Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J. Chem. Soc. Dalton' loop_ _publ_author_name 'Corbella, Montserrat' 'Llobet, Antoni' 'Martell, Arthur' 'Muller, Peter' 'Reibenspies, Joseph' 'Rodriguez, Montserrat' 'Uson, Miguel Angel' _publ_contact_author_name 'Prof. Antoni Llobet' _publ_contact_author_address ; Departament de Quimica Universitat de Girona Campus Montilivi E-17071 Girona. Spain ; _publ_contact_author_email 'antoni.llobet@udg.es ' _publ_section_title ; Solvent controlled complex nuclearity in Cu(II) complexes linked by the CO3 2- ligand: synthesis, structure and magnetic properties. ; data_m-te _database_code_CSD 167772 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu4(m4-CO3)(m-Cl)2(ClO4)2(dpt)4(OH2)](ClO4)2.3CH3OH' _chemical_formula_sum 'C28 H80 Cl6 Cu4 N12 O22' _chemical_formula_weight 1403.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.798(3) _cell_length_b 17.105(3) _cell_length_c 25.802(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.02(3) _cell_angle_gamma 90.00 _cell_volume 5617(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 1.859 _exptl_absorpt_correction_type 'multi-scan, semiempirical (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe Siemens-Huber four circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean '8192 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9571 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9571 _reflns_number_gt 7740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (V. 4.202, Siemens 1996)' _computing_cell_refinement 'Siemens SAINT (V. 5.00, Siemens 1998)' _computing_data_reduction 'Siemens SAINT (V. 5.00, Siemens 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Bruker)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+15.0174P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9571 _refine_ls_number_parameters 737 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 0.37922(8) 0.19098(6) 0.55573(4) 0.0242(2) Uani 1 d . . . O31 O 0.3959(3) 0.1550(2) 0.60604(11) 0.0395(8) Uani 1 d . . . O32 O 0.3242(3) 0.26342(19) 0.55875(13) 0.0381(8) Uani 1 d . . . O33 O 0.3169(3) 0.1386(2) 0.52114(13) 0.0444(9) Uani 1 d . . . O34 O 0.4769(3) 0.2049(2) 0.53587(14) 0.0480(10) Uani 1 d . . . Cl4 Cl 0.11082(9) 0.29612(6) 0.17925(4) 0.0279(3) Uani 1 d . . . O41 O 0.1621(3) 0.2972(2) 0.13322(12) 0.0422(9) Uani 1 d . . . O42 O 0.0957(3) 0.21632(19) 0.19489(14) 0.0444(9) Uani 1 d . . . O43 O 0.1747(4) 0.3344(2) 0.22044(13) 0.0617(12) Uani 1 d . . . O44 O 0.0126(3) 0.3354(3) 0.17101(16) 0.0630(12) Uani 1 d . . . Cl5 Cl 0.39159(11) 0.53741(7) 0.40672(4) 0.0355(3) Uani 1 d . . . O51 O 0.3677(3) 0.45411(17) 0.40249(12) 0.0321(8) Uani 1 d . . . O52 O 0.4881(5) 0.5493(3) 0.4341(3) 0.132(3) Uani 1 d . . . O53 O 0.3106(6) 0.5719(3) 0.4324(2) 0.119(2) Uani 1 d . . . O54 O 0.3858(4) 0.5697(2) 0.35641(15) 0.0669(13) Uani 1 d . . . Cl6 Cl -0.17315(9) 0.52885(7) 0.14410(4) 0.0305(3) Uani 1 d . . . O62 O -0.1858(4) 0.5031(2) 0.09130(13) 0.0577(11) Uani 1 d . . . O61 O -0.1995(3) 0.6115(2) 0.14395(13) 0.0467(9) Uani 1 d . . . O63 O -0.2422(5) 0.4894(3) 0.17322(17) 0.0958(19) Uani 1 d . . . O64 O -0.0687(4) 0.5235(4) 0.1669(2) 0.109(2) Uani 1 d . . . O7 O 0.2546(3) -0.1573(2) 0.43984(14) 0.0545(11) Uani 1 d . . . H7 H 0.2411 -0.1111 0.4302 0.082 Uiso 1 calc R . . C7 C 0.2576(5) -0.2053(4) 0.3960(2) 0.0668(19) Uani 1 d . . . H7A H 0.1974 -0.1934 0.3705 0.100 Uiso 1 calc R . . H7B H 0.2546 -0.2602 0.4065 0.100 Uiso 1 calc R . . H7C H 0.3230 -0.1958 0.3803 0.100 Uiso 1 calc R . . O8 O 0.2599(3) 0.49442(19) 0.23530(12) 0.0372(8) Uani 1 d . . . H8 H 0.2428 0.4760 0.2054 0.056 Uiso 1 calc R . . C8 C 0.3057(4) 0.5695(3) 0.2308(2) 0.0434(13) Uani 1 d . . . H8A H 0.3024 0.5985 0.2633 0.065 Uiso 1 calc R . . H8B H 0.2671 0.5981 0.2020 0.065 Uiso 1 calc R . . H8C H 0.3792 0.5636 0.2240 0.065 Uiso 1 calc R . . O9 O 0.2391(3) 0.4679(2) 0.13155(14) 0.0529(10) Uani 1 d . . . H9 H 0.2467 0.4201 0.1253 0.079 Uiso 1 calc R . . C9 C 0.1410(5) 0.4920(3) 0.1103(2) 0.0521(15) Uani 1 d . . . H9A H 0.1270 0.5446 0.1230 0.078 Uiso 1 calc R . . H9B H 0.0877 0.4557 0.1206 0.078 Uiso 1 calc R . . H9C H 0.1387 0.4929 0.0722 0.078 Uiso 1 calc R . . C1A C 0.3512(4) 0.1160(3) 0.23261(17) 0.0293(10) Uani 1 d . . . H1AA H 0.2976 0.0746 0.2257 0.035 Uiso 1 calc R A 1 H1AB H 0.4140 0.0925 0.2523 0.035 Uiso 1 calc R A 1 C1B C 0.3805(4) 0.1486(3) 0.18151(17) 0.0303(11) Uani 1 d . . . H1BA H 0.3968 0.1046 0.1588 0.036 Uiso 1 calc R . . H1BB H 0.3192 0.1768 0.1639 0.036 Uiso 1 calc R . . C1C C 0.4736(4) 0.2035(3) 0.18780(16) 0.0269(10) Uani 1 d . . . H1CA H 0.5312 0.1782 0.2103 0.032 Uiso 1 calc R B 1 H1CB H 0.4986 0.2122 0.1532 0.032 Uiso 1 calc R B 1 C1D C 0.5451(3) 0.3305(3) 0.20934(17) 0.0269(10) Uani 1 d . . . H1DA H 0.5672 0.3290 0.1737 0.032 Uiso 1 calc R C 1 H1DB H 0.6029 0.3080 0.2333 0.032 Uiso 1 calc R C 1 C1E C 0.5293(4) 0.4153(3) 0.22445(17) 0.0280(10) Uani 1 d . . . H1EA H 0.5902 0.4464 0.2156 0.034 Uiso 1 calc R . . H1EB H 0.4659 0.4359 0.2036 0.034 Uiso 1 calc R . . C1F C 0.5171(4) 0.4261(3) 0.28154(17) 0.0321(11) Uani 1 d . . . H1FA H 0.5770 0.4014 0.3028 0.039 Uiso 1 calc R D 1 H1FB H 0.5173 0.4826 0.2900 0.039 Uiso 1 calc R D 1 C2A C 0.4864(4) 0.0463(2) 0.41174(18) 0.0304(11) Uani 1 d . . . H2AA H 0.5058 0.0446 0.3756 0.036 Uiso 1 calc R E 1 H2AB H 0.4433 -0.0004 0.4173 0.036 Uiso 1 calc R E 1 C2B C 0.5848(4) 0.0451(3) 0.4496(2) 0.0373(12) Uani 1 d . . . H2BA H 0.6176 -0.0072 0.4486 0.045 Uiso 1 calc R . . H2BB H 0.5650 0.0533 0.4853 0.045 Uiso 1 calc R . . C2C C 0.6650(4) 0.1062(3) 0.43860(19) 0.0321(11) Uani 1 d . . . H2CA H 0.7333 0.0928 0.4583 0.039 Uiso 1 calc R F 1 H2CB H 0.6746 0.1048 0.4010 0.039 Uiso 1 calc R F 1 C2D C 0.7223(3) 0.2404(3) 0.44253(19) 0.0332(11) Uani 1 d . . . H2DA H 0.7241 0.2452 0.4044 0.040 Uiso 1 calc R G 1 H2DB H 0.7897 0.2171 0.4572 0.040 Uiso 1 calc R G 1 C2E C 0.7126(4) 0.3213(3) 0.4654(2) 0.0404(13) Uani 1 d . . . H2EA H 0.7038 0.3161 0.5029 0.048 Uiso 1 calc R . . H2EB H 0.7789 0.3501 0.4626 0.048 Uiso 1 calc R . . C2F C 0.6223(4) 0.3689(3) 0.4395(2) 0.0375(12) Uani 1 d . . . H2FA H 0.6251 0.4226 0.4539 0.045 Uiso 1 calc R H 1 H2FB H 0.6280 0.3724 0.4016 0.045 Uiso 1 calc R H 1 C3A C 0.1832(4) 0.4593(3) 0.51321(18) 0.0371(12) Uani 1 d . . . H3AA H 0.1241 0.4808 0.4897 0.044 Uiso 1 calc R I 1 H3AB H 0.2353 0.5015 0.5212 0.044 Uiso 1 calc R I 1 C3B C 0.1431(4) 0.4314(3) 0.56307(18) 0.0399(13) Uani 1 d . . . H3BA H 0.2017 0.4061 0.5850 0.048 Uiso 1 calc R . . H3BB H 0.1208 0.4774 0.5824 0.048 Uiso 1 calc R . . C3C C 0.0528(4) 0.3748(3) 0.55539(17) 0.0335(12) Uani 1 d . . . H3CA H 0.0245 0.3669 0.5893 0.040 Uiso 1 calc R J 1 H3CB H -0.0036 0.3985 0.5312 0.040 Uiso 1 calc R J 1 C3D C -0.0136(3) 0.2458(3) 0.53429(17) 0.0305(11) Uani 1 d . . . H3DA H -0.0699 0.2666 0.5088 0.037 Uiso 1 calc R K 1 H3DB H -0.0394 0.2481 0.5691 0.037 Uiso 1 calc R K 1 C3E C 0.0053(4) 0.1615(3) 0.52122(18) 0.0344(12) Uani 1 d . . . H3EA H -0.0566 0.1304 0.5287 0.041 Uiso 1 calc R . . H3EB H 0.0664 0.1422 0.5444 0.041 Uiso 1 calc R . . C3F C 0.0255(4) 0.1473(3) 0.46542(18) 0.0301(11) Uani 1 d . . . H3FA H 0.0298 0.0904 0.4590 0.036 Uiso 1 calc R L 1 H3FB H -0.0333 0.1687 0.4416 0.036 Uiso 1 calc R L 1 C4A C -0.0783(4) 0.2123(3) 0.30677(19) 0.0355(12) Uani 1 d . . . H4AA H -0.1033 0.2163 0.3417 0.043 Uiso 1 calc R M 1 H4AB H -0.0840 0.1570 0.2955 0.043 Uiso 1 calc R M 1 C4B C -0.1459(4) 0.2632(3) 0.2685(2) 0.0386(12) Uani 1 d . . . H4BA H -0.1167 0.2615 0.2345 0.046 Uiso 1 calc R . . H4BB H -0.2175 0.2405 0.2634 0.046 Uiso 1 calc R . . C4C C -0.1545(4) 0.3475(3) 0.2847(2) 0.0369(12) Uani 1 d . . . H4CA H -0.2095 0.3732 0.2607 0.044 Uiso 1 calc R N 1 H4CB H -0.1776 0.3491 0.3201 0.044 Uiso 1 calc R N 1 C4D C -0.0796(4) 0.4760(3) 0.29646(18) 0.0334(11) Uani 1 d . . . H4DA H -0.1010 0.4789 0.3322 0.040 Uiso 1 calc R O 1 H4DB H -0.1403 0.4930 0.2721 0.040 Uiso 1 calc R O 1 C4E C 0.0102(4) 0.5324(3) 0.2923(2) 0.0398(13) Uani 1 d . . . H4EA H -0.0171 0.5864 0.2934 0.048 Uiso 1 calc R . . H4EB H 0.0372 0.5250 0.2581 0.048 Uiso 1 calc R . . C4F C 0.1011(4) 0.5234(3) 0.33492(19) 0.0359(12) Uani 1 d . . . H4FA H 0.1523 0.5662 0.3324 0.043 Uiso 1 calc R P 1 H4FB H 0.0746 0.5263 0.3696 0.043 Uiso 1 calc R P 1 N11A N 0.3095(3) 0.1787(2) 0.26391(14) 0.0250(8) Uani 0.67 d P Q 1 H11A H 0.2935 0.1565 0.2946 0.030 Uiso 0.67 calc PR Q 1 H11B H 0.2470 0.1950 0.2463 0.030 Uiso 0.67 calc PR Q 1 N12A N 0.4506(3) 0.2808(2) 0.21072(13) 0.0214(8) Uani 0.67 d P Q 1 H12A H 0.3976 0.3037 0.1883 0.026 Uiso 0.67 calc PR Q 1 N13A N 0.4180(3) 0.3907(2) 0.29415(14) 0.0267(9) Uani 0.67 d P Q 1 H13A H 0.3638 0.4161 0.2748 0.032 Uiso 0.67 calc PR Q 1 H13B H 0.4114 0.4010 0.3286 0.032 Uiso 0.67 calc PR Q 1 N21A N 0.4246(3) 0.1178(2) 0.41901(14) 0.0265(8) Uani 0.67 d P Q 1 H21A H 0.3963 0.1127 0.4502 0.032 Uiso 0.67 calc PR Q 1 H21B H 0.3692 0.1182 0.3932 0.032 Uiso 0.67 calc PR Q 1 N22A N 0.6353(3) 0.1869(2) 0.45270(13) 0.0224(8) Uani 0.67 d P Q 1 H22A H 0.6317 0.1872 0.4885 0.027 Uiso 0.67 calc PR Q 1 N23A N 0.5213(3) 0.3316(2) 0.44856(14) 0.0260(8) Uani 0.67 d P Q 1 H23A H 0.4677 0.3638 0.4349 0.031 Uiso 0.67 calc PR Q 1 H23B H 0.5179 0.3291 0.4840 0.031 Uiso 0.67 calc PR Q 1 N31A N 0.2324(3) 0.3943(2) 0.48710(14) 0.0271(9) Uani 0.67 d P R 1 H31A H 0.2887 0.3768 0.5091 0.033 Uiso 0.67 calc PR R 1 H31B H 0.2586 0.4140 0.4579 0.033 Uiso 0.67 calc PR R 1 N32A N 0.0800(3) 0.2977(2) 0.53451(12) 0.0221(8) Uani 0.67 d P R 1 H32A H 0.1315 0.2764 0.5585 0.027 Uiso 0.67 calc PR R 1 N33A N 0.1249(3) 0.1852(2) 0.45496(13) 0.0230(8) Uani 0.67 d P R 1 H33A H 0.1354 0.1742 0.4210 0.028 Uiso 0.67 calc PR R 1 H33B H 0.1783 0.1613 0.4758 0.028 Uiso 0.67 calc PR R 1 N41A N 0.0327(3) 0.2381(2) 0.30937(14) 0.0253(8) Uani 0.67 d P R 1 H41A H 0.0543 0.2316 0.2767 0.030 Uiso 0.67 calc PR R 1 H41B H 0.0720 0.2044 0.3314 0.030 Uiso 0.67 calc PR R 1 N42A N -0.0551(3) 0.3932(2) 0.28486(13) 0.0255(8) Uani 0.67 d P R 1 H42A H -0.0362 0.3920 0.2510 0.031 Uiso 0.67 calc PR R 1 N43A N 0.1528(3) 0.4472(2) 0.32895(14) 0.0261(8) Uani 0.67 d P R 1 H43A H 0.2091 0.4444 0.3541 0.031 Uiso 0.67 calc PR R 1 H43B H 0.1795 0.4476 0.2972 0.031 Uiso 0.67 calc PR R 1 N11B N 0.3095(3) 0.1787(2) 0.26391(14) 0.0250(8) Uani 0.33 d P Q 2 H11C H 0.2978 0.1572 0.2955 0.030 Uiso 0.33 calc PR Q 2 H11D H 0.2448 0.1926 0.2475 0.030 Uiso 0.33 calc PR Q 2 N12B N 0.4506(3) 0.2808(2) 0.21072(13) 0.0214(8) Uani 0.33 d P Q 2 H12B H 0.3992 0.3035 0.1873 0.026 Uiso 0.33 calc PR Q 2 N13B N 0.4180(3) 0.3907(2) 0.29415(14) 0.0267(9) Uani 0.33 d P Q 2 H13C H 0.3640 0.4190 0.2769 0.032 Uiso 0.33 calc PR Q 2 H13D H 0.4142 0.3981 0.3292 0.032 Uiso 0.33 calc PR Q 2 N21B N 0.4246(3) 0.1178(2) 0.41901(14) 0.0265(8) Uani 0.33 d P Q 2 H21C H 0.3945 0.1114 0.4496 0.032 Uiso 0.33 calc PR Q 2 H21D H 0.3704 0.1184 0.3926 0.032 Uiso 0.33 calc PR Q 2 N22B N 0.6353(3) 0.1869(2) 0.45270(13) 0.0224(8) Uani 0.33 d P Q 2 H22B H 0.6337 0.1867 0.4886 0.027 Uiso 0.33 calc PR Q 2 N23B N 0.5213(3) 0.3316(2) 0.44856(14) 0.0260(8) Uani 0.33 d P Q 2 H23C H 0.4683 0.3641 0.4346 0.031 Uiso 0.33 calc PR Q 2 H23D H 0.5179 0.3306 0.4840 0.031 Uiso 0.33 calc PR Q 2 N31B N 0.2324(3) 0.3943(2) 0.48710(14) 0.0271(9) Uani 0.33 d P Q 2 H31C H 0.2901 0.3783 0.5087 0.033 Uiso 0.33 calc PR Q 2 H31D H 0.2568 0.4140 0.4575 0.033 Uiso 0.33 calc PR Q 2 N32B N 0.0800(3) 0.2977(2) 0.53451(12) 0.0221(8) Uani 0.33 d P Q 2 H32B H 0.1302 0.2766 0.5592 0.027 Uiso 0.33 calc PR Q 2 N33B N 0.1249(3) 0.1852(2) 0.45496(13) 0.0230(8) Uani 0.33 d P Q 2 H33C H 0.1337 0.1754 0.4206 0.028 Uiso 0.33 calc PR Q 2 H33D H 0.1782 0.1595 0.4747 0.028 Uiso 0.33 calc PR Q 2 N41B N 0.0327(3) 0.2381(2) 0.30937(14) 0.0253(8) Uani 0.33 d P Q 2 H41C H 0.0553 0.2295 0.2771 0.030 Uiso 0.33 calc PR Q 2 H41D H 0.0716 0.2059 0.3325 0.030 Uiso 0.33 calc PR Q 2 N42B N -0.0551(3) 0.3932(2) 0.28486(13) 0.0255(8) Uani 0.33 d P Q 2 H42B H -0.0374 0.3924 0.2508 0.031 Uiso 0.33 calc PR Q 2 N43B N 0.1528(3) 0.4472(2) 0.32895(14) 0.0261(8) Uani 0.33 d P Q 2 H43C H 0.2071 0.4434 0.3552 0.031 Uiso 0.33 calc PR Q 2 H43D H 0.1824 0.4486 0.2980 0.031 Uiso 0.33 calc PR Q 2 Cu1A Cu 0.3968(5) 0.2770(4) 0.2831(3) 0.0323(12) Uani 0.67 d PD Q 1 Cu2A Cu 0.4941(4) 0.2244(3) 0.41905(15) 0.0339(13) Uani 0.67 d PD Q 1 Cu3A Cu 0.1418(3) 0.3007(2) 0.46494(14) 0.0175(7) Uani 0.67 d PD R 1 Cu4A Cu 0.0707(4) 0.3486(2) 0.33289(17) 0.0263(11) Uani 0.67 d PD R 1 Cl1A Cl 0.54168(19) 0.2219(2) 0.33077(12) 0.0255(6) Uani 0.67 d PD Q 1 Cl2A Cl -0.0304(2) 0.3642(3) 0.41655(15) 0.0269(7) Uani 0.67 d PD R 1 O1A O 0.2810(4) 0.2894(3) 0.33037(16) 0.0213(10) Uani 0.67 d P Q 1 O2A O 0.3369(4) 0.2631(3) 0.41468(16) 0.0204(10) Uani 0.67 d P Q 1 O3A O 0.1769(3) 0.3083(2) 0.39104(14) 0.0182(9) Uani 0.67 d P R 1 Cu1B Cu 0.3873(9) 0.2740(6) 0.2785(5) 0.0156(13) Uani 0.33 d PD Q 2 Cu2B Cu 0.4883(8) 0.2238(6) 0.4215(2) 0.0145(17) Uani 0.33 d PD Q 2 Cu3B Cu 0.1489(9) 0.3008(6) 0.4669(4) 0.049(3) Uani 0.33 d PD Q 2 Cu4B Cu 0.0685(7) 0.3478(4) 0.3295(3) 0.030(2) Uani 0.33 d PD Q 2 Cl1B Cl 0.5839(4) 0.2231(4) 0.3264(2) 0.0246(12) Uani 0.33 d PD Q 2 Cl2B Cl 0.0057(4) 0.3557(5) 0.4119(3) 0.0257(14) Uani 0.33 d PD Q 2 O1B O 0.2780(8) 0.2837(5) 0.4255(3) 0.0193(19) Uani 0.33 d P Q 2 O2B O 0.2158(8) 0.2972(5) 0.3403(3) 0.022(2) Uani 0.33 d P Q 2 O3B O 0.3798(6) 0.2627(5) 0.3625(3) 0.0166(18) Uani 0.33 d P Q 2 C0 C 0.2752(3) 0.2845(2) 0.37785(15) 0.0189(9) Uani 1 d . . . 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 Cl3 0.0259(6) 0.0274(6) 0.0192(5) 0.0011(4) 0.0020(4) 0.0024(5) O31 0.059(2) 0.038(2) 0.0198(16) 0.0050(14) -0.0015(15) 0.0054(18) O32 0.047(2) 0.0285(19) 0.0407(19) 0.0039(15) 0.0114(16) 0.0094(16) O33 0.054(2) 0.034(2) 0.0390(19) -0.0011(16) -0.0222(17) -0.0050(18) O34 0.029(2) 0.069(3) 0.049(2) 0.0056(19) 0.0161(16) 0.0033(19) Cl4 0.0365(7) 0.0268(6) 0.0207(5) 0.0005(4) 0.0040(5) 0.0021(5) O41 0.056(2) 0.044(2) 0.0289(17) -0.0035(16) 0.0174(16) -0.0039(18) O42 0.055(2) 0.0270(19) 0.052(2) 0.0028(16) 0.0105(18) -0.0084(17) O43 0.107(4) 0.042(2) 0.0313(19) -0.0018(17) -0.019(2) -0.018(2) O44 0.048(3) 0.070(3) 0.074(3) 0.020(2) 0.023(2) 0.022(2) Cl5 0.0549(8) 0.0234(6) 0.0287(6) -0.0010(5) 0.0065(5) -0.0049(6) O51 0.042(2) 0.0218(17) 0.0331(17) 0.0021(14) 0.0073(15) 0.0001(15) O52 0.134(5) 0.064(3) 0.173(6) 0.027(4) -0.098(5) -0.043(4) O53 0.210(7) 0.050(3) 0.118(4) -0.004(3) 0.108(5) 0.033(4) O54 0.106(4) 0.051(3) 0.044(2) 0.0180(19) 0.009(2) -0.025(2) Cl6 0.0362(7) 0.0297(6) 0.0257(5) 0.0025(5) 0.0035(5) 0.0045(5) O62 0.105(4) 0.040(2) 0.0312(19) -0.0100(17) 0.020(2) -0.009(2) O61 0.063(3) 0.037(2) 0.041(2) -0.0040(17) 0.0093(18) 0.0030(19) O63 0.141(5) 0.094(4) 0.058(3) -0.004(3) 0.041(3) -0.070(4) O64 0.062(3) 0.139(5) 0.120(5) -0.023(4) -0.026(3) 0.051(3) O7 0.054(3) 0.068(3) 0.040(2) 0.013(2) 0.0002(18) 0.017(2) C7 0.064(4) 0.098(5) 0.043(3) 0.010(4) 0.025(3) 0.007(4) O8 0.047(2) 0.0313(19) 0.0333(18) 0.0004(15) 0.0050(17) -0.0099(16) C8 0.043(3) 0.031(3) 0.055(3) 0.000(2) 0.001(3) -0.002(2) O9 0.080(3) 0.037(2) 0.043(2) 0.0018(18) 0.012(2) 0.003(2) C9 0.048(4) 0.038(3) 0.071(4) -0.005(3) 0.008(3) -0.004(3) C1A 0.034(3) 0.020(2) 0.034(3) -0.004(2) 0.005(2) -0.005(2) C1B 0.039(3) 0.023(2) 0.028(2) -0.008(2) 0.003(2) 0.001(2) C1C 0.031(3) 0.028(3) 0.023(2) -0.0021(19) 0.0084(19) 0.006(2) C1D 0.026(2) 0.031(3) 0.025(2) -0.0004(19) 0.0121(19) -0.002(2) C1E 0.030(3) 0.022(2) 0.034(2) 0.004(2) 0.011(2) -0.007(2) C1F 0.040(3) 0.025(3) 0.033(3) -0.003(2) 0.012(2) -0.012(2) C2A 0.035(3) 0.014(2) 0.041(3) -0.003(2) -0.002(2) 0.000(2) C2B 0.040(3) 0.024(3) 0.046(3) 0.001(2) -0.002(2) 0.009(2) C2C 0.028(3) 0.028(3) 0.040(3) 0.000(2) 0.002(2) 0.010(2) C2D 0.017(2) 0.040(3) 0.042(3) 0.002(2) 0.001(2) 0.001(2) C2E 0.026(3) 0.031(3) 0.061(3) -0.002(2) -0.011(2) -0.005(2) C2F 0.030(3) 0.022(3) 0.057(3) 0.000(2) -0.008(2) -0.004(2) C3A 0.052(3) 0.027(3) 0.034(3) -0.007(2) 0.011(2) -0.002(2) C3B 0.062(4) 0.032(3) 0.027(2) -0.007(2) 0.012(2) 0.006(3) C3C 0.042(3) 0.036(3) 0.025(2) -0.002(2) 0.016(2) 0.010(2) C3D 0.020(2) 0.046(3) 0.028(2) 0.003(2) 0.0103(19) -0.003(2) C3E 0.029(3) 0.039(3) 0.036(3) 0.010(2) 0.010(2) -0.009(2) C3F 0.024(2) 0.028(3) 0.039(3) -0.002(2) 0.004(2) -0.010(2) C4A 0.031(3) 0.031(3) 0.044(3) 0.000(2) 0.003(2) -0.002(2) C4B 0.025(3) 0.043(3) 0.047(3) 0.004(2) -0.004(2) -0.002(2) C4C 0.020(3) 0.045(3) 0.046(3) 0.009(2) 0.002(2) 0.008(2) C4D 0.037(3) 0.031(3) 0.032(3) 0.005(2) 0.005(2) 0.017(2) C4E 0.053(3) 0.024(3) 0.044(3) 0.008(2) 0.007(3) 0.012(2) C4F 0.041(3) 0.024(3) 0.044(3) -0.002(2) 0.008(2) 0.006(2) N11A 0.022(2) 0.023(2) 0.031(2) 0.0027(16) 0.0098(16) 0.0012(16) N12A 0.0214(19) 0.0221(19) 0.0216(17) 0.0001(15) 0.0068(15) 0.0039(16) N13A 0.031(2) 0.024(2) 0.028(2) -0.0022(16) 0.0152(17) -0.0020(17) N21A 0.025(2) 0.025(2) 0.028(2) 0.0000(16) -0.0049(16) -0.0024(17) N22A 0.0201(19) 0.0219(19) 0.0249(18) -0.0039(15) 0.0003(15) 0.0032(16) N23A 0.023(2) 0.026(2) 0.0284(19) -0.0059(16) -0.0018(16) 0.0027(16) N31A 0.027(2) 0.030(2) 0.0252(19) 0.0018(16) 0.0071(16) -0.0022(17) N32A 0.0175(19) 0.031(2) 0.0195(17) 0.0025(15) 0.0072(14) 0.0036(16) N33A 0.024(2) 0.025(2) 0.0199(17) 0.0029(15) 0.0034(15) 0.0036(16) N41A 0.020(2) 0.027(2) 0.0291(19) 0.0037(16) 0.0040(16) 0.0023(16) N42A 0.027(2) 0.028(2) 0.0219(18) 0.0055(16) 0.0032(16) 0.0072(17) N43A 0.027(2) 0.025(2) 0.0263(19) 0.0030(16) 0.0034(16) 0.0045(17) N11B 0.022(2) 0.023(2) 0.031(2) 0.0027(16) 0.0098(16) 0.0012(16) N12B 0.0214(19) 0.0221(19) 0.0216(17) 0.0001(15) 0.0068(15) 0.0039(16) N13B 0.031(2) 0.024(2) 0.028(2) -0.0022(16) 0.0152(17) -0.0020(17) N21B 0.025(2) 0.025(2) 0.028(2) 0.0000(16) -0.0049(16) -0.0024(17) N22B 0.0201(19) 0.0219(19) 0.0249(18) -0.0039(15) 0.0003(15) 0.0032(16) N23B 0.023(2) 0.026(2) 0.0284(19) -0.0059(16) -0.0018(16) 0.0027(16) N31B 0.027(2) 0.030(2) 0.0252(19) 0.0018(16) 0.0071(16) -0.0022(17) N32B 0.0175(19) 0.031(2) 0.0195(17) 0.0025(15) 0.0072(14) 0.0036(16) N33B 0.024(2) 0.025(2) 0.0199(17) 0.0029(15) 0.0034(15) 0.0036(16) N41B 0.020(2) 0.027(2) 0.0291(19) 0.0037(16) 0.0040(16) 0.0023(16) N42B 0.027(2) 0.028(2) 0.0219(18) 0.0055(16) 0.0032(16) 0.0072(17) N43B 0.027(2) 0.025(2) 0.0263(19) 0.0030(16) 0.0034(16) 0.0045(17) Cu1A 0.046(2) 0.0229(14) 0.0327(19) -0.0098(10) 0.0277(16) -0.0127(11) Cu2A 0.0256(19) 0.0162(19) 0.057(2) -0.0006(15) -0.0115(14) 0.0001(13) Cu3A 0.0283(13) 0.0136(14) 0.0129(13) -0.0010(10) 0.0129(9) 0.0000(10) Cu4A 0.0162(19) 0.033(2) 0.0296(13) 0.0049(10) 0.0017(10) 0.0056(13) Cl1A 0.0233(16) 0.0328(11) 0.0203(10) 0.0013(8) 0.0017(12) 0.0020(15) Cl2A 0.0204(19) 0.0389(15) 0.0222(11) 0.0067(9) 0.0063(13) 0.0107(15) O1A 0.021(3) 0.026(3) 0.019(2) -0.0002(19) 0.008(2) 0.003(2) O2A 0.017(3) 0.025(3) 0.018(2) 0.0005(19) 0.000(2) 0.004(2) O3A 0.015(2) 0.023(2) 0.016(2) 0.0006(18) 0.0032(17) 0.0005(18) Cu1B 0.0218(19) 0.008(2) 0.0182(18) 0.0000(18) 0.0101(13) 0.0049(19) Cu2B 0.011(3) 0.021(4) 0.010(2) -0.003(2) -0.0075(17) 0.001(2) Cu3B 0.064(5) 0.045(5) 0.044(5) -0.008(3) 0.029(3) -0.015(3) Cu4B 0.023(4) 0.003(3) 0.061(4) 0.009(2) -0.013(3) -0.002(2) Cl1B 0.020(3) 0.035(2) 0.019(2) 0.0025(16) 0.002(2) -0.001(3) Cl2B 0.016(4) 0.040(3) 0.021(2) 0.0031(18) 0.004(2) 0.010(3) O1B 0.015(5) 0.026(5) 0.017(5) 0.004(4) 0.004(4) 0.007(4) O2B 0.018(5) 0.031(6) 0.017(5) 0.000(4) 0.000(4) 0.010(4) O3B 0.012(4) 0.020(5) 0.019(4) 0.003(3) 0.005(3) 0.001(3) C0 0.027(2) 0.008(2) 0.022(2) -0.0011(17) 0.005(2) -0.0038(17) _geom_special_details ; Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 4.2218 (0.0081) x + 15.9223 (0.0101) y + 3.1383 (0.0321) z = 6.9028 (0.0120) * 0.0706 (0.0045) Cu1A_a * 0.0704 (0.0038) Cu2A_a * -0.0566 (0.0036) Cu3A_a * -0.0088 (0.0035) Cu4A_a * -0.0445 (0.0036) Cl1A_a * 0.0751 (0.0035) Cl2A_a * -0.0710 (0.0042) O1A_a * 0.0102 (0.0041) O2A_a * -0.0203 (0.0039) O3A_a * -0.0250 (0.0037) C0 Rms deviation of fitted atoms = 0.0520 4.0297 (0.0148) x + 16.0813 (0.0127) y + 2.4902 (0.0621) z = 6.6611 (0.0223) Angle to previous plane (with approximate esd) = 1.84 ( 0.12 ) * 0.0000 (0.0083) Cu1B_b * -0.0443 (0.0073) Cu2B_b * -0.0608 (0.0083) Cu3B_b * 0.0279 (0.0063) Cu4B_b * 0.0917 (0.0066) Cl1B_b * 0.1073 (0.0073) Cl2B_b * 0.0808 (0.0082) O1B_b * -0.1643 (0.0085) O2B_b * -0.0026 (0.0076) O3B_b * -0.0357 (0.0045) C0 Rms deviation of fitted atoms = 0.0782 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 Cl3 O34 1.420(3) . ? Cl3 O32 1.431(3) . ? Cl3 O31 1.432(3) . ? Cl3 O33 1.445(3) . ? Cl4 O41 1.416(3) . ? Cl4 O44 1.422(4) . ? Cl4 O43 1.430(4) . ? Cl4 O42 1.442(3) . ? Cl5 O52 1.372(5) . ? Cl5 O54 1.406(4) . ? Cl5 O53 1.415(5) . ? Cl5 O51 1.459(3) . ? Cl6 O63 1.393(4) . ? Cl6 O64 1.406(5) . ? Cl6 O62 1.425(3) . ? Cl6 O61 1.453(4) . ? O7 C7 1.402(7) . ? O7 H7 0.8400 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O8 C8 1.421(6) . ? O8 H8 0.8400 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C9 1.379(7) . ? O9 H9 0.8400 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C1A N11A 1.476(5) . ? C1A C1B 1.514(6) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C1B C1C 1.512(6) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C1C N12A 1.490(5) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C1D N12A 1.482(5) . ? C1D C1E 1.522(6) . ? C1D H1DA 0.9900 . ? C1D H1DB 0.9900 . ? C1E C1F 1.509(6) . ? C1E H1EA 0.9900 . ? C1E H1EB 0.9900 . ? C1F N13A 1.473(5) . ? C1F H1FA 0.9900 . ? C1F H1FB 0.9900 . ? C2A N21A 1.478(5) . ? C2A C2B 1.511(6) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C2B C2C 1.513(7) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C2C N22A 1.487(5) . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C2D N22A 1.485(6) . ? C2D C2E 1.514(7) . ? C2D H2DA 0.9900 . ? C2D H2DB 0.9900 . ? C2E C2F 1.511(7) . ? C2E H2EA 0.9900 . ? C2E H2EB 0.9900 . ? C2F N23A 1.481(6) . ? C2F H2FA 0.9900 . ? C2F H2FB 0.9900 . ? C3A N31A 1.475(6) . ? C3A C3B 1.511(6) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3B C3C 1.504(7) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C3C N32A 1.480(6) . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C3D N32A 1.490(6) . ? C3D C3E 1.506(7) . ? C3D H3DA 0.9900 . ? C3D H3DB 0.9900 . ? C3E C3F 1.509(6) . ? C3E H3EA 0.9900 . ? C3E H3EB 0.9900 . ? C3F N33A 1.477(5) . ? C3F H3FA 0.9900 . ? C3F H3FB 0.9900 . ? C4A N41A 1.483(6) . ? C4A C4B 1.517(7) . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? C4B C4C 1.508(7) . ? C4B H4BA 0.9900 . ? C4B H4BB 0.9900 . ? C4C N42A 1.493(6) . ? C4C H4CA 0.9900 . ? C4C H4CB 0.9900 . ? C4D N42A 1.488(6) . ? C4D C4E 1.513(7) . ? C4D H4DA 0.9900 . ? C4D H4DB 0.9900 . ? C4E C4F 1.521(7) . ? C4E H4EA 0.9900 . ? C4E H4EB 0.9900 . ? C4F N43A 1.477(6) . ? C4F H4FA 0.9900 . ? C4F H4FB 0.9900 . ? N11A Cu1A 2.050(8) . ? N11A H11A 0.9200 . ? N11A H11B 0.9200 . ? N12A Cu1A 2.059(7) . ? N12A H12A 0.9300 . ? N13A Cu1A 1.980(7) . ? N13A H13A 0.9200 . ? N13A H13B 0.9200 . ? N21A Cu2A 2.029(7) . ? N21A H21A 0.9200 . ? N21A H21B 0.9200 . ? N22A Cu2A 2.026(6) . ? N22A H22A 0.9300 . ? N23A Cu2A 2.003(6) . ? N23A H23A 0.9200 . ? N23A H23B 0.9200 . ? N31A Cu3A 2.022(6) . ? N31A H31A 0.9200 . ? N31A H31B 0.9200 . ? N32A Cu3A 2.037(5) . ? N32A H32A 0.9300 . ? N33A Cu3A 2.002(5) . ? N33A H33A 0.9200 . ? N33A H33B 0.9200 . ? N41A Cu4A 2.029(5) . ? N41A H41A 0.9200 . ? N41A H41B 0.9200 . ? N42A Cu4A 2.071(6) . ? N42A H42A 0.9300 . ? N43A Cu4A 1.994(5) . ? N43A H43A 0.9200 . ? N43A H43B 0.9200 . ? Cu1A O1A 2.026(8) . ? Cu1A Cl1A 2.315(6) . ? Cu2A O2A 2.110(7) . ? Cu2A Cl1A 2.419(5) . ? Cu3A O3A 2.008(5) . ? Cu3A Cl2A 2.649(4) . ? Cu4A O3A 2.036(6) . ? Cu4A Cl2A 2.644(4) . ? O1A C0 1.238(6) . ? O2A C0 1.226(6) . ? O3A C0 1.398(6) . ? Cu1B O3B 2.188(14) . ? Cu1B Cl1B 2.822(10) . ? Cu2B O3B 2.060(11) . ? Cu2B Cl1B 2.853(8) . ? Cu3B O1B 2.080(14) . ? Cu3B Cl2B 2.387(10) . ? Cu4B O2B 2.066(13) . ? Cu4B Cl2B 2.355(9) . ? O1B C0 1.226(9) . ? O2B C0 1.188(9) . ? O3B C0 1.483(8) . ? 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 O34 Cl3 O32 109.3(2) . . ? O34 Cl3 O31 110.2(2) . . ? O32 Cl3 O31 110.5(2) . . ? O34 Cl3 O33 109.3(2) . . ? O32 Cl3 O33 109.1(2) . . ? O31 Cl3 O33 108.3(2) . . ? O41 Cl4 O44 110.4(2) . . ? O41 Cl4 O43 109.8(2) . . ? O44 Cl4 O43 108.8(3) . . ? O41 Cl4 O42 109.5(2) . . ? O44 Cl4 O42 110.3(2) . . ? O43 Cl4 O42 108.0(2) . . ? O52 Cl5 O54 112.0(4) . . ? O52 Cl5 O53 111.2(5) . . ? O54 Cl5 O53 107.3(3) . . ? O52 Cl5 O51 110.7(3) . . ? O54 Cl5 O51 108.9(2) . . ? O53 Cl5 O51 106.5(3) . . ? O63 Cl6 O64 111.8(4) . . ? O63 Cl6 O62 110.6(3) . . ? O64 Cl6 O62 112.8(3) . . ? O63 Cl6 O61 108.2(3) . . ? O64 Cl6 O61 105.9(3) . . ? O62 Cl6 O61 107.2(2) . . ? C7 O7 H7 109.5 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 O8 H8 109.5 . . ? O8 C8 H8A 109.5 . . ? O8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O9 H9 109.5 . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N11A C1A C1B 110.2(4) . . ? N11A C1A H1AA 109.6 . . ? C1B C1A H1AA 109.6 . . ? N11A C1A H1AB 109.6 . . ? C1B C1A H1AB 109.6 . . ? H1AA C1A H1AB 108.1 . . ? C1C C1B C1A 113.5(4) . . ? C1C C1B H1BA 108.9 . . ? C1A C1B H1BA 108.9 . . ? C1C C1B H1BB 108.9 . . ? C1A C1B H1BB 108.9 . . ? H1BA C1B H1BB 107.7 . . ? N12A C1C C1B 114.1(4) . . ? N12A C1C H1CA 108.7 . . ? C1B C1C H1CA 108.7 . . ? N12A C1C H1CB 108.7 . . ? C1B C1C H1CB 108.7 . . ? H1CA C1C H1CB 107.6 . . ? N12A C1D C1E 114.1(3) . . ? N12A C1D H1DA 108.7 . . ? C1E C1D H1DA 108.7 . . ? N12A C1D H1DB 108.7 . . ? C1E C1D H1DB 108.7 . . ? H1DA C1D H1DB 107.6 . . ? C1F C1E C1D 113.4(4) . . ? C1F C1E H1EA 108.9 . . ? C1D C1E H1EA 108.9 . . ? C1F C1E H1EB 108.9 . . ? C1D C1E H1EB 108.9 . . ? H1EA C1E H1EB 107.7 . . ? N13A C1F C1E 110.2(4) . . ? N13A C1F H1FA 109.6 . . ? C1E C1F H1FA 109.6 . . ? N13A C1F H1FB 109.6 . . ? C1E C1F H1FB 109.6 . . ? H1FA C1F H1FB 108.1 . . ? N21A C2A C2B 110.5(4) . . ? N21A C2A H2AA 109.5 . . ? C2B C2A H2AA 109.5 . . ? N21A C2A H2AB 109.5 . . ? C2B C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C2A C2B C2C 113.9(4) . . ? C2A C2B H2BA 108.8 . . ? C2C C2B H2BA 108.8 . . ? C2A C2B H2BB 108.8 . . ? C2C C2B H2BB 108.8 . . ? H2BA C2B H2BB 107.7 . . ? N22A C2C C2B 113.5(4) . . ? N22A C2C H2CA 108.9 . . ? C2B C2C H2CA 108.9 . . ? N22A C2C H2CB 108.9 . . ? C2B C2C H2CB 108.9 . . ? H2CA C2C H2CB 107.7 . . ? N22A C2D C2E 113.6(4) . . ? N22A C2D H2DA 108.8 . . ? C2E C2D H2DA 108.8 . . ? N22A C2D H2DB 108.8 . . ? C2E C2D H2DB 108.8 . . ? H2DA C2D H2DB 107.7 . . ? C2F C2E C2D 114.2(4) . . ? C2F C2E H2EA 108.7 . . ? C2D C2E H2EA 108.7 . . ? C2F C2E H2EB 108.7 . . ? C2D C2E H2EB 108.7 . . ? H2EA C2E H2EB 107.6 . . ? N23A C2F C2E 109.8(4) . . ? N23A C2F H2FA 109.7 . . ? C2E C2F H2FA 109.7 . . ? N23A C2F H2FB 109.7 . . ? C2E C2F H2FB 109.7 . . ? H2FA C2F H2FB 108.2 . . ? N31A C3A C3B 110.5(4) . . ? N31A C3A H3AA 109.6 . . ? C3B C3A H3AA 109.6 . . ? N31A C3A H3AB 109.6 . . ? C3B C3A H3AB 109.6 . . ? H3AA C3A H3AB 108.1 . . ? C3C C3B C3A 114.5(4) . . ? C3C C3B H3BA 108.6 . . ? C3A C3B H3BA 108.6 . . ? C3C C3B H3BB 108.6 . . ? C3A C3B H3BB 108.6 . . ? H3BA C3B H3BB 107.6 . . ? N32A C3C C3B 114.5(4) . . ? N32A C3C H3CA 108.6 . . ? C3B C3C H3CA 108.6 . . ? N32A C3C H3CB 108.6 . . ? C3B C3C H3CB 108.6 . . ? H3CA C3C H3CB 107.6 . . ? N32A C3D C3E 115.1(4) . . ? N32A C3D H3DA 108.5 . . ? C3E C3D H3DA 108.5 . . ? N32A C3D H3DB 108.5 . . ? C3E C3D H3DB 108.5 . . ? H3DA C3D H3DB 107.5 . . ? C3D C3E C3F 114.5(4) . . ? C3D C3E H3EA 108.6 . . ? C3F C3E H3EA 108.6 . . ? C3D C3E H3EB 108.6 . . ? C3F C3E H3EB 108.6 . . ? H3EA C3E H3EB 107.6 . . ? N33A C3F C3E 109.9(4) . . ? N33A C3F H3FA 109.7 . . ? C3E C3F H3FA 109.7 . . ? N33A C3F H3FB 109.7 . . ? C3E C3F H3FB 109.7 . . ? H3FA C3F H3FB 108.2 . . ? N41A C4A C4B 109.7(4) . . ? N41A C4A H4AA 109.7 . . ? C4B C4A H4AA 109.7 . . ? N41A C4A H4AB 109.7 . . ? C4B C4A H4AB 109.7 . . ? H4AA C4A H4AB 108.2 . . ? C4C C4B C4A 114.9(4) . . ? C4C C4B H4BA 108.5 . . ? C4A C4B H4BA 108.5 . . ? C4C C4B H4BB 108.5 . . ? C4A C4B H4BB 108.5 . . ? H4BA C4B H4BB 107.5 . . ? N42A C4C C4B 114.6(4) . . ? N42A C4C H4CA 108.6 . . ? C4B C4C H4CA 108.6 . . ? N42A C4C H4CB 108.6 . . ? C4B C4C H4CB 108.6 . . ? H4CA C4C H4CB 107.6 . . ? N42A C4D C4E 114.5(4) . . ? N42A C4D H4DA 108.6 . . ? C4E C4D H4DA 108.6 . . ? N42A C4D H4DB 108.6 . . ? C4E C4D H4DB 108.6 . . ? H4DA C4D H4DB 107.6 . . ? C4D C4E C4F 114.4(4) . . ? C4D C4E H4EA 108.7 . . ? C4F C4E H4EA 108.7 . . ? C4D C4E H4EB 108.7 . . ? C4F C4E H4EB 108.7 . . ? H4EA C4E H4EB 107.6 . . ? N43A C4F C4E 109.3(4) . . ? N43A C4F H4FA 109.8 . . ? C4E C4F H4FA 109.8 . . ? N43A C4F H4FB 109.8 . . ? C4E C4F H4FB 109.8 . . ? H4FA C4F H4FB 108.3 . . ? C1A N11A Cu1A 120.6(3) . . ? C1A N11A H11A 107.2 . . ? Cu1A N11A H11A 107.2 . . ? C1A N11A H11B 107.2 . . ? Cu1A N11A H11B 107.2 . . ? H11A N11A H11B 106.8 . . ? C1D N12A C1C 107.6(3) . . ? C1D N12A Cu1A 113.1(3) . . ? C1C N12A Cu1A 115.5(3) . . ? C1D N12A H12A 106.7 . . ? C1C N12A H12A 106.7 . . ? Cu1A N12A H12A 106.7 . . ? C1F N13A Cu1A 118.8(3) . . ? C1F N13A H13A 107.6 . . ? Cu1A N13A H13A 107.6 . . ? C1F N13A H13B 107.6 . . ? Cu1A N13A H13B 107.6 . . ? H13A N13A H13B 107.1 . . ? C2A N21A Cu2A 120.1(3) . . ? C2A N21A H21A 107.3 . . ? Cu2A N21A H21A 107.3 . . ? C2A N21A H21B 107.3 . . ? Cu2A N21A H21B 107.3 . . ? H21A N21A H21B 106.9 . . ? C2D N22A C2C 108.3(3) . . ? C2D N22A Cu2A 112.4(3) . . ? C2C N22A Cu2A 115.3(3) . . ? C2D N22A H22A 106.8 . . ? C2C N22A H22A 106.8 . . ? Cu2A N22A H22A 106.8 . . ? C2F N23A Cu2A 117.0(3) . . ? C2F N23A H23A 108.0 . . ? Cu2A N23A H23A 108.0 . . ? C2F N23A H23B 108.0 . . ? Cu2A N23A H23B 108.0 . . ? H23A N23A H23B 107.3 . . ? C3A N31A Cu3A 117.8(3) . . ? C3A N31A H31A 107.9 . . ? Cu3A N31A H31A 107.9 . . ? C3A N31A H31B 107.9 . . ? Cu3A N31A H31B 107.9 . . ? H31A N31A H31B 107.2 . . ? C3C N32A C3D 108.3(3) . . ? C3C N32A Cu3A 115.2(3) . . ? C3D N32A Cu3A 113.5(3) . . ? C3C N32A H32A 106.4 . . ? C3D N32A H32A 106.4 . . ? Cu3A N32A H32A 106.4 . . ? C3F N33A Cu3A 119.6(3) . . ? C3F N33A H33A 107.4 . . ? Cu3A N33A H33A 107.4 . . ? C3F N33A H33B 107.4 . . ? Cu3A N33A H33B 107.4 . . ? H33A N33A H33B 107.0 . . ? C4A N41A Cu4A 119.3(3) . . ? C4A N41A H41A 107.5 . . ? Cu4A N41A H41A 107.5 . . ? C4A N41A H41B 107.5 . . ? Cu4A N41A H41B 107.5 . . ? H41A N41A H41B 107.0 . . ? C4D N42A C4C 107.6(4) . . ? C4D N42A Cu4A 113.4(3) . . ? C4C N42A Cu4A 114.7(3) . . ? C4D N42A H42A 106.9 . . ? C4C N42A H42A 106.9 . . ? Cu4A N42A H42A 106.9 . . ? C4F N43A Cu4A 119.8(3) . . ? C4F N43A H43A 107.4 . . ? Cu4A N43A H43A 107.4 . . ? C4F N43A H43B 107.4 . . ? Cu4A N43A H43B 107.4 . . ? H43A N43A H43B 106.9 . . ? N13A Cu1A O1A 84.7(3) . . ? N13A Cu1A N11A 154.5(3) . . ? O1A Cu1A N11A 79.5(3) . . ? N13A Cu1A N12A 92.6(3) . . ? O1A Cu1A N12A 151.4(3) . . ? N11A Cu1A N12A 91.9(3) . . ? N13A Cu1A Cl1A 103.5(3) . . ? O1A Cu1A Cl1A 108.6(3) . . ? N11A Cu1A Cl1A 100.4(3) . . ? N12A Cu1A Cl1A 99.8(3) . . ? N23A Cu2A N22A 90.8(3) . . ? N23A Cu2A N21A 151.9(3) . . ? N22A Cu2A N21A 95.0(3) . . ? N23A Cu2A O2A 81.9(3) . . ? N22A Cu2A O2A 157.7(3) . . ? N21A Cu2A O2A 82.3(3) . . ? N23A Cu2A Cl1A 108.8(3) . . ? N22A Cu2A Cl1A 95.5(2) . . ? N21A Cu2A Cl1A 97.9(2) . . ? O2A Cu2A Cl1A 106.7(2) . . ? N33A Cu3A O3A 88.5(2) . . ? N33A Cu3A N31A 150.3(2) . . ? O3A Cu3A N31A 92.2(2) . . ? N33A Cu3A N32A 92.4(2) . . ? O3A Cu3A N32A 169.9(3) . . ? N31A Cu3A N32A 92.0(2) . . ? N33A Cu3A Cl2A 105.7(2) . . ? O3A Cu3A Cl2A 77.51(17) . . ? N31A Cu3A Cl2A 103.5(2) . . ? N32A Cu3A Cl2A 92.57(19) . . ? N43A Cu4A N41A 152.0(2) . . ? N43A Cu4A O3A 90.6(3) . . ? N41A Cu4A O3A 91.4(2) . . ? N43A Cu4A N42A 92.2(2) . . ? N41A Cu4A N42A 91.0(2) . . ? O3A Cu4A N42A 169.2(2) . . ? N43A Cu4A Cl2A 105.2(2) . . ? N41A Cu4A Cl2A 102.5(2) . . ? O3A Cu4A Cl2A 77.19(17) . . ? N42A Cu4A Cl2A 92.01(19) . . ? Cu1A Cl1A Cu2A 103.1(2) . . ? Cu4A Cl2A Cu3A 83.64(15) . . ? C0 O1A Cu1A 135.4(4) . . ? C0 O2A Cu2A 131.9(4) . . ? C0 O3A Cu3A 120.6(3) . . ? C0 O3A Cu4A 117.9(3) . . ? Cu3A O3A Cu4A 121.6(2) . . ? O3B Cu1B Cl1B 70.6(4) . . ? O3B Cu2B Cl1B 71.5(3) . . ? O1B Cu3B Cl2B 110.7(5) . . ? O2B Cu4B Cl2B 107.2(5) . . ? Cu1B Cl1B Cu2B 86.1(3) . . ? Cu4B Cl2B Cu3B 101.5(4) . . ? C0 O1B Cu3B 124.8(7) . . ? C0 O2B Cu4B 133.1(7) . . ? C0 O3B Cu2B 116.3(5) . . ? C0 O3B Cu1B 112.1(5) . . ? Cu2B O3B Cu1B 131.6(5) . . ? O2B C0 O1B 140.3(8) . . ? O2B C0 O2A 172.9(6) . . ? O1B C0 O2A 43.1(4) . . ? O2B C0 O1A 43.9(5) . . ? O1B C0 O1A 173.9(6) . . ? O2A C0 O1A 133.3(5) . . ? O2B C0 O3A 68.3(6) . . ? O1B C0 O3A 72.1(5) . . ? O2A C0 O3A 114.9(4) . . ? O1A C0 O3A 111.7(4) . . ? O2B C0 O3B 110.3(6) . . ? O1B C0 O3B 109.3(6) . . ? O2A C0 O3B 66.7(4) . . ? O1A C0 O3B 66.6(4) . . ? O3A C0 O3B 177.4(5) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.939 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.083 #end data_am88 _database_code_CSD 167773 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Cu3(m3-CO3)(ClO4)2(dpt)3(OH2)](ClO4)2' _chemical_formula_sum 'C19 H55 Cl4 Cu3 N9 O21' _chemical_formula_weight 1078.14 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.664(5) _cell_length_b 21.033(4) _cell_length_c 17.550(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8366(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5402 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.50 _exptl_crystal_description 'plate' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4440 _exptl_absorpt_coefficient_mu 1.852 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method 'theta-2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1% _diffrn_reflns_number 7330 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7330 _reflns_number_gt 5712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Bruker)' _computing_cell_refinement 'XSCANS (Bruker)' _computing_data_reduction 'XSCANS (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-Plus (Bruker)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0137P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7330 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0181 _refine_ls_R_factor_gt 0.0121 _refine_ls_wR_factor_ref 0.0282 _refine_ls_wR_factor_gt 0.0281 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.343038(6) 0.071275(7) 0.349439(8) 0.05619(4) Uani 1 d . . . Cu2 Cu 0.169506(5) 0.153331(6) 0.465570(8) 0.05025(4) Uani 1 d . . . Cu3 Cu 0.152005(6) -0.067009(5) 0.370596(7) 0.04602(4) Uani 1 d . . . C1 C 0.21841(4) 0.04615(4) 0.39381(5) 0.03748(19) Uani 1 d . . . O1 O 0.26118(3) 0.08493(3) 0.38728(4) 0.04837(16) Uani 1 d . . . O2 O 0.17052(3) 0.06569(3) 0.42553(4) 0.04735(15) Uani 1 d . . . O3 O 0.22235(3) -0.00976(3) 0.36484(4) 0.04812(16) Uani 1 d . . . O4 O 0.32012(6) -0.00078(11) 0.25499(11) 0.1612(9) Uani 1 d . . . H4OA H 0.3253(15) 0.0149(15) 0.207(2) 0.233(16) Uiso 1 d . . . H4OB H 0.2818(14) -0.0081(15) 0.257(2) 0.257(16) Uiso 1 d . . . O5 O 0.44418(6) -0.04280(7) 0.87068(8) 0.0909(3) Uani 1 d . . . H5OC H 0.4673(10) -0.0135(11) 0.8936(13) 0.150(9) Uiso 1 d . . . H5OD H 0.4235(11) -0.0634(11) 0.8987(13) 0.148(10) Uiso 1 d . . . Cl1 Cl 0.085157(13) 0.061332(19) 0.59337(2) 0.07582(10) Uani 1 d . . . O6 O 0.08817(4) 0.11489(4) 0.54374(5) 0.0732(2) Uani 1 d . . . O7 O 0.05529(10) 0.06853(10) 0.66050(11) 0.0998(5) Uani 0.67 d P A 1 O8 O 0.05382(8) 0.01274(8) 0.54725(12) 0.0947(5) Uani 0.67 d P A 1 O9 O 0.14262(17) 0.03510(18) 0.60546(17) 0.0620(7) Uani 0.67 d P A 1 O7' O 0.08724(17) 0.09458(17) 0.6710(2) 0.0933(11) Uani 0.33 d P A 2 O8' O 0.03011(16) 0.03069(19) 0.5908(2) 0.0933(10) Uani 0.33 d P A 2 O9' O 0.1348(3) 0.0221(3) 0.5859(3) 0.0423(9) Uani 0.33 d P A 2 Cl2 Cl 0.257745(13) -0.184944(15) 0.346948(17) 0.06185(7) Uani 1 d . . . O10 O 0.20529(4) -0.15964(5) 0.31854(6) 0.0834(3) Uani 1 d . . . O11 O 0.23834(11) -0.23603(11) 0.40059(13) 0.0991(7) Uani 0.50 d P B 1 O12 O 0.29126(7) -0.21699(8) 0.29163(9) 0.0601(4) Uani 0.50 d P B 1 O13 O 0.29097(11) -0.14221(11) 0.39109(14) 0.0793(6) Uani 0.50 d P B 1 O11' O 0.26320(12) -0.25105(12) 0.33290(16) 0.1077(7) Uani 0.50 d P B 2 O12' O 0.30433(11) -0.15588(12) 0.29854(15) 0.1119(7) Uani 0.50 d P B 2 O13' O 0.27133(8) -0.15955(9) 0.41991(11) 0.0540(4) Uani 0.50 d P B 2 Cl3 Cl 0.406365(16) 0.167869(15) 0.510138(17) 0.06609(8) Uani 1 d . . . O14 O 0.35625(6) 0.18914(7) 0.46890(9) 0.1295(4) Uani 1 d . . . O15 O 0.45480(6) 0.17660(6) 0.46012(7) 0.1142(4) Uani 1 d . . . O16 O 0.39196(7) 0.10400(8) 0.52803(9) 0.1437(5) Uani 1 d . . . O17 O 0.41014(6) 0.20629(6) 0.57698(7) 0.1092(4) Uani 1 d . . . Cl4 Cl 0.30434(2) -0.07042(2) 0.62704(4) 0.11118(17) Uani 1 d . . . O20 O 0.28812(7) -0.10810(8) 0.56553(11) 0.1518(6) Uani 1 d . . . O18 O 0.36973(12) -0.06459(12) 0.61879(14) 0.1306(8) Uani 0.67 d P C 1 O19 O 0.2796(3) -0.0105(4) 0.6297(3) 0.1060(11) Uani 0.67 d P C 1 O21 O 0.2951(2) -0.1036(2) 0.7006(3) 0.2245(19) Uani 0.67 d P C 1 O18' O 0.35403(16) -0.07704(18) 0.6699(2) 0.0907(9) Uani 0.33 d P C 2 O19' O 0.2943(6) -0.0094(8) 0.6019(6) 0.126(3) Uani 0.33 d P C 2 O21' O 0.2569(3) -0.0955(3) 0.6627(4) 0.164(2) Uani 0.33 d P C 2 N1 N 0.34847(5) -0.00353(6) 0.41788(8) 0.0834(3) Uani 1 d . . . H1A H 0.3472 0.0113 0.4660 0.100 Uiso 1 calc R . . H1B H 0.3154 -0.0265 0.4108 0.100 Uiso 1 calc R . . N2 N 0.43178(5) 0.08097(6) 0.32514(7) 0.0824(3) Uani 1 d . . . H2C H 0.4466 0.1076 0.3612 0.099 Uiso 1 calc R . . N3 N 0.32519(5) 0.15383(6) 0.29946(6) 0.0875(4) Uani 1 d . . . H3A H 0.2889 0.1497 0.2792 0.105 Uiso 1 calc R . . H3B H 0.3219 0.1825 0.3373 0.105 Uiso 1 calc R . . N4 N 0.23452(4) 0.13087(5) 0.53870(6) 0.0679(3) Uani 1 d . . . H4A H 0.2321 0.0887 0.5467 0.081 Uiso 1 calc R . . H4B H 0.2687 0.1377 0.5140 0.081 Uiso 1 calc R . . N5 N 0.15110(4) 0.23923(4) 0.50867(8) 0.0683(3) Uani 1 d . . . H5C H 0.1753 0.2665 0.4833 0.082 Uiso 1 calc R . . N6 N 0.12810(5) 0.17697(5) 0.36884(7) 0.0810(3) Uani 1 d . . . H6A H 0.1529 0.2020 0.3422 0.097 Uiso 1 calc R . . H6B H 0.1235 0.1410 0.3417 0.097 Uiso 1 calc R . . N7 N 0.13308(5) -0.03541(5) 0.26722(5) 0.0674(3) Uani 1 d . . . H7A H 0.1069 -0.0036 0.2728 0.081 Uiso 1 calc R . . H7B H 0.1663 -0.0180 0.2484 0.081 Uiso 1 calc R . . N8 N 0.07688(4) -0.11886(4) 0.37258(6) 0.0575(2) Uani 1 d . . . H8C H 0.0475 -0.0900 0.3798 0.069 Uiso 1 calc R . . N9 N 0.17186(5) -0.07871(5) 0.47990(5) 0.0621(2) Uani 1 d . . . H9A H 0.2112 -0.0843 0.4825 0.075 Uiso 1 calc R . . H9B H 0.1640 -0.0416 0.5033 0.075 Uiso 1 calc R . . C2 C 0.39836(8) -0.04796(6) 0.41367(15) 0.1252(8) Uani 1 d . . . H2A H 0.3919 -0.0777 0.3723 0.150 Uiso 1 calc R . . H2B H 0.4007 -0.0721 0.4607 0.150 Uiso 1 calc R . . C3 C 0.45676(7) -0.01281(10) 0.40076(9) 0.1040(6) Uani 1 d . . . H3C H 0.4631 0.0153 0.4438 0.125 Uiso 1 calc R . . H3D H 0.4882 -0.0441 0.4015 0.125 Uiso 1 calc R . . C4 C 0.46299(8) 0.02422(7) 0.33222(11) 0.1066(6) Uani 1 d . . . H4C H 0.5045 0.0340 0.3262 0.128 Uiso 1 calc R . . H4D H 0.4519 -0.0027 0.2897 0.128 Uiso 1 calc R . . C5 C 0.44373(7) 0.11164(7) 0.25060(12) 0.1208(8) Uani 1 d . . . H5A H 0.4861 0.1139 0.2429 0.145 Uiso 1 calc R . . H5B H 0.4274 0.0854 0.2104 0.145 Uiso 1 calc R . . C6 C 0.41887(8) 0.17603(10) 0.24444(10) 0.1095(6) Uani 1 d . . . H6C H 0.4331 0.2003 0.2877 0.131 Uiso 1 calc R . . H6D H 0.4355 0.1955 0.1991 0.131 Uiso 1 calc R . . C7 C 0.36112(8) 0.18357(8) 0.24127(9) 0.1066(6) Uani 1 d . . . H7C H 0.3478 0.1678 0.1922 0.128 Uiso 1 calc R . . H7D H 0.3531 0.2289 0.2424 0.128 Uiso 1 calc R . . C8 C 0.24053(8) 0.16078(8) 0.61414(7) 0.0866(5) Uani 1 d . . . H8A H 0.2800 0.1533 0.6334 0.104 Uiso 1 calc R . . H8B H 0.2128 0.1413 0.6492 0.104 Uiso 1 calc R . . C9 C 0.22925(8) 0.23086(7) 0.61083(8) 0.0900(5) Uani 1 d . . . H9C H 0.2561 0.2499 0.5743 0.108 Uiso 1 calc R . . H9D H 0.2376 0.2493 0.6604 0.108 Uiso 1 calc R . . C10 C 0.16607(6) 0.24718(6) 0.58832(12) 0.0905(6) Uani 1 d . . . H10A H 0.1396 0.2209 0.6183 0.109 Uiso 1 calc R . . H10B H 0.1586 0.2911 0.6022 0.109 Uiso 1 calc R . . C11 C 0.09108(6) 0.26507(6) 0.49730(14) 0.1157(8) Uani 1 d . . . H11A H 0.0625 0.2366 0.5203 0.139 Uiso 1 calc R . . H11B H 0.0880 0.3059 0.5226 0.139 Uiso 1 calc R . . C12 C 0.07752(7) 0.27274(7) 0.41605(12) 0.0983(6) Uani 1 d . . . H12A H 0.1083 0.2982 0.3928 0.118 Uiso 1 calc R . . H12B H 0.0408 0.2961 0.4113 0.118 Uiso 1 calc R . . C13 C 0.07167(7) 0.20847(8) 0.37025(14) 0.1315(9) Uani 1 d . . . H13A H 0.0426 0.1813 0.3944 0.158 Uiso 1 calc R . . H13B H 0.0587 0.2172 0.3186 0.158 Uiso 1 calc R . . C14 C 0.10911(5) -0.07896(6) 0.20688(7) 0.0595(3) Uani 1 d . . . H14A H 0.0997 -0.0546 0.1615 0.071 Uiso 1 calc R . . H14B H 0.1387 -0.1103 0.1935 0.071 Uiso 1 calc R . . C15 C 0.05494(6) -0.11168(7) 0.23517(8) 0.0791(4) Uani 1 d . . . H15A H 0.0259 -0.0794 0.2473 0.095 Uiso 1 calc R . . H15B H 0.0390 -0.1369 0.1937 0.095 Uiso 1 calc R . . C16 C 0.06120(6) -0.15225(7) 0.30027(11) 0.0951(5) Uani 1 d . . . H16A H 0.0915 -0.1836 0.2894 0.114 Uiso 1 calc R . . H16B H 0.0244 -0.1749 0.3079 0.114 Uiso 1 calc R . . C17 C 0.06866(7) -0.16641(6) 0.43364(9) 0.0783(4) Uani 1 d . . . H17A H 0.0948 -0.2022 0.4248 0.094 Uiso 1 calc R . . H17B H 0.0284 -0.1820 0.4325 0.094 Uiso 1 calc R . . C18 C 0.08139(7) -0.13828(10) 0.51025(9) 0.1161(8) Uani 1 d . . . H18A H 0.0622 -0.0971 0.5135 0.139 Uiso 1 calc R . . H18B H 0.0640 -0.1654 0.5490 0.139 Uiso 1 calc R . . C19 C 0.14436(7) -0.13018(8) 0.52735(8) 0.0960(5) Uani 1 d . . . H19A H 0.1648 -0.1699 0.5180 0.115 Uiso 1 calc R . . H19B H 0.1490 -0.1198 0.5809 0.115 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.05055(8) 0.06543(8) 0.05259(8) -0.01900(6) 0.01076(6) -0.00839(6) Cu2 0.04031(6) 0.04823(7) 0.06221(8) 0.00523(6) -0.00014(6) -0.00050(5) Cu3 0.05170(7) 0.04134(6) 0.04503(7) 0.00725(5) 0.00398(5) -0.00005(5) C1 0.0535(5) 0.0339(4) 0.0251(4) -0.0001(3) -0.0078(4) -0.0025(4) O1 0.0366(3) 0.0539(4) 0.0546(4) -0.0079(3) 0.0033(3) -0.0136(3) O2 0.0447(4) 0.0513(4) 0.0461(4) -0.0026(3) 0.0055(3) 0.0067(3) O3 0.0419(4) 0.0441(4) 0.0583(4) -0.0052(3) 0.0059(3) -0.0091(3) O4 0.0729(8) 0.286(2) 0.1242(12) -0.1421(15) 0.0137(7) -0.0226(10) O5 0.0936(8) 0.0843(7) 0.0947(8) 0.0017(7) 0.0007(7) 0.0007(6) Cl1 0.04747(15) 0.1052(3) 0.0748(2) 0.0343(2) 0.00838(13) 0.00355(16) O6 0.0729(5) 0.0749(6) 0.0719(5) -0.0004(5) -0.0009(4) -0.0005(4) O7 0.1076(15) 0.1025(14) 0.0892(12) 0.0078(11) 0.0108(11) 0.0109(11) O8 0.0980(12) 0.0810(11) 0.1050(13) 0.0063(10) -0.0098(11) -0.0038(9) O9 0.0614(13) 0.0714(17) 0.0531(18) -0.0012(11) 0.0007(11) 0.0048(11) O7' 0.086(2) 0.084(2) 0.110(3) 0.000(2) -0.002(2) -0.0269(18) O8' 0.097(3) 0.106(3) 0.077(2) -0.0117(19) 0.0147(18) 0.008(2) O9' 0.0470(19) 0.052(2) 0.028(2) -0.0036(15) -0.0063(14) 0.0020(15) Cl2 0.05513(16) 0.06887(18) 0.06154(16) -0.00234(15) -0.00532(12) 0.00958(13) O10 0.0824(6) 0.0848(6) 0.0830(6) 0.0009(5) 0.0000(5) 0.0018(5) O11 0.1000(16) 0.1063(17) 0.0910(15) -0.0055(13) 0.0021(12) -0.0002(13) O12 0.0632(9) 0.0554(10) 0.0617(9) 0.0047(8) 0.0008(7) -0.0071(8) O13 0.0816(16) 0.0777(15) 0.0787(15) 0.0081(12) 0.0079(11) -0.0043(11) O11' 0.1101(18) 0.0964(17) 0.1166(19) -0.0042(15) -0.0111(15) 0.0055(15) O12' 0.1098(17) 0.1142(19) 0.1116(18) 0.0023(15) 0.0023(16) -0.0036(15) O13' 0.0529(11) 0.0514(11) 0.0576(12) -0.0033(9) -0.0034(8) 0.0015(8) Cl3 0.0852(2) 0.05667(16) 0.05642(15) -0.00017(13) -0.01018(14) -0.01061(14) O14 0.1267(11) 0.1327(11) 0.1292(11) -0.0017(9) -0.0021(9) 0.0002(9) O15 0.1116(9) 0.1188(10) 0.1123(9) 0.0014(8) -0.0025(8) -0.0003(7) O16 0.1460(12) 0.1401(12) 0.1449(12) -0.0038(10) 0.0031(11) -0.0003(10) O17 0.1098(9) 0.1085(8) 0.1094(9) 0.0006(7) -0.0017(7) 0.0007(7) Cl4 0.1129(4) 0.0677(2) 0.1530(5) -0.0365(3) -0.0436(4) -0.0033(2) O20 0.1419(13) 0.1559(14) 0.1576(14) 0.0081(12) 0.0052(11) 0.0031(11) O18 0.136(2) 0.143(2) 0.1133(18) 0.0129(15) 0.0131(15) -0.0066(15) O19 0.112(3) 0.0955(17) 0.110(3) 0.001(2) 0.0042(16) -0.0059(17) O21 0.202(4) 0.257(4) 0.215(5) 0.009(4) -0.035(3) 0.003(3) O18' 0.070(2) 0.096(2) 0.106(3) -0.012(2) -0.0123(19) 0.0059(17) O19' 0.123(7) 0.108(4) 0.147(9) 0.016(6) -0.030(5) -0.005(5) O21' 0.193(7) 0.154(5) 0.144(5) -0.005(4) 0.041(5) -0.023(5) N1 0.0667(7) 0.0786(8) 0.1048(9) -0.0149(7) 0.0149(6) 0.0282(6) N2 0.0602(6) 0.1041(9) 0.0830(8) -0.0220(7) -0.0037(6) 0.0198(6) N3 0.0882(8) 0.1163(10) 0.0578(7) 0.0444(7) 0.0084(6) -0.0176(7) N4 0.0521(5) 0.0813(7) 0.0702(6) -0.0160(5) 0.0054(5) 0.0017(5) N5 0.0519(5) 0.0482(5) 0.1048(9) 0.0049(6) 0.0241(5) -0.0168(4) N6 0.0870(8) 0.0591(6) 0.0969(8) 0.0049(6) -0.0361(7) -0.0256(6) N7 0.0801(7) 0.0689(6) 0.0531(5) 0.0094(5) -0.0039(5) -0.0174(5) N8 0.0428(4) 0.0474(5) 0.0824(7) 0.0216(5) 0.0163(5) 0.0110(4) N9 0.0766(6) 0.0690(6) 0.0409(5) 0.0088(4) 0.0019(4) -0.0011(5) C2 0.1003(12) 0.0347(6) 0.241(2) 0.0315(10) 0.0594(14) 0.0119(7) C3 0.0839(10) 0.1591(17) 0.0691(9) -0.0001(10) 0.0011(8) 0.0634(11) C4 0.1114(13) 0.0713(9) 0.1370(16) -0.0536(10) 0.0555(11) -0.0075(9) C5 0.1101(12) 0.0667(9) 0.1854(18) -0.0111(10) 0.1230(13) -0.0022(8) C6 0.1021(12) 0.1418(17) 0.0847(11) 0.0283(11) 0.0394(10) 0.0012(12) C7 0.1388(15) 0.0898(11) 0.0912(10) 0.0048(9) 0.0816(11) -0.0520(10) C8 0.1075(11) 0.1170(12) 0.0354(6) -0.0326(7) -0.0028(7) -0.0039(9) C9 0.1169(12) 0.0865(10) 0.0666(8) -0.0274(8) 0.0236(8) -0.0348(9) C10 0.0577(8) 0.0448(6) 0.1690(18) -0.0210(8) 0.0524(9) -0.0027(6) C11 0.0574(8) 0.0396(7) 0.250(3) 0.0228(10) 0.0432(12) 0.0202(5) C12 0.0672(9) 0.0590(8) 0.1686(18) 0.0494(10) -0.0217(10) 0.0086(6) C13 0.0661(9) 0.0839(11) 0.245(3) 0.0779(14) -0.0572(12) 0.0100(8) C14 0.0542(6) 0.0702(7) 0.0541(6) 0.0086(6) 0.0088(5) 0.0094(5) C15 0.0620(7) 0.1026(11) 0.0727(8) -0.0489(8) -0.0025(7) 0.0141(7) C16 0.0691(8) 0.0639(8) 0.1524(16) 0.0097(9) -0.0460(10) 0.0141(7) C17 0.0825(9) 0.0629(8) 0.0893(10) 0.0433(7) 0.0038(7) -0.0039(7) C18 0.0800(10) 0.1673(18) 0.1011(13) 0.0944(13) 0.0483(9) 0.0150(10) C19 0.1038(11) 0.1265(13) 0.0576(7) 0.0670(9) -0.0010(8) 0.0223(10) _geom_special_details ; Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 7.1315 (0.0023) x - 7.2241 (0.0022) y + 15.5293 (0.0032) z = 7.3267 (0.0015) * 0.0313 (0.0003) Cu1 * 0.0044 (0.0003) Cu2 * -0.0035 (0.0003) Cu3 * 0.0131 (0.0007) C1 * -0.0636 (0.0006) O1 * 0.0230 (0.0005) O2 * -0.0047 (0.0005) O3 Rms deviation of fitted atoms = 0.0287 6.2000 (0.0044) x - 7.2718 (0.0042) y + 15.7519 (0.0036) z = 7.2098 (0.0017) Angle to previous plane (with approximate esd) = 2.47 ( 0.02 ) * 0.0000 (0.0000) N2 * 0.0000 (0.0000) N5 * 0.0000 (0.0000) N8 Rms deviation of fitted atoms = 0.0000 6.9791 (0.0016) x - 7.2608 (0.0016) y + 15.5589 (0.0031) z = 7.3134 (0.0015) Angle to previous plane (with approximate esd) = 2.07 ( 0.02 ) * 0.0000 (0.0000) Cu1 * 0.0000 (0.0000) Cu2 * 0.0000 (0.0000) Cu3 Rms deviation of fitted atoms = 0.0000 7.9593 (0.0099) x - 6.9072 (0.0090) y + 15.3878 (0.0049) z = 7.4585 (0.0024) Angle to previous plane (with approximate esd) = 2.72 ( 0.04 ) * 0.0211 (0.0007) C1 * -0.0070 (0.0002) O1 * -0.0070 (0.0002) O2 * -0.0071 (0.0002) O3 Rms deviation of fitted atoms = 0.0122 5.3866 (0.0081) x + 11.3738 (0.0088) y + 14.1608 (0.0055) z = 7.7622 (0.0029) Angle to previous plane (with approximate esd) = 52.16 ( 0.03 ) * -0.1554 (0.0005) Cu1 * -0.0078 (0.0006) N1 * 0.0887 (0.0005) N2 * -0.0203 (0.0006) N3 * 0.0948 (0.0006) O1 Rms deviation of fitted atoms = 0.0911 - 17.7132 (0.0068) x - 6.6690 (0.0063) y + 9.4284 (0.0064) z = 0.3045 (0.0039) Angle to previous plane (with approximate esd) = 85.62 ( 0.03 ) * 0.0600 (0.0004) Cu2 * -0.2523 (0.0005) N4 * 0.2196 (0.0004) N5 * -0.2763 (0.0006) N6 * 0.2490 (0.0005) O2 Rms deviation of fitted atoms = 0.2253 7.9593 (0.0099) x - 6.9072 (0.0090) y + 15.3878 (0.0049) z = 7.4585 (0.0024) Angle to previous plane (with approximate esd) = 72.50 ( 0.03 ) * 0.0211 (0.0007) C1 * -0.0070 (0.0002) O1 * -0.0070 (0.0002) O2 * -0.0071 (0.0002) O3 Rms deviation of fitted atoms = 0.0122 12.1294 (0.0060) x - 16.4723 (0.0052) y - 5.5560 (0.0071) z = 0.7934 (0.0031) Angle to previous plane (with approximate esd) = 80.35 ( 0.03 ) * 0.0951 (0.0004) Cu3 * -0.0806 (0.0005) N7 * 0.0269 (0.0004) N8 * -0.0787 (0.0005) N9 * 0.0373 (0.0005) O3 Rms deviation of fitted atoms = 0.0691 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 N1 1.9832(13) . ? Cu1 N3 1.9870(11) . ? Cu1 O1 1.9914(7) . ? Cu1 N2 2.0660(12) . ? Cu1 O4 2.3051(12) . ? Cu2 O2 1.9729(8) . ? Cu2 N6 2.0025(11) . ? Cu2 N5 2.0025(11) . ? Cu2 N4 2.0104(11) . ? Cu2 O6 2.4360(10) . ? Cu3 N7 1.9791(10) . ? Cu3 N9 1.9857(10) . ? Cu3 O3 2.0006(7) . ? Cu3 N8 2.0223(9) . ? Cu3 O10 2.4676(10) . ? C1 O1 1.2720(11) . ? C1 O3 1.2842(11) . ? C1 O2 1.2872(11) . ? O4 H4OA 0.91(3) . ? O4 H4OB 0.88(3) . ? O5 H5OC 0.90(2) . ? O5 H5OD 0.80(2) . ? Cl1 O7 1.3672(19) . ? Cl1 O9' 1.401(7) . ? Cl1 O8' 1.405(4) . ? Cl1 O6 1.4256(10) . ? Cl1 O9 1.430(4) . ? Cl1 O8 1.4846(19) . ? Cl1 O7' 1.531(4) . ? Cl2 O10 1.3946(10) . ? Cl2 O12 1.4049(17) . ? Cl2 O13 1.405(3) . ? Cl2 O11' 1.418(2) . ? Cl2 O13' 1.4212(19) . ? Cl2 O12' 1.487(3) . ? Cl2 O11 1.495(2) . ? Cl3 O15 1.4174(13) . ? Cl3 O16 1.4176(17) . ? Cl3 O14 1.4192(15) . ? Cl3 O17 1.4270(13) . ? Cl4 O21' 1.352(7) . ? Cl4 O18' 1.361(3) . ? Cl4 O19' 1.376(16) . ? Cl4 O19 1.381(8) . ? Cl4 O20 1.3887(18) . ? Cl4 O21 1.482(5) . ? Cl4 O18 1.494(3) . ? N1 C2 1.4688(17) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C4 1.3929(19) . ? N2 C5 1.484(2) . ? N2 H2C 0.9100 . ? N3 C7 1.4482(14) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C8 1.4721(14) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C10 1.448(2) . ? N5 C11 1.4783(16) . ? N5 H5C 0.9100 . ? N6 C13 1.4406(19) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C14 1.5018(16) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C17 1.4777(14) . ? N8 C16 1.493(2) . ? N8 H8C 0.9100 . ? N9 C19 1.5013(16) . ? N9 H9A 0.9000 . ? N9 H9B 0.9000 . ? C2 C3 1.533(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.440(2) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.471(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.320(2) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C8 C9 1.497(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.525(2) . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.468(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.578(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.4925(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.433(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.497(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.468(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 166.72(5) . . ? N1 Cu1 O1 88.30(4) . . ? N3 Cu1 O1 80.30(4) . . ? N1 Cu1 N2 98.21(5) . . ? N3 Cu1 N2 91.20(5) . . ? O1 Cu1 N2 164.06(4) . . ? N1 Cu1 O4 85.86(8) . . ? N3 Cu1 O4 102.20(8) . . ? O1 Cu1 O4 97.16(4) . . ? N2 Cu1 O4 97.80(5) . . ? O2 Cu2 N6 86.30(4) . . ? O2 Cu2 N5 168.50(3) . . ? N6 Cu2 N5 89.92(5) . . ? O2 Cu2 N4 89.96(4) . . ? N6 Cu2 N4 160.57(5) . . ? N5 Cu2 N4 97.10(5) . . ? O2 Cu2 O6 84.22(3) . . ? N6 Cu2 O6 101.84(4) . . ? N5 Cu2 O6 85.93(3) . . ? N4 Cu2 O6 96.73(4) . . ? N7 Cu3 N9 167.50(4) . . ? N7 Cu3 O3 85.66(4) . . ? N9 Cu3 O3 86.72(4) . . ? N7 Cu3 N8 90.82(4) . . ? N9 Cu3 N8 96.16(4) . . ? O3 Cu3 N8 175.19(3) . . ? N7 Cu3 O10 91.82(4) . . ? N9 Cu3 O10 98.56(4) . . ? O3 Cu3 O10 93.81(3) . . ? N8 Cu3 O10 89.58(4) . . ? O1 C1 O3 119.90(9) . . ? O1 C1 O2 118.47(8) . . ? O3 C1 O2 121.49(8) . . ? C1 O1 Cu1 130.35(6) . . ? C1 O2 Cu2 117.53(6) . . ? C1 O3 Cu3 118.41(6) . . ? Cu1 O4 H4OA 113(2) . . ? Cu1 O4 H4OB 108(2) . . ? H4OA O4 H4OB 103(3) . . ? H5OC O5 H5OD 116(2) . . ? O7 Cl1 O9' 122.9(3) . . ? O7 Cl1 O8' 68.82(17) . . ? O9' Cl1 O8' 116.0(3) . . ? O7 Cl1 O6 117.56(9) . . ? O9' Cl1 O6 111.7(3) . . ? O8' Cl1 O6 112.67(16) . . ? O7 Cl1 O9 111.46(16) . . ? O9' Cl1 O9 19.24(19) . . ? O8' Cl1 O9 129.5(2) . . ? O6 Cl1 O9 110.60(17) . . ? O7 Cl1 O8 108.01(13) . . ? O9' Cl1 O8 85.82(19) . . ? O8' Cl1 O8 40.71(13) . . ? O6 Cl1 O8 103.52(8) . . ? O9 Cl1 O8 104.54(13) . . ? O7 Cl1 O7' 36.73(12) . . ? O9' Cl1 O7' 109.1(2) . . ? O8' Cl1 O7' 105.4(2) . . ? O6 Cl1 O7' 100.42(15) . . ? O9 Cl1 O7' 90.94(18) . . ? O8 Cl1 O7' 144.47(15) . . ? Cl1 O6 Cu2 129.99(5) . . ? O10 Cl2 O12 113.39(8) . . ? O10 Cl2 O13 114.18(11) . . ? O12 Cl2 O13 113.46(12) . . ? O10 Cl2 O11' 112.74(11) . . ? O12 Cl2 O11' 50.36(12) . . ? O13 Cl2 O11' 132.57(14) . . ? O10 Cl2 O13' 111.30(9) . . ? O12 Cl2 O13' 133.29(10) . . ? O13 Cl2 O13' 31.45(8) . . ? O11' Cl2 O13' 120.43(13) . . ? O10 Cl2 O12' 104.13(11) . . ? O12 Cl2 O12' 54.44(11) . . ? O13 Cl2 O12' 70.82(14) . . ? O11' Cl2 O12' 104.01(16) . . ? O13' Cl2 O12' 101.91(13) . . ? O10 Cl2 O11 104.41(10) . . ? O12 Cl2 O11 104.44(12) . . ? O13 Cl2 O11 105.68(13) . . ? O11' Cl2 O11 55.25(14) . . ? O13' Cl2 O11 76.49(12) . . ? O12' Cl2 O11 149.82(14) . . ? Cl2 O10 Cu3 125.88(6) . . ? O15 Cl3 O16 115.99(9) . . ? O15 Cl3 O14 105.26(8) . . ? O16 Cl3 O14 103.14(9) . . ? O15 Cl3 O17 112.91(7) . . ? O16 Cl3 O17 111.61(9) . . ? O14 Cl3 O17 106.77(8) . . ? O21' Cl4 O18' 111.3(4) . . ? O21' Cl4 O19' 112.4(5) . . ? O18' Cl4 O19' 114.2(6) . . ? O21' Cl4 O19 91.0(4) . . ? O18' Cl4 O19 114.3(3) . . ? O19' Cl4 O19 24.7(4) . . ? O21' Cl4 O20 85.8(3) . . ? O18' Cl4 O20 126.15(17) . . ? O19' Cl4 O20 103.9(6) . . ? O19 Cl4 O20 116.1(3) . . ? O21' Cl4 O21 45.6(3) . . ? O18' Cl4 O21 65.7(2) . . ? O19' Cl4 O21 134.0(5) . . ? O19 Cl4 O21 110.1(3) . . ? O20 Cl4 O21 111.8(2) . . ? O21' Cl4 O18 150.0(4) . . ? O18' Cl4 O18 40.63(18) . . ? O19' Cl4 O18 93.2(5) . . ? O19 Cl4 O18 109.3(3) . . ? O20 Cl4 O18 103.54(13) . . ? O21 Cl4 O18 105.3(2) . . ? C2 N1 Cu1 121.48(10) . . ? C2 N1 H1A 107.0 . . ? Cu1 N1 H1A 107.0 . . ? C2 N1 H1B 107.0 . . ? Cu1 N1 H1B 107.0 . . ? H1A N1 H1B 106.7 . . ? C4 N2 C5 111.01(12) . . ? C4 N2 Cu1 113.04(11) . . ? C5 N2 Cu1 113.75(10) . . ? C4 N2 H2C 106.1 . . ? C5 N2 H2C 106.1 . . ? Cu1 N2 H2C 106.1 . . ? C7 N3 Cu1 125.04(11) . . ? C7 N3 H3A 106.1 . . ? Cu1 N3 H3A 106.1 . . ? C7 N3 H3B 106.1 . . ? Cu1 N3 H3B 106.1 . . ? H3A N3 H3B 106.3 . . ? C8 N4 Cu2 122.78(9) . . ? C8 N4 H4A 106.6 . . ? Cu2 N4 H4A 106.6 . . ? C8 N4 H4B 106.6 . . ? Cu2 N4 H4B 106.6 . . ? H4A N4 H4B 106.6 . . ? C10 N5 C11 107.66(13) . . ? C10 N5 Cu2 114.84(8) . . ? C11 N5 Cu2 118.19(9) . . ? C10 N5 H5C 104.9 . . ? C11 N5 H5C 104.9 . . ? Cu2 N5 H5C 104.9 . . ? C13 N6 Cu2 121.04(12) . . ? C13 N6 H6A 107.1 . . ? Cu2 N6 H6A 107.1 . . ? C13 N6 H6B 107.1 . . ? Cu2 N6 H6B 107.1 . . ? H6A N6 H6B 106.8 . . ? C14 N7 Cu3 121.33(8) . . ? C14 N7 H7A 107.0 . . ? Cu3 N7 H7A 107.0 . . ? C14 N7 H7B 107.0 . . ? Cu3 N7 H7B 107.0 . . ? H7A N7 H7B 106.7 . . ? C17 N8 C16 105.55(11) . . ? C17 N8 Cu3 118.92(8) . . ? C16 N8 Cu3 116.06(8) . . ? C17 N8 H8C 105.0 . . ? C16 N8 H8C 105.0 . . ? Cu3 N8 H8C 105.0 . . ? C19 N9 Cu3 122.08(9) . . ? C19 N9 H9A 106.8 . . ? Cu3 N9 H9A 106.8 . . ? C19 N9 H9B 106.8 . . ? Cu3 N9 H9B 106.8 . . ? H9A N9 H9B 106.7 . . ? N1 C2 C3 111.43(11) . . ? N1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 117.96(16) . . ? C4 C3 H3C 107.8 . . ? C2 C3 H3C 107.8 . . ? C4 C3 H3D 107.8 . . ? C2 C3 H3D 107.8 . . ? H3C C3 H3D 107.2 . . ? N2 C4 C3 119.23(13) . . ? N2 C4 H4C 107.5 . . ? C3 C4 H4C 107.5 . . ? N2 C4 H4D 107.5 . . ? C3 C4 H4D 107.5 . . ? H4C C4 H4D 107.0 . . ? C6 C5 N2 113.28(12) . . ? C6 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 119.58(18) . . ? C7 C6 H6C 107.4 . . ? C5 C6 H6C 107.4 . . ? C7 C6 H6D 107.4 . . ? C5 C6 H6D 107.4 . . ? H6C C6 H6D 107.0 . . ? C6 C7 N3 118.44(17) . . ? C6 C7 H7C 107.7 . . ? N3 C7 H7C 107.7 . . ? C6 C7 H7D 107.7 . . ? N3 C7 H7D 107.7 . . ? H7C C7 H7D 107.1 . . ? N4 C8 C9 111.72(12) . . ? N4 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N4 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 113.08(13) . . ? C8 C9 H9C 109.0 . . ? C10 C9 H9C 109.0 . . ? C8 C9 H9D 109.0 . . ? C10 C9 H9D 109.0 . . ? H9C C9 H9D 107.8 . . ? N5 C10 C9 116.36(11) . . ? N5 C10 H10A 108.2 . . ? C9 C10 H10A 108.2 . . ? N5 C10 H10B 108.2 . . ? C9 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? C12 C11 N5 111.37(14) . . ? C12 C11 H11A 109.4 . . ? N5 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? N5 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 114.73(12) . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? C11 C12 H12B 108.6 . . ? C13 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N6 C13 C12 109.14(12) . . ? N6 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? N6 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C15 C14 N7 110.13(9) . . ? C15 C14 H14A 109.6 . . ? N7 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? N7 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 117.28(12) . . ? C16 C15 H15A 108.0 . . ? C14 C15 H15A 108.0 . . ? C16 C15 H15B 108.0 . . ? C14 C15 H15B 108.0 . . ? H15A C15 H15B 107.2 . . ? C15 C16 N8 114.90(12) . . ? C15 C16 H16A 108.5 . . ? N8 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? N8 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N8 C17 C18 111.07(12) . . ? N8 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? N8 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C19 C18 C17 114.63(14) . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C18 C19 N9 111.96(10) . . ? C18 C19 H19A 109.2 . . ? N9 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? N9 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5OC O8' 0.90(2) 1.72(2) 2.576(4) 157(2) 6_657 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.148 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.019