# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Tapan Kanti Paine' _publ_contact_author_email ictkp@iacs.res.in loop_ _publ_author_name S.Khanra S.Ghosh E.Zangrando M.Johann E.Rentschler ; T.Weyhermuller ; T.K.Paine data_neu _database_code_depnum_ccdc_archive 'CCDC 760091' #TrackingRef 'Complex_1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H75 Cu6 N12 O14, 3 (B F4), H2 O' _chemical_formula_sum 'C48 H75 B3 Cu6 F12 N12 O15' _chemical_formula_weight 1701.87 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 cubic _symmetry_space_group_name_H-M Pa-3 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 23.8313(9) _cell_length_b 23.8313(9) _cell_length_c 23.8313(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13534.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque block' _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6912 _exptl_absorpt_coefficient_mu 1.953 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5545 _exptl_absorpt_correction_T_max 0.6869 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '497 images at 1.0 deg. stepwise rotation in omega and phi, 15 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 118922 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 27.83 _reflns_number_total 5319 _reflns_number_gt 4508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+38.1927P] 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 5319 _refine_ls_number_parameters 309 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.296288(17) 0.237001(16) 0.186646(16) 0.02244(12) Uani 1 1 d . . . Cu2 Cu 0.350397(17) 0.361641(17) 0.260531(17) 0.02498(13) Uani 1 1 d . . . O1 O 0.30351(10) 0.14769(10) 0.27050(10) 0.0280(5) Uani 1 1 d . . . N2 N 0.32388(12) 0.16783(12) 0.22226(12) 0.0242(5) Uani 1 1 d . . . C3 C 0.36356(14) 0.14145(14) 0.19651(15) 0.0271(7) Uani 1 1 d . . . C4 C 0.37933(15) 0.16835(15) 0.14237(15) 0.0291(7) Uani 1 1 d . . . N5 N 0.35261(12) 0.21348(12) 0.12913(12) 0.0268(6) Uani 1 1 d . . . C6 C 0.36340(15) 0.24403(15) 0.07627(15) 0.0301(7) Uani 1 1 d . . . H6A H 0.3284 0.2621 0.0632 0.036 Uiso 1 1 calc R . . H6B H 0.3759 0.2173 0.0470 0.036 Uiso 1 1 calc R . . C7 C 0.40808(15) 0.28820(15) 0.08530(14) 0.0279(7) Uani 1 1 d . . . C8 C 0.46003(15) 0.28570(16) 0.05912(15) 0.0307(7) Uani 1 1 d . . . H8 H 0.4690 0.2551 0.0352 0.037 Uiso 1 1 calc R . . C9 C 0.49932(15) 0.32868(17) 0.06810(16) 0.0343(8) Uani 1 1 d . . . H9 H 0.5342 0.3279 0.0488 0.041 Uiso 1 1 calc R . . C10 C 0.48773(14) 0.37207(16) 0.10462(15) 0.0307(7) Uani 1 1 d . . . H10 H 0.5149 0.4006 0.1108 0.037 Uiso 1 1 calc R . . C11 C 0.43618(14) 0.37416(15) 0.13261(15) 0.0282(7) Uani 1 1 d . . . C12 C 0.39644(14) 0.33294(15) 0.12147(15) 0.0284(7) Uani 1 1 d . . . H12 H 0.3606 0.3352 0.1388 0.034 Uiso 1 1 calc R . . C13 C 0.42645(15) 0.41964(16) 0.17567(16) 0.0332(8) Uani 1 1 d . . . H13A H 0.4553 0.4164 0.2054 0.040 Uiso 1 1 calc R . . H13B H 0.4312 0.4567 0.1574 0.040 Uiso 1 1 calc R . . N14 N 0.37068(13) 0.41724(12) 0.20165(13) 0.0285(6) Uani 1 1 d . . . C15 C 0.33397(16) 0.45622(14) 0.19476(14) 0.0299(7) Uani 1 1 d . . . C16 C 0.28284(17) 0.45236(15) 0.23047(15) 0.0310(7) Uani 1 1 d . . . N17 N 0.28587(14) 0.41267(13) 0.26757(13) 0.0327(7) Uani 1 1 d . . . O18 O 0.24357(14) 0.40520(13) 0.30367(13) 0.0501(9) Uani 1 1 d . . . C19 C 0.38962(16) 0.08875(15) 0.21782(18) 0.0346(8) Uani 1 1 d . . . H19A H 0.3729 0.0789 0.2541 0.052 Uiso 1 1 calc R . . H19B H 0.4301 0.0944 0.2224 0.052 Uiso 1 1 calc R . . H19C H 0.3830 0.0583 0.1910 0.052 Uiso 1 1 calc R . . C20 C 0.42412(19) 0.14104(18) 0.10751(19) 0.0431(10) Uani 1 1 d . . . H20A H 0.4301 0.1629 0.0732 0.065 Uiso 1 1 calc R . . H20B H 0.4124 0.1029 0.0976 0.065 Uiso 1 1 calc R . . H20C H 0.4591 0.1394 0.1290 0.065 Uiso 1 1 calc R . . C21 C 0.3391(2) 0.50502(17) 0.15550(17) 0.0422(9) Uani 1 1 d . . . H21A H 0.3745 0.5022 0.1347 0.063 Uiso 1 1 calc R . . H21B H 0.3386 0.5401 0.1770 0.063 Uiso 1 1 calc R . . H21C H 0.3076 0.5047 0.1291 0.063 Uiso 1 1 calc R . . C22 C 0.23418(19) 0.49185(17) 0.22580(18) 0.0412(9) Uani 1 1 d . . . H22A H 0.2055 0.4816 0.2534 0.062 Uiso 1 1 calc R . . H22B H 0.2182 0.4895 0.1880 0.062 Uiso 1 1 calc R . . H22C H 0.2470 0.5303 0.2329 0.062 Uiso 1 1 calc R . . O30 O 0.25190(9) 0.25190(9) 0.25190(9) 0.0219(7) Uani 1 3 d SD . . H35 H 0.2824(3) 0.2824(3) 0.2824(3) 0.026 Uiso 1 3 d SD . . O40 O 0.31289(9) 0.31289(9) 0.31289(9) 0.0219(7) Uani 1 3 d SD . . B50 B 0.5523(2) 0.2113(3) -0.0657(3) 0.053(2) Uani 0.67 1 d PD A 1 F51 F 0.5462(4) 0.2671(3) -0.0507(5) 0.079(2) Uani 0.67 1 d PD A 1 F52 F 0.5460(3) 0.2065(6) -0.1236(3) 0.0782(15) Uani 0.67 1 d PD A 1 F53 F 0.6040(2) 0.1918(3) -0.0498(3) 0.0809(19) Uani 0.67 1 d PD A 1 F54 F 0.5092(2) 0.1807(3) -0.0399(3) 0.114(2) Uani 0.67 1 d PD A 1 B50X B 0.5734(4) 0.2201(6) -0.0776(5) 0.053(2) Uani 0.33 1 d PD B 2 F51X F 0.5478(9) 0.2580(7) -0.0419(11) 0.079(2) Uani 0.33 1 d PD B 2 F52X F 0.5362(7) 0.2049(12) -0.1197(7) 0.0782(15) Uani 0.33 1 d PD B 2 F53X F 0.5891(6) 0.1728(6) -0.0476(8) 0.0809(19) Uani 0.33 1 d PD B 2 F54X F 0.6207(5) 0.2440(6) -0.1014(6) 0.114(2) Uani 0.33 1 d PD B 2 O60 O 0.2264(3) 0.1803(3) 0.1350(2) 0.115(2) Uani 1 1 d . . . O70 O 0.4016(2) 0.4206(3) 0.3286(2) 0.0508(12) Uani 0.629(7) 1 d P . . O70X O 0.4280(4) 0.3967(4) 0.3098(4) 0.0508(12) Uani 0.371(7) 1 d P . . O80 O 0.4562(6) 0.5438(6) 0.0438(6) 0.262(11) Uani 1 3 d S . . 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 0.0247(2) 0.0218(2) 0.0208(2) -0.00024(14) 0.00148(14) 0.00135(14) Cu2 0.0249(2) 0.0220(2) 0.0281(2) 0.00184(15) 0.00174(15) -0.00134(15) O1 0.0300(12) 0.0292(12) 0.0248(11) 0.0058(9) 0.0039(9) 0.0048(10) N2 0.0246(13) 0.0231(13) 0.0249(13) 0.0011(11) 0.0009(11) -0.0006(10) C3 0.0269(16) 0.0232(15) 0.0310(17) 0.0000(13) 0.0023(13) -0.0009(12) C4 0.0300(17) 0.0258(16) 0.0315(17) -0.0017(13) 0.0075(14) 0.0006(13) N5 0.0279(14) 0.0253(14) 0.0271(14) -0.0007(11) 0.0052(11) -0.0009(11) C6 0.0353(18) 0.0303(17) 0.0248(16) 0.0005(13) 0.0064(14) 0.0004(14) C7 0.0284(16) 0.0310(17) 0.0242(15) 0.0071(13) 0.0039(13) 0.0032(13) C8 0.0297(17) 0.0345(18) 0.0280(16) 0.0076(14) 0.0035(13) 0.0087(14) C9 0.0208(15) 0.048(2) 0.0345(18) 0.0121(16) 0.0034(14) 0.0048(15) C10 0.0223(15) 0.0403(19) 0.0296(17) 0.0112(14) -0.0025(13) -0.0013(14) C11 0.0258(16) 0.0309(17) 0.0279(16) 0.0091(13) -0.0005(13) 0.0002(13) C12 0.0262(16) 0.0302(17) 0.0287(16) 0.0045(13) 0.0051(13) 0.0005(13) C13 0.0298(17) 0.0334(18) 0.0363(19) 0.0021(15) 0.0043(15) -0.0102(14) N14 0.0289(14) 0.0260(14) 0.0306(15) -0.0013(11) 0.0040(12) -0.0062(11) C15 0.0398(19) 0.0257(16) 0.0241(16) -0.0017(13) 0.0012(14) -0.0038(14) C16 0.041(2) 0.0240(16) 0.0278(17) -0.0026(13) 0.0040(14) 0.0036(14) N17 0.0405(17) 0.0248(14) 0.0329(16) 0.0039(12) 0.0114(13) 0.0084(12) O18 0.0571(19) 0.0436(16) 0.0496(17) 0.0215(14) 0.0302(15) 0.0262(14) C19 0.0314(18) 0.0263(17) 0.046(2) 0.0062(15) 0.0056(16) 0.0067(14) C20 0.044(2) 0.036(2) 0.049(2) 0.0061(18) 0.0222(19) 0.0111(17) C21 0.061(3) 0.034(2) 0.0314(19) 0.0056(16) 0.0060(18) -0.0028(19) C22 0.057(3) 0.0328(19) 0.0342(19) 0.0052(16) 0.0082(18) 0.0180(18) O30 0.0219(7) 0.0219(7) 0.0219(7) 0.0005(9) 0.0005(9) 0.0005(9) O40 0.0219(7) 0.0219(7) 0.0219(7) -0.0002(8) -0.0002(8) -0.0002(8) B50 0.026(4) 0.082(6) 0.051(5) -0.016(4) -0.002(4) 0.009(4) F51 0.071(2) 0.104(4) 0.063(4) -0.030(3) -0.002(3) 0.029(3) F52 0.065(4) 0.109(3) 0.061(2) -0.029(2) -0.019(2) 0.029(3) F53 0.050(4) 0.101(5) 0.092(3) -0.025(4) -0.035(3) 0.005(3) F54 0.071(4) 0.151(6) 0.119(5) -0.006(4) -0.009(3) -0.010(4) B50X 0.026(4) 0.082(6) 0.051(5) -0.016(4) -0.002(4) 0.009(4) F51X 0.071(2) 0.104(4) 0.063(4) -0.030(3) -0.002(3) 0.029(3) F52X 0.065(4) 0.109(3) 0.061(2) -0.029(2) -0.019(2) 0.029(3) F53X 0.050(4) 0.101(5) 0.092(3) -0.025(4) -0.035(3) 0.005(3) F54X 0.071(4) 0.151(6) 0.119(5) -0.006(4) -0.009(3) -0.010(4) O60 0.106(4) 0.154(6) 0.084(4) -0.001(4) -0.014(3) -0.042(4) O70 0.053(3) 0.064(3) 0.035(2) 0.010(2) -0.008(2) -0.006(2) O70X 0.053(3) 0.064(3) 0.035(2) 0.010(2) -0.008(2) -0.006(2) O80 0.262(11) 0.262(11) 0.262(11) -0.037(11) 0.037(11) 0.037(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O30 1.9140(11) . ? Cu1 O1 1.937(2) 5 ? Cu1 N2 1.967(3) . ? Cu1 N5 1.999(3) . ? Cu1 O60 2.473(6) . ? Cu2 O40 1.9250(10) . ? Cu2 O18 1.944(3) 9 ? Cu2 N17 1.968(3) . ? Cu2 N14 1.989(3) . ? Cu2 O70X 2.345(9) . ? Cu2 O70 2.470(6) . ? O1 N2 1.337(4) . ? O1 Cu1 1.937(2) 9 ? N2 C3 1.291(4) . ? C3 C4 1.489(5) . ? C3 C19 1.490(5) . ? C4 N5 1.289(5) . ? C4 C20 1.501(5) . ? N5 C6 1.477(4) . ? C6 C7 1.513(5) . ? C7 C8 1.388(5) . ? C7 C12 1.399(5) . ? C8 C9 1.404(6) . ? C9 C10 1.379(6) . ? C10 C11 1.399(5) . ? C11 C12 1.390(5) . ? C11 C13 1.511(5) . ? C13 N14 1.467(5) . ? N14 C15 1.287(5) . ? C15 C16 1.489(5) . ? C15 C21 1.498(5) . ? C16 N17 1.297(5) . ? C16 C22 1.497(5) . ? N17 O18 1.337(4) . ? O18 Cu2 1.944(3) 5 ? O30 Cu1 1.9140(11) 5 ? O30 Cu1 1.9141(11) 9 ? O40 Cu2 1.9250(10) 9 ? O40 Cu2 1.9252(10) 5 ? B50 F53 1.370(6) . ? B50 F51 1.386(6) . ? B50 F52 1.391(6) . ? B50 F54 1.402(6) . ? B50X F51X 1.382(7) . ? B50X F54X 1.385(7) . ? B50X F53X 1.387(7) . ? B50X F52X 1.388(7) . ? O70 O70X 0.960(11) . ? 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 O30 Cu1 O1 93.57(7) . 5 ? O30 Cu1 N2 89.41(8) . . ? O1 Cu1 N2 176.88(11) 5 . ? O30 Cu1 N5 168.64(10) . . ? O1 Cu1 N5 96.54(11) 5 . ? N2 Cu1 N5 80.58(12) . . ? O30 Cu1 O60 97.67(19) . . ? O1 Cu1 O60 89.71(18) 5 . ? N2 Cu1 O60 88.96(19) . . ? N5 Cu1 O60 87.58(18) . . ? O40 Cu2 O18 91.02(8) . 9 ? O40 Cu2 N17 87.41(9) . . ? O18 Cu2 N17 169.16(16) 9 . ? O40 Cu2 N14 166.39(11) . . ? O18 Cu2 N14 99.41(12) 9 . ? N17 Cu2 N14 80.70(13) . . ? O40 Cu2 O70X 104.9(2) . . ? O18 Cu2 O70X 80.1(3) 9 . ? N17 Cu2 O70X 110.7(3) . . ? N14 Cu2 O70X 85.7(2) . . ? O40 Cu2 O70 98.46(17) . . ? O18 Cu2 O70 102.07(19) 9 . ? N17 Cu2 O70 88.77(18) . . ? N14 Cu2 O70 87.96(15) . . ? O70X Cu2 O70 22.8(3) . . ? N2 O1 Cu1 113.44(18) . 9 ? C3 N2 O1 120.0(3) . . ? C3 N2 Cu1 116.6(2) . . ? O1 N2 Cu1 123.4(2) . . ? N2 C3 C4 112.8(3) . . ? N2 C3 C19 123.6(3) . . ? C4 C3 C19 123.6(3) . . ? N5 C4 C3 116.5(3) . . ? N5 C4 C20 125.3(3) . . ? C3 C4 C20 118.2(3) . . ? C4 N5 C6 122.3(3) . . ? C4 N5 Cu1 113.4(2) . . ? C6 N5 Cu1 124.3(2) . . ? N5 C6 C7 110.1(3) . . ? C8 C7 C12 119.1(3) . . ? C8 C7 C6 122.3(3) . . ? C12 C7 C6 118.6(3) . . ? C7 C8 C9 119.7(4) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C11 120.2(3) . . ? C12 C11 C10 118.8(3) . . ? C12 C11 C13 122.2(3) . . ? C10 C11 C13 119.0(3) . . ? C11 C12 C7 121.4(3) . . ? N14 C13 C11 113.4(3) . . ? C15 N14 C13 122.3(3) . . ? C15 N14 Cu2 113.9(2) . . ? C13 N14 Cu2 122.9(2) . . ? N14 C15 C16 116.0(3) . . ? N14 C15 C21 125.8(4) . . ? C16 C15 C21 118.2(3) . . ? N17 C16 C15 112.9(3) . . ? N17 C16 C22 123.5(3) . . ? C15 C16 C22 123.5(3) . . ? C16 N17 O18 119.6(3) . . ? C16 N17 Cu2 115.9(3) . . ? O18 N17 Cu2 124.2(2) . . ? N17 O18 Cu2 113.0(2) . 5 ? Cu1 O30 Cu1 113.63(9) 5 . ? Cu1 O30 Cu1 113.62(9) 5 9 ? Cu1 O30 Cu1 113.63(9) . 9 ? Cu2 O40 Cu2 114.32(9) 9 . ? Cu2 O40 Cu2 114.32(9) 9 5 ? Cu2 O40 Cu2 114.32(9) . 5 ? F53 B50 F51 110.3(5) . . ? F53 B50 F52 110.2(5) . . ? F51 B50 F52 108.8(5) . . ? F53 B50 F54 111.2(5) . . ? F51 B50 F54 108.0(5) . . ? F52 B50 F54 108.3(5) . . ? F51X B50X F54X 110.1(6) . . ? F51X B50X F53X 109.5(6) . . ? F54X B50X F53X 109.1(6) . . ? F51X B50X F52X 109.5(6) . . ? F54X B50X F52X 109.4(6) . . ? F53X B50X F52X 109.3(6) . . ? O70X O70 Cu2 71.2(7) . . ? O70 O70X Cu2 86.0(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.677 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.103 # Attachment 'Complex_1b.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 760092' #TrackingRef 'Complex_1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H73 Cu6 N12 O14 3+, 3(Cl O4 1-) (H2 O)' _chemical_formula_sum 'C48 H75 Cl3 Cu6 N12 O27' _chemical_formula_weight 1739.79 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 cubic _symmetry_space_group_name_H-M 'P a-3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' '-z, -x, -y' 'z, -x-1/2, y-1/2' 'z-1/2, x, -y-1/2' '-z-1/2, x-1/2, y' _cell_length_a 23.960(4) _cell_length_b 23.960(4) _cell_length_c 23.960(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13755(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour black _exptl_crystal_size_max .32 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7104 _exptl_absorpt_coefficient_mu 2.025 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5663 _exptl_absorpt_correction_T_max 0.6034 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123688 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.08 _reflns_number_total 5067 _reflns_number_gt 3786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1378P)^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 5067 _refine_ls_number_parameters 294 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.35093(2) 0.36055(2) 0.26145(2) 0.0647(2) Uani 1 1 d . . . Cu2 Cu 0.295905(19) 0.236757(19) 0.186855(18) 0.05725(19) Uani 1 1 d . . . O1 O 0.24603(14) 0.40651(14) 0.30381(14) 0.0808(8) Uani 1 1 d . . . O2 O 0.30361(12) 0.14876(12) 0.27095(12) 0.0680(7) Uani 1 1 d . . . O3 O 0.31238(11) 0.31238(11) 0.31238(11) 0.0626(11) Uani 1 3 d SD . . O4 O 0.25162(11) 0.25162(11) 0.25162(11) 0.0569(9) Uani 1 3 d SD . . H34 H 0.2820(3) 0.2820(3) 0.2820(3) 0.068 Uiso 1 3 d SD . . N1 N 0.28832(15) 0.41252(15) 0.26762(15) 0.0686(8) Uani 1 1 d . . . N2 N 0.37330(15) 0.41617(15) 0.20456(15) 0.0676(8) Uani 1 1 d . . . N3 N 0.35309(13) 0.21379(13) 0.13112(14) 0.0599(7) Uani 1 1 d . . . N4 N 0.32374(13) 0.16853(13) 0.22314(13) 0.0585(7) Uani 1 1 d . . . C1 C 0.2397(2) 0.4924(2) 0.2269(2) 0.0856(13) Uani 1 1 d . . . H1A H 0.2106 0.4822 0.2526 0.128 Uiso 1 1 calc R . . H1B H 0.2253 0.4917 0.1895 0.128 Uiso 1 1 calc R . . H1C H 0.2528 0.5293 0.2355 0.128 Uiso 1 1 calc R . . C2 C 0.28609(19) 0.45259(18) 0.23172(17) 0.0692(10) Uani 1 1 d . . . C3 C 0.3377(2) 0.45468(18) 0.19645(17) 0.0700(10) Uani 1 1 d . . . C4 C 0.3422(3) 0.5022(2) 0.1556(2) 0.0939(15) Uani 1 1 d . . . H4A H 0.3513 0.5359 0.1753 0.141 Uiso 1 1 calc R . . H4B H 0.3073 0.5069 0.1366 0.141 Uiso 1 1 calc R . . H4C H 0.3710 0.4942 0.1289 0.141 Uiso 1 1 calc R . . C5 C 0.42925(19) 0.41711(19) 0.1783(2) 0.0757(11) Uani 1 1 d . . . H5A H 0.4573 0.4122 0.2071 0.091 Uiso 1 1 calc R . . H5B H 0.4352 0.4534 0.1614 0.091 Uiso 1 1 calc R . . C6 C 0.43707(16) 0.37317(18) 0.13493(16) 0.0639(9) Uani 1 1 d . . . C7 C 0.48786(17) 0.37118(19) 0.10643(18) 0.0703(10) Uani 1 1 d . . . H7 H 0.5145 0.3987 0.1126 0.084 Uiso 1 1 calc R . . C8 C 0.49877(17) 0.3287(2) 0.06929(19) 0.0738(11) Uani 1 1 d . . . H8 H 0.5324 0.3282 0.0500 0.089 Uiso 1 1 calc R . . C9 C 0.45932(17) 0.28605(19) 0.06034(17) 0.0681(10) Uani 1 1 d . . . H9 H 0.4672 0.2566 0.0363 0.082 Uiso 1 1 calc R . . C10 C 0.40902(16) 0.28857(16) 0.08773(16) 0.0612(9) Uani 1 1 d . . . C11 C 0.39824(15) 0.33198(17) 0.12387(16) 0.0625(9) Uani 1 1 d . . . H11 H 0.3637 0.3336 0.1414 0.075 Uiso 1 1 calc R . . C12 C 0.36423(18) 0.24461(18) 0.07854(17) 0.0661(9) Uani 1 1 d . . . H12A H 0.3302 0.2624 0.0658 0.079 Uiso 1 1 calc R . . H12B H 0.3764 0.2187 0.0499 0.079 Uiso 1 1 calc R . . C13 C 0.4263(2) 0.1445(2) 0.1114(2) 0.0815(13) Uani 1 1 d . . . H13A H 0.4314 0.1652 0.0775 0.122 Uiso 1 1 calc R . . H13B H 0.4168 0.1065 0.1027 0.122 Uiso 1 1 calc R . . H13C H 0.4603 0.1452 0.1327 0.122 Uiso 1 1 calc R . . C14 C 0.38046(17) 0.17015(16) 0.14470(16) 0.0616(8) Uani 1 1 d . . . C15 C 0.36406(17) 0.14309(16) 0.19858(17) 0.0612(9) Uani 1 1 d . . . C16 C 0.3895(2) 0.09140(19) 0.2204(2) 0.0780(12) Uani 1 1 d . . . H16A H 0.3721 0.0816 0.2551 0.117 Uiso 1 1 calc R . . H16B H 0.4287 0.0972 0.2262 0.117 Uiso 1 1 calc R . . H16C H 0.3842 0.0617 0.1939 0.117 Uiso 1 1 calc R . . O1W O 0.4166(4) 0.4051(4) 0.3282(4) 0.218(4) Uani 1 1 d . . . O2W O 0.2281(3) 0.1741(4) 0.1353(3) 0.168(2) Uani 1 1 d . . . Cl1 Cl 0.05358(10) 0.20587(10) 0.56653(9) 0.1458(9) Uani 1 1 d . . . O11 O 0.0457(3) 0.2591(3) 0.5460(3) 0.183(3) Uani 1 1 d . . . O12 O 0.0409(3) 0.2020(3) 0.6219(3) 0.174(3) Uani 1 1 d . . . O13 O 0.1042(3) 0.1854(4) 0.5563(3) 0.207(4) Uani 1 1 d . . . O14 O 0.0074(5) 0.1791(6) 0.5313(5) 0.293(6) Uani 1 1 d . . . O3W O 0.0230(6) 0.4770(6) 0.5230(6) 0.302(13) Uani 1 3 d S . . 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 0.0630(3) 0.0611(3) 0.0700(3) 0.0014(2) 0.0028(2) -0.0024(2) Cu2 0.0579(3) 0.0585(3) 0.0553(3) 0.00085(18) 0.00201(18) 0.00289(18) O1 0.0759(18) 0.083(2) 0.0831(19) 0.0184(16) 0.0218(15) 0.0146(15) O2 0.0699(16) 0.0688(16) 0.0652(15) 0.0103(13) 0.0066(13) 0.0105(12) O3 0.0626(11) 0.0626(11) 0.0626(11) -0.0028(11) -0.0028(11) -0.0028(11) O4 0.0569(9) 0.0569(9) 0.0569(9) 0.0012(11) 0.0012(11) 0.0012(11) N1 0.075(2) 0.0653(19) 0.0657(19) -0.0005(16) 0.0029(16) 0.0014(16) N2 0.071(2) 0.0620(18) 0.070(2) -0.0091(15) 0.0058(16) -0.0128(16) N3 0.0615(17) 0.0603(17) 0.0579(16) -0.0005(14) 0.0033(13) -0.0047(14) N4 0.0584(17) 0.0601(17) 0.0569(16) 0.0011(14) 0.0044(13) 0.0000(14) C1 0.101(4) 0.076(3) 0.080(3) 0.004(2) 0.009(3) 0.018(2) C2 0.082(3) 0.063(2) 0.062(2) -0.0066(18) -0.0030(19) 0.001(2) C3 0.085(3) 0.063(2) 0.061(2) -0.0054(17) 0.0035(19) -0.014(2) C4 0.120(4) 0.088(3) 0.073(3) 0.014(2) 0.007(3) -0.011(3) C5 0.068(2) 0.072(2) 0.087(3) -0.008(2) 0.010(2) -0.019(2) C6 0.059(2) 0.070(2) 0.062(2) 0.0087(17) -0.0007(16) -0.0017(17) C7 0.056(2) 0.081(3) 0.073(2) 0.008(2) 0.0008(18) -0.0073(19) C8 0.052(2) 0.093(3) 0.076(3) 0.012(2) 0.0078(18) 0.006(2) C9 0.065(2) 0.076(2) 0.063(2) 0.0071(19) 0.0047(17) 0.0093(19) C10 0.063(2) 0.065(2) 0.0556(19) 0.0106(16) 0.0000(16) 0.0017(16) C11 0.0545(19) 0.072(2) 0.061(2) 0.0064(17) 0.0043(16) 0.0001(17) C12 0.070(2) 0.075(2) 0.0533(19) -0.0021(17) 0.0039(17) -0.0035(18) C13 0.077(3) 0.083(3) 0.084(3) 0.007(2) 0.022(2) 0.018(2) C14 0.0586(19) 0.062(2) 0.064(2) -0.0043(16) 0.0042(16) 0.0011(17) C15 0.060(2) 0.058(2) 0.066(2) -0.0017(16) 0.0011(16) 0.0007(16) C16 0.078(3) 0.073(3) 0.083(3) 0.012(2) 0.012(2) 0.013(2) O1W 0.231(8) 0.221(8) 0.201(7) 0.003(6) -0.061(7) -0.082(7) O2W 0.147(4) 0.223(7) 0.134(5) -0.032(5) -0.010(4) -0.052(5) Cl1 0.1427(17) 0.177(2) 0.1176(13) 0.0384(13) 0.0320(12) 0.0707(15) O11 0.189(6) 0.181(6) 0.179(6) 0.059(5) -0.029(5) 0.049(5) O12 0.169(5) 0.239(7) 0.113(4) 0.045(4) 0.038(4) 0.077(5) O13 0.147(5) 0.290(9) 0.184(6) 0.064(6) 0.061(5) 0.100(6) O14 0.245(10) 0.379(15) 0.257(12) 0.009(11) -0.091(10) -0.085(11) O3W 0.302(13) 0.302(13) 0.302(13) -0.087(14) 0.087(14) -0.087(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.9169(13) . ? Cu1 O1 1.939(3) 5 ? Cu1 N1 1.955(4) . ? Cu1 N2 1.980(4) . ? Cu1 O1W 2.485(7) . ? Cu2 O4 1.9133(13) . ? Cu2 O2 1.938(3) 9 ? Cu2 N4 1.968(3) . ? Cu2 N3 1.991(3) . ? Cu2 O2W 2.534(6) . ? O1 N1 1.342(5) . ? O1 Cu1 1.939(3) 9 ? O2 N4 1.330(4) . ? O2 Cu2 1.938(3) 5 ? O3 Cu1 1.9169(13) 9 ? O3 Cu1 1.9169(13) 5 ? O3 H34 1.261(11) . ? O4 Cu2 1.9133(13) 9 ? O4 Cu2 1.9133(13) 5 ? O4 H34 1.260(11) . ? N1 C2 1.290(5) . ? N2 C3 1.271(6) . ? N2 C5 1.481(6) . ? N3 C14 1.276(5) . ? N3 C12 1.485(5) . ? N4 C15 1.285(5) . ? C1 C2 1.470(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.499(6) . ? C3 C4 1.505(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.491(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C11 1.382(6) . ? C6 C7 1.396(5) . ? C7 C8 1.377(6) . ? C7 H7 0.9300 . ? C8 C9 1.408(7) . ? C8 H8 0.9300 . ? C9 C10 1.374(6) . ? C9 H9 0.9300 . ? C10 C11 1.378(6) . ? C10 C12 1.520(6) . ? C11 H11 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.491(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.497(5) . ? C15 C16 1.476(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Cl1 O13 1.332(6) . ? Cl1 O12 1.364(6) . ? Cl1 O11 1.379(6) . ? Cl1 O14 1.531(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O1 91.73(9) . 5 ? O3 Cu1 N1 88.03(10) . . ? O1 Cu1 N1 171.15(16) 5 . ? O3 Cu1 N2 166.88(13) . . ? O1 Cu1 N2 98.90(14) 5 . ? N1 Cu1 N2 80.28(15) . . ? O3 Cu1 O1W 98.9(2) . . ? O1 Cu1 O1W 89.4(3) 5 . ? N1 Cu1 O1W 99.4(3) . . ? N2 Cu1 O1W 89.0(2) . . ? O4 Cu2 O2 93.27(8) . 9 ? O4 Cu2 N4 89.10(9) . . ? O2 Cu2 N4 177.57(12) 9 . ? O4 Cu2 N3 167.73(12) . . ? O2 Cu2 N3 97.17(13) 9 . ? N4 Cu2 N3 80.42(13) . . ? O4 Cu2 O2W 98.6(2) . . ? O2 Cu2 O2W 93.6(2) 9 . ? N4 Cu2 O2W 86.6(2) . . ? N3 Cu2 O2W 87.17(18) . . ? N1 O1 Cu1 112.5(2) . 9 ? N4 O2 Cu2 113.4(2) . 5 ? Cu1 O3 Cu1 113.58(11) 9 . ? Cu1 O3 Cu1 113.58(11) 9 5 ? Cu1 O3 Cu1 113.58(11) . 5 ? Cu1 O3 H34 104.97(13) 9 . ? Cu1 O3 H34 104.97(13) . . ? Cu1 O3 H34 104.97(13) 5 . ? Cu2 O4 Cu2 113.70(10) 9 . ? Cu2 O4 Cu2 113.70(10) 9 5 ? Cu2 O4 Cu2 113.70(10) . 5 ? Cu2 O4 H34 104.81(13) 9 . ? Cu2 O4 H34 104.81(13) . . ? Cu2 O4 H34 104.81(13) 5 . ? C2 N1 O1 118.6(4) . . ? C2 N1 Cu1 117.1(3) . . ? O1 N1 Cu1 124.1(3) . . ? C3 N2 C5 122.1(4) . . ? C3 N2 Cu1 114.3(3) . . ? C5 N2 Cu1 123.2(3) . . ? C14 N3 C12 122.1(3) . . ? C14 N3 Cu2 114.1(3) . . ? C12 N3 Cu2 123.8(3) . . ? C15 N4 O2 119.9(3) . . ? C15 N4 Cu2 116.5(3) . . ? O2 N4 Cu2 123.6(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 124.5(4) . . ? N1 C2 C3 111.5(4) . . ? C1 C2 C3 124.0(4) . . ? N2 C3 C2 116.3(4) . . ? N2 C3 C4 126.9(4) . . ? C2 C3 C4 116.8(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C11 C6 C7 117.9(4) . . ? C11 C6 C5 123.6(4) . . ? C7 C6 C5 118.3(4) . . ? C8 C7 C6 120.4(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.0(4) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 C12 121.3(4) . . ? C11 C10 C12 118.8(3) . . ? C10 C11 C6 122.2(4) . . ? C10 C11 H11 118.9 . . ? C6 C11 H11 118.9 . . ? N3 C12 C10 110.4(3) . . ? N3 C12 H12A 109.6 . . ? C10 C12 H12A 109.6 . . ? N3 C12 H12B 109.6 . . ? C10 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C13 125.5(4) . . ? N3 C14 C15 116.1(3) . . ? C13 C14 C15 118.4(4) . . ? N4 C15 C16 123.1(4) . . ? N4 C15 C14 112.8(3) . . ? C16 C15 C14 124.1(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O13 Cl1 O12 110.9(4) . . ? O13 Cl1 O11 113.5(5) . . ? O12 Cl1 O11 112.4(5) . . ? O13 Cl1 O14 113.7(8) . . ? O12 Cl1 O14 110.3(6) . . ? O11 Cl1 O14 95.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 O3 Cu1 163.4(2) 5 . . 9 ? N1 Cu1 O3 Cu1 -25.4(2) . . . 9 ? N2 Cu1 O3 Cu1 -52.4(8) . . . 9 ? O1W Cu1 O3 Cu1 73.8(3) . . . 9 ? O1 Cu1 O3 Cu1 31.6(2) 5 . . 5 ? N1 Cu1 O3 Cu1 -157.3(2) . . . 5 ? N2 Cu1 O3 Cu1 175.8(5) . . . 5 ? O1W Cu1 O3 Cu1 -58.0(3) . . . 5 ? O2 Cu2 O4 Cu2 26.4(2) 9 . . 9 ? N4 Cu2 O4 Cu2 -154.2(2) . . . 9 ? N3 Cu2 O4 Cu2 174.7(6) . . . 9 ? O2W Cu2 O4 Cu2 -67.8(3) . . . 9 ? O2 Cu2 O4 Cu2 158.6(2) 9 . . 5 ? N4 Cu2 O4 Cu2 -21.9(2) . . . 5 ? N3 Cu2 O4 Cu2 -53.1(8) . . . 5 ? O2W Cu2 O4 Cu2 64.5(3) . . . 5 ? Cu1 O1 N1 C2 -172.1(3) 9 . . . ? Cu1 O1 N1 Cu1 13.1(4) 9 . . . ? O3 Cu1 N1 C2 -167.4(3) . . . . ? O1 Cu1 N1 C2 -78.8(10) 5 . . . ? N2 Cu1 N1 C2 6.7(3) . . . . ? O1W Cu1 N1 C2 94.0(4) . . . . ? O3 Cu1 N1 O1 7.5(4) . . . . ? O1 Cu1 N1 O1 96.1(10) 5 . . . ? N2 Cu1 N1 O1 -178.5(4) . . . . ? O1W Cu1 N1 O1 -91.2(4) . . . . ? O3 Cu1 N2 C3 23.2(8) . . . . ? O1 Cu1 N2 C3 166.9(3) 5 . . . ? N1 Cu1 N2 C3 -4.1(3) . . . . ? O1W Cu1 N2 C3 -103.9(4) . . . . ? O3 Cu1 N2 C5 -163.7(6) . . . . ? O1 Cu1 N2 C5 -20.0(3) 5 . . . ? N1 Cu1 N2 C5 169.0(3) . . . . ? O1W Cu1 N2 C5 69.2(4) . . . . ? O4 Cu2 N3 C14 29.4(8) . . . . ? O2 Cu2 N3 C14 177.5(3) 9 . . . ? N4 Cu2 N3 C14 -2.3(3) . . . . ? O2W Cu2 N3 C14 -89.3(3) . . . . ? O4 Cu2 N3 C12 -149.7(6) . . . . ? O2 Cu2 N3 C12 -1.6(3) 9 . . . ? N4 Cu2 N3 C12 178.7(3) . . . . ? O2W Cu2 N3 C12 91.7(3) . . . . ? Cu2 O2 N4 C15 -172.1(3) 5 . . . ? Cu2 O2 N4 Cu2 8.9(4) 5 . . . ? O4 Cu2 N4 C15 -171.0(3) . . . . ? O2 Cu2 N4 C15 -4(3) 9 . . . ? N3 Cu2 N4 C15 2.6(3) . . . . ? O2W Cu2 N4 C15 90.3(3) . . . . ? O4 Cu2 N4 O2 8.1(3) . . . . ? O2 Cu2 N4 O2 176(27) 9 . . . ? N3 Cu2 N4 O2 -178.3(3) . . . . ? O2W Cu2 N4 O2 -90.6(3) . . . . ? O1 N1 C2 C1 -0.8(7) . . . . ? Cu1 N1 C2 C1 174.3(4) . . . . ? O1 N1 C2 C3 177.5(3) . . . . ? Cu1 N1 C2 C3 -7.4(5) . . . . ? C5 N2 C3 C2 -171.7(4) . . . . ? Cu1 N2 C3 C2 1.5(5) . . . . ? C5 N2 C3 C4 7.7(7) . . . . ? Cu1 N2 C3 C4 -179.1(4) . . . . ? N1 C2 C3 N2 3.8(6) . . . . ? C1 C2 C3 N2 -177.9(4) . . . . ? N1 C2 C3 C4 -175.7(4) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C3 N2 C5 C6 -111.0(5) . . . . ? Cu1 N2 C5 C6 76.4(5) . . . . ? N2 C5 C6 C11 -6.0(6) . . . . ? N2 C5 C6 C7 178.4(4) . . . . ? C11 C6 C7 C8 -1.1(6) . . . . ? C5 C6 C7 C8 174.7(4) . . . . ? C6 C7 C8 C9 -1.3(6) . . . . ? C7 C8 C9 C10 2.3(6) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C8 C9 C10 C12 178.3(4) . . . . ? C9 C10 C11 C6 -1.6(6) . . . . ? C12 C10 C11 C6 179.2(4) . . . . ? C7 C6 C11 C10 2.6(6) . . . . ? C5 C6 C11 C10 -173.0(4) . . . . ? C14 N3 C12 C10 -88.8(4) . . . . ? Cu2 N3 C12 C10 90.3(4) . . . . ? C9 C10 C12 N3 116.7(4) . . . . ? C11 C10 C12 N3 -64.0(5) . . . . ? C12 N3 C14 C13 0.4(6) . . . . ? Cu2 N3 C14 C13 -178.7(4) . . . . ? C12 N3 C14 C15 -179.2(3) . . . . ? Cu2 N3 C14 C15 1.7(5) . . . . ? O2 N4 C15 C16 1.0(6) . . . . ? Cu2 N4 C15 C16 -179.9(3) . . . . ? O2 N4 C15 C14 178.5(3) . . . . ? Cu2 N4 C15 C14 -2.4(4) . . . . ? N3 C14 C15 N4 0.4(5) . . . . ? C13 C14 C15 N4 -179.2(4) . . . . ? N3 C14 C15 C16 177.9(4) . . . . ? C13 C14 C15 C16 -1.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.571 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.126