# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Ashutosh Ghosh' _publ_contact_author_address ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; _publ_contact_author_email 'ghosh 59@yahoo.com' loop_ _publ_author_name _publ_author_address 'M.Sinha Ray' ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; A.Das ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; M.G.B.Drew ; Department of Chemistry The University of Reading PO BOX 224,Whiteknights Reading RG6 6AD,UK ; J.Ribas-Arino ; Departament de Quimica Fisica and CeRQT Universitat de Barcelona Av. Diagonal, 647 08028-Barcelona Spain ; J.Novoa ; Departament de Quimica Fisica and CeRQT Universitat de Barcelona Av. Diagonal, 647 08028-Barcelona Spain ; J.Ribas ; Departament de Quimica Inorganica Facultat de Quimica Universitat de Barcelona Av. Diagonal, 647 08028-Barcelona Spain ; ; A.Ghosh ; ; Department of Chemistry University of Calcutta 92 Acharya Prafulla Chandra Road Kolkata 700 009 India ; _publ_section_title ; A new tetrameric CuII cluster with square topology exhibiting ferro- and antiferromagnetic magnetic pathways : which is which? ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 207155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H53 Cl4 Cu4 N10 O29.5 ' _chemical_formula_weight 1637.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.275(16) _cell_length_b 14.520(16) _cell_length_c 20.52(2) _cell_angle_alpha 86.969(10) _cell_angle_beta 77.615(10) _cell_angle_gamma 73.435(10) _cell_volume 3145(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9549 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 26.21 _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1654 _exptl_absorpt_coefficient_mu 1.601 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9549 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.21 _reflns_number_total 9549 _reflns_number_gt 4875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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^)+(0.1313P)^2^+3.0849P] 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 SHELXL _refine_ls_extinction_coef 0.0009(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9549 _refine_ls_number_parameters 841 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1669 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2352 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _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 Cu1A Cu 0.33578(12) 0.34924(11) 0.44174(7) 0.0509(4) Uani 1 d . . . Cu2A Cu 0.29787(12) 0.71487(10) 0.43213(7) 0.0465(4) Uani 1 d . . . O10A O 0.4164(9) 0.8147(8) 0.4186(5) 0.089(3) Uani 1 d . . . O20A O 0.3964(16) 0.1724(13) 0.4466(9) 0.073(5) Uiso 0.50 d P . . N11A N 0.2151(7) 0.3656(7) 0.5273(4) 0.047(2) Uani 1 d . . . C12A C 0.2400(12) 0.3758(10) 0.5872(7) 0.067(4) Uani 1 d . . . H12A H 0.3216 0.3748 0.5899 0.080 Uiso 1 calc R . . C13A C 0.1477(12) 0.3877(10) 0.6447(6) 0.067(4) Uani 1 d . . . H13A H 0.1670 0.3888 0.6865 0.080 Uiso 1 calc R . . C14A C 0.0240(12) 0.3980(9) 0.6379(7) 0.064(3) Uani 1 d . . . H14A H -0.0401 0.4081 0.6760 0.077 Uiso 1 calc R . . C15A C -0.0059(10) 0.3938(8) 0.5784(6) 0.053(3) Uani 1 d . . . H15A H -0.0890 0.4023 0.5745 0.063 Uiso 1 calc R . . C16A C 0.0938(10) 0.3760(8) 0.5228(6) 0.052(3) Uani 1 d . . . C17A C 0.0725(9) 0.3679(8) 0.4544(5) 0.043(3) Uani 1 d . . . C18A C -0.0394(11) 0.3763(9) 0.4390(8) 0.068(4) Uani 1 d . . . H18A H -0.1123 0.3867 0.4724 0.082 Uiso 1 calc R . . C19A C -0.0459(14) 0.3691(11) 0.3718(9) 0.092(5) Uani 1 d . . . H19A H -0.1239 0.3812 0.3598 0.110 Uiso 1 calc R . . C20A C 0.0620(12) 0.3445(10) 0.3250(8) 0.073(4) Uani 1 d . . . H20A H 0.0647 0.3311 0.2808 0.088 Uiso 1 calc R . . C21A C 0.1669(12) 0.3413(9) 0.3491(6) 0.057(3) Uani 1 d . . . H21A H 0.2416 0.3310 0.3171 0.068 Uiso 1 calc R . . N22A N 0.1783(8) 0.3505(7) 0.4100(5) 0.052(2) Uani 1 d . . . N31A N 0.1315(9) 0.8113(7) 0.4706(5) 0.052(2) Uani 1 d . . . C32A C 0.0942(13) 0.8365(10) 0.5357(7) 0.070(4) Uani 1 d . . . H32A H 0.1493 0.8150 0.5646 0.084 Uiso 1 calc R . . C33A C -0.0290(18) 0.8955(13) 0.5593(7) 0.117(7) Uani 1 d . . . H33A H -0.0540 0.9182 0.6031 0.141 Uiso 1 calc R . . C34A C -0.1129(17) 0.9197(15) 0.5163(10) 0.127(7) Uani 1 d . . . H34A H -0.1977 0.9508 0.5329 0.153 Uiso 1 calc R . . C35A C -0.0709(14) 0.8976(13) 0.4487(9) 0.096(5) Uani 1 d . . . H35A H -0.1238 0.9189 0.4186 0.115 Uiso 1 calc R . . C36A C 0.0552(11) 0.8416(10) 0.4277(7) 0.066(4) Uani 1 d . . . C37A C 0.1072(12) 0.8055(9) 0.3572(6) 0.056(3) Uani 1 d . . . C38A C 0.0481(11) 0.8323(9) 0.3086(6) 0.053(3) Uani 1 d . . . H38A H -0.0318 0.8762 0.3167 0.064 Uiso 1 calc R . . C39 C 0.1015(14) 0.7970(11) 0.2472(7) 0.077(4) Uani 1 d . . . H39A H 0.0590 0.8122 0.2122 0.093 Uiso 1 calc R . . C40A C 0.2222(14) 0.7373(11) 0.2386(7) 0.079(5) Uani 1 d . . . H40A H 0.2647 0.7151 0.1958 0.094 Uiso 1 calc R . . C41A C 0.2804(11) 0.7103(9) 0.2885(6) 0.052(3) Uani 1 d . . . H41A H 0.3609 0.6673 0.2815 0.063 Uiso 1 calc R . . N42A N 0.2217(8) 0.7456(6) 0.3493(5) 0.044(2) Uani 1 d . . . C53A C 0.4214(14) 0.5302(11) 0.3945(6) 0.063(4) Uani 1 d . . . O51A O 0.3260(9) 0.5105(7) 0.4247(4) 0.076(3) Uani 1 d . . . O52A O 0.4369(6) 0.6116(6) 0.3899(3) 0.0436(18) Uani 1 d . . . C54A C 0.5396(17) 0.4495(11) 0.3640(9) 0.105(6) Uani 1 d . . . H54A H 0.5322 0.4438 0.3183 0.126 Uiso 1 calc R . . H54B H 0.6095 0.4770 0.3614 0.126 Uiso 1 calc R . . C55A C 0.5823(16) 0.3611(18) 0.3827(8) 0.128(9) Uani 1 d . . . H55A H 0.6638 0.3281 0.3544 0.153 Uiso 1 calc R . . N56A N 0.4573(11) 0.3354(12) 0.3586(6) 0.107(5) Uani 1 d . . . H56A H 0.4796 0.2753 0.3420 0.128 Uiso 1 calc R . . H56B H 0.4275 0.3774 0.3281 0.128 Uiso 1 calc R . . C57A C 0.5818(11) 0.3431(9) 0.4546(6) 0.055(3) Uani 1 d . . . O58A O 0.4811(7) 0.3313(7) 0.4836(4) 0.074(3) Uani 1 d . . . O59A O 0.6819(7) 0.3256(6) 0.4764(4) 0.055(2) Uani 1 d . . . Cu2B Cu 0.08907(12) 1.21169(10) 0.92467(6) 0.0442(4) Uani 1 d . . . Cu1B Cu 0.32237(12) 0.85040(11) 0.93896(7) 0.0492(4) Uani 1 d . . . O10B O 0.0877(9) 0.6878(7) 1.1011(5) 0.083(3) Uani 1 d . . . O20B O 0.398(2) 0.6653(16) 0.9301(11) 0.100(7) Uiso 0.50 d P . . N11B N 0.3630(8) 0.8720(6) 1.0249(4) 0.042(2) Uani 1 d . . . C12B C 0.2783(12) 0.8922(9) 1.0822(6) 0.056(3) Uani 1 d . . . H12B H 0.1951 0.8919 1.0848 0.067 Uiso 1 calc R . . C13B C 0.3179(14) 0.9140(9) 1.1396(6) 0.067(4) Uani 1 d . . . H13B H 0.2613 0.9247 1.1806 0.081 Uiso 1 calc R . . C14B C 0.4386(15) 0.9194(10) 1.1348(8) 0.074(4) Uani 1 d . . . H14B H 0.4632 0.9354 1.1721 0.088 Uiso 1 calc R . . C15B C 0.5222(14) 0.9014(10) 1.0759(8) 0.072(4) Uani 1 d . . . H15B H 0.6046 0.9041 1.0727 0.087 Uiso 1 calc R . . C16B C 0.4855(12) 0.8791(9) 1.0211(7) 0.062(3) Uani 1 d . . . C17B C 0.5679(11) 0.8580(8) 0.9514(6) 0.049(3) Uani 1 d . . . C18B C 0.6998(14) 0.8490(11) 0.9391(9) 0.079(4) Uani 1 d . . . H18B H 0.7393 0.8592 0.9723 0.095 Uiso 1 calc R . . C19B C 0.7603(12) 0.8259(11) 0.8794(9) 0.079(4) Uani 1 d . . . H19B H 0.8470 0.8183 0.8695 0.095 Uiso 1 calc R . . C20B C 0.7024(13) 0.8112(11) 0.8279(7) 0.080(4) Uani 1 d . . . H20B H 0.7483 0.7983 0.7844 0.096 Uiso 1 calc R . . C21B C 0.5697(13) 0.8168(12) 0.8448(7) 0.084(5) Uani 1 d . . . H21B H 0.5288 0.8036 0.8131 0.100 Uiso 1 calc R . . N22B N 0.5076(8) 0.8413(7) 0.9067(5) 0.054(3) Uani 1 d . . . N42B N 0.2148(9) 1.2251(6) 0.8452(4) 0.046(2) Uani 1 d . . . C37B C 0.2774(10) 1.2921(9) 0.8479(5) 0.050(3) Uani 1 d . . . C38B C 0.2448(12) 1.1807(9) 0.7864(6) 0.058(3) Uani 1 d . . . H38B H 0.2008 1.1373 0.7808 0.070 Uiso 1 calc R . . C39B C 0.3346(14) 1.1936(11) 0.7338(7) 0.073(4) Uani 1 d . . . H39B H 0.3540 1.1557 0.6957 0.088 Uiso 1 calc R . . C40B C 0.3945(13) 1.2582(10) 0.7354(7) 0.072(4) Uani 1 d . . . H40B H 0.4514 1.2709 0.6984 0.086 Uiso 1 calc R . . C41B C 0.3669(11) 1.3079(11) 0.7972(7) 0.070(4) Uani 1 d . . . H41B H 0.4109 1.3513 0.8025 0.084 Uiso 1 calc R . . C36B C 0.2446(11) 1.3421(9) 0.9134(5) 0.050(3) Uani 1 d . . . C35B C 0.2898(15) 1.4097(12) 0.9281(9) 0.094(5) Uani 1 d . . . H35B H 0.3514 1.4290 0.8973 0.113 Uiso 1 calc R . . C34B C 0.2435(15) 1.4524(12) 0.9913(8) 0.091(5) Uani 1 d . . . H34B H 0.2766 1.4989 1.0039 0.109 Uiso 1 calc R . . C33B C 0.1510(17) 1.4260(12) 1.0335(8) 0.094(5) Uani 1 d . . . H33B H 0.1174 1.4557 1.0751 0.112 Uiso 1 calc R . . C32B C 0.1080(14) 1.3580(10) 1.0162(6) 0.066(4) Uani 1 d . . . H32B H 0.0469 1.3382 1.0471 0.080 Uiso 1 calc R . . N31B N 0.1486(9) 1.3161(7) 0.9559(5) 0.055(3) Uani 1 d . . . C57B C 0.0729(13) 0.8391(10) 0.9520(7) 0.063(4) Uani 1 d . . . O58B O 0.1645(8) 0.8249(7) 0.9845(4) 0.067(2) Uani 1 d . . . O59B O -0.0304(6) 0.8205(5) 0.9826(3) 0.0433(18) Uani 1 d . . . C55B C 0.1023(19) 0.8556(18) 0.8839(8) 0.126(9) Uani 1 d . . . H55B H 0.0640 0.8230 0.8571 0.151 Uiso 1 calc R . . C54B C 0.104(3) 0.9425(13) 0.8635(11) 0.185(14) Uani 1 d . . . H54C H 0.0192 0.9721 0.8560 0.222 Uiso 1 calc R . . H54D H 0.1586 0.9327 0.8195 0.222 Uiso 1 calc R . . C53B C 0.1368(16) 1.0212(10) 0.8940(6) 0.068(4) Uani 1 d . . . N56B N 0.2634(12) 0.8337(12) 0.8577(6) 0.115(5) Uani 1 d . . . H56D H 0.2823 0.8756 0.8261 0.138 Uiso 1 calc R . . H56C H 0.2990 0.7736 0.8412 0.138 Uiso 1 calc R . . O51B O 0.2202(11) 1.0108(8) 0.9239(5) 0.100(4) Uani 1 d . . . O52B O 0.0598(7) 1.1015(7) 0.8887(3) 0.052(2) Uani 1 d . . . Cl3 Cl 0.3715(8) 1.0357(6) 0.3174(4) 0.138(2) Uani 1 d . . . O32 O 0.2940(19) 0.9920(16) 0.3096(10) 0.188(8) Uani 1 d . . . O33 O 0.4139(16) 1.0065(12) 0.3761(8) 0.157(6) Uani 1 d . . . O34 O 0.4880(18) 1.0187(12) 0.2632(9) 0.161(6) Uani 1 d . . . O31 O 0.301(2) 1.1240(16) 0.3305(10) 0.237(12) Uani 1 d . . . Cl2 Cl 0.7308(4) 1.0906(4) 0.3319(2) 0.0873(12) Uani 1 d . . . O21 O 0.7526(14) 0.9950(12) 0.3143(8) 0.155(6) Uani 1 d . . . O22 O 0.6689(12) 1.1064(12) 0.4012(7) 0.152(6) Uani 1 d . . . O23 O 0.6469(13) 1.1553(12) 0.2935(8) 0.163(6) Uani 1 d . . . O24 O 0.8375(16) 1.1251(16) 0.3242(8) 0.196(8) Uani 1 d . . . Cl1 Cl 0.1612(5) 0.6140(4) 0.8092(2) 0.0959(14) Uani 1 d . . . O14 O 0.214(2) 0.6647(17) 0.7664(10) 0.249(12) Uani 1 d . . . O11 O 0.198(2) 0.5227(14) 0.7864(10) 0.227(10) Uani 1 d . . . O12 O 0.1965(12) 0.6174(10) 0.8681(6) 0.121(4) Uani 1 d . . . O13 O 0.0316(18) 0.6445(14) 0.8197(8) 0.182(7) Uani 1 d . . . Cl41 Cl 0.4133(11) 0.4466(8) 1.1857(5) 0.124(2) Uiso 0.583(9) d PD A 1 O41 O 0.4696(18) 0.5250(12) 1.1653(10) 0.124(2) Uiso 0.583(9) d PD A 1 O42 O 0.4996(17) 0.3607(11) 1.2073(10) 0.124(2) Uiso 0.583(9) d PD A 1 O43 O 0.3469(18) 0.4260(16) 1.1386(8) 0.124(2) Uiso 0.583(9) d PD A 1 O44 O 0.3149(17) 0.4860(14) 1.2513(8) 0.124(2) Uiso 0.583(9) d PD A 1 Cl51 Cl 0.3458(14) 0.4803(10) 1.1916(7) 0.124(2) Uiso 0.417(9) d PD A 2 O51 O 0.437(2) 0.5316(18) 1.2053(14) 0.124(2) Uiso 0.417(9) d PD A 2 O52 O 0.413(2) 0.3770(12) 1.1860(14) 0.124(2) Uiso 0.417(9) d PD A 2 O53 O 0.307(2) 0.517(2) 1.1289(9) 0.124(2) Uiso 0.417(9) d PD A 2 O54 O 0.235(2) 0.4997(19) 1.2462(10) 0.124(2) Uiso 0.417(9) d PD A 2 O400 O 0.0520(12) 0.5501(10) 1.1961(7) 0.128(4) Uiso 1 d . . . O401 O 0.3462(17) 0.6527(14) 1.0677(9) 0.081(5) Uiso 0.50 d P . . O403 O 0.376(3) 0.122(2) 0.5532(16) 0.163(11) Uiso 0.50 d P . . O404 O 0.072(3) 1.072(2) 1.2429(13) 0.134(9) Uiso 0.50 d P . . 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 Cu1A 0.0421(7) 0.0579(11) 0.0527(9) -0.0051(7) -0.0120(7) -0.0116(7) Cu2A 0.0447(7) 0.0469(10) 0.0471(8) 0.0040(7) -0.0103(6) -0.0119(7) O10A 0.104(7) 0.107(9) 0.074(6) -0.003(6) -0.011(6) -0.065(7) N11A 0.031(4) 0.053(7) 0.054(6) -0.001(5) -0.005(4) -0.012(4) C12A 0.056(8) 0.068(11) 0.075(10) -0.005(7) -0.017(7) -0.010(7) C13A 0.069(8) 0.074(11) 0.051(8) 0.005(7) -0.010(7) -0.012(7) C14A 0.055(8) 0.058(10) 0.077(10) 0.000(7) -0.006(7) -0.018(7) C15A 0.038(6) 0.040(8) 0.073(9) -0.007(6) 0.009(6) -0.013(5) C16A 0.051(7) 0.033(8) 0.066(8) 0.007(6) -0.009(6) -0.003(6) C17A 0.038(6) 0.039(8) 0.052(7) -0.004(5) -0.003(5) -0.015(5) C18A 0.050(7) 0.053(10) 0.116(12) 0.019(8) -0.034(8) -0.027(6) C19A 0.061(9) 0.088(13) 0.141(15) -0.020(10) -0.063(11) -0.011(8) C20A 0.057(8) 0.068(11) 0.092(11) 0.000(8) -0.011(8) -0.017(7) C21A 0.060(7) 0.059(10) 0.055(8) -0.001(6) -0.016(6) -0.019(6) N22A 0.046(5) 0.055(7) 0.057(6) -0.003(5) -0.004(5) -0.022(5) N31A 0.060(6) 0.044(7) 0.047(6) -0.002(5) -0.002(5) -0.014(5) C32A 0.075(9) 0.063(10) 0.070(10) 0.000(8) -0.024(7) -0.007(8) C33A 0.147(16) 0.098(15) 0.043(9) 0.004(9) 0.006(10) 0.046(13) C34A 0.090(12) 0.14(2) 0.104(15) -0.010(14) -0.007(11) 0.031(12) C35A 0.064(9) 0.111(15) 0.094(12) 0.008(10) -0.032(9) 0.014(9) C36A 0.053(7) 0.071(10) 0.063(9) 0.038(7) -0.002(7) -0.013(7) C37A 0.072(8) 0.049(9) 0.066(9) 0.020(6) -0.041(7) -0.031(7) C38A 0.053(7) 0.041(8) 0.061(8) 0.015(6) -0.014(6) -0.006(6) C39 0.088(10) 0.067(11) 0.071(10) 0.028(8) -0.024(8) -0.010(9) C40A 0.084(10) 0.088(12) 0.084(10) 0.045(9) -0.049(9) -0.040(9) C41A 0.059(7) 0.048(9) 0.047(7) -0.003(6) -0.010(6) -0.010(6) N42A 0.047(5) 0.032(6) 0.056(6) 0.005(5) -0.013(5) -0.016(5) C53A 0.087(10) 0.064(11) 0.036(7) 0.005(7) -0.005(7) -0.025(9) O51A 0.078(6) 0.089(8) 0.059(6) 0.002(5) -0.003(5) -0.031(6) O52A 0.048(4) 0.036(5) 0.042(4) 0.009(4) -0.006(3) -0.009(4) C54A 0.127(14) 0.053(11) 0.088(12) -0.006(9) 0.047(11) -0.002(10) C55A 0.091(12) 0.19(2) 0.055(10) 0.044(12) -0.003(9) 0.016(14) N56A 0.075(8) 0.167(15) 0.085(9) -0.033(9) 0.003(7) -0.052(9) C57A 0.041(6) 0.067(10) 0.041(7) -0.004(6) -0.005(6) 0.009(6) O58A 0.045(5) 0.115(9) 0.061(6) -0.002(5) -0.016(4) -0.016(5) O59A 0.044(4) 0.062(6) 0.049(5) -0.001(4) -0.012(4) 0.000(4) Cu2B 0.0478(7) 0.0433(10) 0.0442(8) 0.0003(6) -0.0094(6) -0.0171(7) Cu1B 0.0461(8) 0.0548(11) 0.0479(8) -0.0016(7) -0.0121(6) -0.0140(7) O10B 0.085(6) 0.057(7) 0.109(8) 0.026(6) -0.042(6) -0.011(5) N11B 0.040(5) 0.042(6) 0.047(6) -0.002(4) -0.011(4) -0.014(4) C12B 0.063(7) 0.058(9) 0.051(8) 0.005(6) -0.011(6) -0.023(7) C13B 0.089(10) 0.052(9) 0.056(8) -0.013(7) -0.022(7) -0.005(7) C14B 0.090(11) 0.062(11) 0.073(10) -0.010(8) -0.036(9) -0.012(8) C15B 0.073(9) 0.061(10) 0.095(11) 0.007(8) -0.058(9) -0.009(8) C16B 0.069(8) 0.043(9) 0.072(9) -0.002(7) -0.025(7) -0.003(7) C17B 0.057(7) 0.030(7) 0.055(7) 0.017(6) -0.009(6) -0.011(6) C18B 0.069(9) 0.065(11) 0.114(14) 0.004(10) -0.032(10) -0.024(8) C19B 0.041(7) 0.096(13) 0.106(12) 0.003(10) -0.016(8) -0.028(8) C20B 0.061(8) 0.100(13) 0.078(10) 0.006(9) 0.004(8) -0.033(8) C21B 0.073(9) 0.109(14) 0.072(10) -0.008(9) -0.007(8) -0.034(9) N22B 0.045(5) 0.061(8) 0.053(6) -0.006(5) 0.003(5) -0.019(5) N42B 0.065(6) 0.037(6) 0.044(6) 0.005(5) -0.016(5) -0.025(5) C37B 0.053(7) 0.045(8) 0.042(7) 0.017(6) -0.006(6) -0.004(6) C38B 0.072(8) 0.057(9) 0.052(8) 0.008(7) -0.007(7) -0.036(7) C39B 0.094(11) 0.067(11) 0.065(9) -0.001(8) -0.028(8) -0.025(9) C40B 0.073(9) 0.068(11) 0.076(10) 0.017(8) -0.011(8) -0.030(8) C41B 0.049(7) 0.089(12) 0.070(9) -0.014(8) -0.009(7) -0.018(7) C36B 0.058(7) 0.051(9) 0.046(7) -0.007(6) -0.007(6) -0.027(6) C35B 0.096(11) 0.086(13) 0.104(13) -0.018(10) -0.003(10) -0.041(10) C34B 0.105(12) 0.100(14) 0.078(11) -0.028(10) -0.008(9) -0.049(11) C33B 0.129(14) 0.078(13) 0.080(11) -0.015(9) 0.003(10) -0.054(11) C32B 0.107(11) 0.060(10) 0.039(7) -0.006(6) -0.016(7) -0.032(8) N31B 0.068(6) 0.047(7) 0.051(6) 0.013(5) -0.012(5) -0.022(5) C57B 0.077(9) 0.064(10) 0.069(9) -0.001(7) -0.027(7) -0.045(7) O58B 0.061(5) 0.091(8) 0.057(5) -0.003(5) -0.010(4) -0.032(5) O59B 0.046(4) 0.052(5) 0.039(4) 0.001(3) -0.005(3) -0.027(4) C55B 0.146(17) 0.24(3) 0.062(11) 0.016(13) -0.038(10) -0.150(19) C54B 0.41(4) 0.039(12) 0.110(16) -0.012(11) -0.13(2) -0.006(18) C53B 0.114(12) 0.039(9) 0.039(7) 0.006(6) -0.008(8) -0.011(9) N56B 0.083(9) 0.154(15) 0.083(9) -0.035(9) -0.022(7) 0.017(9) O51B 0.122(9) 0.088(9) 0.055(6) -0.001(5) -0.019(6) 0.026(7) O52B 0.054(5) 0.063(7) 0.045(5) -0.001(4) -0.018(4) -0.019(4) Cl3 0.147(6) 0.122(6) 0.136(6) 0.015(4) -0.040(5) -0.019(5) O32 0.171(17) 0.23(2) 0.182(18) 0.010(15) -0.047(14) -0.082(17) O33 0.183(15) 0.161(15) 0.133(12) -0.002(11) -0.055(11) -0.044(12) O34 0.193(16) 0.145(15) 0.167(15) -0.013(11) -0.066(14) -0.059(12) O31 0.29(3) 0.139(17) 0.197(19) -0.010(14) -0.037(17) 0.073(18) Cl2 0.083(3) 0.090(4) 0.092(3) 0.014(3) -0.025(2) -0.026(2) O21 0.142(12) 0.136(14) 0.181(15) -0.062(11) -0.056(11) -0.002(10) O22 0.112(10) 0.198(17) 0.112(11) -0.038(10) 0.010(8) -0.010(10) O23 0.121(10) 0.165(15) 0.197(15) 0.070(12) -0.051(11) -0.030(10) O24 0.146(13) 0.32(3) 0.146(14) 0.009(14) -0.043(11) -0.092(15) Cl1 0.112(4) 0.091(4) 0.064(3) 0.000(2) -0.011(2) 0.000(3) O14 0.31(3) 0.20(2) 0.150(17) 0.006(15) 0.054(17) -0.008(19) O11 0.27(2) 0.125(16) 0.24(2) -0.065(15) -0.089(18) 0.057(15) O12 0.124(9) 0.147(12) 0.095(9) 0.027(8) -0.027(8) -0.047(9) O13 0.169(15) 0.197(18) 0.149(14) -0.041(12) -0.052(12) 0.022(13) _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 Cu1A N56A 1.925(12) . ? Cu1A N11A 1.956(9) . ? Cu1A O58A 1.957(8) . ? Cu1A N22A 2.013(9) . ? Cu1A O51A 2.324(10) . ? Cu1A O20A 2.465(19) . ? Cu2A O52A 1.916(8) . ? Cu2A O59A 1.977(8) 2_666 ? Cu2A N31A 2.022(10) . ? Cu2A N42A 2.037(9) . ? Cu2A O10A 2.206(9) . ? Cu2A C53A 2.712(15) . ? N11A C12A 1.342(15) . ? N11A C16A 1.356(14) . ? C12A C13A 1.377(17) . ? C13A C14A 1.397(17) . ? C14A C15A 1.343(17) . ? C15A C16A 1.395(15) . ? C16A C17A 1.490(16) . ? C17A N22A 1.305(13) . ? C17A C18A 1.337(15) . ? C18A C19A 1.41(2) . ? C19A C20A 1.35(2) . ? C20A C21A 1.364(17) . ? C21A N22A 1.301(14) . ? N31A C36A 1.332(15) . ? N31A C32A 1.348(16) . ? C32A C33A 1.41(2) . ? C33A C34A 1.39(2) . ? C34A C35A 1.39(2) . ? C35A C36A 1.408(18) . ? C36A C37A 1.501(18) . ? C37A C38A 1.299(15) . ? C37A N42A 1.316(15) . ? C38A C39 1.334(18) . ? C39 C40A 1.369(19) . ? C40A C41A 1.317(15) . ? C41A N42A 1.333(14) . ? C53A O51A 1.222(15) . ? C53A O52A 1.239(15) . ? C53A C54A 1.540(19) . ? C54A C55A 1.30(2) . ? C55A C57A 1.483(18) . ? C55A N56A 1.73(2) . ? C57A O58A 1.217(14) . ? C57A O59A 1.258(13) . ? O59A Cu2A 1.977(8) 2_666 ? Cu2B O52B 1.935(8) . ? Cu2B O59B 1.954(7) 2_577 ? Cu2B N42B 1.959(9) . ? Cu2B N31B 2.006(10) . ? Cu2B O10B 2.257(9) 2_577 ? Cu2B C53B 2.743(14) . ? Cu1B O58B 1.950(8) . ? Cu1B N56B 1.973(12) . ? Cu1B N11B 1.976(9) . ? Cu1B N22B 2.019(9) . ? Cu1B O51B 2.322(10) . ? Cu1B O20B 2.58(2) . ? O10B Cu2B 2.257(9) 2_577 ? N11B C12B 1.333(14) . ? N11B C16B 1.399(15) . ? C12B C13B 1.426(16) . ? C13B C14B 1.368(19) . ? C14B C15B 1.349(19) . ? C15B C16B 1.362(17) . ? C16B C17B 1.522(17) . ? C17B N22B 1.323(14) . ? C17B C18B 1.422(17) . ? C18B C19B 1.277(19) . ? C19B C20B 1.410(19) . ? C20B C21B 1.441(18) . ? C21B N22B 1.323(16) . ? N42B C38B 1.330(14) . ? N42B C37B 1.366(14) . ? C37B C41B 1.345(16) . ? C37B C36B 1.486(16) . ? C38B C39B 1.358(17) . ? C39B C40B 1.308(18) . ? C40B C41B 1.423(18) . ? C36B C35B 1.303(18) . ? C36B N31B 1.367(14) . ? C35B C34B 1.40(2) . ? C34B C33B 1.34(2) . ? C33B C32B 1.311(18) . ? C32B N31B 1.339(15) . ? C57B O59B 1.293(13) . ? C57B O58B 1.310(14) . ? C57B C55B 1.391(19) . ? O59B Cu2B 1.954(7) 2_577 ? C55B C54B 1.31(2) . ? C55B N56B 1.72(2) . ? C54B C53B 1.50(2) . ? C53B O51B 1.201(17) . ? C53B O52B 1.255(15) . ? Cl3 O32 1.256(19) . ? Cl3 O31 1.308(19) . ? Cl3 O33 1.393(15) . ? Cl3 O34 1.496(19) . ? Cl2 O21 1.392(15) . ? Cl2 O24 1.407(17) . ? Cl2 O22 1.442(13) . ? Cl2 O23 1.461(14) . ? Cl1 O14 1.27(2) . ? Cl1 O11 1.349(18) . ? Cl1 O12 1.360(12) . ? Cl1 O13 1.372(18) . ? Cl41 O43 1.432(13) . ? Cl41 O41 1.456(13) . ? Cl41 O42 1.461(13) . ? Cl41 O44 1.565(14) . ? Cl51 O54 1.460(15) . ? Cl51 O53 1.472(15) . ? Cl51 O52 1.473(15) . ? Cl51 O51 1.504(15) . ? 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 N56A Cu1A N11A 178.2(5) . . ? N56A Cu1A O58A 85.4(5) . . ? N11A Cu1A O58A 93.2(4) . . ? N56A Cu1A N22A 101.2(5) . . ? N11A Cu1A N22A 80.3(4) . . ? O58A Cu1A N22A 170.0(4) . . ? N56A Cu1A O51A 81.9(5) . . ? N11A Cu1A O51A 96.9(3) . . ? O58A Cu1A O51A 90.2(4) . . ? N22A Cu1A O51A 98.0(4) . . ? N56A Cu1A O20A 87.0(6) . . ? N11A Cu1A O20A 94.0(5) . . ? O58A Cu1A O20A 82.1(5) . . ? N22A Cu1A O20A 90.8(5) . . ? O51A Cu1A O20A 167.0(5) . . ? O52A Cu2A O59A 94.3(3) . 2_666 ? O52A Cu2A N31A 169.6(4) . . ? O59A Cu2A N31A 89.5(4) 2_666 . ? O52A Cu2A N42A 94.0(3) . . ? O59A Cu2A N42A 160.8(3) 2_666 . ? N31A Cu2A N42A 79.6(4) . . ? O52A Cu2A O10A 92.0(4) . . ? O59A Cu2A O10A 96.9(3) 2_666 . ? N31A Cu2A O10A 97.2(4) . . ? N42A Cu2A O10A 100.1(3) . . ? O52A Cu2A C53A 24.1(3) . . ? O59A Cu2A C53A 86.6(3) 2_666 . ? N31A Cu2A C53A 147.2(4) . . ? N42A Cu2A C53A 94.0(4) . . ? O10A Cu2A C53A 115.5(4) . . ? C12A N11A C16A 118.9(10) . . ? C12A N11A Cu1A 126.2(8) . . ? C16A N11A Cu1A 114.7(8) . . ? N11A C12A C13A 121.7(11) . . ? C12A C13A C14A 117.4(12) . . ? C15A C14A C13A 122.5(12) . . ? C14A C15A C16A 116.8(11) . . ? N11A C16A C15A 122.5(11) . . ? N11A C16A C17A 115.9(10) . . ? C15A C16A C17A 121.6(10) . . ? N22A C17A C18A 123.1(12) . . ? N22A C17A C16A 111.5(9) . . ? C18A C17A C16A 125.4(11) . . ? C17A C18A C19A 119.3(13) . . ? C20A C19A C18A 119.4(13) . . ? C19A C20A C21A 113.2(14) . . ? N22A C21A C20A 129.9(13) . . ? C21A N22A C17A 114.8(10) . . ? C21A N22A Cu1A 127.8(8) . . ? C17A N22A Cu1A 117.3(8) . . ? C36A N31A C32A 121.8(11) . . ? C36A N31A Cu2A 114.5(8) . . ? C32A N31A Cu2A 123.3(9) . . ? N31A C32A C33A 119.3(13) . . ? C34A C33A C32A 119.1(15) . . ? C35A C34A C33A 120.5(15) . . ? C34A C35A C36A 117.1(14) . . ? N31A C36A C35A 121.7(13) . . ? N31A C36A C37A 116.3(11) . . ? C35A C36A C37A 121.8(12) . . ? C38A C37A N42A 123.3(13) . . ? C38A C37A C36A 124.0(12) . . ? N42A C37A C36A 112.6(10) . . ? C37A C38A C39 120.3(13) . . ? C38A C39 C40A 116.3(13) . . ? C41A C40A C39 122.5(15) . . ? C40A C41A N42A 118.8(13) . . ? C37A N42A C41A 118.7(10) . . ? C37A N42A Cu2A 116.8(8) . . ? C41A N42A Cu2A 124.5(8) . . ? O51A C53A O52A 125.3(13) . . ? O51A C53A C54A 120.1(14) . . ? O52A C53A C54A 114.3(13) . . ? O51A C53A Cu2A 86.3(9) . . ? O52A C53A Cu2A 39.1(6) . . ? C54A C53A Cu2A 153.2(11) . . ? C53A O51A Cu1A 117.9(9) . . ? C53A O52A Cu2A 116.9(8) . . ? C55A C54A C53A 131.1(15) . . ? C54A C55A C57A 118(2) . . ? C54A C55A N56A 88.3(14) . . ? C57A C55A N56A 112.7(14) . . ? C55A N56A Cu1A 101.6(8) . . ? O58A C57A O59A 127.0(11) . . ? O58A C57A C55A 110.5(12) . . ? O59A C57A C55A 121.2(12) . . ? C57A O58A Cu1A 123.5(8) . . ? C57A O59A Cu2A 126.5(7) . 2_666 ? O52B Cu2B O59B 94.0(3) . 2_577 ? O52B Cu2B N42B 93.3(3) . . ? O59B Cu2B N42B 155.6(3) 2_577 . ? O52B Cu2B N31B 170.9(4) . . ? O59B Cu2B N31B 89.8(3) 2_577 . ? N42B Cu2B N31B 79.9(4) . . ? O52B Cu2B O10B 92.3(4) . 2_577 ? O59B Cu2B O10B 102.6(3) 2_577 2_577 ? N42B Cu2B O10B 100.3(4) . 2_577 ? N31B Cu2B O10B 94.9(4) . 2_577 ? O52B Cu2B C53B 24.0(4) . . ? O59B Cu2B C53B 87.5(3) 2_577 . ? N42B Cu2B C53B 89.8(4) . . ? N31B Cu2B C53B 148.5(5) . . ? O10B Cu2B C53B 116.3(5) 2_577 . ? O58B Cu1B N56B 83.6(5) . . ? O58B Cu1B N11B 91.3(3) . . ? N56B Cu1B N11B 174.1(4) . . ? O58B Cu1B N22B 162.9(4) . . ? N56B Cu1B N22B 104.6(5) . . ? N11B Cu1B N22B 81.1(4) . . ? O58B Cu1B O51B 91.9(4) . . ? N56B Cu1B O51B 82.4(5) . . ? N11B Cu1B O51B 94.9(4) . . ? N22B Cu1B O51B 104.0(4) . . ? O58B Cu1B O20B 82.0(6) . . ? N56B Cu1B O20B 80.9(7) . . ? N11B Cu1B O20B 101.4(5) . . ? N22B Cu1B O20B 84.4(6) . . ? O51B Cu1B O20B 162.8(6) . . ? C12B N11B C16B 119.7(10) . . ? C12B N11B Cu1B 124.3(7) . . ? C16B N11B Cu1B 115.4(8) . . ? N11B C12B C13B 118.7(11) . . ? C14B C13B C12B 120.3(13) . . ? C15B C14B C13B 120.1(13) . . ? C14B C15B C16B 119.8(13) . . ? C15B C16B N11B 121.2(13) . . ? C15B C16B C17B 126.0(12) . . ? N11B C16B C17B 112.8(10) . . ? N22B C17B C18B 124.7(12) . . ? N22B C17B C16B 113.7(10) . . ? C18B C17B C16B 121.4(12) . . ? C19B C18B C17B 115.7(13) . . ? C18B C19B C20B 123.3(12) . . ? C19B C20B C21B 117.9(13) . . ? N22B C21B C20B 118.3(13) . . ? C17B N22B C21B 120.0(10) . . ? C17B N22B Cu1B 116.7(8) . . ? C21B N22B Cu1B 123.3(8) . . ? C38B N42B C37B 113.8(10) . . ? C38B N42B Cu2B 129.0(8) . . ? C37B N42B Cu2B 117.1(7) . . ? C41B C37B N42B 123.2(12) . . ? C41B C37B C36B 122.4(12) . . ? N42B C37B C36B 114.2(10) . . ? N42B C38B C39B 125.2(12) . . ? C40B C39B C38B 121.5(14) . . ? C39B C40B C41B 115.8(13) . . ? C37B C41B C40B 120.1(13) . . ? C35B C36B N31B 122.4(12) . . ? C35B C36B C37B 125.9(12) . . ? N31B C36B C37B 111.4(10) . . ? C36B C35B C34B 118.4(15) . . ? C33B C34B C35B 119.4(15) . . ? C32B C33B C34B 119.9(15) . . ? C33B C32B N31B 122.5(14) . . ? C32B N31B C36B 117.2(11) . . ? C32B N31B Cu2B 125.6(9) . . ? C36B N31B Cu2B 117.1(8) . . ? O59B C57B O58B 117.6(11) . . ? O59B C57B C55B 124.2(11) . . ? O58B C57B C55B 117.0(13) . . ? C57B O58B Cu1B 118.4(8) . . ? C57B O59B Cu2B 131.9(7) . 2_577 ? C54B C55B C57B 119(2) . . ? C54B C55B N56B 82.1(17) . . ? C57B C55B N56B 109.7(14) . . ? C55B C54B C53B 131.7(16) . . ? O51B C53B O52B 122.4(14) . . ? O51B C53B C54B 126.0(16) . . ? O52B C53B C54B 111.4(16) . . ? O51B C53B Cu2B 83.6(9) . . ? O52B C53B Cu2B 38.9(6) . . ? C54B C53B Cu2B 150.4(14) . . ? C55B N56B Cu1B 104.3(8) . . ? C53B O51B Cu1B 112.9(11) . . ? C53B O52B Cu2B 117.0(9) . . ? O32 Cl3 O31 103.5(16) . . ? O32 Cl3 O33 110.1(13) . . ? O31 Cl3 O33 103.5(13) . . ? O32 Cl3 O34 114.8(13) . . ? O31 Cl3 O34 118.5(14) . . ? O33 Cl3 O34 105.8(11) . . ? O21 Cl2 O24 116.8(11) . . ? O21 Cl2 O22 110.2(10) . . ? O24 Cl2 O22 105.5(10) . . ? O21 Cl2 O23 111.4(10) . . ? O24 Cl2 O23 105.7(10) . . ? O22 Cl2 O23 106.7(9) . . ? O14 Cl1 O11 108.7(14) . . ? O14 Cl1 O12 109.4(14) . . ? O11 Cl1 O12 110.1(10) . . ? O14 Cl1 O13 112.5(14) . . ? O11 Cl1 O13 107.3(13) . . ? O12 Cl1 O13 108.8(9) . . ? O43 Cl41 O41 113.3(11) . . ? O43 Cl41 O42 113.0(12) . . ? O41 Cl41 O42 114.2(11) . . ? O43 Cl41 O44 108.3(10) . . ? O41 Cl41 O44 103.2(11) . . ? O42 Cl41 O44 103.7(10) . . ? O54 Cl51 O53 109.5(13) . . ? O54 Cl51 O52 111.3(13) . . ? O53 Cl51 O52 111.2(13) . . ? O54 Cl51 O51 109.2(13) . . ? O53 Cl51 O51 108.2(13) . . ? O52 Cl51 O51 107.3(13) . . ? _refine_diff_density_max 0.693 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.115