(9) 0.0004(11) -0.0131(10) O1 0.033(2) 0.032(2) 0.037(2) -0.0041(18) -0.0181(19) -0.0068(18) O2 0.031(2) 0.033(2) 0.031(2) -0.0014(17) -0.0159(18) -0.0057(17) O3 0.027(2) 0.030(2) 0.036(2) -0.0003(17) -0.0147(18) -0.0038(17) N1 0.027(3) 0.029(3) 0.036(3) 0.000(2) -0.015(2) -0.007(2) N2 0.024(3) 0.028(3) 0.039(3) -0.001(2) -0.017(2) -0.006(2) N3 0.060(4) 0.052(4) 0.121(6) 0.002(4) -0.067(5) 0.009(3) N4 0.052(4) 0.083(5) 0.070(5) 0.018(4) -0.032(4) -0.001(4) N5 0.027(3) 0.044(3) 0.058(4) 0.007(3) -0.023(3) -0.004(2) N6 0.032(3) 0.030(3) 0.034(3) -0.006(2) -0.014(2) -0.009(2) N7 0.025(3) 0.032(3) 0.040(3) -0.008(2) -0.012(2) -0.008(2) N8 0.083(6) 0.131(8) 0.110(7) -0.056(6) -0.033(5) -0.054(6) N9 0.050(4) 0.130(7) 0.092(6) -0.046(6) -0.039(4) -0.014(5) N10 0.039(3) 0.070(4) 0.048(3) -0.018(3) -0.022(3) -0.023(3) N11 0.032(3) 0.034(3) 0.037(3) -0.001(2) -0.014(2) -0.006(2) N12 0.041(3) 0.028(3) 0.034(3) 0.000(2) -0.015(2) -0.002(2) C1 0.030(3) 0.052(4) 0.057(4) 0.006(3) -0.021(3) -0.013(3) C2 0.025(3) 0.029(3) 0.037(3) 0.000(3) -0.011(3) -0.005(2) C3 0.023(3) 0.032(3) 0.052(4) -0.003(3) -0.016(3) 0.002(3) C4 0.029(3) 0.025(3) 0.043(4) 0.000(3) -0.019(3) -0.005(3) C5 0.040(4) 0.040(4) 0.078(5) 0.024(3) -0.029(4) -0.012(3) C6 0.048(5) 0.044(4) 0.104(7) -0.014(4) -0.036(5) 0.003(4) C7 0.049(5) 0.089(6) 0.052(5) 0.011(4) -0.028(4) -0.003(4) C8 0.040(4) 0.066(5) 0.049(4) -0.023(4) -0.012(3) -0.018(3) C9 0.029(3) 0.037(3) 0.038(3) -0.009(3) -0.016(3) -0.007(3) C10 0.038(4) 0.042(4) 0.042(4) -0.008(3) -0.020(3) -0.014(3) C11 0.029(3) 0.041(4) 0.042(4) -0.006(3) -0.014(3) -0.010(3) C12 0.032(4) 0.071(5) 0.057(4) -0.020(4) -0.012(3) -0.019(3) C13 0.081(6) 0.093(7) 0.086(6) -0.033(5) -0.028(5) -0.043(5) C14 0.056(5) 0.108(7) 0.069(6) -0.026(5) -0.027(5) -0.022(5) C15 0.066(5) 0.039(4) 0.054(4) 0.014(3) -0.028(4) -0.010(3) C16 0.049(4) 0.038(4) 0.039(4) 0.002(3) -0.018(3) -0.013(3) C17 0.075(5) 0.048(4) 0.023(3) 0.008(3) -0.024(3) -0.013(4) C18 0.053(4) 0.039(4) 0.025(3) -0.003(3) -0.019(3) -0.002(3) C19 0.098(6) 0.051(4) 0.035(4) -0.009(3) -0.028(4) -0.005(4) N15 0.124(6) 0.062(4) 0.045(4) 0.007(3) -0.048(4) -0.019(4) N13 0.184(13) 0.127(12) 0.070(8) 0.042(8) -0.062(9) -0.028(10) N14 0.182(12) 0.116(11) 0.068(8) 0.049(8) -0.075(9) -0.041(9) C20 0.169(15) 0.114(14) 0.050(9) 0.064(10) -0.062(10) -0.041(11) C21 0.170(12) 0.095(13) 0.066(10) 0.035(10) -0.079(10) -0.015(10) C20A 0.183(13) 0.109(12) 0.061(8) 0.056(8) -0.083(9) -0.068(10) C21A 0.164(12) 0.141(15) 0.063(9) 0.037(10) -0.088(9) -0.024(11) N13A 0.186(13) 0.109(11) 0.074(9) 0.039(8) -0.075(9) -0.050(10) N14A 0.166(12) 0.131(12) 0.075(9) 0.050(9) -0.088(9) -0.056(9) O4 0.080(5) 0.087(4) 0.138(6) 0.031(4) -0.062(5) -0.031(4) O5 0.121(5) 0.054(4) 0.103(5) -0.028(3) -0.082(4) 0.018(4) O6 0.075(4) 0.116(5) 0.049(4) 0.000(4) -0.009(3) 0.021(4) C22 0.067(8) 0.167(12) 0.141(12) 0.054(10) -0.021(8) -0.034(8) C23 0.181(15) 0.089(9) 0.278(19) 0.036(11) -0.193(15) -0.056(10) C24 0.195(16) 0.072(9) 0.223(17) -0.036(10) -0.173(15) 0.005(9) C25 0.174(13) 0.118(10) 0.090(9) -0.078(8) -0.082(9) 0.076(10) C26 0.143(11) 0.118(10) 0.062(7) -0.034(7) -0.031(7) 0.043(8) C27 0.064(7) 0.231(17) 0.079(8) 0.040(10) -0.001(6) -0.017(9) C28 0.059(9) 0.062(8) 0.069(9) 0.001(7) -0.055(8) -0.005(7) Cl2 0.078(2) 0.060(2) 0.094(3) 0.0004(18) -0.025(2) -0.0144(17) Cl3 0.078(2) 0.069(2) 0.074(2) -0.0130(17) -0.0301(18) -0.0049(17) Cl4 0.064(3) 0.073(2) 0.066(3) -0.0009(19) -0.0183(19) -0.018(2) C29 0.123(10) 0.124(10) 0.110(9) 0.019(7) -0.011(7) -0.054(8) Cl5 0.120(3) 0.154(4) 0.184(4) 0.001(3) -0.040(3) -0.065(3) Cl6 0.137(4) 0.217(5) 0.146(4) -0.073(3) -0.015(3) -0.059(3) Cl7 0.193(5) 0.153(4) 0.295(7) 0.118(5) -0.075(5) -0.062(4) O7 0.104(5) 0.072(4) 0.129(6) 0.007(4) -0.070(5) -0.020(4) C30 0.116(8) 0.116(8) 0.070(6) -0.018(6) 0.010(6) -0.085(7) C31 0.078(7) 0.082(7) 0.107(8) -0.024(6) -0.019(6) -0.026(6) O8 0.135(8) 0.216(11) 0.105(7) 0.033(7) -0.042(6) 0.051(7) C32 0.160(12) 0.114(9) 0.064(7) -0.006(7) -0.059(9) -0.035(9) C33 0.093(8) 0.103(9) 0.090(9) -0.025(7) 0.006(7) -0.010(7) O9 0.102(10) 0.093(8) 0.151(10) -0.028(8) -0.086(9) 0.011(7) O10 0.086(9) 0.105(9) 0.133(10) 0.006(8) -0.076(8) -0.008(7) C34 0.132(11) 0.114(9) 0.152(10) -0.043(8) -0.119(9) 0.008(9) C35 0.110(11) 0.141(11) 0.146(12) -0.035(10) -0.087(10) 0.005(10) C36 0.096(11) 0.091(9) 0.122(10) 0.018(8) -0.065(9) -0.020(8) C37 0.103(11) 0.090(9) 0.112(10) 0.012(8) -0.071(9) 0.011(8) O9A 0.117(10) 0.090(8) 0.117(9) -0.024(8) -0.092(8) 0.030(7) O10A 0.120(9) 0.074(7) 0.111(9) 0.015(7) -0.075(8) -0.011(7) C34A 0.148(12) 0.125(10) 0.152(10) -0.037(9) -0.085(11) 0.021(10) C35A 0.166(12) 0.079(10) 0.141(12) -0.020(9) -0.096(10) -0.025(9) C36A 0.115(11) 0.070(8) 0.122(10) 0.013(8) -0.082(9) -0.051(8) C37A 0.108(10) 0.098(9) 0.132(11) 0.010(9) -0.069(9) -0.014(8) _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 O2 1.929(3) . ? Cu1 O1 1.936(3) . ? Cu1 N1 1.956(5) . ? Cu1 N12 1.968(5) 2_755 ? Cu1 Cl1 3.1509(7) . ? Cu2 O3 1.930(4) . ? Cu2 O2 1.939(4) . ? Cu2 N2 1.955(4) . ? Cu2 N6 1.959(4) . ? Cu2 Cl1 3.0549(6) . ? Cu3 O3 1.924(4) . ? Cu3 O1 1.942(4) 2_755 ? Cu3 N11 1.952(5) . ? Cu3 N7 1.962(4) . ? Cu3 Cl1 3.0594(7) . ? K1 O9A 2.67(2) . ? K1 O9A 2.67(2) 2_666 ? K1 O9 2.68(2) . ? K1 O9 2.68(2) 2_666 ? K1 O5 2.772(5) . ? K1 O5 2.772(5) 2_666 ? K1 O6 2.784(6) . ? K1 O6 2.784(6) 2_666 ? K1 O4 2.806(6) . ? K1 O4 2.806(6) 2_666 ? K1 C34 3.40(2) . ? K1 C34 3.40(2) 2_666 ? O1 Cu3 1.942(4) 2_755 ? O1 H1W 0.8502 . ? O2 H2W 0.8525 . ? O3 H3W 0.8573 . ? N1 C2 1.346(7) . ? N1 N2 1.377(6) . ? N2 C4 1.335(7) . ? N3 C6 1.306(9) . ? N3 N4 1.340(9) . ? N4 C7 1.306(9) . ? N5 C6 1.337(8) . ? N5 C7 1.343(8) . ? N5 C3 1.432(7) . ? N6 C9 1.334(6) . ? N6 N7 1.374(6) . ? N7 C11 1.339(6) . ? N8 C13 1.305(10) . ? N8 N9 1.342(11) . ? N9 C14 1.340(10) . ? N10 C14 1.329(9) . ? N10 C13 1.335(10) . ? N10 C10 1.427(7) . ? N11 C16 1.345(7) . ? N11 N12 1.376(6) . ? N12 C18 1.344(7) . ? N12 Cu1 1.968(5) 2_755 ? C1 C2 1.499(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.383(8) . ? C3 C4 1.399(7) . ? C4 C5 1.478(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.489(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.397(8) . ? C10 C11 1.389(8) . ? C11 C12 1.474(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.482(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.382(8) . ? C17 C18 1.384(8) . ? C17 N15 1.416(8) . ? C18 C19 1.500(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N15 C20A 1.352(9) . ? N15 C21 1.353(10) . ? N15 C21A 1.373(10) . ? N15 C20 1.387(10) . ? N13 C20 1.306(10) . ? N13 N14 1.396(10) . ? N14 C21 1.308(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C20A N13A 1.307(10) . ? C20A H20A 0.9500 . ? C21A N14A 1.317(10) . ? C21A H21A 0.9500 . ? N13A N14A 1.393(10) . ? O4 C22 1.421(13) . ? O4 C23 1.467(13) . ? O5 C24 1.405(16) . ? O5 C25 1.460(14) . ? O6 C26 1.429(12) . ? O6 C27 1.435(15) . ? C22 C27 1.434(15) 2_666 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.497(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.431(17) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C22 1.434(15) 2_666 ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 Cl3 1.726(14) . ? C28 Cl2 1.740(14) . ? C28 Cl4 1.783(15) . ? C28 H28 1.0000 . ? C29 Cl7 1.704(7) . ? C29 Cl6 1.709(7) . ? C29 Cl5 1.759(8) . ? C29 H29 1.0000 . ? O7 C31 1.369(10) . ? O7 C30 1.506(10) . ? C30 C31 1.420(11) 2_765 ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C30 1.420(11) 2_765 ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O8 C32 1.254(13) . ? O8 C33 1.390(13) . ? C32 C33 1.457(15) 2_766 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C32 1.457(15) 2_766 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O9 C37 1.433(7) . ? O9 C34 1.438(7) . ? O10 C36 1.418(7) . ? O10 C35 1.432(7) . ? C34 C35 1.501(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.483(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O9A C37A 1.436(7) . ? O9A C34A 1.442(7) . ? O10A C36A 1.424(7) . ? O10A C35A 1.440(7) . ? C34A C35A 1.499(7) . ? C34A H34C 0.9900 . ? C34A H34D 0.9900 . ? C35A H35C 0.9900 . ? C35A H35D 0.9900 . ? C36A C37A 1.476(7) . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? 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 O2 Cu1 O1 165.31(15) . . ? O2 Cu1 N1 86.60(17) . . ? O1 Cu1 N1 95.57(16) . . ? O2 Cu1 N12 94.74(17) . 2_755 ? O1 Cu1 N12 86.07(17) . 2_755 ? N1 Cu1 N12 168.35(19) . 2_755 ? O2 Cu1 Cl1 82.43(11) . . ? O1 Cu1 Cl1 82.90(11) . . ? N1 Cu1 Cl1 95.82(13) . . ? N12 Cu1 Cl1 95.83(14) 2_755 . ? O3 Cu2 O2 166.53(14) . . ? O3 Cu2 N2 94.40(17) . . ? O2 Cu2 N2 86.52(17) . . ? O3 Cu2 N6 86.23(17) . . ? O2 Cu2 N6 96.31(17) . . ? N2 Cu2 N6 165.20(18) . . ? O3 Cu2 Cl1 81.62(10) . . ? O2 Cu2 Cl1 84.94(10) . . ? N2 Cu2 Cl1 97.55(13) . . ? N6 Cu2 Cl1 97.17(13) . . ? O3 Cu3 O1 166.93(16) . 2_755 ? O3 Cu3 N11 94.56(17) . . ? O1 Cu3 N11 86.70(17) 2_755 . ? O3 Cu3 N7 86.08(17) . . ? O1 Cu3 N7 95.84(17) 2_755 . ? N11 Cu3 N7 166.0(2) . . ? O3 Cu3 Cl1 81.58(11) . . ? O1 Cu3 Cl1 85.35(11) 2_755 . ? N11 Cu3 Cl1 97.15(14) . . ? N7 Cu3 Cl1 96.78(14) . . ? O9A K1 O9A 180.000(1) . 2_666 ? O9A K1 O9 12.9(8) . . ? O9A K1 O9 167.1(8) 2_666 . ? O9A K1 O9 167.1(8) . 2_666 ? O9A K1 O9 12.9(8) 2_666 2_666 ? O9 K1 O9 180.000(2) . 2_666 ? O9A K1 O5 78.2(4) . . ? O9A K1 O5 101.8(4) 2_666 . ? O9 K1 O5 78.6(4) . . ? O9 K1 O5 101.4(4) 2_666 . ? O9A K1 O5 101.8(4) . 2_666 ? O9A K1 O5 78.2(4) 2_666 2_666 ? O9 K1 O5 101.4(4) . 2_666 ? O9 K1 O5 78.6(4) 2_666 2_666 ? O5 K1 O5 180.000(1) . 2_666 ? O9A K1 O6 97.6(4) . . ? O9A K1 O6 82.4(4) 2_666 . ? O9 K1 O6 86.9(5) . . ? O9 K1 O6 93.1(5) 2_666 . ? O5 K1 O6 58.8(2) . . ? O5 K1 O6 121.2(2) 2_666 . ? O9A K1 O6 82.4(4) . 2_666 ? O9A K1 O6 97.6(4) 2_666 2_666 ? O9 K1 O6 93.1(5) . 2_666 ? O9 K1 O6 86.9(5) 2_666 2_666 ? O5 K1 O6 121.2(2) . 2_666 ? O5 K1 O6 58.8(2) 2_666 2_666 ? O6 K1 O6 180.000(1) . 2_666 ? O9A K1 O4 82.1(5) . . ? O9A K1 O4 97.9(5) 2_666 . ? O9 K1 O4 93.6(5) . . ? O9 K1 O4 86.4(5) 2_666 . ? O5 K1 O4 61.1(2) . . ? O5 K1 O4 118.9(2) 2_666 . ? O6 K1 O4 118.5(2) . . ? O6 K1 O4 61.5(2) 2_666 . ? O9A K1 O4 97.9(5) . 2_666 ? O9A K1 O4 82.1(5) 2_666 2_666 ? O9 K1 O4 86.4(5) . 2_666 ? O9 K1 O4 93.6(5) 2_666 2_666 ? O5 K1 O4 118.9(2) . 2_666 ? O5 K1 O4 61.1(2) 2_666 2_666 ? O6 K1 O4 61.5(2) . 2_666 ? O6 K1 O4 118.5(2) 2_666 2_666 ? O4 K1 O4 180.000(1) . 2_666 ? O9A K1 C34 23.1(7) . . ? O9A K1 C34 156.9(7) 2_666 . ? O9 K1 C34 23.8(3) . . ? O9 K1 C34 156.2(3) 2_666 . ? O5 K1 C34 100.9(4) . . ? O5 K1 C34 79.1(4) 2_666 . ? O6 K1 C34 105.6(5) . . ? O6 K1 C34 74.4(5) 2_666 . ? O4 K1 C34 97.2(5) . . ? O4 K1 C34 82.8(5) 2_666 . ? O9A K1 C34 156.9(7) . 2_666 ? O9A K1 C34 23.1(7) 2_666 2_666 ? O9 K1 C34 156.2(3) . 2_666 ? O9 K1 C34 23.8(3) 2_666 2_666 ? O5 K1 C34 79.1(4) . 2_666 ? O5 K1 C34 100.9(4) 2_666 2_666 ? O6 K1 C34 74.4(5) . 2_666 ? O6 K1 C34 105.6(5) 2_666 2_666 ? O4 K1 C34 82.8(5) . 2_666 ? O4 K1 C34 97.2(5) 2_666 2_666 ? C34 K1 C34 180.000(1) . 2_666 ? Cu2 Cl1 Cu3 60.966(17) . . ? Cu2 Cl1 Cu1 59.516(17) . . ? Cu3 Cl1 Cu1 120.481(17) . . ? Cu1 O1 Cu3 105.37(16) . 2_755 ? Cu1 O1 H1W 110.6 . . ? Cu3 O1 H1W 110.4 2_755 . ? Cu1 O2 Cu2 105.63(16) . . ? Cu1 O2 H2W 110.7 . . ? Cu2 O2 H2W 110.5 . . ? Cu3 O3 Cu2 107.18(17) . . ? Cu3 O3 H3W 110.4 . . ? Cu2 O3 H3W 109.8 . . ? C2 N1 N2 108.0(4) . . ? C2 N1 Cu1 136.2(4) . . ? N2 N1 Cu1 115.8(3) . . ? C4 N2 N1 109.6(4) . . ? C4 N2 Cu2 134.6(4) . . ? N1 N2 Cu2 115.9(3) . . ? C6 N3 N4 106.5(6) . . ? C7 N4 N3 107.6(6) . . ? C6 N5 C7 103.6(6) . . ? C6 N5 C3 129.7(6) . . ? C7 N5 C3 126.6(6) . . ? C9 N6 N7 109.5(4) . . ? C9 N6 Cu2 134.4(4) . . ? N7 N6 Cu2 115.9(3) . . ? C11 N7 N6 109.0(4) . . ? C11 N7 Cu3 134.2(4) . . ? N6 N7 Cu3 116.4(3) . . ? C13 N8 N9 107.5(7) . . ? C14 N9 N8 106.1(7) . . ? C14 N10 C13 104.4(6) . . ? C14 N10 C10 127.0(7) . . ? C13 N10 C10 128.5(7) . . ? C16 N11 N12 108.4(4) . . ? C16 N11 Cu3 135.6(4) . . ? N12 N11 Cu3 116.0(4) . . ? C18 N12 N11 108.8(5) . . ? C18 N12 Cu1 135.4(4) . 2_755 ? N11 N12 Cu1 115.7(3) . 2_755 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.1(5) . . ? N1 C2 C1 123.4(5) . . ? C3 C2 C1 128.5(5) . . ? C2 C3 C4 107.2(5) . . ? C2 C3 N5 128.9(5) . . ? C4 C3 N5 123.9(5) . . ? N2 C4 C3 107.2(5) . . ? N2 C4 C5 123.9(5) . . ? C3 C4 C5 128.9(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N5 111.6(7) . . ? N3 C6 H6 124.2 . . ? N5 C6 H6 124.2 . . ? N4 C7 N5 110.7(7) . . ? N4 C7 H7 124.7 . . ? N5 C7 H7 124.7 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 106.5(5) . . ? N6 C9 C8 123.7(5) . . ? C10 C9 C8 129.7(5) . . ? C11 C10 C9 108.1(5) . . ? C11 C10 N10 125.7(5) . . ? C9 C10 N10 126.2(5) . . ? N7 C11 C10 106.8(5) . . ? N7 C11 C12 123.8(5) . . ? C10 C11 C12 129.4(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N8 C13 N10 111.4(9) . . ? N8 C13 H13 124.3 . . ? N10 C13 H13 124.3 . . ? N10 C14 N9 110.6(9) . . ? N10 C14 H14 124.7 . . ? N9 C14 H14 124.7 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 C17 107.7(5) . . ? N11 C16 C15 124.0(5) . . ? C17 C16 C15 128.3(6) . . ? C16 C17 C18 107.7(5) . . ? C16 C17 N15 126.3(6) . . ? C18 C17 N15 126.0(6) . . ? N12 C18 C17 107.4(5) . . ? N12 C18 C19 122.9(5) . . ? C17 C18 C19 129.6(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20A N15 C21A 101.3(13) . . ? C21 N15 C20 105.9(12) . . ? C21A N15 C20 112.5(13) . . ? C20A N15 C17 135.7(11) . . ? C21 N15 C17 133.7(11) . . ? C21A N15 C17 121.4(10) . . ? C20 N15 C17 120.3(9) . . ? C20 N13 N14 101.1(18) . . ? C21 N14 N13 114(2) . . ? N13 C20 N15 112.5(15) . . ? N13 C20 H20 123.8 . . ? N15 C20 H20 123.8 . . ? N14 C21 N15 105.7(18) . . ? N14 C21 H21 127.1 . . ? N15 C21 H21 127.1 . . ? N13A C20A N15 114.8(16) . . ? N13A C20A H20A 122.6 . . ? N15 C20A H20A 122.6 . . ? N14A C21A N15 111.2(16) . . ? N14A C21A H21A 124.4 . . ? N15 C21A H21A 124.4 . . ? C20A N13A N14A 104.2(18) . . ? C21A N14A N13A 107.3(18) . . ? C22 O4 C23 115.0(11) . . ? C22 O4 K1 109.7(6) . . ? C23 O4 K1 111.9(7) . . ? C24 O5 C25 113.6(11) . . ? C24 O5 K1 115.8(7) . . ? C25 O5 K1 116.5(7) . . ? C26 O6 C27 110.2(10) . . ? C26 O6 K1 116.7(7) . . ? C27 O6 K1 111.7(6) . . ? O4 C22 C27 110.2(10) . 2_666 ? O4 C22 H22A 109.6 . . ? C27 C22 H22A 109.6 2_666 . ? O4 C22 H22B 109.6 . . ? C27 C22 H22B 109.6 2_666 . ? H22A C22 H22B 108.1 . . ? O4 C23 C24 107.9(9) . . ? O4 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O4 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? O5 C24 C23 108.8(10) . . ? O5 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O5 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C26 C25 O5 109.4(9) . . ? C26 C25 H25A 109.8 . . ? O5 C25 H25A 109.8 . . ? C26 C25 H25B 109.8 . . ? O5 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? O6 C26 C25 106.4(10) . . ? O6 C26 H26A 110.5 . . ? C25 C26 H26A 110.5 . . ? O6 C26 H26B 110.5 . . ? C25 C26 H26B 110.5 . . ? H26A C26 H26B 108.6 . . ? C22 C27 O6 108.1(11) 2_666 . ? C22 C27 H27A 110.1 2_666 . ? O6 C27 H27A 110.1 . . ? C22 C27 H27B 110.1 2_666 . ? O6 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? Cl3 C28 Cl2 111.0(8) . . ? Cl3 C28 Cl4 110.6(8) . . ? Cl2 C28 Cl4 109.2(7) . . ? Cl3 C28 H28 108.7 . . ? Cl2 C28 H28 108.7 . . ? Cl4 C28 H28 108.7 . . ? Cl7 C29 Cl6 115.9(5) . . ? Cl7 C29 Cl5 108.5(5) . . ? Cl6 C29 Cl5 109.2(5) . . ? Cl7 C29 H29 107.6 . . ? Cl6 C29 H29 107.6 . . ? Cl5 C29 H29 107.6 . . ? C31 O7 C30 108.6(8) . . ? C31 C30 O7 109.4(7) 2_765 . ? C31 C30 H30A 109.8 2_765 . ? O7 C30 H30A 109.8 . . ? C31 C30 H30B 109.8 2_765 . ? O7 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? O7 C31 C30 115.1(8) . 2_765 ? O7 C31 H31A 108.5 . . ? C30 C31 H31A 108.5 2_765 . ? O7 C31 H31B 108.5 . . ? C30 C31 H31B 108.5 2_765 . ? H31A C31 H31B 107.5 . . ? C32 O8 C33 117.4(9) . . ? O8 C32 C33 114.4(9) . 2_766 ? O8 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 2_766 . ? O8 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 2_766 . ? H32A C32 H32B 107.6 . . ? O8 C33 C32 116.3(9) . 2_766 ? O8 C33 H33A 108.2 . . ? C32 C33 H33A 108.2 2_766 . ? O8 C33 H33B 108.2 . . ? C32 C33 H33B 108.2 2_766 . ? H33A C33 H33B 107.4 . . ? C37 O9 C34 123(2) . . ? C37 O9 K1 127.5(15) . . ? C34 O9 K1 107.3(13) . . ? C36 O10 C35 115.3(17) . . ? O9 C34 C35 110.4(19) . . ? O9 C34 K1 48.9(10) . . ? C35 C34 K1 136.0(19) . . ? O9 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? K1 C34 H34A 61.9 . . ? O9 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? K1 C34 H34B 114.1 . . ? H34A C34 H34B 108.1 . . ? O10 C35 C34 114.1(16) . . ? O10 C35 H35A 108.7 . . ? C34 C35 H35A 108.7 . . ? O10 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? O10 C36 C37 113.4(16) . . ? O10 C36 H36A 108.9 . . ? C37 C36 H36A 108.9 . . ? O10 C36 H36B 108.9 . . ? C37 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O9 C37 C36 117.3(19) . . ? O9 C37 H37A 108.0 . . ? C36 C37 H37A 108.0 . . ? O9 C37 H37B 108.0 . . ? C36 C37 H37B 108.0 . . ? H37A C37 H37B 107.2 . . ? C37A O9A C34A 102(2) . . ? C37A O9A K1 128.1(14) . . ? C34A O9A K1 128.0(16) . . ? C36A O10A C35A 103.6(13) . . ? O9A C34A C35A 107(2) . . ? O9A C34A H34C 110.4 . . ? C35A C34A H34C 110.4 . . ? O9A C34A H34D 110.4 . . ? C35A C34A H34D 110.4 . . ? H34C C34A H34D 108.6 . . ? O10A C35A C34A 107.3(19) . . ? O10A C35A H35C 110.3 . . ? C34A C35A H35C 110.3 . . ? O10A C35A H35D 110.3 . . ? C34A C35A H35D 110.3 . . ? H35C C35A H35D 108.5 . . ? O10A C36A C37A 124.5(17) . . ? O10A C36A H36C 106.2 . . ? C37A C36A H36C 106.2 . . ? O10A C36A H36D 106.2 . . ? C37A C36A H36D 106.2 . . ? H36C C36A H36D 106.4 . . ? O9A C37A C36A 102.5(17) . . ? O9A C37A H37C 111.3 . . ? C36A C37A H37C 111.3 . . ? O9A C37A H37D 111.3 . . ? C36A C37A H37D 111.3 . . ? H37C C37A H37D 109.2 . . ? 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 O3 Cu2 Cl1 Cu3 30.95(10) . . . . ? O2 Cu2 Cl1 Cu3 -149.88(10) . . . . ? N2 Cu2 Cl1 Cu3 124.32(14) . . . . ? N6 Cu2 Cl1 Cu3 -54.13(14) . . . . ? O3 Cu2 Cl1 Cu1 -148.65(10) . . . . ? O2 Cu2 Cl1 Cu1 30.52(10) . . . . ? N2 Cu2 Cl1 Cu1 -55.29(14) . . . . ? N6 Cu2 Cl1 Cu1 126.26(14) . . . . ? O3 Cu3 Cl1 Cu2 -31.06(10) . . . . ? O1 Cu3 Cl1 Cu2 149.28(10) 2_755 . . . ? N11 Cu3 Cl1 Cu2 -124.65(14) . . . . ? N7 Cu3 Cl1 Cu2 53.94(13) . . . . ? O3 Cu3 Cl1 Cu1 -30.67(11) . . . . ? O1 Cu3 Cl1 Cu1 149.68(10) 2_755 . . . ? N11 Cu3 Cl1 Cu1 -124.25(14) . . . . ? N7 Cu3 Cl1 Cu1 54.33(14) . . . . ? O2 Cu1 Cl1 Cu2 -30.86(11) . . . . ? O1 Cu1 Cl1 Cu2 149.82(11) . . . . ? N1 Cu1 Cl1 Cu2 54.91(12) . . . . ? N12 Cu1 Cl1 Cu2 -124.89(13) 2_755 . . . ? O2 Cu1 Cl1 Cu3 -31.27(11) . . . . ? O1 Cu1 Cl1 Cu3 149.42(11) . . . . ? N1 Cu1 Cl1 Cu3 54.51(12) . . . . ? N12 Cu1 Cl1 Cu3 -125.29(13) 2_755 . . . ? O2 Cu1 O1 Cu3 43.1(7) . . . 2_755 ? N1 Cu1 O1 Cu3 140.9(2) . . . 2_755 ? N12 Cu1 O1 Cu3 -50.6(2) 2_755 . . 2_755 ? Cl1 Cu1 O1 Cu3 45.76(14) . . . 2_755 ? O1 Cu1 O2 Cu2 49.0(7) . . . . ? N1 Cu1 O2 Cu2 -50.01(19) . . . . ? N12 Cu1 O2 Cu2 141.59(19) 2_755 . . . ? Cl1 Cu1 O2 Cu2 46.32(13) . . . . ? O3 Cu2 O2 Cu1 -44.4(7) . . . . ? N2 Cu2 O2 Cu1 49.97(19) . . . . ? N6 Cu2 O2 Cu1 -144.61(19) . . . . ? Cl1 Cu2 O2 Cu1 -47.93(14) . . . . ? O1 Cu3 O3 Cu2 49.9(7) 2_755 . . . ? N11 Cu3 O3 Cu2 144.94(19) . . . . ? N7 Cu3 O3 Cu2 -49.08(19) . . . . ? Cl1 Cu3 O3 Cu2 48.37(13) . . . . ? O2 Cu2 O3 Cu3 -52.0(7) . . . . ? N2 Cu2 O3 Cu3 -145.46(18) . . . . ? N6 Cu2 O3 Cu3 49.36(19) . . . . ? Cl1 Cu2 O3 Cu3 -48.46(13) . . . . ? O2 Cu1 N1 C2 -149.0(5) . . . . ? O1 Cu1 N1 C2 45.5(5) . . . . ? N12 Cu1 N1 C2 -52.1(11) 2_755 . . . ? Cl1 Cu1 N1 C2 128.9(5) . . . . ? O2 Cu1 N1 N2 31.2(3) . . . . ? O1 Cu1 N1 N2 -134.2(4) . . . . ? N12 Cu1 N1 N2 128.2(8) 2_755 . . . ? Cl1 Cu1 N1 N2 -50.8(3) . . . . ? C2 N1 N2 C4 -0.8(6) . . . . ? Cu1 N1 N2 C4 179.0(3) . . . . ? C2 N1 N2 Cu2 180.0(3) . . . . ? Cu1 N1 N2 Cu2 -0.2(5) . . . . ? O3 Cu2 N2 C4 -43.2(5) . . . . ? O2 Cu2 N2 C4 150.3(5) . . . . ? N6 Cu2 N2 C4 48.7(10) . . . . ? Cl1 Cu2 N2 C4 -125.3(5) . . . . ? O3 Cu2 N2 N1 135.8(4) . . . . ? O2 Cu2 N2 N1 -30.7(3) . . . . ? N6 Cu2 N2 N1 -132.3(7) . . . . ? Cl1 Cu2 N2 N1 53.7(3) . . . . ? C6 N3 N4 C7 0.7(9) . . . . ? O3 Cu2 N6 C9 143.4(6) . . . . ? O2 Cu2 N6 C9 -49.9(6) . . . . ? N2 Cu2 N6 C9 50.5(11) . . . . ? Cl1 Cu2 N6 C9 -135.5(5) . . . . ? O3 Cu2 N6 N7 -30.2(4) . . . . ? O2 Cu2 N6 N7 136.5(4) . . . . ? N2 Cu2 N6 N7 -123.1(7) . . . . ? Cl1 Cu2 N6 N7 50.8(4) . . . . ? C9 N6 N7 C11 -0.9(6) . . . . ? Cu2 N6 N7 C11 174.3(4) . . . . ? C9 N6 N7 Cu3 -174.9(4) . . . . ? Cu2 N6 N7 Cu3 0.3(5) . . . . ? O3 Cu3 N7 C11 -142.2(6) . . . . ? O1 Cu3 N7 C11 50.8(6) 2_755 . . . ? N11 Cu3 N7 C11 -49.0(11) . . . . ? Cl1 Cu3 N7 C11 136.8(5) . . . . ? O3 Cu3 N7 N6 29.9(4) . . . . ? O1 Cu3 N7 N6 -137.1(4) 2_755 . . . ? N11 Cu3 N7 N6 123.0(7) . . . . ? Cl1 Cu3 N7 N6 -51.1(4) . . . . ? C13 N8 N9 C14 -0.6(10) . . . . ? O3 Cu3 N11 C16 41.2(6) . . . . ? O1 Cu3 N11 C16 -151.9(6) 2_755 . . . ? N7 Cu3 N11 C16 -50.9(11) . . . . ? Cl1 Cu3 N11 C16 123.2(6) . . . . ? O3 Cu3 N11 N12 -137.1(4) . . . . ? O1 Cu3 N11 N12 29.8(4) 2_755 . . . ? N7 Cu3 N11 N12 130.8(7) . . . . ? Cl1 Cu3 N11 N12 -55.0(4) . . . . ? C16 N11 N12 C18 -0.4(6) . . . . ? Cu3 N11 N12 C18 178.3(4) . . . . ? C16 N11 N12 Cu1 -176.9(4) . . . 2_755 ? Cu3 N11 N12 Cu1 1.9(5) . . . 2_755 ? N2 N1 C2 C3 1.1(6) . . . . ? Cu1 N1 C2 C3 -178.7(4) . . . . ? N2 N1 C2 C1 -179.1(5) . . . . ? Cu1 N1 C2 C1 1.1(9) . . . . ? N1 C2 C3 C4 -1.0(6) . . . . ? C1 C2 C3 C4 179.2(6) . . . . ? N1 C2 C3 N5 178.3(5) . . . . ? C1 C2 C3 N5 -1.5(10) . . . . ? C6 N5 C3 C2 88.5(9) . . . . ? C7 N5 C3 C2 -95.3(9) . . . . ? C6 N5 C3 C4 -92.3(9) . . . . ? C7 N5 C3 C4 83.9(8) . . . . ? N1 N2 C4 C3 0.2(6) . . . . ? Cu2 N2 C4 C3 179.2(4) . . . . ? N1 N2 C4 C5 178.8(5) . . . . ? Cu2 N2 C4 C5 -2.2(9) . . . . ? C2 C3 C4 N2 0.5(6) . . . . ? N5 C3 C4 N2 -178.8(5) . . . . ? C2 C3 C4 C5 -178.0(6) . . . . ? N5 C3 C4 C5 2.7(10) . . . . ? N4 N3 C6 N5 0.2(9) . . . . ? C7 N5 C6 N3 -0.9(9) . . . . ? C3 N5 C6 N3 175.9(6) . . . . ? N3 N4 C7 N5 -1.3(9) . . . . ? C6 N5 C7 N4 1.4(8) . . . . ? C3 N5 C7 N4 -175.6(6) . . . . ? N7 N6 C9 C10 0.9(6) . . . . ? Cu2 N6 C9 C10 -173.0(4) . . . . ? N7 N6 C9 C8 179.7(6) . . . . ? Cu2 N6 C9 C8 5.8(9) . . . . ? N6 C9 C10 C11 -0.6(7) . . . . ? C8 C9 C10 C11 -179.3(7) . . . . ? N6 C9 C10 N10 177.6(6) . . . . ? C8 C9 C10 N10 -1.1(11) . . . . ? C14 N10 C10 C11 -84.1(9) . . . . ? C13 N10 C10 C11 92.1(9) . . . . ? C14 N10 C10 C9 98.0(9) . . . . ? C13 N10 C10 C9 -85.8(9) . . . . ? N6 N7 C11 C10 0.5(7) . . . . ? Cu3 N7 C11 C10 172.9(4) . . . . ? N6 N7 C11 C12 -179.8(6) . . . . ? Cu3 N7 C11 C12 -7.3(10) . . . . ? C9 C10 C11 N7 0.1(7) . . . . ? N10 C10 C11 N7 -178.1(6) . . . . ? C9 C10 C11 C12 -179.6(7) . . . . ? N10 C10 C11 C12 2.1(11) . . . . ? N9 N8 C13 N10 0.1(10) . . . . ? C14 N10 C13 N8 0.4(9) . . . . ? C10 N10 C13 N8 -176.4(6) . . . . ? C13 N10 C14 N9 -0.8(8) . . . . ? C10 N10 C14 N9 176.1(6) . . . . ? N8 N9 C14 N10 0.9(9) . . . . ? N12 N11 C16 C17 0.7(7) . . . . ? Cu3 N11 C16 C17 -177.7(5) . . . . ? N12 N11 C16 C15 -180.0(6) . . . . ? Cu3 N11 C16 C15 1.6(10) . . . . ? N11 C16 C17 C18 -0.7(8) . . . . ? C15 C16 C17 C18 -180.0(6) . . . . ? N11 C16 C17 N15 177.2(7) . . . . ? C15 C16 C17 N15 -2.1(12) . . . . ? N11 N12 C18 C17 0.0(7) . . . . ? Cu1 N12 C18 C17 175.4(5) 2_755 . . . ? N11 N12 C18 C19 179.9(6) . . . . ? Cu1 N12 C18 C19 -4.7(10) 2_755 . . . ? C16 C17 C18 N12 0.5(8) . . . . ? N15 C17 C18 N12 -177.4(7) . . . . ? C16 C17 C18 C19 -179.5(7) . . . . ? N15 C17 C18 C19 2.6(13) . . . . ? C16 C17 N15 C20A 70.9(19) . . . . ? C18 C17 N15 C20A -111.5(18) . . . . ? C16 C17 N15 C21 -57.9(19) . . . . ? C18 C17 N15 C21 119.7(16) . . . . ? C16 C17 N15 C21A -92.3(16) . . . . ? C18 C17 N15 C21A 85.3(17) . . . . ? C16 C17 N15 C20 116.7(13) . . . . ? C18 C17 N15 C20 -65.8(15) . . . . ? C20 N13 N14 C21 -11(4) . . . . ? N14 N13 C20 N15 10(3) . . . . ? C20A N15 C20 N13 -56(2) . . . . ? C21 N15 C20 N13 -7(2) . . . . ? C21A N15 C20 N13 24(2) . . . . ? C17 N15 C20 N13 177.4(14) . . . . ? N13 N14 C21 N15 7(3) . . . . ? C20A N15 C21 N14 28(2) . . . . ? C21A N15 C21 N14 -108(4) . . . . ? C20 N15 C21 N14 -1(2) . . . . ? C17 N15 C21 N14 174.5(17) . . . . ? C21 N15 C20A N13A -28(2) . . . . ? C21A N15 C20A N13A -8(3) . . . . ? C20 N15 C20A N13A 104(3) . . . . ? C17 N15 C20A N13A -173.0(17) . . . . ? C20A N15 C21A N14A 11(2) . . . . ? C21 N15 C21A N14A 54(3) . . . . ? C20 N15 C21A N14A -28(2) . . . . ? C17 N15 C21A N14A 178.7(14) . . . . ? N15 C20A N13A N14A 2(3) . . . . ? N15 C21A N14A N13A -10(3) . . . . ? C20A N13A N14A C21A 5(3) . . . . ? O9A K1 O4 C22 67.7(8) . . . . ? O9A K1 O4 C22 -112.3(8) 2_666 . . . ? O9 K1 O4 C22 73.7(8) . . . . ? O9 K1 O4 C22 -106.3(8) 2_666 . . . ? O5 K1 O4 C22 148.5(7) . . . . ? O5 K1 O4 C22 -31.5(7) 2_666 . . . ? O6 K1 O4 C22 162.1(7) . . . . ? O6 K1 O4 C22 -17.9(7) 2_666 . . . ? C34 K1 O4 C22 50.0(8) . . . . ? C34 K1 O4 C22 -130.0(8) 2_666 . . . ? O9A K1 O4 C23 -61.2(8) . . . . ? O9A K1 O4 C23 118.8(8) 2_666 . . . ? O9 K1 O4 C23 -55.2(8) . . . . ? O9 K1 O4 C23 124.8(8) 2_666 . . . ? O5 K1 O4 C23 19.7(7) . . . . ? O5 K1 O4 C23 -160.3(7) 2_666 . . . ? O6 K1 O4 C23 33.2(8) . . . . ? O6 K1 O4 C23 -146.8(8) 2_666 . . . ? C34 K1 O4 C23 -78.9(8) . . . . ? C34 K1 O4 C23 101.1(8) 2_666 . . . ? O9A K1 O5 C24 102.9(9) . . . . ? O9A K1 O5 C24 -77.1(9) 2_666 . . . ? O9 K1 O5 C24 116.1(9) . . . . ? O9 K1 O5 C24 -63.9(9) 2_666 . . . ? O6 K1 O5 C24 -150.6(8) . . . . ? O6 K1 O5 C24 29.4(8) 2_666 . . . ? O4 K1 O5 C24 15.5(7) . . . . ? O4 K1 O5 C24 -164.5(7) 2_666 . . . ? C34 K1 O5 C24 107.7(9) . . . . ? C34 K1 O5 C24 -72.3(9) 2_666 . . . ? O9A K1 O5 C25 -119.6(8) . . . . ? O9A K1 O5 C25 60.4(8) 2_666 . . . ? O9 K1 O5 C25 -106.3(8) . . . . ? O9 K1 O5 C25 73.7(8) 2_666 . . . ? O6 K1 O5 C25 -13.1(7) . . . . ? O6 K1 O5 C25 166.9(7) 2_666 . . . ? O4 K1 O5 C25 153.0(7) . . . . ? O4 K1 O5 C25 -27.0(7) 2_666 . . . ? C34 K1 O5 C25 -114.8(8) . . . . ? C34 K1 O5 C25 65.2(8) 2_666 . . . ? O9A K1 O6 C26 50.3(9) . . . . ? O9A K1 O6 C26 -129.7(9) 2_666 . . . ? O9 K1 O6 C26 57.5(8) . . . . ? O9 K1 O6 C26 -122.5(8) 2_666 . . . ? O5 K1 O6 C26 -21.0(7) . . . . ? O5 K1 O6 C26 159.0(7) 2_666 . . . ? O4 K1 O6 C26 -34.9(8) . . . . ? O4 K1 O6 C26 145.1(8) 2_666 . . . ? C34 K1 O6 C26 72.5(8) . . . . ? C34 K1 O6 C26 -107.5(8) 2_666 . . . ? O9A K1 O6 C27 -77.8(8) . . . . ? O9A K1 O6 C27 102.2(8) 2_666 . . . ? O9 K1 O6 C27 -70.5(8) . . . . ? O9 K1 O6 C27 109.5(8) 2_666 . . . ? O5 K1 O6 C27 -149.1(7) . . . . ? O5 K1 O6 C27 30.9(7) 2_666 . . . ? O4 K1 O6 C27 -162.9(7) . . . . ? O4 K1 O6 C27 17.1(7) 2_666 . . . ? C34 K1 O6 C27 -55.6(8) . . . . ? C34 K1 O6 C27 124.4(8) 2_666 . . . ? C23 O4 C22 C27 -179.4(11) . . . 2_666 ? K1 O4 C22 C27 53.5(12) . . . 2_666 ? C22 O4 C23 C24 -177.6(11) . . . . ? K1 O4 C23 C24 -51.6(11) . . . . ? C25 O5 C24 C23 172.9(8) . . . . ? K1 O5 C24 C23 -48.4(10) . . . . ? O4 C23 C24 O5 67.1(12) . . . . ? C24 O5 C25 C26 -175.7(9) . . . . ? K1 O5 C25 C26 45.9(11) . . . . ? C27 O6 C26 C25 -178.7(9) . . . . ? K1 O6 C26 C25 52.5(11) . . . . ? O5 C25 C26 O6 -63.1(11) . . . . ? C26 O6 C27 C22 177.3(9) . . . 2_666 ? K1 O6 C27 C22 -51.2(11) . . . 2_666 ? C31 O7 C30 C31 -53.7(11) . . . 2_765 ? C30 O7 C31 C30 57.0(11) . . . 2_765 ? C33 O8 C32 C33 38.5(19) . . . 2_766 ? C32 O8 C33 C32 -39(2) . . . 2_766 ? O9A K1 O9 C37 90(4) . . . . ? O9A K1 O9 C37 -90(4) 2_666 . . . ? O5 K1 O9 C37 3(2) . . . . ? O5 K1 O9 C37 -177(2) 2_666 . . . ? O6 K1 O9 C37 -56(2) . . . . ? O6 K1 O9 C37 124(2) 2_666 . . . ? O4 K1 O9 C37 62(2) . . . . ? O4 K1 O9 C37 -118(2) 2_666 . . . ? C34 K1 O9 C37 162(3) . . . . ? C34 K1 O9 C37 -18(3) 2_666 . . . ? O9A K1 O9 C34 -72(4) . . . . ? O9A K1 O9 C34 108(4) 2_666 . . . ? O5 K1 O9 C34 -159.1(16) . . . . ? O5 K1 O9 C34 20.9(16) 2_666 . . . ? O6 K1 O9 C34 142.1(15) . . . . ? O6 K1 O9 C34 -37.9(15) 2_666 . . . ? O4 K1 O9 C34 -99.6(15) . . . . ? O4 K1 O9 C34 80.4(15) 2_666 . . . ? C37 O9 C34 C35 -29(3) . . . . ? K1 O9 C34 C35 133.9(18) . . . . ? C36 O10 C35 C34 -56(3) . . . . ? O9 C34 C35 O10 44(3) . . . . ? C35 O10 C36 C37 46(3) . . . . ? C34 O9 C37 C36 22(4) . . . . ? K1 O9 C37 C36 -137.1(18) . . . . ? O10 C36 C37 O9 -29(3) . . . . ? O9 K1 O9A C37A -106(4) . . . . ? O9 K1 O9A C37A 74(4) 2_666 . . . ? O5 K1 O9A C37A -15.3(19) . . . . ? O5 K1 O9A C37A 164.7(19) 2_666 . . . ? O6 K1 O9A C37A -71.1(19) . . . . ? O6 K1 O9A C37A 108.9(19) 2_666 . . . ? O4 K1 O9A C37A 46.7(19) . . . . ? O4 K1 O9A C37A -133.3(19) 2_666 . . . ? C34 K1 O9A C37A 177(3) . . . . ? C34 K1 O9A C37A -3(3) 2_666 . . . ? O5 K1 O9A C34A -178(2) . . . . ? O5 K1 O9A C34A 2(2) 2_666 . . . ? O6 K1 O9A C34A 127(2) . . . . ? O6 K1 O9A C34A -53(2) 2_666 . . . ? O4 K1 O9A C34A -116(2) . . . . ? O4 K1 O9A C34A 64(2) 2_666 . . . ? C37A O9A C34A C35A 79(2) . . . . ? K1 O9A C34A C35A -115(2) . . . . ? C36A O10A C35A C34A 52(2) . . . . ? O9A C34A C35A O10A -74(3) . . . . ? C35A O10A C36A C37A -50(3) . . . . ? C34A O9A C37A C36A -63(2) . . . . ? K1 O9A C37A C36A 131.5(17) . . . . ? O10A C36A C37A O9A 56(3) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.933 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.105 #============================================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 796879' #TrackingRef '- Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-tetrahydrofurane-(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium \m6-chlorido-hexakis-[\m-(4-(1,2,4-triazol-4-yl)-3,5-dimethylpyrazolato]- hexa-\m-hydroxido-hexacopper(II) Solvate with 2 Dichloromethane and 4 Tetrahydrofurane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 Cl Cu6 N30 O6, C20 H40 K O8, 4(C4 H8 O), 2(C H2 Cl2)' _chemical_formula_sum 'C80 H130 Cl5 Cu6 K N30 O18' _chemical_formula_weight 2397.73 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9956(8) _cell_length_b 14.3194(8) _cell_length_c 14.6356(10) _cell_angle_alpha 88.431(3) _cell_angle_beta 71.096(3) _cell_angle_gamma 74.869(2) _cell_volume 2673.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17403 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 25.83 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7107 _exptl_absorpt_correction_T_max 0.7657 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 17403 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.83 _reflns_number_total 10018 _reflns_number_gt 6948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _refine_special_details ; Main problem of the refinement was connected with modeling disorder of THF molecules. The coordinated THF molecule of the centrosymmetric [K(18c6)(THF)2]+ cation (18c6 ligand itself adopts the most typical nearly D3d conformation) is disordered. This was resolved with two equal contributions from two of the methylene carbon atoms and with restraints in geometry and thermal parameters (DFIX/SIMU) (Figure S1). Atoms of this molecule were left isotropic (Uiso = 0.069-0.140 A^2) and the hydrogen atoms were not added. Also, two of three independent solvate THF molecules are disordered over a center of inversion (no hydrogen atoms added here). One of them was refined isotropically (Uiso = 0.063-0.124 A^2) and with restraints in geometry. In all other cases, non-hydrogen atoms were refined anisotropically and CH hydrogen atoms were placed in calculated positions and refined within a riding model, with Uiso = 1.2Ueq of the carrier atom. OH hydrogen atoms were located and then fixed with Uiso = 1.5Ueq(O). 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^)+(0.0807P)^2^+0.0000P] 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_number_reflns 10018 _refine_ls_number_parameters 643 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _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 0.90709(5) 0.71231(5) 0.06456(5) 0.02531(19) Uani 1 1 d . . . Cu2 Cu 0.78426(5) 0.56925(5) 0.16799(5) 0.02471(19) Uani 1 1 d . . . Cu3 Cu 0.88228(5) 0.35437(5) 0.10270(5) 0.02501(19) Uani 1 1 d . . . K1 K 0.5000 0.0000 0.5000 0.0485(5) Uani 1 2 d S . . Cl1 Cl 1.0000 0.5000 0.0000 0.0324(5) Uani 1 2 d S . . O1 O 0.8461(3) 0.6679(3) 0.1906(3) 0.0283(9) Uani 1 1 d . . . H1W H 0.8915 0.6467 0.2196 0.043 Uiso 1 1 d . . . O2 O 0.7572(3) 0.4585(2) 0.1198(2) 0.0250(8) Uani 1 1 d . . . H2W H 0.7487 0.4699 0.0642 0.038 Uiso 1 1 d . . . O3 O 1.0231(3) 0.2735(3) 0.0703(3) 0.0275(9) Uani 1 1 d . . . H3W H 1.0537 0.2964 0.1036 0.041 Uiso 1 1 d . . . O4 O 0.6067(4) 0.1462(3) 0.4502(4) 0.0570(13) Uani 1 1 d . . . O5 O 0.6591(4) -0.0153(4) 0.3187(3) 0.0610(14) Uani 1 1 d . . . O6 O 0.5190(4) -0.1316(3) 0.3580(4) 0.0552(13) Uani 1 1 d . . . N1 N 0.7706(3) 0.7276(3) 0.0489(3) 0.0243(10) Uani 1 1 d . . . N2 N 0.7164(3) 0.6627(3) 0.0924(3) 0.0264(10) Uani 1 1 d . . . N3 N 0.4199(4) 0.9081(4) -0.0625(5) 0.0486(15) Uani 1 1 d . . . N4 N 0.4727(4) 0.8423(4) -0.1414(4) 0.0480(15) Uani 1 1 d . . . N5 N 0.5463(3) 0.8027(3) -0.0281(3) 0.0302(11) Uani 1 1 d . . . N6 N 1.0299(3) 0.7324(3) 0.0899(3) 0.0266(10) Uani 1 1 d . . . N7 N 1.1223(3) 0.7050(3) 0.0144(3) 0.0276(11) Uani 1 1 d . . . N8 N 1.3065(5) 0.8280(6) 0.2625(4) 0.0629(18) Uani 1 1 d . . . N9 N 1.2748(5) 0.9180(5) 0.2273(5) 0.0656(18) Uani 1 1 d . . . N10 N 1.2034(4) 0.8172(4) 0.1807(3) 0.0363(12) Uani 1 1 d . . . N11 N 0.8247(3) 0.4851(3) 0.2652(3) 0.0278(11) Uani 1 1 d . . . N12 N 0.8696(3) 0.3887(3) 0.2351(3) 0.0275(11) Uani 1 1 d . . . N13 N 0.9653(6) 0.3761(6) 0.5828(5) 0.082(2) Uani 1 1 d . . . N14 N 0.8668(5) 0.3708(5) 0.6275(4) 0.0637(18) Uani 1 1 d . . . N15 N 0.8877(4) 0.3928(4) 0.4749(3) 0.0360(12) Uani 1 1 d . . . C1 C 0.7509(4) 0.8674(4) -0.0555(4) 0.0361(15) Uani 1 1 d . . . H1A H 0.7130 0.9290 -0.0174 0.054 Uiso 1 1 calc R . . H1B H 0.7361 0.8695 -0.1167 0.054 Uiso 1 1 calc R . . H1C H 0.8264 0.8570 -0.0690 0.054 Uiso 1 1 calc R . . C2 C 0.7164(4) 0.7864(4) 0.0000(4) 0.0250(12) Uani 1 1 d . . . C3 C 0.6245(4) 0.7596(4) 0.0147(4) 0.0279(13) Uani 1 1 d . . . C4 C 0.6259(4) 0.6819(4) 0.0725(4) 0.0260(12) Uani 1 1 d . . . C5 C 0.5447(4) 0.6272(4) 0.1107(4) 0.0344(14) Uani 1 1 d . . . H5A H 0.5784 0.5610 0.1225 0.052 Uiso 1 1 calc R . . H5B H 0.5094 0.6248 0.0632 0.052 Uiso 1 1 calc R . . H5C H 0.4930 0.6598 0.1714 0.052 Uiso 1 1 calc R . . C6 C 0.4657(5) 0.8826(4) 0.0029(5) 0.0420(16) Uani 1 1 d . . . H6 H 0.4447 0.9162 0.0643 0.050 Uiso 1 1 calc R . . C7 C 0.5477(5) 0.7816(5) -0.1189(4) 0.0370(15) Uani 1 1 d . . . H7 H 0.5973 0.7289 -0.1608 0.044 Uiso 1 1 calc R . . C8 C 0.9608(5) 0.8172(5) 0.2540(4) 0.0381(15) Uani 1 1 d . . . H8A H 0.8927 0.8202 0.2471 0.057 Uiso 1 1 calc R . . H8B H 0.9631 0.8825 0.2696 0.057 Uiso 1 1 calc R . . H8C H 0.9705 0.7752 0.3061 0.057 Uiso 1 1 calc R . . C9 C 1.0466(4) 0.7766(4) 0.1606(4) 0.0289(13) Uani 1 1 d . . . C10 C 1.1509(4) 0.7768(4) 0.1292(4) 0.0304(13) Uani 1 1 d . . . C11 C 1.1952(4) 0.7318(4) 0.0383(4) 0.0287(13) Uani 1 1 d . . . C12 C 1.3058(4) 0.7152(5) -0.0283(5) 0.0413(16) Uani 1 1 d . . . H12A H 1.3312 0.6489 -0.0579 0.062 Uiso 1 1 calc R . . H12B H 1.3504 0.7244 0.0084 0.062 Uiso 1 1 calc R . . H12C H 1.3083 0.7614 -0.0792 0.062 Uiso 1 1 calc R . . C13 C 1.2633(6) 0.7695(6) 0.2347(5) 0.057(2) Uani 1 1 d . . . H13 H 1.2716 0.7034 0.2493 0.068 Uiso 1 1 calc R . . C14 C 1.2155(6) 0.9073(5) 0.1803(5) 0.0537(19) Uani 1 1 d . . . H14 H 1.1831 0.9581 0.1482 0.064 Uiso 1 1 calc R . . C15 C 0.7809(5) 0.5945(5) 0.4101(5) 0.0442(16) Uani 1 1 d . . . H15A H 0.7360 0.6390 0.3794 0.066 Uiso 1 1 calc R . . H15B H 0.8385 0.6212 0.4107 0.066 Uiso 1 1 calc R . . H15C H 0.7395 0.5866 0.4767 0.066 Uiso 1 1 calc R . . C16 C 0.8244(4) 0.4987(4) 0.3548(4) 0.0307(13) Uani 1 1 d . . . C17 C 0.8690(4) 0.4097(4) 0.3841(4) 0.0318(14) Uani 1 1 d . . . C18 C 0.8960(4) 0.3423(4) 0.3076(4) 0.0291(13) Uani 1 1 d . . . C19 C 0.9480(5) 0.2373(4) 0.3004(5) 0.0437(17) Uani 1 1 d . . . H19A H 0.9347 0.2051 0.2494 0.066 Uiso 1 1 calc R . . H19B H 0.9202 0.2097 0.3624 0.066 Uiso 1 1 calc R . . H19C H 1.0237 0.2275 0.2849 0.066 Uiso 1 1 calc R . . C20 C 0.9761(6) 0.3855(8) 0.4924(6) 0.089(3) Uani 1 1 d . . . H20 H 1.0401 0.3869 0.4441 0.107 Uiso 1 1 calc R . . C21 C 0.8214(6) 0.3816(6) 0.5616(5) 0.065(2) Uani 1 1 d . . . H21 H 0.7506 0.3816 0.5734 0.078 Uiso 1 1 calc R . . C22 C 0.6177(7) 0.1850(6) 0.5330(6) 0.072(3) Uani 1 1 d . . . H22A H 0.6459 0.2421 0.5160 0.087 Uiso 1 1 calc R . . H22B H 0.6680 0.1360 0.5558 0.087 Uiso 1 1 calc R . . C23 C 0.7008(7) 0.1169(7) 0.3726(7) 0.074(3) Uani 1 1 d . . . H23A H 0.7531 0.0685 0.3937 0.089 Uiso 1 1 calc R . . H23B H 0.7289 0.1735 0.3517 0.089 Uiso 1 1 calc R . . C24 C 0.6835(7) 0.0742(7) 0.2905(6) 0.073(2) Uani 1 1 d . . . H24A H 0.6249 0.1187 0.2743 0.088 Uiso 1 1 calc R . . H24B H 0.7473 0.0627 0.2328 0.088 Uiso 1 1 calc R . . C25 C 0.6389(7) -0.0623(6) 0.2442(5) 0.073(3) Uani 1 1 d . . . H25A H 0.7011 -0.0755 0.1848 0.088 Uiso 1 1 calc R . . H25B H 0.5790 -0.0196 0.2284 0.088 Uiso 1 1 calc R . . C26 C 0.6150(7) -0.1539(6) 0.2785(6) 0.072(3) Uani 1 1 d . . . H26A H 0.6081 -0.1905 0.2256 0.087 Uiso 1 1 calc R . . H26B H 0.6723 -0.1944 0.2994 0.087 Uiso 1 1 calc R . . C27 C 0.4840(7) -0.2137(6) 0.3893(6) 0.066(2) Uani 1 1 d . . . H27A H 0.5357 -0.2593 0.4134 0.079 Uiso 1 1 calc R . . H27B H 0.4769 -0.2472 0.3345 0.079 Uiso 1 1 calc R . . Cl2 Cl 0.85503(18) 0.61540(18) -0.22060(17) 0.0816(7) Uani 1 1 d . . . Cl3 Cl 0.72081(17) 0.49782(15) -0.11772(15) 0.0682(6) Uani 1 1 d . . . C28 C 0.8510(6) 0.5016(5) -0.1711(5) 0.062(2) Uani 1 1 d . . . H28A H 0.8881 0.4492 -0.2229 0.074 Uiso 1 1 calc R . . H28B H 0.8869 0.4914 -0.1220 0.074 Uiso 1 1 calc R . . O7 O 0.3308(6) 0.0859(6) 0.4523(6) 0.131(3) Uiso 1 1 d DU . . C29 C 0.3350(10) 0.0762(10) 0.3457(9) 0.140(4) Uiso 1 1 d DU . . C30 C 0.2501(9) 0.1552(8) 0.3369(8) 0.107(3) Uiso 1 1 d DU . . C31A C 0.1872(15) 0.1976(16) 0.4360(13) 0.125(5) Uiso 0.50 1 d PDU . . C31B C 0.2842(19) 0.2285(12) 0.3895(15) 0.123(5) Uiso 0.50 1 d PDU . . C32A C 0.2373(13) 0.1529(13) 0.5076(12) 0.086(4) Uiso 0.50 1 d PDU . . C32B C 0.3162(13) 0.1795(11) 0.4739(11) 0.069(4) Uiso 0.50 1 d PDU . . O8 O 0.4392(5) 0.5264(6) 0.3637(6) 0.114(2) Uani 1 1 d . . . C33 C 0.4355(9) 0.4429(9) 0.3098(10) 0.113(4) Uani 1 1 d . . . H33A H 0.3652 0.4312 0.3343 0.136 Uiso 1 1 calc R . . H33B H 0.4525 0.4538 0.2400 0.136 Uiso 1 1 calc R . . C34 C 0.5134(10) 0.3620(9) 0.3264(10) 0.124(4) Uani 1 1 d . . . H34A H 0.5493 0.3175 0.2677 0.149 Uiso 1 1 calc R . . H34B H 0.4806 0.3254 0.3806 0.149 Uiso 1 1 calc R . . C35 C 0.5873(7) 0.4041(7) 0.3501(8) 0.090(3) Uani 1 1 d . . . H35A H 0.6550 0.3886 0.2967 0.108 Uiso 1 1 calc R . . H35B H 0.5997 0.3773 0.4096 0.108 Uiso 1 1 calc R . . C36 C 0.5416(7) 0.5109(7) 0.3652(6) 0.072(2) Uani 1 1 d . . . H36A H 0.5413 0.5349 0.4281 0.086 Uiso 1 1 calc R . . H36B H 0.5821 0.5446 0.3129 0.086 Uiso 1 1 calc R . . O9 O 1.0582(9) 1.0143(8) 0.0785(8) 0.070(3) Uani 0.50 1 d PD . . C37 C 1.110(3) 0.995(3) -0.0284(16) 0.103(15) Uani 0.50 1 d PD . . C38 C 1.018(2) 0.9652(16) -0.056(2) 0.081(9) Uani 0.50 1 d P . . C39 C 0.918(2) 1.0035(15) 0.0342(17) 0.044(6) Uani 0.50 1 d P . . C40 C 0.9475(16) 1.059(2) 0.110(3) 0.109(13) Uani 0.50 1 d PD . . O10 O 0.9305(13) 0.0751(13) 0.4670(13) 0.124(5) Uiso 0.50 1 d PD . . C41 C 0.9546(16) 0.0879(14) 0.5520(14) 0.080(6) Uiso 0.50 1 d PD . . C42 C 1.0319(16) -0.0014(14) 0.5681(14) 0.072(6) Uiso 0.50 1 d PD . . C43 C 1.061(2) -0.0674(15) 0.4734(16) 0.100(8) Uiso 0.50 1 d PD . . C44 C 1.0153(15) 0.0030(12) 0.4092(13) 0.063(5) Uiso 0.50 1 d PD . . 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 0.0215(4) 0.0283(4) 0.0265(4) -0.0008(3) -0.0095(3) -0.0050(3) Cu2 0.0243(4) 0.0251(4) 0.0245(4) 0.0004(3) -0.0106(3) -0.0030(3) Cu3 0.0242(4) 0.0253(4) 0.0250(4) -0.0017(3) -0.0096(3) -0.0033(3) K1 0.0528(13) 0.0554(13) 0.0346(12) -0.0145(10) -0.0162(10) -0.0056(11) Cl1 0.0353(11) 0.0289(10) 0.0329(11) 0.0008(9) -0.0115(9) -0.0080(9) O1 0.029(2) 0.030(2) 0.028(2) -0.0003(17) -0.0119(18) -0.0069(17) O2 0.027(2) 0.029(2) 0.022(2) -0.0001(16) -0.0120(17) -0.0064(17) O3 0.025(2) 0.027(2) 0.031(2) 0.0008(17) -0.0143(18) -0.0018(16) O4 0.056(3) 0.058(3) 0.065(4) 0.004(3) -0.035(3) -0.009(3) O5 0.066(3) 0.067(3) 0.041(3) -0.003(3) -0.022(3) 0.005(3) O6 0.064(3) 0.040(3) 0.056(3) -0.018(2) -0.028(3) 0.006(2) N1 0.020(2) 0.025(2) 0.028(3) 0.005(2) -0.010(2) -0.005(2) N2 0.019(2) 0.025(2) 0.032(3) 0.001(2) -0.007(2) -0.001(2) N3 0.042(3) 0.039(3) 0.070(4) 0.014(3) -0.033(3) -0.003(3) N4 0.038(3) 0.062(4) 0.046(4) 0.022(3) -0.022(3) -0.009(3) N5 0.023(3) 0.029(3) 0.033(3) 0.002(2) -0.010(2) 0.003(2) N6 0.021(2) 0.030(3) 0.026(3) -0.004(2) -0.008(2) -0.001(2) N7 0.022(2) 0.033(3) 0.028(3) -0.001(2) -0.007(2) -0.009(2) N8 0.054(4) 0.099(6) 0.052(4) -0.011(4) -0.028(3) -0.032(4) N9 0.058(4) 0.080(5) 0.071(5) -0.018(4) -0.023(4) -0.033(4) N10 0.029(3) 0.051(3) 0.031(3) -0.007(2) -0.010(2) -0.013(2) N11 0.032(3) 0.025(2) 0.025(3) -0.003(2) -0.013(2) -0.001(2) N12 0.028(3) 0.030(3) 0.024(3) 0.001(2) -0.011(2) -0.004(2) N13 0.067(5) 0.138(7) 0.050(4) 0.027(4) -0.034(4) -0.029(5) N14 0.073(5) 0.095(5) 0.029(3) 0.015(3) -0.025(3) -0.022(4) N15 0.037(3) 0.045(3) 0.023(3) 0.002(2) -0.012(2) -0.003(2) C1 0.031(3) 0.036(3) 0.046(4) 0.012(3) -0.020(3) -0.007(3) C2 0.022(3) 0.025(3) 0.027(3) -0.005(2) -0.007(2) -0.005(2) C3 0.024(3) 0.025(3) 0.031(3) -0.001(2) -0.011(3) 0.001(2) C4 0.021(3) 0.028(3) 0.028(3) -0.006(2) -0.010(2) -0.001(2) C5 0.019(3) 0.038(3) 0.042(4) 0.004(3) -0.009(3) -0.003(3) C6 0.036(4) 0.032(3) 0.057(4) -0.004(3) -0.018(3) -0.003(3) C7 0.034(4) 0.045(4) 0.034(4) 0.008(3) -0.014(3) -0.011(3) C8 0.039(4) 0.046(4) 0.032(3) -0.012(3) -0.012(3) -0.012(3) C9 0.033(3) 0.030(3) 0.025(3) -0.003(2) -0.008(3) -0.010(3) C10 0.024(3) 0.034(3) 0.035(3) -0.004(3) -0.012(3) -0.008(3) C11 0.029(3) 0.031(3) 0.026(3) 0.000(3) -0.008(3) -0.010(3) C12 0.031(3) 0.051(4) 0.044(4) -0.010(3) -0.009(3) -0.017(3) C13 0.055(5) 0.079(5) 0.046(4) 0.000(4) -0.023(4) -0.025(4) C14 0.055(5) 0.049(4) 0.067(5) -0.012(4) -0.029(4) -0.019(4) C15 0.050(4) 0.043(4) 0.036(4) -0.007(3) -0.018(3) -0.001(3) C16 0.034(3) 0.036(3) 0.023(3) -0.001(3) -0.011(3) -0.007(3) C17 0.031(3) 0.044(4) 0.020(3) 0.004(3) -0.011(3) -0.008(3) C18 0.025(3) 0.032(3) 0.030(3) 0.010(3) -0.010(3) -0.006(3) C19 0.046(4) 0.039(4) 0.040(4) 0.013(3) -0.014(3) -0.002(3) C20 0.053(5) 0.188(11) 0.044(5) 0.041(6) -0.028(4) -0.053(6) C21 0.064(5) 0.104(7) 0.031(4) 0.014(4) -0.015(4) -0.029(5) C22 0.090(7) 0.071(6) 0.085(7) 0.008(5) -0.064(6) -0.028(5) C23 0.061(6) 0.085(6) 0.082(7) 0.023(5) -0.032(5) -0.020(5) C24 0.061(5) 0.086(7) 0.056(5) 0.014(5) -0.005(4) -0.011(5) C25 0.082(6) 0.079(6) 0.034(4) -0.014(4) -0.009(4) 0.010(5) C26 0.085(6) 0.068(6) 0.046(5) -0.029(4) -0.023(5) 0.015(5) C27 0.070(6) 0.059(5) 0.073(6) -0.020(4) -0.040(5) 0.003(4) Cl2 0.0790(15) 0.0954(17) 0.0717(15) 0.0162(13) -0.0148(12) -0.0394(13) Cl3 0.0756(14) 0.0634(12) 0.0629(13) 0.0017(10) -0.0166(11) -0.0213(11) C28 0.065(5) 0.056(5) 0.060(5) -0.006(4) -0.037(4) 0.013(4) O8 0.066(4) 0.094(5) 0.155(7) -0.007(5) -0.018(4) 0.002(4) C33 0.093(8) 0.107(9) 0.167(12) 0.036(9) -0.069(8) -0.042(7) C34 0.104(9) 0.098(9) 0.164(12) -0.032(8) -0.039(9) -0.018(8) C35 0.058(6) 0.084(7) 0.103(8) 0.014(6) -0.003(5) -0.009(5) C36 0.061(6) 0.097(7) 0.056(5) 0.005(5) -0.013(4) -0.026(5) O9 0.075(8) 0.066(7) 0.080(9) 0.013(6) -0.038(7) -0.021(6) C37 0.11(3) 0.18(3) 0.068(18) 0.028(17) -0.047(17) -0.11(2) C38 0.092(18) 0.029(11) 0.16(3) 0.014(14) -0.08(2) -0.024(12) C39 0.027(9) 0.025(8) 0.077(15) -0.010(8) -0.015(9) -0.004(8) C40 0.076(19) 0.09(2) 0.17(3) -0.057(18) -0.067(19) -0.003(14) _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 O3 1.930(4) 2_765 ? Cu1 O1 1.932(4) . ? Cu1 N1 1.952(4) . ? Cu1 N6 1.963(4) . ? Cu1 Cl1 3.0206(7) . ? Cu2 O1 1.924(4) . ? Cu2 O2 1.926(4) . ? Cu2 N2 1.963(4) . ? Cu2 N11 1.967(4) . ? Cu2 Cl1 3.1473(7) . ? Cu3 O3 1.919(3) . ? Cu3 O2 1.930(3) . ? Cu3 N12 1.952(4) . ? Cu3 N7 1.961(5) 2_765 ? Cu3 Cl1 3.0561(7) . ? K1 O7 2.666(7) . ? K1 O7 2.666(7) 2_656 ? K1 O6 2.746(5) 2_656 ? K1 O6 2.746(4) . ? K1 O4 2.826(5) 2_656 ? K1 O4 2.826(5) . ? K1 O5 2.828(5) . ? K1 O5 2.828(5) 2_656 ? O4 C23 1.403(9) . ? O4 C22 1.416(8) . ? O5 C24 1.427(9) . ? O5 C25 1.436(9) . ? O6 C27 1.399(9) . ? O6 C26 1.430(9) . ? N1 C2 1.335(6) . ? N1 N2 1.366(6) . ? N2 C4 1.349(6) . ? N3 C6 1.310(7) . ? N3 N4 1.382(8) . ? N4 C7 1.302(7) . ? N5 C6 1.346(7) . ? N5 C7 1.365(7) . ? N5 C3 1.429(6) . ? N6 C9 1.341(7) . ? N6 N7 1.370(6) . ? N7 C11 1.324(7) . ? N8 C13 1.295(9) . ? N8 N9 1.392(9) . ? N9 C14 1.275(8) . ? N10 C14 1.344(8) . ? N10 C13 1.376(8) . ? N10 C10 1.431(7) . ? N11 C16 1.329(7) . ? N11 N12 1.377(6) . ? N12 C18 1.339(6) . ? N13 C20 1.290(9) . ? N13 N14 1.342(8) . ? N14 C21 1.302(8) . ? N15 C20 1.320(8) . ? N15 C21 1.341(8) . ? N15 C17 1.437(7) . ? C1 C2 1.493(7) . ? C2 C3 1.386(7) . ? C3 C4 1.378(7) . ? C4 C5 1.500(7) . ? C8 C9 1.505(8) . ? C9 C10 1.381(7) . ? C10 C11 1.369(8) . ? C11 C12 1.499(7) . ? C15 C16 1.489(8) . ? C16 C17 1.388(8) . ? C17 C18 1.387(8) . ? C18 C19 1.480(8) . ? C22 C27 1.469(11) 2_656 ? C23 C24 1.477(11) . ? C25 C26 1.474(11) . ? Cl2 C28 1.772(8) . ? Cl3 C28 1.750(8) . ? O7 C32B 1.334(13) . ? O7 C32A 1.411(14) . ? O7 C29 1.552(12) . ? C29 C30 1.448(12) . ? C30 C31A 1.480(16) . ? C30 C31B 1.570(16) . ? C31A C32A 1.484(16) . ? C31B C32B 1.537(15) . ? O8 C36 1.398(9) . ? O8 C33 1.471(13) . ? C33 C34 1.444(13) . ? C34 C35 1.456(13) . ? C35 C36 1.488(12) . ? O9 C40 1.435(18) . ? O9 C37 1.494(19) . ? C37 C38 1.62(4) . ? C38 C39 1.57(4) . ? C39 C40 1.60(4) . ? O10 C44 1.40(2) . ? O10 C41 1.419(17) . ? C41 C42 1.512(16) . ? C42 C43 1.576(18) . ? C43 C44 1.520(17) . ? 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 O3 Cu1 O1 167.22(15) 2_765 . ? O3 Cu1 N1 94.26(16) 2_765 . ? O1 Cu1 N1 85.84(16) . . ? O3 Cu1 N6 87.33(17) 2_765 . ? O1 Cu1 N6 95.80(16) . . ? N1 Cu1 N6 165.38(18) . . ? O3 Cu1 Cl1 81.71(11) 2_765 . ? O1 Cu1 Cl1 85.63(11) . . ? N1 Cu1 Cl1 98.20(13) . . ? N6 Cu1 Cl1 96.42(13) . . ? O1 Cu2 O2 165.10(16) . . ? O1 Cu2 N2 86.79(17) . . ? O2 Cu2 N2 95.26(16) . . ? O1 Cu2 N11 94.56(17) . . ? O2 Cu2 N11 86.45(16) . . ? N2 Cu2 N11 168.24(19) . . ? O1 Cu2 Cl1 82.21(11) . . ? O2 Cu2 Cl1 82.90(11) . . ? N2 Cu2 Cl1 95.21(13) . . ? N11 Cu2 Cl1 96.55(13) . . ? O3 Cu3 O2 166.29(15) . . ? O3 Cu3 N12 95.12(16) . . ? O2 Cu3 N12 86.92(16) . . ? O3 Cu3 N7 86.45(17) . 2_765 ? O2 Cu3 N7 94.96(16) . 2_765 ? N12 Cu3 N7 165.53(19) . 2_765 ? O3 Cu3 Cl1 80.91(11) . . ? O2 Cu3 Cl1 85.38(10) . . ? N12 Cu3 Cl1 98.23(13) . . ? N7 Cu3 Cl1 96.22(13) 2_765 . ? O7 K1 O7 180.0(3) . 2_656 ? O7 K1 O6 99.9(2) . 2_656 ? O7 K1 O6 80.1(2) 2_656 2_656 ? O7 K1 O6 80.1(2) . . ? O7 K1 O6 99.9(2) 2_656 . ? O6 K1 O6 180.0 2_656 . ? O7 K1 O4 81.5(2) . 2_656 ? O7 K1 O4 98.5(2) 2_656 2_656 ? O6 K1 O4 119.09(16) 2_656 2_656 ? O6 K1 O4 60.91(16) . 2_656 ? O7 K1 O4 98.5(2) . . ? O7 K1 O4 81.5(2) 2_656 . ? O6 K1 O4 60.91(16) 2_656 . ? O6 K1 O4 119.09(16) . . ? O4 K1 O4 180.00(10) 2_656 . ? O7 K1 O5 100.7(2) . . ? O7 K1 O5 79.3(2) 2_656 . ? O6 K1 O5 119.57(16) 2_656 . ? O6 K1 O5 60.43(16) . . ? O4 K1 O5 119.83(16) 2_656 . ? O4 K1 O5 60.17(16) . . ? O7 K1 O5 79.3(2) . 2_656 ? O7 K1 O5 100.7(2) 2_656 2_656 ? O6 K1 O5 60.43(16) 2_656 2_656 ? O6 K1 O5 119.57(16) . 2_656 ? O4 K1 O5 60.17(16) 2_656 2_656 ? O4 K1 O5 119.83(16) . 2_656 ? O5 K1 O5 180.0 . 2_656 ? Cu1 Cl1 Cu3 118.773(17) . . ? Cu1 Cl1 Cu2 59.662(17) . . ? Cu3 Cl1 Cu2 59.117(17) . . ? Cu2 O1 Cu1 105.51(17) . . ? Cu2 O2 Cu3 105.11(16) . . ? Cu3 O3 Cu1 107.03(16) . 2_765 ? C23 O4 C22 113.9(6) . . ? C23 O4 K1 113.1(5) . . ? C22 O4 K1 110.8(5) . . ? C24 O5 C25 112.2(6) . . ? C24 O5 K1 113.6(4) . . ? C25 O5 K1 112.4(5) . . ? C27 O6 C26 112.6(6) . . ? C27 O6 K1 116.3(4) . . ? C26 O6 K1 116.7(4) . . ? C2 N1 N2 108.9(4) . . ? C2 N1 Cu1 134.4(4) . . ? N2 N1 Cu1 116.5(3) . . ? C4 N2 N1 108.8(4) . . ? C4 N2 Cu2 136.1(4) . . ? N1 N2 Cu2 115.0(3) . . ? C6 N3 N4 107.4(5) . . ? C7 N4 N3 106.0(5) . . ? C6 N5 C7 103.7(5) . . ? C6 N5 C3 128.7(5) . . ? C7 N5 C3 126.7(5) . . ? C9 N6 N7 108.4(4) . . ? C9 N6 Cu1 135.8(4) . . ? N7 N6 Cu1 115.3(3) . . ? C11 N7 N6 108.4(4) . . ? C11 N7 Cu3 134.6(4) . 2_765 ? N6 N7 Cu3 116.8(3) . 2_765 ? C13 N8 N9 107.8(6) . . ? C14 N9 N8 105.7(6) . . ? C14 N10 C13 103.2(5) . . ? C14 N10 C10 128.9(5) . . ? C13 N10 C10 127.6(6) . . ? C16 N11 N12 109.1(4) . . ? C16 N11 Cu2 135.4(4) . . ? N12 N11 Cu2 115.3(3) . . ? C18 N12 N11 108.0(4) . . ? C18 N12 Cu3 136.4(4) . . ? N11 N12 Cu3 115.6(3) . . ? C20 N13 N14 107.0(6) . . ? C21 N14 N13 106.3(6) . . ? C20 N15 C21 103.2(6) . . ? C20 N15 C17 127.4(6) . . ? C21 N15 C17 129.4(5) . . ? N1 C2 C3 107.3(5) . . ? N1 C2 C1 124.0(5) . . ? C3 C2 C1 128.7(5) . . ? C4 C3 C2 107.9(5) . . ? C4 C3 N5 127.1(5) . . ? C2 C3 N5 124.9(5) . . ? N2 C4 C3 107.0(5) . . ? N2 C4 C5 123.9(5) . . ? C3 C4 C5 129.2(5) . . ? N3 C6 N5 111.1(6) . . ? N4 C7 N5 111.8(6) . . ? N6 C9 C10 107.4(5) . . ? N6 C9 C8 122.3(5) . . ? C10 C9 C8 130.2(5) . . ? C11 C10 C9 107.1(5) . . ? C11 C10 N10 125.9(5) . . ? C9 C10 N10 127.0(5) . . ? N7 C11 C10 108.6(5) . . ? N7 C11 C12 122.9(5) . . ? C10 C11 C12 128.4(5) . . ? N8 C13 N10 109.9(7) . . ? N9 C14 N10 113.4(7) . . ? N11 C16 C17 107.9(5) . . ? N11 C16 C15 123.5(5) . . ? C17 C16 C15 128.6(5) . . ? C18 C17 C16 106.7(5) . . ? C18 C17 N15 127.2(5) . . ? C16 C17 N15 126.0(5) . . ? N12 C18 C17 108.2(5) . . ? N12 C18 C19 123.1(5) . . ? C17 C18 C19 128.7(5) . . ? N13 C20 N15 112.1(7) . . ? N14 C21 N15 111.2(7) . . ? O4 C22 C27 110.4(6) . 2_656 ? O4 C23 C24 110.6(7) . . ? O5 C24 C23 107.7(7) . . ? O5 C25 C26 108.9(6) . . ? O6 C26 C25 108.4(6) . . ? O6 C27 C22 109.8(7) . 2_656 ? Cl3 C28 Cl2 109.9(4) . . ? C32B O7 C32A 52.2(10) . . ? C32B O7 C29 107.2(9) . . ? C32A O7 C29 110.8(9) . . ? C32B O7 K1 103.1(8) . . ? C32A O7 K1 129.4(9) . . ? C29 O7 K1 119.2(7) . . ? C30 C29 O7 105.1(9) . . ? C29 C30 C31A 106.8(10) . . ? C30 C31A C32A 111.3(12) . . ? C32B C31B C30 109.1(11) . . ? O7 C32A C31A 104.9(12) . . ? O7 C32B C31B 102.5(11) . . ? C36 O8 C33 107.9(7) . . ? C34 C33 O8 104.9(9) . . ? C33 C34 C35 105.7(10) . . ? C34 C35 C36 108.0(8) . . ? O8 C36 C35 105.1(8) . . ? C40 O9 C37 116(2) . . ? O9 C37 C38 100(2) . . ? C39 C38 C37 104(2) . . ? C38 C39 C40 109(2) . . ? C44 O10 C41 105.4(15) . . ? O10 C41 C42 111.4(16) . . ? C41 C42 C43 102.3(13) . . ? C44 C43 C42 102.1(13) . . ? O10 C44 C43 109.4(16) . . ? 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 O3 Cu1 Cl1 Cu3 -148.86(10) 2_765 . . . ? O1 Cu1 Cl1 Cu3 29.44(10) . . . . ? N1 Cu1 Cl1 Cu3 -55.72(13) . . . . ? N6 Cu1 Cl1 Cu3 124.80(13) . . . . ? O3 Cu1 Cl1 Cu2 -147.97(10) 2_765 . . . ? O1 Cu1 Cl1 Cu2 30.32(10) . . . . ? N1 Cu1 Cl1 Cu2 -54.83(13) . . . . ? N6 Cu1 Cl1 Cu2 125.68(13) . . . . ? O3 Cu3 Cl1 Cu1 -148.57(11) . . . . ? O2 Cu3 Cl1 Cu1 31.54(10) . . . . ? N12 Cu3 Cl1 Cu1 -54.67(13) . . . . ? N7 Cu3 Cl1 Cu1 126.04(13) 2_765 . . . ? O3 Cu3 Cl1 Cu2 -149.46(11) . . . . ? O2 Cu3 Cl1 Cu2 30.65(10) . . . . ? N12 Cu3 Cl1 Cu2 -55.55(13) . . . . ? N7 Cu3 Cl1 Cu2 125.16(13) 2_765 . . . ? O1 Cu2 Cl1 Cu1 -30.68(10) . . . . ? O2 Cu2 Cl1 Cu1 150.02(10) . . . . ? N2 Cu2 Cl1 Cu1 55.35(13) . . . . ? N11 Cu2 Cl1 Cu1 -124.40(13) . . . . ? O1 Cu2 Cl1 Cu3 148.42(10) . . . . ? O2 Cu2 Cl1 Cu3 -30.88(10) . . . . ? N2 Cu2 Cl1 Cu3 -125.55(13) . . . . ? N11 Cu2 Cl1 Cu3 54.69(13) . . . . ? O2 Cu2 O1 Cu1 48.3(6) . . . . ? N2 Cu2 O1 Cu1 -50.12(18) . . . . ? N11 Cu2 O1 Cu1 141.60(18) . . . . ? Cl1 Cu2 O1 Cu1 45.59(13) . . . . ? O3 Cu1 O1 Cu2 -40.1(7) 2_765 . . . ? N1 Cu1 O1 Cu2 50.87(18) . . . . ? N6 Cu1 O1 Cu2 -143.72(18) . . . . ? Cl1 Cu1 O1 Cu2 -47.70(13) . . . . ? O1 Cu2 O2 Cu3 43.6(6) . . . . ? N2 Cu2 O2 Cu3 140.87(18) . . . . ? N11 Cu2 O2 Cu3 -50.80(18) . . . . ? Cl1 Cu2 O2 Cu3 46.26(12) . . . . ? O3 Cu3 O2 Cu2 -48.3(7) . . . . ? N12 Cu3 O2 Cu2 50.73(19) . . . . ? N7 Cu3 O2 Cu2 -143.65(18) 2_765 . . . ? Cl1 Cu3 O2 Cu2 -47.79(13) . . . . ? O2 Cu3 O3 Cu1 -47.9(7) . . . 2_765 ? N12 Cu3 O3 Cu1 -145.96(19) . . . 2_765 ? N7 Cu3 O3 Cu1 48.46(19) 2_765 . . 2_765 ? Cl1 Cu3 O3 Cu1 -48.42(14) . . . 2_765 ? O7 K1 O4 C23 -114.3(5) . . . . ? O7 K1 O4 C23 65.7(5) 2_656 . . . ? O6 K1 O4 C23 149.1(5) 2_656 . . . ? O6 K1 O4 C23 -30.9(5) . . . . ? O5 K1 O4 C23 -16.8(4) . . . . ? O5 K1 O4 C23 163.2(4) 2_656 . . . ? C32B K1 O4 C23 -127.5(5) . . . . ? C32B K1 O4 C23 52.5(5) 2_656 . . . ? O7 K1 O4 C22 116.5(5) . . . . ? O7 K1 O4 C22 -63.5(5) 2_656 . . . ? O6 K1 O4 C22 19.9(5) 2_656 . . . ? O6 K1 O4 C22 -160.1(5) . . . . ? O5 K1 O4 C22 -146.0(5) . . . . ? O5 K1 O4 C22 34.0(5) 2_656 . . . ? C32B K1 O4 C22 103.2(5) . . . . ? C32B K1 O4 C22 -76.8(5) 2_656 . . . ? O7 K1 O5 C24 75.5(5) . . . . ? O7 K1 O5 C24 -104.5(5) 2_656 . . . ? O6 K1 O5 C24 -32.4(5) 2_656 . . . ? O6 K1 O5 C24 147.6(5) . . . . ? O4 K1 O5 C24 161.8(4) 2_656 . . . ? O4 K1 O5 C24 -18.2(4) . . . . ? C32B K1 O5 C24 51.5(5) . . . . ? C32B K1 O5 C24 -128.5(5) 2_656 . . . ? O7 K1 O5 C25 -53.3(5) . . . . ? O7 K1 O5 C25 126.7(5) 2_656 . . . ? O6 K1 O5 C25 -161.2(4) 2_656 . . . ? O6 K1 O5 C25 18.8(4) . . . . ? O4 K1 O5 C25 32.9(5) 2_656 . . . ? O4 K1 O5 C25 -147.1(5) . . . . ? C32B K1 O5 C25 -77.4(5) . . . . ? C32B K1 O5 C25 102.6(5) 2_656 . . . ? O7 K1 O6 C27 -99.2(5) . . . . ? O7 K1 O6 C27 80.8(5) 2_656 . . . ? O4 K1 O6 C27 -13.5(4) 2_656 . . . ? O4 K1 O6 C27 166.5(4) . . . . ? O5 K1 O6 C27 152.5(5) . . . . ? O5 K1 O6 C27 -27.5(5) 2_656 . . . ? C32B K1 O6 C27 -110.1(5) . . . . ? C32B K1 O6 C27 69.9(5) 2_656 . . . ? O7 K1 O6 C26 124.0(5) . . . . ? O7 K1 O6 C26 -56.0(5) 2_656 . . . ? O4 K1 O6 C26 -150.3(5) 2_656 . . . ? O4 K1 O6 C26 29.7(5) . . . . ? O5 K1 O6 C26 15.6(4) . . . . ? O5 K1 O6 C26 -164.4(4) 2_656 . . . ? C32B K1 O6 C26 113.1(5) . . . . ? C32B K1 O6 C26 -66.9(5) 2_656 . . . ? O3 Cu1 N1 C2 -42.2(5) 2_765 . . . ? O1 Cu1 N1 C2 150.6(5) . . . . ? N6 Cu1 N1 C2 53.6(10) . . . . ? Cl1 Cu1 N1 C2 -124.4(5) . . . . ? O3 Cu1 N1 N2 134.1(4) 2_765 . . . ? O1 Cu1 N1 N2 -33.1(4) . . . . ? N6 Cu1 N1 N2 -130.2(7) . . . . ? Cl1 Cu1 N1 N2 51.9(4) . . . . ? C2 N1 N2 C4 -1.3(6) . . . . ? Cu1 N1 N2 C4 -178.4(3) . . . . ? C2 N1 N2 Cu2 179.8(3) . . . . ? Cu1 N1 N2 Cu2 2.7(5) . . . . ? O1 Cu2 N2 C4 -149.1(5) . . . . ? O2 Cu2 N2 C4 45.7(5) . . . . ? N11 Cu2 N2 C4 -52.2(12) . . . . ? Cl1 Cu2 N2 C4 129.0(5) . . . . ? O1 Cu2 N2 N1 29.4(4) . . . . ? O2 Cu2 N2 N1 -135.8(4) . . . . ? N11 Cu2 N2 N1 126.3(9) . . . . ? Cl1 Cu2 N2 N1 -52.5(3) . . . . ? C6 N3 N4 C7 -0.4(7) . . . . ? O3 Cu1 N6 C9 143.6(5) 2_765 . . . ? O1 Cu1 N6 C9 -48.8(5) . . . . ? N1 Cu1 N6 C9 46.9(10) . . . . ? Cl1 Cu1 N6 C9 -135.1(5) . . . . ? O3 Cu1 N6 N7 -27.5(3) 2_765 . . . ? O1 Cu1 N6 N7 140.0(3) . . . . ? N1 Cu1 N6 N7 -124.2(7) . . . . ? Cl1 Cu1 N6 N7 53.8(3) . . . . ? C9 N6 N7 C11 0.2(6) . . . . ? Cu1 N6 N7 C11 173.7(3) . . . . ? C9 N6 N7 Cu3 -176.2(3) . . . 2_765 ? Cu1 N6 N7 Cu3 -2.7(5) . . . 2_765 ? C13 N8 N9 C14 -0.5(8) . . . . ? O1 Cu2 N11 C16 42.9(6) . . . . ? O2 Cu2 N11 C16 -152.0(6) . . . . ? N2 Cu2 N11 C16 -53.2(12) . . . . ? Cl1 Cu2 N11 C16 125.6(6) . . . . ? O1 Cu2 N11 N12 -133.0(4) . . . . ? O2 Cu2 N11 N12 32.1(4) . . . . ? N2 Cu2 N11 N12 130.9(8) . . . . ? Cl1 Cu2 N11 N12 -50.3(4) . . . . ? C16 N11 N12 C18 0.7(6) . . . . ? Cu2 N11 N12 C18 177.7(3) . . . . ? C16 N11 N12 Cu3 -177.8(4) . . . . ? Cu2 N11 N12 Cu3 -0.8(5) . . . . ? O3 Cu3 N12 C18 -42.3(6) . . . . ? O2 Cu3 N12 C18 151.3(6) . . . . ? N7 Cu3 N12 C18 53.3(10) 2_765 . . . ? Cl1 Cu3 N12 C18 -123.9(5) . . . . ? O3 Cu3 N12 N11 135.6(4) . . . . ? O2 Cu3 N12 N11 -30.8(4) . . . . ? N7 Cu3 N12 N11 -128.7(7) 2_765 . . . ? Cl1 Cu3 N12 N11 54.1(4) . . . . ? C20 N13 N14 C21 -2.8(10) . . . . ? N2 N1 C2 C3 1.4(6) . . . . ? Cu1 N1 C2 C3 177.9(4) . . . . ? N2 N1 C2 C1 179.1(5) . . . . ? Cu1 N1 C2 C1 -4.4(8) . . . . ? N1 C2 C3 C4 -1.1(6) . . . . ? C1 C2 C3 C4 -178.6(6) . . . . ? N1 C2 C3 N5 -177.7(5) . . . . ? C1 C2 C3 N5 4.7(9) . . . . ? C6 N5 C3 C4 98.5(8) . . . . ? C7 N5 C3 C4 -94.0(8) . . . . ? C6 N5 C3 C2 -85.5(8) . . . . ? C7 N5 C3 C2 82.0(8) . . . . ? N1 N2 C4 C3 0.6(6) . . . . ? Cu2 N2 C4 C3 179.1(4) . . . . ? N1 N2 C4 C5 -178.1(5) . . . . ? Cu2 N2 C4 C5 0.5(9) . . . . ? C2 C3 C4 N2 0.3(6) . . . . ? N5 C3 C4 N2 176.9(5) . . . . ? C2 C3 C4 C5 178.9(6) . . . . ? N5 C3 C4 C5 -4.5(10) . . . . ? N4 N3 C6 N5 -0.3(7) . . . . ? C7 N5 C6 N3 0.8(7) . . . . ? C3 N5 C6 N3 170.5(5) . . . . ? N3 N4 C7 N5 1.0(7) . . . . ? C6 N5 C7 N4 -1.1(7) . . . . ? C3 N5 C7 N4 -171.1(5) . . . . ? N7 N6 C9 C10 -0.1(6) . . . . ? Cu1 N6 C9 C10 -171.7(4) . . . . ? N7 N6 C9 C8 179.2(5) . . . . ? Cu1 N6 C9 C8 7.6(9) . . . . ? N6 C9 C10 C11 0.1(6) . . . . ? C8 C9 C10 C11 -179.2(6) . . . . ? N6 C9 C10 N10 179.4(5) . . . . ? C8 C9 C10 N10 0.2(10) . . . . ? C14 N10 C10 C11 89.2(8) . . . . ? C13 N10 C10 C11 -83.3(8) . . . . ? C14 N10 C10 C9 -90.0(8) . . . . ? C13 N10 C10 C9 97.5(8) . . . . ? N6 N7 C11 C10 -0.1(6) . . . . ? Cu3 N7 C11 C10 175.3(4) 2_765 . . . ? N6 N7 C11 C12 -178.7(5) . . . . ? Cu3 N7 C11 C12 -3.3(9) 2_765 . . . ? C9 C10 C11 N7 0.0(6) . . . . ? N10 C10 C11 N7 -179.3(5) . . . . ? C9 C10 C11 C12 178.5(6) . . . . ? N10 C10 C11 C12 -0.9(10) . . . . ? N9 N8 C13 N10 0.5(8) . . . . ? C14 N10 C13 N8 -0.3(8) . . . . ? C10 N10 C13 N8 173.7(6) . . . . ? N8 N9 C14 N10 0.3(9) . . . . ? C13 N10 C14 N9 -0.1(8) . . . . ? C10 N10 C14 N9 -173.9(6) . . . . ? N12 N11 C16 C17 -0.5(6) . . . . ? Cu2 N11 C16 C17 -176.6(4) . . . . ? N12 N11 C16 C15 -179.6(5) . . . . ? Cu2 N11 C16 C15 4.3(9) . . . . ? N11 C16 C17 C18 0.0(7) . . . . ? C15 C16 C17 C18 179.1(6) . . . . ? N11 C16 C17 N15 177.2(5) . . . . ? C15 C16 C17 N15 -3.7(10) . . . . ? C20 N15 C17 C18 79.4(10) . . . . ? C21 N15 C17 C18 -101.2(9) . . . . ? C20 N15 C17 C16 -97.2(9) . . . . ? C21 N15 C17 C16 82.2(9) . . . . ? N11 N12 C18 C17 -0.7(6) . . . . ? Cu3 N12 C18 C17 177.4(4) . . . . ? N11 N12 C18 C19 -179.0(5) . . . . ? Cu3 N12 C18 C19 -0.9(9) . . . . ? C16 C17 C18 N12 0.4(6) . . . . ? N15 C17 C18 N12 -176.8(5) . . . . ? C16 C17 C18 C19 178.6(6) . . . . ? N15 C17 C18 C19 1.5(10) . . . . ? N14 N13 C20 N15 4.0(12) . . . . ? C21 N15 C20 N13 -3.4(11) . . . . ? C17 N15 C20 N13 176.1(7) . . . . ? N13 N14 C21 N15 0.7(10) . . . . ? C20 N15 C21 N14 1.6(10) . . . . ? C17 N15 C21 N14 -177.9(6) . . . . ? C23 O4 C22 C27 -180.0(7) . . . 2_656 ? K1 O4 C22 C27 -51.1(7) . . . 2_656 ? C22 O4 C23 C24 178.0(6) . . . . ? K1 O4 C23 C24 50.3(7) . . . . ? C25 O5 C24 C23 179.0(6) . . . . ? K1 O5 C24 C23 50.0(7) . . . . ? O4 C23 C24 O5 -68.3(8) . . . . ? C24 O5 C25 C26 179.7(6) . . . . ? K1 O5 C25 C26 -50.7(7) . . . . ? C27 O6 C26 C25 173.9(6) . . . . ? K1 O6 C26 C25 -47.7(7) . . . . ? O5 C25 C26 O6 65.5(8) . . . . ? C26 O6 C27 C22 -176.7(6) . . . 2_656 ? K1 O6 C27 C22 44.7(7) . . . 2_656 ? O6 K1 O7 C32B 27.5(9) 2_656 . . . ? O6 K1 O7 C32B -152.5(9) . . . . ? O4 K1 O7 C32B 145.8(9) 2_656 . . . ? O4 K1 O7 C32B -34.2(9) . . . . ? O5 K1 O7 C32B -95.3(9) . . . . ? O5 K1 O7 C32B 84.7(9) 2_656 . . . ? O6 K1 O7 C32A -24.0(12) 2_656 . . . ? O6 K1 O7 C32A 156.0(12) . . . . ? O4 K1 O7 C32A 94.3(12) 2_656 . . . ? O4 K1 O7 C32A -85.7(12) . . . . ? O5 K1 O7 C32A -146.8(12) . . . . ? O5 K1 O7 C32A 33.2(12) 2_656 . . . ? O6 K1 O7 C29 146.1(7) 2_656 . . . ? O6 K1 O7 C29 -33.9(7) . . . . ? O4 K1 O7 C29 -95.7(8) 2_656 . . . ? O4 K1 O7 C29 84.3(8) . . . . ? O5 K1 O7 C29 23.2(8) . . . . ? O5 K1 O7 C29 -156.8(8) 2_656 . . . ? K1 O7 C29 C30 -160.3(7) . . . . ? O7 C29 C30 C31A -9.9(16) . . . . ? O7 C29 C30 C31B 46.9(13) . . . . ? C29 C30 C31A C32A 6(2) . . . . ? C29 C30 C31B C32B -40.5(17) . . . . ? C29 O7 C32A C31A -7.7(19) . . . . ? K1 O7 C32A C31A 163.0(12) . . . . ? C30 C31A C32A O7 1(2) . . . . ? C30 C31A C32A C31B 60.2(13) . . . . ? C30 C31B C32B O7 17(2) . . . . ? C36 O8 C33 C34 30.2(12) . . . . ? O8 C33 C34 C35 -23.9(13) . . . . ? C33 C34 C35 C36 10.4(13) . . . . ? C33 O8 C36 C35 -23.2(10) . . . . ? C34 C35 C36 O8 8.0(11) . . . . ? C40 O9 C37 C38 -37(3) . . . . ? O9 C37 C38 C39 17(3) . . . . ? C37 C38 C39 C40 3(4) . . . . ? C37 O9 C40 C39 38(3) . . . . ? C38 C39 C40 O9 -23(3) . . . . ? C44 O10 C41 C42 -23(2) . . . . ? O10 C41 C42 C43 6(3) . . . . ? C41 C42 C43 C44 12(2) . . . . ? C41 O10 C44 C43 32(2) . . . . ? C42 C43 C44 O10 -28(2) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.866 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.103 #============================================================================== data_(3) _database_code_depnum_ccdc_archive 'CCDC 796880' #TrackingRef '- Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cadmium(II) Tetrachlorocadmato(II)-hexakis-[\m-(4-(1,2,4-triazol-4-yl)- 3,5-dimethylpyrazolato]-hexa-\m-hydroxido-hexacopper(II) Solvate 13 Ethanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H132 Cd2 Cl4 Cu6 N30 O19' _chemical_formula_weight 2421.88 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 205 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' 'y, z, x' '-z+1/2, -x, y+1/2' '-y, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y' '-y+1/2, -z, x+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-z, -x, -y' '-y, -z, -x' 'z-1/2, x, -y-1/2' 'y, -z-1/2, x-1/2' '-z-1/2, x-1/2, y' 'y-1/2, z, -x-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' _cell_length_a 22.6467(10) _cell_length_b 22.6467(10) _cell_length_c 22.6467(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11614.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 31909 _cell_measurement_theta_min 5.04 _cell_measurement_theta_max 25.07 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4960 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7012 _exptl_absorpt_correction_T_max 0.7626 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 31909 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.04 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3333 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT (Bruker, 1998)' _computing_cell_refinement 'SAINT-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _refine_special_details ; [CdCl4 Cu6(OH)6(pztr)6]2- moiety has centrosymmetric structure and is situated over -3 axis. Therefore, only 1/6 of the molecule is independent. Due to the centrosymmetric structure of this host-guest complex, the incorporated CdCl42- anion is equally disordered over two positions (one guest anion per two cages). Atoms of the tetrachlorocadmate were refined anisotropically without any restraints. Another cage of the "metallacontainer" is populated with ethanol molecule (two other ethanol molecules are located in the framework voids amounting a total solvate composition 13EtOH per single [CdCl4 Cu6(OH)6(pztr)6]2-). This ethanol molecule is disordered by symmetry over three position (3 axis) and considering the 50/50 disorder of the guests (CdCl42-/EtOH), atoms of this ethanol were refined with partial contribution factors 1/6. The bond lengths were restrained (0.01 A) and hydrogen atoms were not added. One of two solvate ethanol molecules was refined isotropically. Second EtOH molecule exhibits complicated disorder over several positions, which cannot be satisfactorily resolved. Therefore, in the final refinement, the contribution from this moiety was modeled using SQUEEZE routine implemented in the PLATON program (A.L. Spek, PLATON, University of Utrecht, The Netherlands, 2001.). In addition, very high anisotropy for thermal motion of the triazole ring atoms also indicated possible disorder. The refined model in depicted in Figure S2: two contributions of the disorder are related as rotation around N5---N3 axis. Thus N3 and N5 atoms of the ring are orderd, while other three atoms are equally disordered over two positions (C6 and C6A; C7 and C7A; N4 and N4A, N4---N4A 0.74 A). Soft geometry restraints for geometry of triazole ring were applied (DFIX/FLAT) and the H atoms were added with partial occupancy factors 0.5 (Uiso = 1.5Ueq(C). Methyl CH hydrogen atoms were placed in calculated positions and refined within a riding model, with Uiso = 1.5Ueq of the carrier atom. 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^)+(0.1152P)^2^+5.8590P] 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_number_reflns 3333 _refine_ls_number_parameters 197 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1859 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _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 0.00213(3) 0.09624(3) 0.90254(3) 0.0359(3) Uani 1 1 d . . . Cd1 Cd 0.0000 0.0000 0.5000 0.0259(3) Uani 1 6 d S . . Cd2 Cd -0.07944(6) -0.07944(6) 0.92056(6) 0.0860(7) Uani 0.50 3 d SP . . Cl1 Cl -0.01139(16) -0.01139(16) 0.98861(16) 0.0596(19) Uani 0.50 3 d SP . . Cl2 Cl -0.1376(3) -0.0223(2) 0.8552(3) 0.1034(16) Uani 0.50 1 d P . . O3 O 0.1117(11) 0.1124(11) 1.0326(9) 0.039(5) Uiso 0.17 1 d PDU . . C10 C 0.1229(14) 0.112(3) 1.0929(9) 0.059(8) Uiso 0.17 1 d PDU . . C11 C 0.077(2) 0.091(2) 1.1375(13) 0.073(10) Uiso 0.17 1 d PDU . . O1 O -0.08294(18) 0.09280(19) 0.91384(18) 0.0446(10) Uani 1 1 d . . . H1W H -0.0967 0.0600 0.9002 0.067 Uiso 1 1 d . . . N1 N 0.0039(2) 0.0434(2) 0.8345(2) 0.0434(12) Uani 1 1 d . . . N2 N 0.0449(2) -0.0012(2) 0.8349(2) 0.0434(12) Uani 1 1 d . . . C1 C -0.0738(4) 0.0820(4) 0.7663(3) 0.072(2) Uani 1 1 d . . . H1A H -0.1044 0.0809 0.7963 0.109 Uiso 1 1 calc R . . H1B H -0.0903 0.0704 0.7286 0.109 Uiso 1 1 calc R . . H1C H -0.0580 0.1217 0.7634 0.109 Uiso 1 1 calc R . . C2 C -0.0260(3) 0.0408(3) 0.7826(3) 0.0483(15) Uani 1 1 d . . . C3 C -0.0033(3) -0.0063(3) 0.7512(3) 0.0485(16) Uani 1 1 d . A . C4 C 0.0414(3) -0.0310(3) 0.7841(3) 0.0452(14) Uani 1 1 d . . . C5 C 0.0807(4) -0.0823(4) 0.7701(3) 0.072(2) Uani 1 1 d . . . H5A H 0.1215 -0.0714 0.7775 0.108 Uiso 1 1 calc R . . H5B H 0.0761 -0.0931 0.7290 0.108 Uiso 1 1 calc R . . H5C H 0.0701 -0.1156 0.7950 0.108 Uiso 1 1 calc R . . O2 O -0.1349(6) 0.1979(6) 0.8619(6) 0.182(4) Uiso 1 1 d . . . H2W H -0.1198 0.1657 0.8790 0.273 Uiso 1 1 d . . . C8 C -0.1030(14) 0.2503(16) 0.8808(15) 0.235(11) Uiso 1 1 d . . . H8A H -0.1112 0.2563 0.9229 0.282 Uiso 1 1 calc R . . H8B H -0.0607 0.2420 0.8772 0.282 Uiso 1 1 calc R . . C9 C -0.1142(17) 0.3026(18) 0.8520(18) 0.290(15) Uiso 1 1 d . . . H9A H -0.0887 0.3333 0.8676 0.435 Uiso 1 1 calc R . . H9B H -0.1552 0.3137 0.8580 0.435 Uiso 1 1 calc R . . H9C H -0.1067 0.2977 0.8101 0.435 Uiso 1 1 calc R . . N3 N -0.0248(2) -0.0225(2) 0.59695(19) 0.0442(12) Uani 1 1 d D . . N5 N -0.0208(2) -0.0218(2) 0.69224(18) 0.0458(12) Uani 1 1 d D . . N4 N -0.0575(7) -0.0726(7) 0.6175(7) 0.060(4) Uani 0.50 1 d PDU A -1 C6 C -0.0036(4) 0.0068(4) 0.6422(4) 0.033(3) Uani 0.50 1 d PD A -1 H6 H 0.0193 0.0414 0.6405 0.040 Uiso 0.50 1 calc PR A -1 C7 C -0.0530(7) -0.0693(8) 0.6746(8) 0.063(4) Uani 0.50 1 d PDU A -1 H7 H -0.0700 -0.0967 0.7008 0.076 Uiso 0.50 1 calc PR A -1 N4A N -0.0768(8) -0.0461(7) 0.6178(8) 0.062(4) Uani 0.50 1 d PDU A -2 C6A C 0.0093(4) -0.0078(4) 0.6418(4) 0.039(4) Uani 0.50 1 d PD A -2 H6A H 0.0471 0.0092 0.6396 0.047 Uiso 0.50 1 calc PR A -2 C7A C -0.0732(10) -0.0451(7) 0.6767(10) 0.066(4) Uani 0.50 1 d PDU A -2 H7A H -0.1025 -0.0584 0.7030 0.079 Uiso 0.50 1 calc PR A -2 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 0.0387(4) 0.0344(4) 0.0347(4) -0.0033(3) -0.0019(3) -0.0023(3) Cd1 0.0259(3) 0.0259(3) 0.0259(3) 0.00011(19) -0.00011(19) -0.00011(19) Cd2 0.0860(7) 0.0860(7) 0.0860(7) -0.0095(7) -0.0095(7) -0.0095(7) Cl1 0.0596(19) 0.0596(19) 0.0596(19) 0.014(2) 0.014(2) 0.014(2) Cl2 0.107(4) 0.075(3) 0.128(5) -0.008(3) -0.014(4) -0.008(3) O1 0.040(2) 0.054(2) 0.040(2) -0.0061(19) -0.0043(17) -0.0008(19) N1 0.048(3) 0.047(3) 0.035(3) 0.001(2) -0.011(2) 0.005(2) N2 0.053(3) 0.044(3) 0.033(3) -0.002(2) -0.001(2) 0.006(2) C1 0.094(6) 0.072(5) 0.052(4) 0.004(4) -0.022(4) 0.021(4) C2 0.052(4) 0.061(4) 0.031(3) 0.001(3) -0.008(3) -0.003(3) C3 0.058(4) 0.065(4) 0.022(3) -0.007(3) 0.000(3) 0.000(3) C4 0.059(4) 0.048(3) 0.029(3) -0.005(3) 0.004(3) 0.002(3) C5 0.079(5) 0.094(6) 0.043(4) -0.024(4) -0.008(4) 0.030(5) N3 0.047(3) 0.057(3) 0.029(2) -0.001(2) -0.001(2) -0.010(2) N5 0.056(3) 0.060(3) 0.021(2) 0.000(2) -0.003(2) -0.009(3) N4 0.083(12) 0.076(11) 0.021(4) -0.001(7) 0.008(6) -0.043(8) C6 0.041(8) 0.037(7) 0.023(7) 0.000(5) 0.001(5) 0.008(6) C7 0.085(12) 0.078(11) 0.025(5) -0.004(7) 0.010(7) -0.044(8) N4A 0.068(10) 0.085(12) 0.034(5) 0.003(8) 0.002(6) -0.029(8) C6A 0.038(8) 0.035(8) 0.044(9) -0.014(6) -0.001(6) 0.010(6) C7A 0.073(10) 0.086(12) 0.039(6) 0.005(8) 0.001(7) -0.028(8) _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 O1 1.930(4) 17_656 ? Cu1 O1 1.945(4) . ? Cu1 N1 1.952(5) . ? Cu1 N2 1.963(5) 18_566 ? Cu1 Cl1 3.1359(12) . ? Cd1 N3 2.323(5) 19_556 ? Cd1 N3 2.323(5) 8_545 ? Cd1 N3 2.323(5) . ? Cd1 N3 2.323(5) 20_566 ? Cd1 N3 2.323(5) 13_556 ? Cd1 N3 2.323(5) 7 ? Cd2 Cl2 2.367(7) 6_546 ? Cd2 Cl2 2.367(7) 5_456 ? Cd2 Cl2 2.367(7) . ? Cd2 Cl1 2.669(7) . ? O3 C10 1.388(10) . ? C10 C11 1.525(10) . ? O1 Cu1 1.930(4) 18_566 ? O1 H1W 0.8628 . ? N1 C2 1.357(8) . ? N1 N2 1.370(7) . ? N2 C4 1.337(8) . ? N2 Cu1 1.963(5) 17_656 ? C1 C2 1.474(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.382(9) . ? C3 C4 1.376(9) . ? C3 N5 1.436(7) . ? C4 C5 1.497(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? O2 C8 1.45(3) . ? O2 H2W 0.8923 . ? C8 C9 1.38(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? N3 C6 1.312(9) . ? N3 C6A 1.318(9) . ? N3 N4A 1.38(2) . ? N3 N4 1.434(18) . ? N5 C7A 1.34(2) . ? N5 C7 1.36(2) . ? N5 C6 1.363(9) . ? N5 C6A 1.368(9) . ? N4 C7 1.300(19) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? N4A C7A 1.34(2) . ? C6A H6A 0.9400 . ? C7A H7A 0.9400 . ? 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 O1 Cu1 O1 164.5(2) 17_656 . ? O1 Cu1 N1 85.84(19) 17_656 . ? O1 Cu1 N1 95.71(19) . . ? O1 Cu1 N2 95.84(19) 17_656 18_566 ? O1 Cu1 N2 86.61(19) . 18_566 ? N1 Cu1 N2 165.2(2) . 18_566 ? O1 Cu1 Cl1 86.62(14) 17_656 . ? O1 Cu1 Cl1 77.90(15) . . ? N1 Cu1 Cl1 90.93(18) . . ? N2 Cu1 Cl1 103.84(18) 18_566 . ? N3 Cd1 N3 88.19(19) 19_556 8_545 ? N3 Cd1 N3 88.19(18) 19_556 . ? N3 Cd1 N3 91.81(19) 8_545 . ? N3 Cd1 N3 91.81(19) 19_556 20_566 ? N3 Cd1 N3 180.0 8_545 20_566 ? N3 Cd1 N3 88.19(19) . 20_566 ? N3 Cd1 N3 91.81(19) 19_556 13_556 ? N3 Cd1 N3 88.19(19) 8_545 13_556 ? N3 Cd1 N3 180.0 . 13_556 ? N3 Cd1 N3 91.81(18) 20_566 13_556 ? N3 Cd1 N3 180.0(3) 19_556 7 ? N3 Cd1 N3 91.81(18) 8_545 7 ? N3 Cd1 N3 91.81(19) . 7 ? N3 Cd1 N3 88.19(19) 20_566 7 ? N3 Cd1 N3 88.19(19) 13_556 7 ? Cl2 Cd2 Cl2 107.32(15) 6_546 . ? Cl2 Cd2 Cl2 107.32(15) 5_456 . ? Cl2 Cd2 Cl1 111.55(14) 6_546 . ? Cl2 Cd2 Cl1 111.55(14) 5_456 . ? Cl2 Cd2 Cl1 111.55(14) . . ? Cl1 Cl1 Cd2 180.0(14) 13_557 . ? Cl1 Cl1 Cu1 81.59(12) 13_557 . ? Cd2 Cl1 Cu1 98.41(12) . . ? O3 C10 C11 121.9(13) . . ? Cu1 O1 Cu1 106.4(2) 18_566 . ? Cu1 O1 H1W 110.1 18_566 . ? Cu1 O1 H1W 110.2 . . ? C2 N1 N2 108.2(5) . . ? C2 N1 Cu1 134.4(5) . . ? N2 N1 Cu1 117.4(3) . . ? C4 N2 N1 109.0(5) . . ? C4 N2 Cu1 135.6(4) . 17_656 ? N1 N2 Cu1 115.1(3) . 17_656 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.0(6) . . ? N1 C2 C1 123.8(6) . . ? C3 C2 C1 129.2(6) . . ? C4 C3 C2 108.0(5) . . ? C4 C3 N5 127.3(6) . . ? C2 C3 N5 124.4(6) . . ? N2 C4 C3 107.7(6) . . ? N2 C4 C5 122.6(6) . . ? C3 C4 C5 129.8(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C8 O2 H2W 110.3 . . ? C9 C8 O2 118(3) . . ? C9 C8 H8A 107.8 . . ? O2 C8 H8A 107.8 . . ? C9 C8 H8B 107.8 . . ? O2 C8 H8B 107.8 . . ? H8A C8 H8B 107.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 N3 N4A 104.0(9) . . ? C6A N3 N4A 109.5(10) . . ? C6 N3 N4 109.6(9) . . ? C6A N3 N4 104.6(8) . . ? C6 N3 Cd1 122.6(5) . . ? C6A N3 Cd1 122.1(5) . . ? N4A N3 Cd1 128.0(8) . . ? N4 N3 Cd1 127.2(7) . . ? C7A N5 C6 102.8(10) . . ? C7 N5 C6 106.6(10) . . ? C7A N5 C6A 108.3(11) . . ? C7 N5 C6A 101.9(9) . . ? C7A N5 C3 125.6(10) . . ? C7 N5 C3 128.0(9) . . ? C6 N5 C3 125.2(6) . . ? C6A N5 C3 125.5(6) . . ? C7 N4 N3 103.7(12) . . ? N3 C6 N5 107.7(8) . . ? N3 C6 H6 126.2 . . ? N5 C6 H6 126.2 . . ? N4 C7 N5 112.4(13) . . ? N4 C7 H7 123.8 . . ? N5 C7 H7 123.8 . . ? C7A N4A N3 106.5(13) . . ? N3 C6A N5 107.0(8) . . ? N3 C6A H6A 126.5 . . ? N5 C6A H6A 126.5 . . ? N4A C7A N5 108.7(15) . . ? N4A C7A H7A 125.7 . . ? N5 C7A H7A 125.7 . . ? 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 C10 Cd2 Cl1 Cu1 110(7) 17_656 . . . ? C10 Cd2 Cl1 Cu1 -130(7) 13_557 . . . ? C10 Cd2 Cl1 Cu1 -10(7) 18_566 . . . ? C11 Cd2 Cl1 Cu1 162(3) 18_566 . . . ? C11 Cd2 Cl1 Cu1 42(3) 13_557 . . . ? C11 Cd2 Cl1 Cu1 -78(3) 17_656 . . . ? O3 Cd2 Cl1 Cu1 88.6(9) 17_656 . . . ? O3 Cd2 Cl1 Cu1 -151.4(9) 13_557 . . . ? O3 Cd2 Cl1 Cu1 -31.4(9) 18_566 . . . ? Cl2 Cd2 Cl1 Cu1 92.06(17) 6_546 . . . ? Cl2 Cd2 Cl1 Cu1 -147.94(17) 5_456 . . . ? Cl2 Cd2 Cl1 Cu1 -27.94(17) . . . . ? O1 Cu1 Cl1 Cl1 58.26(12) 17_656 . . 13_557 ? O1 Cu1 Cl1 Cl1 -120.33(12) . . . 13_557 ? N1 Cu1 Cl1 Cl1 144.03(15) . . . 13_557 ? N2 Cu1 Cl1 Cl1 -36.93(15) 18_566 . . 13_557 ? O1 Cu1 Cl1 Cd2 -121.74(12) 17_656 . . . ? O1 Cu1 Cl1 Cd2 59.67(12) . . . . ? N1 Cu1 Cl1 Cd2 -35.97(15) . . . . ? N2 Cu1 Cl1 Cd2 143.07(15) 18_566 . . . ? O1 Cu1 O1 Cu1 50.6(4) 17_656 . . 18_566 ? N1 Cu1 O1 Cu1 145.6(2) . . . 18_566 ? N2 Cu1 O1 Cu1 -49.1(2) 18_566 . . 18_566 ? Cl1 Cu1 O1 Cu1 55.8(2) . . . 18_566 ? O1 Cu1 N1 C2 -144.9(6) 17_656 . . . ? O1 Cu1 N1 C2 50.6(6) . . . . ? N2 Cu1 N1 C2 -47.8(12) 18_566 . . . ? Cl1 Cu1 N1 C2 128.5(6) . . . . ? O1 Cu1 N1 N2 32.2(4) 17_656 . . . ? O1 Cu1 N1 N2 -132.3(4) . . . . ? N2 Cu1 N1 N2 129.3(6) 18_566 . . . ? Cl1 Cu1 N1 N2 -54.3(4) . . . . ? C2 N1 N2 C4 0.6(7) . . . . ? Cu1 N1 N2 C4 -177.3(4) . . . . ? C2 N1 N2 Cu1 175.6(4) . . . 17_656 ? Cu1 N1 N2 Cu1 -2.2(5) . . . 17_656 ? N2 N1 C2 C3 0.5(7) . . . . ? Cu1 N1 C2 C3 177.9(5) . . . . ? N2 N1 C2 C1 180.0(7) . . . . ? Cu1 N1 C2 C1 -2.7(11) . . . . ? N1 C2 C3 C4 -1.4(8) . . . . ? C1 C2 C3 C4 179.2(8) . . . . ? N1 C2 C3 N5 -176.2(6) . . . . ? C1 C2 C3 N5 4.4(12) . . . . ? N1 N2 C4 C3 -1.4(7) . . . . ? Cu1 N2 C4 C3 -175.0(5) 17_656 . . . ? N1 N2 C4 C5 179.4(7) . . . . ? Cu1 N2 C4 C5 5.8(11) 17_656 . . . ? C2 C3 C4 N2 1.8(8) . . . . ? N5 C3 C4 N2 176.4(6) . . . . ? C2 C3 C4 C5 -179.2(8) . . . . ? N5 C3 C4 C5 -4.5(12) . . . . ? N3 Cd1 N3 C6 63.4(5) 19_556 . . . ? N3 Cd1 N3 C6 -24.8(5) 8_545 . . . ? N3 Cd1 N3 C6 155.2(5) 20_566 . . . ? N3 Cd1 N3 C6 -116.6(5) 7 . . . ? N3 Cd1 N3 C6A 40.5(5) 19_556 . . . ? N3 Cd1 N3 C6A -47.7(5) 8_545 . . . ? N3 Cd1 N3 C6A 132.3(5) 20_566 . . . ? N3 Cd1 N3 C6A -139.5(5) 7 . . . ? N3 Cd1 N3 N4A 125.1(7) 8_545 . . . ? N3 Cd1 N3 N4A -54.9(7) 20_566 . . . ? N3 Cd1 N3 N4A 50.9(8) 13_556 . . . ? N3 Cd1 N3 N4A 33.2(8) 7 . . . ? N3 Cd1 N3 N4 -108.0(8) 19_556 . . . ? N3 Cd1 N3 N4 163.9(8) 8_545 . . . ? N3 Cd1 N3 N4 -16.1(8) 20_566 . . . ? N3 Cd1 N3 N4 72.0(8) 7 . . . ? C4 C3 N5 C7A 115.4(10) . . . . ? C2 C3 N5 C7A -70.8(10) . . . . ? C4 C3 N5 C7 76.9(11) . . . . ? C2 C3 N5 C7 -109.3(10) . . . . ? C4 C3 N5 C6 -97.5(9) . . . . ? C2 C3 N5 C6 76.4(9) . . . . ? C4 C3 N5 C6A -74.6(9) . . . . ? C2 C3 N5 C6A 99.2(8) . . . . ? C6 N3 N4 C7 -0.2(2) . . . . ? C6A N3 N4 C7 19.3(4) . . . . ? Cd1 N3 N4 C7 172.0(5) . . . . ? C6A N3 C6 N5 -78(2) . . . . ? N4A N3 C6 N5 31.5(6) . . . . ? N4 N3 C6 N5 0.12(13) . . . . ? Cd1 N3 C6 N5 -172.6(4) . . . . ? C7A N5 C6 N3 -31.5(6) . . . . ? C7 N5 C6 N3 0.04(13) . . . . ? C6A N5 C6 N3 78(2) . . . . ? C3 N5 C6 N3 175.4(6) . . . . ? N3 N4 C7 N5 0.3(3) . . . . ? C6 N5 C7 N4 -0.2(3) . . . . ? C6A N5 C7 N4 -18.8(4) . . . . ? C3 N5 C7 N4 -175.4(7) . . . . ? C6 N3 N4A C7A -19.1(4) . . . . ? C6A N3 N4A C7A 0.2(3) . . . . ? Cd1 N3 N4A C7A -173.3(5) . . . . ? C6 N3 C6A N5 76(2) . . . . ? N4A N3 C6A N5 -0.12(13) . . . . ? N4 N3 C6A N5 -31.7(5) . . . . ? Cd1 N3 C6A N5 173.8(4) . . . . ? C7A N5 C6A N3 0.00(13) . . . . ? C7 N5 C6A N3 31.2(6) . . . . ? C6 N5 C6A N3 -76(2) . . . . ? C3 N5 C6A N3 -171.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.568 _refine_diff_density_min -1.438 _refine_diff_density_rms 0.100 # ------------- END of CIF -----------------#