# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'R Mukherjee' _publ_contact_author_email RNM@IITK.AC.IN _publ_section_title ; Molecular squares of NiII and CuII: ferromagnetic exchange interaction mediated by syn-anti carboxylate-bridging ; loop_ _publ_author_name 'R Mukherjee' 'Himanshu Arora' 'F Lloret' # Attachment 'CIF_tetramer_DT1.cif' data_19febcm _database_code_depnum_ccdc_archive 'CCDC 718562' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H84 Cl4 N16 Ni4 O24' _chemical_formula_sum 'C72 H84 Cl4 N16 Ni4 O24' _chemical_formula_weight 1934.19 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.656(5) _cell_length_b 17.656(5) _cell_length_c 13.203(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4116(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.28 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8076 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26849 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5117 _reflns_number_gt 3235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WingX publication routine (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^)+(0.0695P)^2^+0.6152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5117 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.32809(2) 0.09103(2) 0.78157(3) 0.03170(15) Uani 1 1 d . . . Cl Cl 0.43649(6) -0.21534(6) 0.84447(8) 0.0541(3) Uani 1 1 d . . . O1 O 0.22773(13) 0.12843(13) 0.72286(16) 0.0352(5) Uani 1 1 d . . . O2 O 0.16377(13) 0.18196(13) 0.59943(17) 0.0369(5) Uani 1 1 d . . . O3 O 0.40102(19) -0.2399(2) 0.9361(2) 0.0868(11) Uani 1 1 d . . . O4 O 0.3861(2) -0.2258(2) 0.7612(2) 0.0811(10) Uani 1 1 d . . . O5 O 0.50305(19) -0.2585(2) 0.8271(3) 0.0849(11) Uani 1 1 d . . . O6 O 0.4549(2) -0.13713(17) 0.8535(3) 0.0800(10) Uani 1 1 d . . . N1 N 0.28315(16) -0.00107(16) 0.8533(2) 0.0381(7) Uani 1 1 d . . . N2 N 0.36026(15) 0.03813(15) 0.6473(2) 0.0347(6) Uani 1 1 d . . . N3 N 0.44121(16) 0.07390(16) 0.8130(2) 0.0372(7) Uani 1 1 d . . . N1S N 0.5833(5) -0.1363(5) 0.6319(5) 0.191(4) Uani 1 1 d . . . C1 C 0.2669(2) 0.0058(2) 0.9533(3) 0.0457(9) Uani 1 1 d . . . H1 H 0.2772 0.0517 0.9849 0.055 Uiso 1 1 calc R . . C2 C 0.2363(2) -0.0512(2) 1.0099(3) 0.0556(11) Uani 1 1 d . . . H2 H 0.2251 -0.0440 1.0781 0.067 Uiso 1 1 calc R . . C3 C 0.2226(2) -0.1195(3) 0.9634(4) 0.0619(12) Uani 1 1 d . . . H3 H 0.2027 -0.1598 1.0001 0.074 Uiso 1 1 calc R . . C4 C 0.2384(2) -0.1277(2) 0.8632(3) 0.0564(11) Uani 1 1 d . . . H4 H 0.2290 -0.1737 0.8314 0.068 Uiso 1 1 calc R . . C5 C 0.2685(2) -0.0677(2) 0.8079(3) 0.0419(9) Uani 1 1 d . . . C6 C 0.2831(2) -0.0757(2) 0.6967(3) 0.0524(10) Uani 1 1 d . . . H6A H 0.2432 -0.0495 0.6604 0.063 Uiso 1 1 calc R . . H6B H 0.2798 -0.1289 0.6792 0.063 Uiso 1 1 calc R . . C7 C 0.3586(2) -0.04570(19) 0.6597(3) 0.0448(9) Uani 1 1 d . . . H7A H 0.3976 -0.0604 0.7075 0.054 Uiso 1 1 calc R . . H7B H 0.3704 -0.0692 0.5952 0.054 Uiso 1 1 calc R . . C8 C 0.4404(2) 0.0622(2) 0.6316(3) 0.0456(9) Uani 1 1 d . . . H8A H 0.4412 0.1120 0.6007 0.055 Uiso 1 1 calc R . . H8B H 0.4650 0.0271 0.5857 0.055 Uiso 1 1 calc R . . C9 C 0.4831(2) 0.06451(19) 0.7294(3) 0.0378(8) Uani 1 1 d . . . C10 C 0.5612(2) 0.0612(2) 0.7327(3) 0.0516(10) Uani 1 1 d . . . H10 H 0.5893 0.0536 0.6740 0.062 Uiso 1 1 calc R . . C11 C 0.5965(2) 0.0693(3) 0.8253(4) 0.0614(12) Uani 1 1 d . . . H11 H 0.6491 0.0694 0.8293 0.074 Uiso 1 1 calc R . . C12 C 0.5540(2) 0.0774(2) 0.9114(3) 0.0517(10) Uani 1 1 d . . . H12 H 0.5771 0.0815 0.9745 0.062 Uiso 1 1 calc R . . C13 C 0.4766(2) 0.0795(2) 0.9026(3) 0.0442(9) Uani 1 1 d . . . H13 H 0.4476 0.0849 0.9610 0.053 Uiso 1 1 calc R . . C14 C 0.3153(2) 0.06023(19) 0.5561(2) 0.0384(8) Uani 1 1 d . . . H14A H 0.2715 0.0273 0.5505 0.046 Uiso 1 1 calc R . . H14B H 0.3461 0.0531 0.4960 0.046 Uiso 1 1 calc R . . C15 C 0.28876(19) 0.14218(19) 0.5607(3) 0.0373(8) Uani 1 1 d . . . H15A H 0.3305 0.1740 0.5825 0.045 Uiso 1 1 calc R . . H15B H 0.2737 0.1585 0.4935 0.045 Uiso 1 1 calc R . . C16 C 0.22351(18) 0.15220(18) 0.6319(2) 0.0314(7) Uani 1 1 d . . . C1S C 0.6109(5) -0.1356(4) 0.7123(6) 0.129(3) Uani 1 1 d . . . C2S C 0.6427(4) -0.1302(4) 0.8103(5) 0.121(2) Uani 1 1 d . . . H2S1 H 0.6688 -0.0828 0.8170 0.181 Uiso 1 1 calc R . . H2S2 H 0.6777 -0.1711 0.8205 0.181 Uiso 1 1 calc R . . H2S3 H 0.6031 -0.1331 0.8600 0.181 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0352(3) 0.0354(3) 0.0245(2) 0.00039(18) 0.00170(18) 0.00046(18) Cl 0.0663(7) 0.0515(6) 0.0445(6) 0.0013(5) -0.0004(5) 0.0054(5) O1 0.0381(13) 0.0418(13) 0.0257(12) 0.0022(10) -0.0005(10) 0.0014(10) O2 0.0378(13) 0.0432(14) 0.0299(13) 0.0045(10) 0.0036(10) 0.0009(11) O3 0.085(2) 0.111(3) 0.065(2) 0.026(2) 0.0044(18) -0.017(2) O4 0.102(3) 0.087(2) 0.054(2) -0.0126(17) -0.0221(19) 0.018(2) O5 0.076(2) 0.077(2) 0.101(3) 0.006(2) 0.010(2) 0.0236(18) O6 0.113(3) 0.0532(19) 0.074(2) -0.0088(17) 0.003(2) -0.0022(18) N1 0.0370(16) 0.0410(17) 0.0363(16) 0.0078(13) -0.0015(13) 0.0013(13) N2 0.0386(16) 0.0371(16) 0.0285(15) -0.0018(12) 0.0027(12) 0.0021(12) N3 0.0391(16) 0.0380(16) 0.0343(16) 0.0026(13) 0.0009(13) 0.0036(13) N1S 0.244(9) 0.246(9) 0.083(4) -0.026(5) 0.042(5) -0.161(7) C1 0.043(2) 0.059(2) 0.035(2) 0.0064(18) 0.0011(16) -0.0040(18) C2 0.046(2) 0.070(3) 0.050(3) 0.018(2) 0.0069(19) 0.002(2) C3 0.054(3) 0.060(3) 0.072(3) 0.026(2) 0.013(2) -0.008(2) C4 0.058(3) 0.042(2) 0.069(3) 0.008(2) 0.006(2) -0.0057(19) C5 0.037(2) 0.041(2) 0.047(2) 0.0069(17) -0.0018(16) -0.0014(16) C6 0.065(3) 0.044(2) 0.049(2) -0.0056(18) -0.003(2) -0.0117(19) C7 0.058(2) 0.037(2) 0.039(2) -0.0081(16) 0.0037(18) 0.0084(17) C8 0.045(2) 0.055(2) 0.037(2) -0.0017(17) 0.0099(17) 0.0021(18) C9 0.039(2) 0.038(2) 0.037(2) 0.0001(15) 0.0052(16) 0.0026(15) C10 0.038(2) 0.068(3) 0.049(2) -0.005(2) 0.0040(18) 0.0035(19) C11 0.036(2) 0.078(3) 0.070(3) -0.006(2) -0.009(2) 0.006(2) C12 0.042(2) 0.068(3) 0.045(2) -0.006(2) -0.0089(19) 0.0052(19) C13 0.050(2) 0.047(2) 0.036(2) -0.0003(17) -0.0022(17) 0.0018(17) C14 0.044(2) 0.047(2) 0.0241(17) -0.0055(15) 0.0041(15) -0.0013(16) C15 0.0388(19) 0.044(2) 0.0295(19) 0.0049(15) 0.0023(15) 0.0023(15) C16 0.0359(19) 0.0327(18) 0.0256(18) -0.0011(14) 0.0013(14) -0.0021(14) C1S 0.173(8) 0.130(6) 0.085(5) -0.029(5) 0.060(5) -0.083(6) C2S 0.138(6) 0.131(6) 0.093(5) 0.020(4) -0.003(4) -0.041(5) _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 Ni O2 2.037(2) 8_657 ? Ni N1 2.042(3) . ? Ni O1 2.044(2) . ? Ni N3 2.062(3) . ? Ni N2 2.083(3) . ? Cl O5 1.419(3) . ? Cl O6 1.424(3) . ? Cl O4 1.427(3) . ? Cl O3 1.430(3) . ? O1 C16 1.274(4) . ? O2 C16 1.254(4) . ? O2 Ni 2.037(2) 7_567 ? N1 C5 1.346(5) . ? N1 C1 1.356(4) . ? N2 C7 1.490(4) . ? N2 C8 1.491(4) . ? N2 C14 1.494(4) . ? N3 C9 1.338(4) . ? N3 C13 1.342(5) . ? N1S C1S 1.169(10) . ? C1 C2 1.365(5) . ? C1 H1 0.9300 . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.359(6) . ? C3 H3 0.9300 . ? C4 C5 1.393(5) . ? C4 H4 0.9300 . ? C5 C6 1.497(5) . ? C6 C7 1.514(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.496(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.381(5) . ? C10 C11 1.380(6) . ? C10 H10 0.9300 . ? C11 C12 1.370(6) . ? C11 H11 0.9300 . ? C12 C13 1.371(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.522(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.497(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C1S C2S 1.413(9) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni N1 96.35(11) 8_657 . ? O2 Ni O1 90.76(9) 8_657 . ? N1 Ni O1 95.53(10) . . ? O2 Ni N3 91.25(11) 8_657 . ? N1 Ni N3 99.58(11) . . ? O1 Ni N3 164.45(10) . . ? O2 Ni N2 164.36(10) 8_657 . ? N1 Ni N2 98.26(12) . . ? O1 Ni N2 93.35(10) . . ? N3 Ni N2 80.86(11) . . ? O5 Cl O6 110.1(2) . . ? O5 Cl O4 108.8(2) . . ? O6 Cl O4 109.4(2) . . ? O5 Cl O3 109.7(2) . . ? O6 Cl O3 108.9(2) . . ? O4 Cl O3 109.9(2) . . ? C16 O1 Ni 121.0(2) . . ? C16 O2 Ni 103.3(2) . 7_567 ? C5 N1 C1 118.1(3) . . ? C5 N1 Ni 124.3(2) . . ? C1 N1 Ni 117.5(2) . . ? C7 N2 C8 108.5(3) . . ? C7 N2 C14 109.7(3) . . ? C8 N2 C14 108.5(3) . . ? C7 N2 Ni 110.2(2) . . ? C8 N2 Ni 104.4(2) . . ? C14 N2 Ni 115.1(2) . . ? C9 N3 C13 118.6(3) . . ? C9 N3 Ni 112.8(2) . . ? C13 N3 Ni 128.1(3) . . ? N1 C1 C2 123.4(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.1(4) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 120.3(4) . . ? N1 C5 C6 119.1(3) . . ? C4 C5 C6 120.6(4) . . ? C5 C6 C7 115.8(3) . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? N2 C7 C6 113.6(3) . . ? N2 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N2 C8 C9 111.5(3) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N3 C9 C10 122.1(3) . . ? N3 C9 C8 115.8(3) . . ? C10 C9 C8 122.0(3) . . ? C11 C10 C9 118.3(4) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.6(4) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? N3 C13 C12 122.4(4) . . ? N3 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? N2 C14 C15 112.3(3) . . ? N2 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N2 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.0(3) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O2 C16 O1 120.6(3) . . ? O2 C16 C15 118.8(3) . . ? O1 C16 C15 120.5(3) . . ? N1S C1S C2S 176.6(11) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.430 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.080 #===END data_2augam _database_code_depnum_ccdc_archive 'CCDC 718563' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Cu4 F12 N8 O24 S4' _chemical_formula_sum 'C48 H60 Cu4 F12 N8 O24 S4' _chemical_formula_weight 1743.44 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 19.7752(8) _cell_length_b 19.7752(8) _cell_length_c 8.4849(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3318.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8340 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10684 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3988 _reflns_number_gt 3671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WingX publication routine (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^)+(0.0575P)^2^+7.9807P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.046(16) _refine_ls_number_reflns 3988 _refine_ls_number_parameters 227 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Cu Cu 0.37108(2) 0.09403(2) 0.29499(5) 0.01564(12) Uani 1 1 d . . . S1 S 0.22460(5) 0.09010(5) 0.48983(12) 0.0198(2) Uani 1 1 d . . . F1 F 0.10035(14) 0.05258(15) 0.5499(4) 0.0446(8) Uani 1 1 d . . . F2 F 0.17470(14) -0.02506(14) 0.5903(4) 0.0383(7) Uani 1 1 d . . . F3 F 0.14650(15) 0.00116(16) 0.3527(4) 0.0428(8) Uani 1 1 d . . . O1 O 0.38992(14) 0.00441(13) 0.2014(3) 0.0187(5) Uani 1 1 d . . . O2 O 0.43270(13) 0.06664(13) 0.4701(3) 0.0171(5) Uani 1 1 d . . . O3 O 0.28160(14) 0.05128(15) 0.4275(4) 0.0251(6) Uani 1 1 d . . . O4 O 0.19846(15) 0.14043(15) 0.3838(4) 0.0255(6) Uani 1 1 d . . . O5 O 0.23098(17) 0.11082(17) 0.6508(4) 0.0314(7) Uani 1 1 d . . . O1W O 0.0699(5) 0.0123(4) 0.9859(14) 0.149(4) Uani 1 1 d . . . N1 N 0.36802(17) 0.18740(16) 0.3973(4) 0.0185(7) Uani 1 1 d . . . N2 N 0.33261(17) 0.12331(17) 0.0861(4) 0.0186(6) Uani 1 1 d . . . C1 C 0.3684(2) 0.1894(2) 0.5570(5) 0.0222(8) Uani 1 1 d . . . H1 H 0.3632 0.1484 0.6140 0.027 Uiso 1 1 calc R . . C2 C 0.3762(2) 0.2490(2) 0.6397(5) 0.0237(9) Uani 1 1 d . . . H2 H 0.3772 0.2484 0.7516 0.028 Uiso 1 1 calc R . . C3 C 0.3825(2) 0.3093(2) 0.5598(6) 0.0281(9) Uani 1 1 d . . . H3 H 0.3881 0.3508 0.6148 0.034 Uiso 1 1 calc R . . C4 C 0.3802(2) 0.3076(2) 0.3975(5) 0.0259(9) Uani 1 1 d . . . H4 H 0.3842 0.3484 0.3391 0.031 Uiso 1 1 calc R . . C5 C 0.37197(19) 0.2460(2) 0.3179(5) 0.0204(8) Uani 1 1 d . . . C6 C 0.3677(2) 0.2433(2) 0.1409(5) 0.0208(8) Uani 1 1 d . . . H6A H 0.4118 0.2284 0.0981 0.025 Uiso 1 1 calc R . . H6B H 0.3585 0.2893 0.1001 0.025 Uiso 1 1 calc R . . C7 C 0.3127(2) 0.1956(2) 0.0830(5) 0.0210(8) Uani 1 1 d . . . H7A H 0.2720 0.2017 0.1494 0.025 Uiso 1 1 calc R . . H7B H 0.3005 0.2081 -0.0263 0.025 Uiso 1 1 calc R . . C8 C 0.2725(2) 0.0830(2) 0.0400(5) 0.0225(8) Uani 1 1 d D . . H8A H 0.2852(2) 0.0298(2) 0.0412(5) 0.034 Uiso 1 1 calc RD . . H8B H 0.2566(2) 0.0975(2) -0.0774(5) 0.034 Uiso 1 1 calc RD . . H8C H 0.2317(2) 0.0924(2) 0.1225(5) 0.034 Uiso 1 1 calc RD . . C9 C 0.3903(2) 0.1133(2) -0.0273(5) 0.0218(8) Uani 1 1 d . . . H9A H 0.4315 0.1333 0.0196 0.026 Uiso 1 1 calc R . . H9B H 0.3802 0.1387 -0.1250 0.026 Uiso 1 1 calc R . . C10 C 0.4056(2) 0.0404(2) -0.0714(5) 0.0220(8) Uani 1 1 d . . . H10A H 0.4486 0.0396 -0.1309 0.026 Uiso 1 1 calc R . . H10B H 0.3696 0.0244 -0.1433 0.026 Uiso 1 1 calc R . . C11 C 0.41121(19) -0.0092(2) 0.0647(5) 0.0174(7) Uani 1 1 d . . . C12 C 0.1582(2) 0.0269(2) 0.4972(6) 0.0274(9) Uani 1 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 Cu 0.0188(2) 0.0174(2) 0.0107(2) 0.00084(17) -0.00040(17) 0.00110(17) S1 0.0206(4) 0.0204(4) 0.0185(5) 0.0012(4) 0.0036(4) 0.0015(3) F1 0.0230(13) 0.0373(16) 0.074(2) 0.0060(15) 0.0179(14) 0.0045(11) F2 0.0326(14) 0.0281(14) 0.0541(19) 0.0125(14) 0.0159(14) 0.0044(11) F3 0.0362(15) 0.0431(17) 0.049(2) -0.0088(14) -0.0030(14) -0.0125(12) O1 0.0259(13) 0.0192(12) 0.0109(12) 0.0003(11) 0.0015(12) 0.0033(10) O2 0.0170(13) 0.0224(13) 0.0120(13) 0.0042(10) -0.0021(10) 0.0030(10) O3 0.0185(14) 0.0267(15) 0.0302(17) -0.0002(13) 0.0082(12) 0.0024(11) O4 0.0290(15) 0.0239(15) 0.0236(16) 0.0024(12) 0.0022(12) 0.0040(12) O5 0.0376(18) 0.0370(18) 0.0195(16) -0.0046(13) 0.0020(13) 0.0055(14) O1W 0.172(8) 0.067(4) 0.209(11) -0.025(6) -0.066(8) 0.040(5) N1 0.0237(17) 0.0161(15) 0.0157(17) 0.0025(13) -0.0016(13) -0.0013(12) N2 0.0233(16) 0.0216(16) 0.0110(15) 0.0007(13) 0.0002(13) 0.0031(13) C1 0.029(2) 0.023(2) 0.0143(19) 0.0021(15) 0.0024(15) -0.0010(16) C2 0.031(2) 0.025(2) 0.0148(19) -0.0054(16) -0.0005(16) -0.0010(17) C3 0.034(2) 0.024(2) 0.027(2) -0.0052(17) 0.0007(19) -0.0006(17) C4 0.032(2) 0.023(2) 0.023(2) 0.0034(17) -0.0014(18) 0.0004(17) C5 0.0187(18) 0.0219(19) 0.021(2) 0.0022(16) 0.0022(16) 0.0023(14) C6 0.024(2) 0.0189(18) 0.0195(19) 0.0039(15) 0.0032(16) 0.0032(14) C7 0.0230(19) 0.025(2) 0.0151(19) 0.0027(16) -0.0001(15) 0.0075(15) C8 0.0166(18) 0.028(2) 0.022(2) 0.0003(16) -0.0020(15) 0.0040(15) C9 0.029(2) 0.022(2) 0.0143(18) 0.0057(15) 0.0021(16) 0.0018(14) C10 0.027(2) 0.025(2) 0.0142(19) 0.0000(16) -0.0006(16) 0.0072(15) C11 0.0146(17) 0.0224(18) 0.0151(19) 0.0014(15) 0.0032(14) -0.0043(14) C12 0.024(2) 0.0207(19) 0.037(3) 0.0010(19) 0.0106(19) 0.0056(15) _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 Cu O1 1.978(3) . ? Cu O2 1.997(3) . ? Cu N2 2.014(3) . ? Cu N1 2.041(3) . ? Cu O3 2.261(3) . ? S1 O5 1.432(3) . ? S1 O4 1.438(3) . ? S1 O3 1.463(3) . ? S1 C12 1.814(4) . ? F1 C12 1.330(5) . ? F2 C12 1.335(5) . ? F3 C12 1.347(6) . ? O1 C11 1.263(5) . ? O2 C11 1.264(5) 7 ? N1 C5 1.342(5) . ? N1 C1 1.356(5) . ? N2 C7 1.483(5) . ? N2 C8 1.484(5) . ? N2 C9 1.505(5) . ? C1 C2 1.380(6) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 C4 1.378(7) . ? C3 H3 0.9500 . ? C4 C5 1.403(6) . ? C4 H4 0.9500 . ? C5 C6 1.505(6) . ? C6 C7 1.520(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 1.0828 . ? C8 H8B 1.0828 . ? C8 H8C 1.0828 . ? C9 C10 1.519(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.264(5) 8_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu O2 86.61(11) . . ? O1 Cu N2 88.59(13) . . ? O2 Cu N2 164.50(12) . . ? O1 Cu N1 170.78(12) . . ? O2 Cu N1 86.96(12) . . ? N2 Cu N1 95.91(13) . . ? O1 Cu O3 90.69(11) . . ? O2 Cu O3 90.35(11) . . ? N2 Cu O3 104.45(13) . . ? N1 Cu O3 95.94(12) . . ? O5 S1 O4 115.5(2) . . ? O5 S1 O3 115.3(2) . . ? O4 S1 O3 114.47(18) . . ? O5 S1 C12 103.2(2) . . ? O4 S1 C12 103.8(2) . . ? O3 S1 C12 102.02(18) . . ? C11 O1 Cu 128.5(3) . . ? C11 O2 Cu 106.6(2) 7 . ? S1 O3 Cu 125.93(18) . . ? C5 N1 C1 118.4(4) . . ? C5 N1 Cu 124.4(3) . . ? C1 N1 Cu 116.8(3) . . ? C7 N2 C8 107.5(3) . . ? C7 N2 C9 108.5(3) . . ? C8 N2 C9 111.6(3) . . ? C7 N2 Cu 113.1(3) . . ? C8 N2 Cu 112.4(3) . . ? C9 N2 Cu 103.8(2) . . ? N1 C1 C2 122.3(4) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 120.0(4) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 117.8(4) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 117.8(4) . . ? C4 C5 C6 121.2(4) . . ? C5 C6 C7 112.6(3) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C6 113.8(3) . . ? N2 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 115.7(3) . . ? N2 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N2 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 116.1(3) . . ? C9 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? C9 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? O1 C11 O2 121.6(4) . 8_545 ? O1 C11 C10 122.4(3) . . ? O2 C11 C10 115.8(3) 8_545 . ? F1 C12 F2 107.8(4) . . ? F1 C12 F3 107.5(4) . . ? F2 C12 F3 106.8(4) . . ? F1 C12 S1 111.8(3) . . ? F2 C12 S1 112.0(3) . . ? F3 C12 S1 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.953 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.100 #===END data_3sepbm _database_code_depnum_ccdc_archive 'CCDC 718564' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H68 Cl4 Cu4 N12 O24' _chemical_formula_sum 'C56 H68 Cl4 Cu4 N12 O24' _chemical_formula_weight 1689.18 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 Tetragonal _symmetry_space_group_name_H-M P-421c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 20.532(5) _cell_length_b 20.532(5) _cell_length_c 8.217(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 3464(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8685 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23088 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4296 _reflns_number_gt 3205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WingX publication routine (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^)+(0.0627P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 4296 _refine_ls_number_parameters 246 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.994 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.11090(2) 0.10458(2) 0.05696(6) 0.01847(13) Uani 1 1 d . . . Cl Cl 0.23697(5) 0.05413(5) 0.34535(13) 0.0235(2) Uani 1 1 d . . . O1 O 0.11085(13) 0.01845(12) -0.0367(3) 0.0199(6) Uani 1 1 d . . . O2 O 0.07651(14) -0.04796(14) -0.2285(3) 0.0199(6) Uani 1 1 d . . . O3 O 0.19825(14) 0.09956(16) 0.2515(4) 0.0304(7) Uani 1 1 d . . . O4 O 0.27532(14) 0.09031(16) 0.4598(4) 0.0333(8) Uani 1 1 d . . . O5 O 0.19378(15) 0.01020(14) 0.4286(4) 0.0304(7) Uani 1 1 d . . . O6 O 0.27884(16) 0.01744(15) 0.2381(4) 0.0352(8) Uani 1 1 d . . . N1 N 0.10250(17) 0.19544(16) 0.1319(4) 0.0213(7) Uani 1 1 d . . . N2 N 0.15047(16) 0.14750(16) -0.1469(4) 0.0194(7) Uani 1 1 d . . . N1S N 0.0789(3) 0.4647(3) 0.0039(8) 0.078(2) Uani 1 1 d . . . C1 C 0.0933(2) 0.2166(2) 0.2845(5) 0.0269(10) Uani 1 1 d . . . H1 H 0.0931 0.1867 0.3695 0.032 Uiso 1 1 calc R . . C2 C 0.0841(2) 0.2812(2) 0.3179(6) 0.0304(11) Uani 1 1 d . . . H2 H 0.0766 0.2948 0.4241 0.037 Uiso 1 1 calc R . . C3 C 0.0859(2) 0.3257(2) 0.1932(6) 0.0330(12) Uani 1 1 d . . . H3 H 0.0812 0.3699 0.2147 0.040 Uiso 1 1 calc R . . C4 C 0.0949(2) 0.3040(2) 0.0350(6) 0.0297(10) Uani 1 1 d . . . H4 H 0.0956 0.3332 -0.0515 0.036 Uiso 1 1 calc R . . C5 C 0.1029(2) 0.2384(2) 0.0088(5) 0.0233(9) Uani 1 1 d . . . C6 C 0.1089(2) 0.20636(19) -0.1588(5) 0.0232(9) Uani 1 1 d . . . H6A H 0.0661 0.1944 -0.1984 0.028 Uiso 1 1 calc R . . H6B H 0.1280 0.2369 -0.2352 0.028 Uiso 1 1 calc R . . C7 C 0.2217(2) 0.1663(2) -0.1205(6) 0.0275(10) Uani 1 1 d . . . H7 H 0.2241 0.1892 -0.0161 0.033 Uiso 1 1 calc R . . C8 C 0.2643(2) 0.1055(2) -0.1058(5) 0.0328(11) Uani 1 1 d . . . H8A H 0.2467 0.0773 -0.0236 0.049 Uiso 1 1 calc R . . H8B H 0.3077 0.1180 -0.0764 0.049 Uiso 1 1 calc R . . H8C H 0.2651 0.0830 -0.2083 0.049 Uiso 1 1 calc R . . C9 C 0.2487(2) 0.2115(2) -0.2477(6) 0.0370(12) Uani 1 1 d . . . H9A H 0.2220 0.2497 -0.2545 0.055 Uiso 1 1 calc R . . H9B H 0.2492 0.1898 -0.3512 0.055 Uiso 1 1 calc R . . H9C H 0.2923 0.2237 -0.2185 0.055 Uiso 1 1 calc R . . C10 C 0.1411(2) 0.1088(2) -0.2986(5) 0.0237(9) Uani 1 1 d D . . H10A H 0.1837(2) 0.0787(2) -0.3180(5) 0.028 Uiso 1 1 calc RD . . H10B H 0.1372(2) 0.1419(2) -0.4007(5) 0.028 Uiso 1 1 calc RD . . C11 C 0.0809(2) 0.0653(2) -0.2946(5) 0.0207(9) Uani 1 1 d . . . H11A H 0.0435 0.0908 -0.2607 0.025 Uiso 1 1 calc R . . H11B H 0.0723 0.0489 -0.4032 0.025 Uiso 1 1 calc R . . C12 C 0.08974(19) 0.0087(2) -0.1794(5) 0.0191(9) Uani 1 1 d . . . C1SA C 0.0695(6) 0.5203(6) -0.0585(17) 0.061(3) Uani 0.55 1 d P A 1 C2SA C 0.0659(7) 0.5804(6) -0.1356(18) 0.064(4) Uani 0.50 1 d P A 1 C1SB C 0.0828(6) 0.5086(6) 0.1042(19) 0.050(4) Uani 0.45 1 d P A 2 C2SB C 0.0768(7) 0.5652(7) 0.211(2) 0.083(5) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0201(3) 0.0195(2) 0.0158(2) 0.0003(2) 0.0001(2) -0.0012(2) Cl 0.0252(5) 0.0237(5) 0.0215(5) -0.0012(4) -0.0011(4) -0.0010(5) O1 0.0224(14) 0.0159(13) 0.0214(14) 0.0010(11) 0.0008(13) 0.0001(12) O2 0.0224(15) 0.0187(14) 0.0185(15) -0.0003(12) 0.0017(12) 0.0045(13) O3 0.0252(16) 0.0352(19) 0.0307(18) 0.0033(15) -0.0072(14) 0.0020(15) O4 0.0298(16) 0.0390(18) 0.0311(18) -0.0040(16) -0.0122(15) -0.0065(15) O5 0.0365(18) 0.0282(17) 0.0263(16) 0.0011(15) 0.0054(16) -0.0091(14) O6 0.0333(18) 0.0339(19) 0.039(2) -0.0070(16) 0.0087(16) 0.0001(15) N1 0.0224(19) 0.0221(17) 0.0195(17) -0.0015(15) -0.0034(16) -0.0020(16) N2 0.0185(17) 0.0202(17) 0.0195(18) -0.0008(15) 0.0004(15) -0.0024(15) N1S 0.075(4) 0.063(4) 0.095(5) 0.016(3) 0.037(4) 0.009(3) C1 0.030(3) 0.028(2) 0.023(2) -0.0028(18) -0.0039(19) -0.002(2) C2 0.033(3) 0.033(3) 0.026(2) -0.007(2) -0.002(2) -0.004(2) C3 0.040(3) 0.019(2) 0.040(3) -0.007(2) 0.000(2) -0.008(2) C4 0.032(3) 0.022(2) 0.035(3) 0.002(2) -0.003(2) -0.002(2) C5 0.019(2) 0.023(2) 0.028(2) -0.0009(17) -0.0020(18) -0.0057(19) C6 0.028(2) 0.021(2) 0.021(2) 0.0049(17) 0.000(2) -0.004(2) C7 0.022(2) 0.036(3) 0.025(2) -0.003(2) 0.0016(18) -0.012(2) C8 0.021(2) 0.053(3) 0.024(2) -0.002(2) 0.0011(18) -0.001(2) C9 0.029(3) 0.044(3) 0.037(3) -0.006(2) 0.008(2) -0.012(2) C10 0.026(2) 0.028(2) 0.017(2) -0.0001(19) 0.0001(17) -0.002(2) C11 0.025(2) 0.019(2) 0.018(2) -0.0015(16) 0.0011(17) 0.0011(18) C12 0.0149(19) 0.026(2) 0.017(2) -0.0020(17) 0.0005(16) -0.0023(17) C1SA 0.055(7) 0.055(7) 0.073(8) 0.019(7) -0.005(7) 0.004(6) C2SA 0.079(10) 0.043(7) 0.069(9) 0.021(7) -0.018(8) -0.010(7) C1SB 0.030(6) 0.042(7) 0.077(11) -0.007(7) 0.018(6) 0.001(6) C2SB 0.043(8) 0.069(10) 0.137(16) -0.037(11) 0.032(10) -0.004(7) _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 Cu O1 1.929(3) . ? Cu N1 1.972(3) . ? Cu O2 1.997(3) 7 ? Cu N2 2.060(4) . ? Cu O3 2.405(3) . ? Cl O4 1.434(3) . ? Cl O5 1.438(3) . ? Cl O6 1.443(3) . ? Cl O3 1.448(3) . ? O1 C12 1.266(5) . ? O2 C12 1.261(5) . ? O2 Cu 1.997(3) 8 ? N1 C1 1.341(5) . ? N1 C5 1.342(5) . ? N2 C6 1.482(5) . ? N2 C10 1.490(5) . ? N2 C7 1.527(5) . ? N1S C1SB 1.224(14) . ? N1S C1SA 1.267(12) . ? C1 C2 1.367(6) . ? C1 H1 0.9300 . ? C2 C3 1.373(7) . ? C2 H2 0.9300 . ? C3 C4 1.387(6) . ? C3 H3 0.9300 . ? C4 C5 1.373(6) . ? C4 H4 0.9300 . ? C5 C6 1.531(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.503(6) . ? C7 C8 1.529(7) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.527(6) . ? C10 H10A 1.0827 . ? C10 H10B 1.0827 . ? C11 C12 1.510(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C1SA C2SA 1.390(15) . ? C1SB C2SB 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu N1 172.71(13) . . ? O1 Cu O2 90.95(12) . 7 ? N1 Cu O2 89.78(13) . 7 ? O1 Cu N2 93.89(13) . . ? N1 Cu N2 83.32(13) . . ? O2 Cu N2 162.29(12) 7 . ? O1 Cu O3 103.09(11) . . ? N1 Cu O3 84.16(13) . . ? O2 Cu O3 90.07(11) 7 . ? N2 Cu O3 105.35(12) . . ? O4 Cl O5 110.6(2) . . ? O4 Cl O6 110.1(2) . . ? O5 Cl O6 109.29(19) . . ? O4 Cl O3 108.48(18) . . ? O5 Cl O3 108.59(19) . . ? O6 Cl O3 109.8(2) . . ? C12 O1 Cu 121.0(3) . . ? C12 O2 Cu 108.0(3) . 8 ? Cl O3 Cu 142.29(19) . . ? C1 N1 C5 119.5(4) . . ? C1 N1 Cu 127.7(3) . . ? C5 N1 Cu 112.7(3) . . ? C6 N2 C10 107.8(3) . . ? C6 N2 C7 110.7(3) . . ? C10 N2 C7 112.1(3) . . ? C6 N2 Cu 100.1(2) . . ? C10 N2 Cu 113.7(2) . . ? C7 N2 Cu 111.7(3) . . ? C1SB N1S C1SA 67.6(10) . . ? N1 C1 C2 121.4(4) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.6(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 113.3(3) . . ? C4 C5 C6 124.9(4) . . ? N2 C6 C5 109.7(3) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C9 C7 N2 114.3(4) . . ? C9 C7 C8 110.3(4) . . ? N2 C7 C8 110.6(3) . . ? C9 C7 H7 107.1 . . ? N2 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 113.5(3) . . ? N2 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N2 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 111.5(4) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? O2 C12 O1 121.1(4) . . ? O2 C12 C11 118.9(4) . . ? O1 C12 C11 120.0(4) . . ? N1S C1SA C2SA 173.6(13) . . ? N1S C1SB C2SB 169.9(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.741 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.108 #===END data_26febbm _database_code_depnum_ccdc_archive 'CCDC 718565' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H59 Cl4 Cu4 N9 O38' _chemical_formula_sum 'C51 H59 Cl4 Cu4 N9 O38' _chemical_formula_weight 1802.03 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.960(5) _cell_length_b 14.823(5) _cell_length_c 25.883(5) _cell_angle_alpha 76.241(5) _cell_angle_beta 87.467(5) _cell_angle_gamma 68.532(5) _cell_volume 3797(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 28.32 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7752 _exptl_absorpt_correction_T_max 0.8775 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25319 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.32 _reflns_number_total 18004 _reflns_number_gt 8824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WingX publication routine (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^)+(0.1690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18004 _refine_ls_number_parameters 956 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.3031 _refine_ls_wR_factor_gt 0.2547 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 0.17262(8) 0.42442(6) 0.12671(3) 0.0425(2) Uani 1 1 d . . . Cu2 Cu 0.02528(8) 0.67239(6) 0.21543(3) 0.0459(2) Uani 1 1 d . . . Cu3 Cu 0.22827(9) 0.43085(7) 0.36777(4) 0.0569(3) Uani 1 1 d . . . Cu4 Cu 0.42554(9) 0.21335(7) 0.26874(4) 0.0549(3) Uani 1 1 d . . . Cl1 Cl 0.3795(2) 0.85435(16) 0.09329(10) 0.0687(6) Uani 1 1 d . . . Cl2 Cl 0.2056(3) 0.8032(2) 0.92849(11) 0.0855(7) Uani 1 1 d . . . Cl3 Cl 0.8571(4) 0.2855(4) 0.39000(18) 0.1448(15) Uani 1 1 d . . . Cl4 Cl 0.5584(4) 0.7234(4) 0.39365(14) 0.1241(13) Uani 1 1 d . . . O1 O -0.0068(5) 0.5058(4) 0.0715(2) 0.0630(14) Uani 1 1 d . . . O2 O -0.1220(6) 0.6640(4) 0.0320(2) 0.0764(17) Uani 1 1 d . . . O3 O 0.1442(4) 0.5347(3) 0.15950(19) 0.0475(11) Uani 1 1 d . . . O4 O 0.2112(4) 0.6299(4) 0.19488(19) 0.0493(11) Uani 1 1 d . . . O5 O 0.0440(6) 0.7829(4) 0.2566(2) 0.0709(15) Uani 1 1 d . . . O6 O 0.0229(7) 0.8210(5) 0.3347(2) 0.093(2) Uani 1 1 d . . . O7 O 0.0826(5) 0.5665(4) 0.28053(19) 0.0537(12) Uani 1 1 d . . . O8 O 0.0727(5) 0.4288(4) 0.3325(2) 0.0666(15) Uani 1 1 d . . . O9 O 0.2544(6) 0.2973(5) 0.4357(2) 0.0786(17) Uani 1 1 d . . . O10 O 0.4027(8) 0.1480(5) 0.4696(3) 0.097(2) Uani 1 1 d . . . O11 O 0.3438(5) 0.3471(4) 0.3240(2) 0.0572(13) Uani 1 1 d . . . O12 O 0.4859(5) 0.3283(4) 0.2623(2) 0.0573(13) Uani 1 1 d . . . O13 O 0.5339(8) 0.1526(5) 0.2026(3) 0.101(2) Uani 1 1 d . . . O14 O 0.6188(8) 0.0400(6) 0.1577(4) 0.114(3) Uani 1 1 d . . . O15 O 0.2819(5) 0.3004(4) 0.2183(2) 0.0675(15) Uani 1 1 d . . . O16 O 0.0809(5) 0.3634(4) 0.1840(2) 0.0541(12) Uani 1 1 d . . . O17 O 0.4592(8) 0.8760(8) 0.0519(4) 0.135(3) Uani 1 1 d . . . O18 O 0.2475(6) 0.9203(5) 0.0801(3) 0.105(2) Uani 1 1 d . . . O19 O 0.4231(8) 0.8691(7) 0.1398(3) 0.116(3) Uani 1 1 d . . . O20 O 0.3879(10) 0.7556(5) 0.1012(4) 0.148(4) Uani 1 1 d . . . O21 O 0.0911(11) 0.8061(12) 0.9185(7) 0.285(11) Uani 1 1 d . . . O22 O 0.2459(15) 0.8611(13) 0.8891(5) 0.247(8) Uani 1 1 d . . . O23 O 0.2864(11) 0.7229(11) 0.9455(12) 0.390(18) Uani 1 1 d . . . O24 O 0.191(3) 0.851(2) 0.9655(8) 0.409(17) Uani 1 1 d . . . O25 O 0.845(3) 0.373(2) 0.4101(8) 0.366(17) Uani 1 1 d . . . O26 O 0.9877(13) 0.2373(16) 0.4012(8) 0.313(12) Uani 1 1 d . . . O27 O 0.7760(13) 0.2498(12) 0.4271(6) 0.239(7) Uani 1 1 d . . . O28 O 0.8157(11) 0.3066(10) 0.3368(4) 0.166(4) Uani 1 1 d . . . O29 O 0.6312(9) 0.7475(9) 0.4294(5) 0.163(4) Uani 1 1 d . . . O30 O 0.6088(16) 0.6327(8) 0.4036(6) 0.227(8) Uani 1 1 d . . . O31 O 0.5521(12) 0.7686(14) 0.3449(4) 0.254(9) Uani 1 1 d . . . O32 O 0.4299(14) 0.7528(18) 0.4092(5) 0.278(11) Uani 1 1 d . . . O1W O 0.8347(9) 0.1120(7) 0.5370(4) 0.139(3) Uani 1 1 d . . . O2W O 0.3691(9) 0.7263(7) 0.2339(3) 0.126(3) Uani 1 1 d . . . O3W O 0.2543(9) 0.8300(7) 0.3121(4) 0.140(4) Uani 1 1 d . . . O4W O 0.6676(7) 0.6386(5) 0.0731(3) 0.097(2) Uani 1 1 d . . . O5W O 0.7969(13) -0.0740(16) 0.5369(4) 0.274(9) Uani 1 1 d . . . O1S O 0.0572(19) 0.9971(11) 0.1844(7) 0.248(8) Uani 1 1 d . . . N1 N 0.2329(6) 0.3060(4) 0.0966(2) 0.0484(14) Uani 1 1 d . . . N2 N 0.2955(5) 0.4689(4) 0.0736(2) 0.0478(13) Uani 1 1 d . . . N3 N -0.0426(6) 0.7659(4) 0.1457(2) 0.0480(14) Uani 1 1 d . . . N4 N -0.1700(6) 0.7052(5) 0.2300(2) 0.0541(15) Uani 1 1 d . . . N5 N 0.1192(8) 0.5280(7) 0.4080(3) 0.085(3) Uani 1 1 d . . . N6 N 0.3807(7) 0.4589(5) 0.3947(2) 0.0622(17) Uani 1 1 d . . . N8 N 0.3447(7) 0.1056(5) 0.2901(3) 0.0656(18) Uani 1 1 d . . . N7 N 0.5601(7) 0.1230(5) 0.3243(3) 0.0656(18) Uani 1 1 d . . . N1S N 0.2993(15) 0.5178(13) 0.8351(8) 0.193(8) Uani 1 1 d . . . C1 C 0.1753(8) 0.2392(5) 0.0991(3) 0.0534(18) Uani 1 1 d . . . H1 H 0.0950 0.2494 0.1149 0.064 Uiso 1 1 calc R . . C2 C 0.2330(10) 0.1551(6) 0.0787(3) 0.068(2) Uani 1 1 d . . . H2 H 0.1920 0.1094 0.0810 0.081 Uiso 1 1 calc R . . C3 C 0.3518(9) 0.1406(6) 0.0549(4) 0.073(2) Uani 1 1 d . . . H3 H 0.3929 0.0846 0.0414 0.088 Uiso 1 1 calc R . . C4 C 0.4082(9) 0.2115(6) 0.0517(3) 0.068(2) Uani 1 1 d . . . H4 H 0.4879 0.2034 0.0357 0.082 Uiso 1 1 calc R . . C5 C 0.3472(7) 0.2929(5) 0.0720(3) 0.0525(17) Uani 1 1 d . . . C6 C 0.4018(7) 0.3719(5) 0.0721(3) 0.0535(18) Uani 1 1 d . . . H6A H 0.4618 0.3506 0.1028 0.064 Uiso 1 1 calc R . . H6B H 0.4508 0.3807 0.0403 0.064 Uiso 1 1 calc R . . C7 C 0.2276(7) 0.5144(5) 0.0198(3) 0.0520(17) Uani 1 1 d . . . H7A H 0.2053 0.4646 0.0081 0.062 Uiso 1 1 calc R . . H7B H 0.2877 0.5334 -0.0051 0.062 Uiso 1 1 calc R . . C8 C 0.1033(8) 0.6056(6) 0.0182(3) 0.062(2) Uani 1 1 d . . . H8A H 0.1233 0.6500 0.0356 0.074 Uiso 1 1 calc R . . H8B H 0.0785 0.6406 -0.0187 0.074 Uiso 1 1 calc R . . C9 C -0.0118(8) 0.5853(6) 0.0435(3) 0.0565(19) Uani 1 1 d . . . C10 C 0.3571(7) 0.5351(6) 0.0888(3) 0.0533(18) Uani 1 1 d . . . H10A H 0.3054 0.6042 0.0722 0.064 Uiso 1 1 calc R . . H10B H 0.4444 0.5199 0.0751 0.064 Uiso 1 1 calc R . . C11 C 0.3669(6) 0.5226(6) 0.1493(3) 0.0533(18) Uani 1 1 d . . . H11A H 0.4084 0.4525 0.1668 0.064 Uiso 1 1 calc R . . H11B H 0.4202 0.5576 0.1575 0.064 Uiso 1 1 calc R . . C12 C 0.2327(6) 0.5638(5) 0.1690(2) 0.0419(15) Uani 1 1 d . . . C13 C 0.0253(9) 0.8111(6) 0.1105(3) 0.067(2) Uani 1 1 d . . . H13 H 0.1147 0.7935 0.1172 0.080 Uiso 1 1 calc R . . C14 C -0.0354(11) 0.8824(7) 0.0651(3) 0.082(3) Uani 1 1 d . . . H14 H 0.0116 0.9130 0.0411 0.098 Uiso 1 1 calc R . . C15 C -0.1705(9) 0.9072(6) 0.0564(3) 0.073(2) Uani 1 1 d . . . H15 H -0.2144 0.9546 0.0260 0.087 Uiso 1 1 calc R . . C16 C -0.2377(9) 0.8618(6) 0.0923(3) 0.068(2) Uani 1 1 d . . . H16 H -0.3274 0.8787 0.0870 0.081 Uiso 1 1 calc R . . C17 C -0.1720(8) 0.7925(6) 0.1353(3) 0.0546(18) Uani 1 1 d . . . C18 C -0.2326(7) 0.7317(6) 0.1762(3) 0.064(2) Uani 1 1 d . . . H18A H -0.3256 0.7696 0.1772 0.077 Uiso 1 1 calc R . . H18B H -0.2234 0.6710 0.1656 0.077 Uiso 1 1 calc R . . C19 C -0.2192(8) 0.7938(6) 0.2522(3) 0.070(2) Uani 1 1 d . . . H19A H -0.3113 0.8076 0.2590 0.084 Uiso 1 1 calc R . . H19B H -0.2143 0.8501 0.2252 0.084 Uiso 1 1 calc R . . C20 C -0.1505(9) 0.7890(7) 0.3028(4) 0.075(2) Uani 1 1 d . . . H20A H -0.2058 0.8429 0.3183 0.090 Uiso 1 1 calc R . . H20B H -0.1414 0.7267 0.3280 0.090 Uiso 1 1 calc R . . C21 C -0.0191(10) 0.7961(6) 0.2960(4) 0.069(2) Uani 1 1 d . . . C22 C -0.1991(8) 0.6204(6) 0.2650(3) 0.063(2) Uani 1 1 d . . . H22A H -0.2835 0.6230 0.2534 0.075 Uiso 1 1 calc R . . H22B H -0.2061 0.6290 0.3011 0.075 Uiso 1 1 calc R . . C23 C -0.0966(7) 0.5178(5) 0.2651(3) 0.0552(18) Uani 1 1 d . . . H23A H -0.1301 0.4665 0.2824 0.066 Uiso 1 1 calc R . . H23B H -0.0786 0.5121 0.2287 0.066 Uiso 1 1 calc R . . C24 C 0.0290(7) 0.5028(6) 0.2943(3) 0.0530(17) Uani 1 1 d . . . C25 C -0.0017(11) 0.5426(11) 0.4221(4) 0.127(6) Uani 1 1 d . . . H25 H -0.0468 0.5067 0.4121 0.153 Uiso 1 1 calc R . . C26 C -0.0630(17) 0.6124(15) 0.4523(6) 0.156(9) Uani 1 1 d . . . H26 H -0.1479 0.6220 0.4632 0.187 Uiso 1 1 calc R . . C27 C 0.000(3) 0.6634(14) 0.4648(10) 0.216(17) Uani 1 1 d . . . H27 H -0.0437 0.7134 0.4824 0.259 Uiso 1 1 calc R . . C28 C 0.1285(19) 0.6471(9) 0.4534(6) 0.152(7) Uani 1 1 d . . . H28 H 0.1769 0.6784 0.4658 0.183 Uiso 1 1 calc R . . C29 C 0.1791(15) 0.5811(8) 0.4223(4) 0.105(4) Uani 1 1 d . . . C30 C 0.3113(13) 0.5649(7) 0.4008(4) 0.099(4) Uani 1 1 d . . . H30A H 0.3642 0.5792 0.4245 0.119 Uiso 1 1 calc R . . H30B H 0.3028 0.6110 0.3664 0.119 Uiso 1 1 calc R . . C31 C 0.4329(9) 0.3922(7) 0.4488(3) 0.074(2) Uani 1 1 d . . . H31A H 0.3653 0.4092 0.4741 0.089 Uiso 1 1 calc R . . H31B H 0.5069 0.4056 0.4596 0.089 Uiso 1 1 calc R . . C32 C 0.4771(9) 0.2793(7) 0.4516(4) 0.078(3) Uani 1 1 d . . . H32A H 0.5308 0.2646 0.4217 0.094 Uiso 1 1 calc R . . H32B H 0.5314 0.2423 0.4839 0.094 Uiso 1 1 calc R . . C33 C 0.3667(10) 0.2439(7) 0.4511(3) 0.070(2) Uani 1 1 d . . . C34 C 0.4889(9) 0.4545(7) 0.3580(3) 0.069(2) Uani 1 1 d . . . H34A H 0.5604 0.3908 0.3698 0.083 Uiso 1 1 calc R . . H34B H 0.5211 0.5066 0.3597 0.083 Uiso 1 1 calc R . . C35 C 0.4487(8) 0.4667(6) 0.3004(3) 0.062(2) Uani 1 1 d . . . H35A H 0.3695 0.5255 0.2897 0.075 Uiso 1 1 calc R . . H35B H 0.5176 0.4759 0.2774 0.075 Uiso 1 1 calc R . . C36 C 0.4246(7) 0.3763(5) 0.2947(3) 0.0480(16) Uani 1 1 d . . . C37 C 0.6779(10) 0.1263(8) 0.3313(4) 0.088(3) Uani 1 1 d . . . H37 H 0.6991 0.1785 0.3104 0.106 Uiso 1 1 calc R . . C38 C 0.7725(14) 0.0511(12) 0.3703(6) 0.134(5) Uani 1 1 d . . . H38 H 0.8562 0.0515 0.3743 0.161 Uiso 1 1 calc R . . C39 C 0.734(2) -0.0210(11) 0.4013(6) 0.148(7) Uani 1 1 d . . . H39 H 0.7919 -0.0698 0.4279 0.178 Uiso 1 1 calc R . . C40 C 0.6163(16) -0.0229(10) 0.3943(5) 0.120(5) Uani 1 1 d . . . H40 H 0.5933 -0.0742 0.4151 0.144 Uiso 1 1 calc R . . C41 C 0.5256(11) 0.0523(7) 0.3557(4) 0.079(3) Uani 1 1 d . . . C42 C 0.3936(10) 0.0558(7) 0.3456(3) 0.081(3) Uani 1 1 d . . . H42A H 0.3342 0.0911 0.3692 0.097 Uiso 1 1 calc R . . H42B H 0.3943 -0.0117 0.3536 0.097 Uiso 1 1 calc R . . C43 C 0.384(2) 0.0378(15) 0.2581(5) 0.199(11) Uani 1 1 d . . . H43A H 0.4193 -0.0257 0.2840 0.238 Uiso 1 1 calc R . . H43B H 0.3005 0.0400 0.2454 0.238 Uiso 1 1 calc R . . C44 C 0.4527(12) 0.0227(9) 0.2204(8) 0.140(6) Uani 1 1 d . . . H44A H 0.3939 0.0259 0.1925 0.168 Uiso 1 1 calc R . . H44B H 0.5107 -0.0467 0.2313 0.168 Uiso 1 1 calc R . . C45 C 0.5387(9) 0.0770(6) 0.1925(4) 0.072(2) Uani 1 1 d . . . C46 C 0.2062(13) 0.1495(14) 0.2886(9) 0.274(16) Uani 1 1 d . . . H46A H 0.1766 0.1073 0.2730 0.329 Uiso 1 1 calc R . . H46B H 0.1841 0.1372 0.3257 0.329 Uiso 1 1 calc R . . C47 C 0.1244(10) 0.2412(6) 0.2673(4) 0.080(3) Uani 1 1 d . . . H47A H 0.1020 0.2769 0.2954 0.096 Uiso 1 1 calc R . . H47B H 0.0444 0.2364 0.2559 0.096 Uiso 1 1 calc R . . C48 C 0.1660(8) 0.3045(6) 0.2214(3) 0.0539(18) Uani 1 1 d . . . C1S C 0.2664(13) 0.5989(16) 0.8189(6) 0.134(6) Uani 1 1 d . . . C2S C 0.2301(13) 0.6956(10) 0.7981(5) 0.112(4) Uani 1 1 d . . . H2S1 H 0.2900 0.7202 0.8107 0.169 Uiso 1 1 calc R . . H2S2 H 0.1432 0.7291 0.8085 0.169 Uiso 1 1 calc R . . H2S3 H 0.2306 0.7077 0.7600 0.169 Uiso 1 1 calc R . . C3S C -0.044(2) 1.0477(13) 0.2388(11) 0.238(12) Uani 1 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 Cu1 0.0377(4) 0.0426(5) 0.0483(5) -0.0134(4) 0.0040(3) -0.0147(4) Cu2 0.0439(5) 0.0474(5) 0.0475(5) -0.0134(4) 0.0013(4) -0.0164(4) Cu3 0.0478(5) 0.0684(6) 0.0464(5) -0.0090(4) 0.0031(4) -0.0150(5) Cu4 0.0612(6) 0.0550(6) 0.0497(5) -0.0063(4) -0.0001(4) -0.0261(5) Cl1 0.0571(12) 0.0603(12) 0.0945(16) -0.0301(11) 0.0132(11) -0.0220(10) Cl2 0.0768(17) 0.0934(18) 0.0940(18) -0.0175(14) 0.0180(13) -0.0444(15) Cl3 0.090(2) 0.210(5) 0.138(3) -0.028(3) 0.011(2) -0.068(3) Cl4 0.135(3) 0.176(4) 0.098(2) -0.008(2) -0.006(2) -0.112(3) O1 0.045(3) 0.058(3) 0.081(4) -0.004(3) -0.013(3) -0.019(3) O2 0.068(4) 0.056(3) 0.084(4) -0.014(3) -0.002(3) 0.001(3) O3 0.041(2) 0.053(3) 0.057(3) -0.022(2) 0.008(2) -0.022(2) O4 0.046(3) 0.054(3) 0.054(3) -0.017(2) 0.003(2) -0.023(2) O5 0.089(4) 0.070(4) 0.071(4) -0.034(3) 0.004(3) -0.038(3) O6 0.137(6) 0.103(5) 0.053(4) -0.031(3) -0.007(4) -0.052(5) O7 0.052(3) 0.053(3) 0.055(3) -0.003(2) -0.007(2) -0.023(2) O8 0.049(3) 0.081(4) 0.057(3) 0.007(3) -0.004(2) -0.022(3) O9 0.062(4) 0.085(4) 0.075(4) 0.010(3) 0.000(3) -0.029(3) O10 0.124(6) 0.052(4) 0.098(5) -0.002(3) -0.007(4) -0.020(4) O11 0.055(3) 0.060(3) 0.061(3) -0.017(3) 0.011(2) -0.026(3) O12 0.062(3) 0.063(3) 0.054(3) -0.016(3) 0.007(3) -0.031(3) O13 0.173(8) 0.087(5) 0.071(4) -0.040(4) 0.042(4) -0.071(5) O14 0.102(6) 0.089(5) 0.158(7) -0.076(5) 0.046(5) -0.020(4) O15 0.061(3) 0.073(4) 0.069(3) 0.014(3) -0.016(3) -0.042(3) O16 0.046(3) 0.057(3) 0.066(3) -0.021(3) 0.012(2) -0.023(2) O17 0.112(6) 0.210(10) 0.139(7) -0.083(7) 0.072(6) -0.102(7) O18 0.064(4) 0.084(5) 0.156(7) -0.039(5) 0.004(4) -0.009(4) O19 0.124(6) 0.157(7) 0.095(5) -0.051(5) 0.008(5) -0.072(6) O20 0.182(9) 0.058(4) 0.198(10) -0.020(5) -0.055(7) -0.037(5) O21 0.111(8) 0.310(17) 0.339(19) 0.190(16) -0.079(10) -0.126(10) O22 0.251(15) 0.36(2) 0.176(11) 0.002(12) 0.085(11) -0.221(16) O23 0.073(7) 0.150(12) 0.79(5) 0.083(19) 0.037(15) 0.016(7) O24 0.56(4) 0.55(4) 0.25(2) -0.30(3) 0.10(2) -0.25(4) O25 0.53(4) 0.56(4) 0.31(2) -0.30(3) 0.21(2) -0.45(4) O26 0.103(10) 0.36(2) 0.35(2) 0.100(19) 0.007(12) -0.057(12) O27 0.156(10) 0.303(17) 0.242(15) 0.005(13) 0.084(10) -0.118(12) O28 0.190(10) 0.252(13) 0.085(6) -0.030(7) -0.009(6) -0.118(10) O29 0.119(7) 0.200(10) 0.197(11) -0.051(9) -0.031(7) -0.080(7) O30 0.311(19) 0.073(6) 0.286(17) -0.035(8) -0.135(14) -0.048(8) O31 0.158(11) 0.44(2) 0.073(6) 0.006(10) 0.009(6) -0.042(12) O32 0.173(12) 0.59(3) 0.161(11) -0.089(16) 0.014(9) -0.238(18) O1W 0.124(7) 0.138(7) 0.177(9) -0.034(7) 0.003(6) -0.075(6) O2W 0.134(7) 0.137(7) 0.123(7) -0.011(5) -0.019(5) -0.078(6) O3W 0.152(8) 0.128(7) 0.153(8) -0.004(6) -0.065(6) -0.075(6) O4W 0.081(5) 0.101(5) 0.090(5) -0.025(4) 0.017(4) -0.013(4) O5W 0.151(10) 0.52(3) 0.096(8) -0.005(12) 0.006(7) -0.096(14) O1S 0.32(2) 0.177(12) 0.269(17) 0.037(12) -0.094(15) -0.158(14) N1 0.053(3) 0.038(3) 0.056(4) -0.014(3) 0.004(3) -0.017(3) N2 0.045(3) 0.049(3) 0.053(3) -0.015(3) 0.010(3) -0.021(3) N3 0.057(4) 0.049(3) 0.042(3) -0.012(3) 0.002(3) -0.023(3) N4 0.046(3) 0.060(4) 0.051(4) -0.014(3) 0.001(3) -0.013(3) N5 0.067(5) 0.093(6) 0.056(5) -0.007(4) 0.004(4) 0.008(5) N6 0.080(5) 0.063(4) 0.052(4) -0.016(3) -0.003(3) -0.034(4) N8 0.081(5) 0.061(4) 0.054(4) 0.001(3) 0.009(3) -0.035(4) N7 0.066(4) 0.054(4) 0.063(4) -0.014(3) -0.012(3) -0.005(3) N1S 0.122(11) 0.185(15) 0.218(17) 0.055(13) -0.006(11) -0.056(11) C1 0.060(5) 0.054(4) 0.050(4) -0.015(3) 0.005(3) -0.024(4) C2 0.094(7) 0.059(5) 0.055(5) -0.015(4) 0.006(4) -0.032(5) C3 0.068(6) 0.048(5) 0.091(7) -0.014(4) 0.005(5) -0.008(4) C4 0.071(5) 0.059(5) 0.061(5) -0.020(4) -0.001(4) -0.005(4) C5 0.051(4) 0.042(4) 0.058(4) -0.009(3) 0.000(3) -0.010(3) C6 0.039(4) 0.056(4) 0.062(5) -0.021(4) 0.011(3) -0.011(3) C7 0.061(5) 0.050(4) 0.044(4) -0.007(3) 0.005(3) -0.022(4) C8 0.070(5) 0.057(5) 0.061(5) -0.001(4) -0.007(4) -0.033(4) C9 0.062(5) 0.051(4) 0.049(4) -0.013(4) -0.010(4) -0.010(4) C10 0.045(4) 0.067(5) 0.053(4) -0.016(4) 0.009(3) -0.026(4) C11 0.039(4) 0.068(5) 0.057(4) -0.021(4) 0.003(3) -0.021(4) C12 0.046(4) 0.046(4) 0.034(3) -0.007(3) 0.001(3) -0.019(3) C13 0.080(6) 0.060(5) 0.061(5) -0.008(4) -0.005(4) -0.032(5) C14 0.116(8) 0.071(6) 0.058(5) 0.008(4) -0.007(5) -0.048(6) C15 0.086(7) 0.060(5) 0.057(5) -0.002(4) -0.020(5) -0.014(5) C16 0.068(5) 0.070(5) 0.059(5) -0.009(4) -0.020(4) -0.020(5) C17 0.061(5) 0.055(4) 0.049(4) -0.021(4) 0.004(4) -0.018(4) C18 0.044(4) 0.071(5) 0.070(5) -0.011(4) -0.004(4) -0.016(4) C19 0.063(5) 0.065(5) 0.070(5) -0.026(4) 0.019(4) -0.005(4) C20 0.080(6) 0.078(6) 0.065(5) -0.036(5) 0.013(5) -0.018(5) C21 0.086(7) 0.042(4) 0.068(6) -0.005(4) -0.012(5) -0.012(4) C22 0.055(5) 0.067(5) 0.060(5) -0.013(4) 0.010(4) -0.018(4) C23 0.048(4) 0.054(4) 0.064(5) -0.012(4) 0.002(3) -0.019(3) C24 0.051(4) 0.060(5) 0.047(4) -0.015(4) 0.009(3) -0.018(4) C25 0.076(7) 0.176(13) 0.046(5) -0.003(6) 0.009(5) 0.035(8) C26 0.103(11) 0.171(19) 0.072(9) 0.036(11) 0.026(8) 0.045(12) C27 0.28(4) 0.091(13) 0.151(18) -0.020(11) 0.08(2) 0.065(16) C28 0.216(19) 0.066(8) 0.132(12) -0.036(8) 0.074(12) -0.003(10) C29 0.133(11) 0.073(7) 0.063(6) 0.002(5) 0.031(7) 0.001(7) C30 0.163(12) 0.068(6) 0.072(6) -0.027(5) 0.009(7) -0.044(7) C31 0.081(6) 0.089(7) 0.056(5) -0.012(5) -0.008(4) -0.038(5) C32 0.066(6) 0.083(6) 0.070(6) -0.001(5) -0.016(4) -0.019(5) C33 0.077(6) 0.084(7) 0.045(4) -0.013(4) 0.005(4) -0.026(5) C34 0.078(6) 0.083(6) 0.061(5) -0.021(4) 0.010(4) -0.045(5) C35 0.066(5) 0.061(5) 0.062(5) -0.014(4) 0.018(4) -0.027(4) C36 0.046(4) 0.046(4) 0.052(4) -0.009(3) 0.001(3) -0.018(3) C37 0.080(7) 0.095(7) 0.079(7) -0.023(6) -0.012(5) -0.017(6) C38 0.104(10) 0.146(13) 0.135(12) -0.035(10) -0.059(9) -0.019(9) C39 0.211(19) 0.098(10) 0.111(11) 0.002(8) -0.083(12) -0.036(11) C40 0.157(13) 0.104(9) 0.088(8) 0.004(7) -0.048(8) -0.045(9) C41 0.109(8) 0.057(5) 0.059(5) -0.003(4) -0.019(5) -0.021(5) C42 0.116(8) 0.064(6) 0.058(5) 0.008(4) 0.004(5) -0.041(6) C43 0.39(3) 0.27(2) 0.112(10) -0.120(13) 0.123(15) -0.29(2) C44 0.098(9) 0.084(8) 0.28(2) -0.119(11) 0.087(11) -0.047(7) C45 0.078(6) 0.051(5) 0.084(6) -0.011(5) -0.013(5) -0.023(5) C46 0.078(9) 0.239(19) 0.38(3) 0.22(2) -0.041(13) -0.084(11) C47 0.090(7) 0.057(5) 0.082(6) -0.009(5) 0.039(5) -0.023(5) C48 0.068(5) 0.054(4) 0.047(4) -0.015(3) 0.016(4) -0.031(4) C1S 0.076(9) 0.181(17) 0.114(11) 0.027(11) -0.007(7) -0.050(11) C2S 0.107(9) 0.110(10) 0.107(9) -0.005(8) 0.010(7) -0.038(8) C3S 0.21(2) 0.116(14) 0.25(2) 0.101(15) -0.008(18) -0.001(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 Cu1 O3 1.937(5) . ? Cu1 N1 1.969(6) . ? Cu1 O16 1.981(5) . ? Cu1 N2 2.048(5) . ? Cu1 O1 2.249(5) . ? Cu2 O7 1.952(5) . ? Cu2 N3 1.977(6) . ? Cu2 O4 1.989(5) . ? Cu2 N4 2.053(6) . ? Cu2 O5 2.226(5) . ? Cu3 O11 1.955(5) . ? Cu3 O8 1.982(5) . ? Cu3 N5 1.983(9) . ? Cu3 N6 2.049(6) . ? Cu3 O9 2.251(6) . ? Cu4 O15 1.934(5) . ? Cu4 N7 1.965(6) . ? Cu4 O12 2.012(5) . ? Cu4 N8 2.053(6) . ? Cu4 O13 2.219(6) . ? Cl1 O20 1.397(7) . ? Cl1 O17 1.405(8) . ? Cl1 O19 1.407(7) . ? Cl1 O18 1.419(7) . ? Cl2 O23 1.187(12) . ? Cl2 O21 1.276(10) . ? Cl2 O24 1.295(15) . ? Cl2 O22 1.339(10) . ? Cl3 O26 1.354(13) . ? Cl3 O28 1.394(9) . ? Cl3 O27 1.420(11) . ? Cl3 O25 1.472(18) . ? Cl4 O30 1.218(10) . ? Cl4 O31 1.272(11) . ? Cl4 O32 1.386(14) . ? Cl4 O29 1.433(10) . ? O1 C9 1.211(9) . ? O2 C9 1.321(9) . ? O3 C12 1.251(7) . ? O4 C12 1.263(8) . ? O5 C21 1.221(11) . ? O6 C21 1.300(10) . ? O7 C24 1.262(9) . ? O8 C24 1.246(9) . ? O9 C33 1.216(10) . ? O10 C33 1.300(11) . ? O11 C36 1.269(8) . ? O12 C36 1.243(8) . ? O13 C45 1.192(10) . ? O14 C45 1.302(12) . ? O15 C48 1.250(9) . ? O16 C48 1.284(9) . ? O1S C3S 1.88(3) . ? N1 C1 1.343(9) . ? N1 C5 1.352(9) . ? N2 C7 1.491(9) . ? N2 C6 1.491(9) . ? N2 C10 1.506(9) . ? N3 C17 1.346(9) . ? N3 C13 1.359(10) . ? N4 C19 1.470(9) . ? N4 C18 1.481(9) . ? N4 C22 1.491(10) . ? N5 C25 1.312(14) . ? N5 C29 1.314(16) . ? N6 C34 1.479(10) . ? N6 C31 1.503(10) . ? N6 C30 1.518(11) . ? N8 C43 1.388(16) . ? N8 C46 1.415(15) . ? N8 C42 1.473(10) . ? N7 C41 1.326(11) . ? N7 C37 1.332(12) . ? N1S C1S 1.10(2) . ? C1 C2 1.395(11) . ? C1 H1 0.9300 . ? C2 C3 1.380(12) . ? C2 H2 0.9300 . ? C3 C4 1.387(12) . ? C3 H3 0.9300 . ? C4 C5 1.364(10) . ? C4 H4 0.9300 . ? C5 C6 1.497(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.522(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.491(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.536(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.490(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.380(11) . ? C13 H13 0.9300 . ? C14 C15 1.404(13) . ? C14 H14 0.9300 . ? C15 C16 1.365(12) . ? C15 H15 0.9300 . ? C16 C17 1.341(10) . ? C16 H16 0.9300 . ? C17 C18 1.514(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.515(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.482(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C23 1.524(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.518(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C26 1.40(2) . ? C25 H25 0.9300 . ? C26 C27 1.29(3) . ? C26 H26 0.9300 . ? C27 C28 1.37(3) . ? C27 H27 0.9300 . ? C28 C29 1.361(16) . ? C28 H28 0.9300 . ? C29 C30 1.484(17) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.547(12) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.486(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C34 C35 1.523(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.498(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C37 C38 1.433(15) . ? C37 H37 0.9300 . ? C38 C39 1.36(2) . ? C38 H38 0.9300 . ? C39 C40 1.32(2) . ? C39 H39 0.9300 . ? C40 C41 1.406(14) . ? C40 H40 0.9300 . ? C41 C42 1.462(14) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.221(16) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.509(15) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C46 C47 1.323(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.495(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C1S C2S 1.32(2) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? 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 N1 170.4(2) . . ? O3 Cu1 O16 91.0(2) . . ? N1 Cu1 O16 92.6(2) . . ? O3 Cu1 N2 91.6(2) . . ? N1 Cu1 N2 83.4(2) . . ? O16 Cu1 N2 170.4(2) . . ? O3 Cu1 O1 94.1(2) . . ? N1 Cu1 O1 94.5(2) . . ? O16 Cu1 O1 94.6(2) . . ? N2 Cu1 O1 94.4(2) . . ? O7 Cu2 N3 171.3(2) . . ? O7 Cu2 O4 87.9(2) . . ? N3 Cu2 O4 94.0(2) . . ? O7 Cu2 N4 93.2(2) . . ? N3 Cu2 N4 83.8(2) . . ? O4 Cu2 N4 172.3(2) . . ? O7 Cu2 O5 91.1(2) . . ? N3 Cu2 O5 97.2(2) . . ? O4 Cu2 O5 93.6(2) . . ? N4 Cu2 O5 93.9(2) . . ? O11 Cu3 O8 90.2(2) . . ? O11 Cu3 N5 173.3(3) . . ? O8 Cu3 N5 92.8(3) . . ? O11 Cu3 N6 91.7(2) . . ? O8 Cu3 N6 169.2(2) . . ? N5 Cu3 N6 84.2(4) . . ? O11 Cu3 O9 91.6(2) . . ? O8 Cu3 O9 96.8(2) . . ? N5 Cu3 O9 94.0(3) . . ? N6 Cu3 O9 93.7(2) . . ? O15 Cu4 N7 175.1(3) . . ? O15 Cu4 O12 88.5(2) . . ? N7 Cu4 O12 94.1(3) . . ? O15 Cu4 N8 93.0(2) . . ? N7 Cu4 N8 83.5(3) . . ? O12 Cu4 N8 167.3(3) . . ? O15 Cu4 O13 88.8(3) . . ? N7 Cu4 O13 94.9(3) . . ? O12 Cu4 O13 98.5(2) . . ? N8 Cu4 O13 94.2(3) . . ? O20 Cl1 O17 110.0(6) . . ? O20 Cl1 O19 110.2(6) . . ? O17 Cl1 O19 108.2(5) . . ? O20 Cl1 O18 109.9(5) . . ? O17 Cl1 O18 109.4(6) . . ? O19 Cl1 O18 109.2(5) . . ? O23 Cl2 O21 116.3(11) . . ? O23 Cl2 O24 106.3(19) . . ? O21 Cl2 O24 104.9(16) . . ? O23 Cl2 O22 114.0(12) . . ? O21 Cl2 O22 112.5(9) . . ? O24 Cl2 O22 100.8(15) . . ? O26 Cl3 O28 115.9(12) . . ? O26 Cl3 O27 115.0(10) . . ? O28 Cl3 O27 114.4(9) . . ? O26 Cl3 O25 96.1(13) . . ? O28 Cl3 O25 115.1(12) . . ? O27 Cl3 O25 97.3(10) . . ? O30 Cl4 O31 116.0(12) . . ? O30 Cl4 O32 110.4(12) . . ? O31 Cl4 O32 105.3(9) . . ? O30 Cl4 O29 102.1(8) . . ? O31 Cl4 O29 116.2(10) . . ? O32 Cl4 O29 106.6(8) . . ? C9 O1 Cu1 115.0(5) . . ? C12 O3 Cu1 124.1(4) . . ? C12 O4 Cu2 109.3(4) . . ? C21 O5 Cu2 118.3(6) . . ? C24 O7 Cu2 121.5(5) . . ? C24 O8 Cu3 110.6(5) . . ? C33 O9 Cu3 116.6(6) . . ? C36 O11 Cu3 120.5(5) . . ? C36 O12 Cu4 106.8(4) . . ? C45 O13 Cu4 124.7(7) . . ? C48 O15 Cu4 125.8(5) . . ? C48 O16 Cu1 108.3(4) . . ? C1 N1 C5 119.0(6) . . ? C1 N1 Cu1 127.7(5) . . ? C5 N1 Cu1 113.3(5) . . ? C7 N2 C6 108.4(5) . . ? C7 N2 C10 111.0(5) . . ? C6 N2 C10 108.2(5) . . ? C7 N2 Cu1 109.8(4) . . ? C6 N2 Cu1 102.1(4) . . ? C10 N2 Cu1 116.7(4) . . ? C17 N3 C13 118.4(7) . . ? C17 N3 Cu2 114.9(5) . . ? C13 N3 Cu2 126.4(5) . . ? C19 N4 C18 108.4(6) . . ? C19 N4 C22 111.0(6) . . ? C18 N4 C22 110.5(6) . . ? C19 N4 Cu2 109.5(5) . . ? C18 N4 Cu2 103.2(4) . . ? C22 N4 Cu2 113.9(4) . . ? C25 N5 C29 118.3(12) . . ? C25 N5 Cu3 127.5(10) . . ? C29 N5 Cu3 114.2(8) . . ? C34 N6 C31 110.5(7) . . ? C34 N6 C30 110.1(7) . . ? C31 N6 C30 108.4(7) . . ? C34 N6 Cu3 115.2(5) . . ? C31 N6 Cu3 110.9(5) . . ? C30 N6 Cu3 101.2(6) . . ? C43 N8 C46 110.1(15) . . ? C43 N8 C42 110.7(11) . . ? C46 N8 C42 109.1(10) . . ? C43 N8 Cu4 112.1(7) . . ? C46 N8 Cu4 110.6(8) . . ? C42 N8 Cu4 104.1(5) . . ? C41 N7 C37 120.1(8) . . ? C41 N7 Cu4 113.7(6) . . ? C37 N7 Cu4 126.2(7) . . ? N1 C1 C2 121.7(7) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.0(8) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.4(8) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.2(9) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 121.6(7) . . ? N1 C5 C6 113.9(6) . . ? C4 C5 C6 124.4(7) . . ? N2 C6 C5 111.4(6) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 113.6(6) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 115.8(6) . . ? C9 C8 H8A 108.3 . . ? C7 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C7 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? O1 C9 O2 122.9(8) . . ? O1 C9 C8 124.5(7) . . ? O2 C9 C8 112.6(7) . . ? N2 C10 C11 112.8(6) . . ? N2 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C10 109.3(6) . . ? C12 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? O3 C12 O4 121.3(6) . . ? O3 C12 C11 121.0(6) . . ? O4 C12 C11 117.7(6) . . ? N3 C13 C14 121.5(8) . . ? N3 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 117.8(9) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C16 C15 C14 120.1(8) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 118.9(8) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 N3 123.4(8) . . ? C16 C17 C18 124.2(8) . . ? N3 C17 C18 112.3(6) . . ? N4 C18 C17 111.9(6) . . ? N4 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N4 C19 C20 117.2(7) . . ? N4 C19 H19A 108.0 . . ? C20 C19 H19A 108.0 . . ? N4 C19 H19B 108.0 . . ? C20 C19 H19B 108.0 . . ? H19A C19 H19B 107.2 . . ? C21 C20 C19 115.1(8) . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? O5 C21 O6 122.0(9) . . ? O5 C21 C20 123.3(8) . . ? O6 C21 C20 114.7(9) . . ? N4 C22 C23 114.3(6) . . ? N4 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N4 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 110.0(6) . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? C22 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O8 C24 O7 122.5(7) . . ? O8 C24 C23 117.9(7) . . ? O7 C24 C23 119.5(7) . . ? N5 C25 C26 120.0(16) . . ? N5 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 119(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 123(2) . . ? C26 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C29 C28 C27 114(2) . . ? C29 C28 H28 123.0 . . ? C27 C28 H28 123.0 . . ? N5 C29 C28 125.2(15) . . ? N5 C29 C30 114.2(10) . . ? C28 C29 C30 120.6(16) . . ? C29 C30 N6 112.3(9) . . ? C29 C30 H30A 109.1 . . ? N6 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? N6 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? N6 C31 C32 114.6(7) . . ? N6 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? N6 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 113.9(8) . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? O9 C33 O10 122.8(9) . . ? O9 C33 C32 124.9(9) . . ? O10 C33 C32 112.3(9) . . ? N6 C34 C35 113.4(7) . . ? N6 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? N6 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C34 110.0(7) . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? O12 C36 O11 119.8(7) . . ? O12 C36 C35 120.2(7) . . ? O11 C36 C35 119.9(7) . . ? N7 C37 C38 121.2(12) . . ? N7 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 116.8(13) . . ? C39 C38 H38 121.6 . . ? C37 C38 H38 121.6 . . ? C40 C39 C38 121.3(13) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 120.4(14) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? N7 C41 C40 120.0(11) . . ? N7 C41 C42 116.1(7) . . ? C40 C41 C42 123.8(10) . . ? C41 C42 N8 112.5(7) . . ? C41 C42 H42A 109.1 . . ? N8 C42 H42A 109.1 . . ? C41 C42 H42B 109.1 . . ? N8 C42 H42B 109.1 . . ? H42A C42 H42B 107.8 . . ? C44 C43 N8 138.8(11) . . ? C44 C43 H43A 102.4 . . ? N8 C43 H43A 102.4 . . ? C44 C43 H43B 102.4 . . ? N8 C43 H43B 102.4 . . ? H43A C43 H43B 104.9 . . ? C43 C44 C45 129.4(11) . . ? C43 C44 H44A 104.9 . . ? C45 C44 H44A 104.9 . . ? C43 C44 H44B 104.9 . . ? C45 C44 H44B 104.9 . . ? H44A C44 H44B 105.8 . . ? O13 C45 O14 120.4(9) . . ? O13 C45 C44 120.2(10) . . ? O14 C45 C44 119.3(9) . . ? C47 C46 N8 131.5(10) . . ? C47 C46 H46A 104.4 . . ? N8 C46 H46A 104.4 . . ? C47 C46 H46B 104.4 . . ? N8 C46 H46B 104.4 . . ? H46A C46 H46B 105.6 . . ? C46 C47 C48 119.4(10) . . ? C46 C47 H47A 107.5 . . ? C48 C47 H47A 107.5 . . ? C46 C47 H47B 107.5 . . ? C48 C47 H47B 107.5 . . ? H47A C47 H47B 107.0 . . ? O15 C48 O16 119.4(6) . . ? O15 C48 C47 121.4(8) . . ? O16 C48 C47 119.2(7) . . ? N1S C1S C2S 178(2) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.224 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.130 #===END