# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email reedijk@chem.leidenuniv.nl _publ_contact_author_name 'Prof. Dr. Jan Reedijk' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0440 _publ_contact_author_address ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden the Netherlands ; _publ_contact_author_phone -31-71-5274459 _publ_contact_author_fax -31-71-5274451 _publ_requested_coeditor_name ? _publ_contact_letter ; This CIf file is for submission for a paper in New Journal of Chemistry ; _publ_section_title ; A unique methoxo-fluoro-bridged triangular trinuclear Cu(II) species linked in a lattice via mononuclear Cu(II) units. Synthesis, X-ray structure and magnetism of [Cu4(2-aminopyrimidine)6(mu-3-OCH3)2(mu-F)3(F)2](BF4). ; _publ_section_exptl_prep ; A crystal was selected for the X--ray measurements and mounted to the glass fiber using the oil drop method (Kottke & Stalke, 1993) and data were collected at 193 K. ; _publ_section_exptl_refinement ; The intensity data were corrected for Lorentz and polarization effects and for absorption. The H atoms were introduced in calculated positions and refined with fixed geometry with respect to their carrier atoms. The disordered tetrafluoroborate anion was refined in two positions as rigid groups. ; _publ_section_references ; Kottke, T. and Stalke, D. (1993). J. Appl. Crystallogr. 26, 615--619. North, A.C.T, Phillips,D.C. and Mathews, F.S. (1968). Acta Crystallogr. A24, 351--359. Sheldrick, G. M. (1994). SHELXTL--PC. Realease 5.03 Siemens Analytical X--Ray Instruments Inc., Madison, WI 53719, USA. Sheldrick, G. M., SHELXL--97. Program for the Refinement of Crystal Structures. University of Gottingen, Germany. TEXSAN (1993). Single Crystal Structure Analysis Software, Version 1.6 Molecular Structure Corporation, The Woodlands, TX. 77381, USA. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'G.A.van Albada' ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden the Netherlands ; O.Roubeau ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden the Netherlands ; I.Mutikainen ; Laboratory of Inorganic Chemistry Department of Chemistry P.O. Box 55 (A. I. Virtasen aukio 1) FIN-00014 University of Helsinki Finland ; U.Turpeinen ; Laboratory of Inorganic Chemistry Department of Chemistry P.O. Box 55 (A. I. Virtasen aukio 1) FIN-00014 University of Helsinki Finland ; J.Reedijk ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden the Netherlands ; data_cuamp5 _database_code_CSD 209271 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H36 Cu4 F5 N18 O2, B F4' _chemical_formula_sum 'C26 H36 B Cu4 F9 N18 O2' _chemical_formula_weight 1068.70 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.899(6) _cell_length_b 21.435(8) _cell_length_c 16.727(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.64(4) _cell_angle_gamma 90.00 _cell_volume 4043(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 7.0 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'North etal. (1968). Acta Cryst. A24, 351-359' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku AFC-7S' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 7437 _diffrn_reflns_av_R_equivalents 0.1482 _diffrn_reflns_av_sigmaI/netI 0.2075 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.30 _reflns_number_total 3654 _reflns_number_gt 1623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku AFC-7S software' _computing_cell_refinement 'Rigaku AFC-7S software' _computing_data_reduction Texsan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC V. 5.03 (Sheldrick, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0528P)^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 3654 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1752 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.02844(8) 0.2500 0.0344(5) Uani 1 d S . . Cu2 Cu -0.12826(10) -0.08938(5) 0.22681(8) 0.0332(4) Uani 1 d . . . Cu3 Cu -0.2500 -0.2500 0.5000 0.0363(5) Uani 1 d S . . N11 N -0.0072(8) 0.0998(4) 0.1555(6) 0.047(2) Uani 1 d . . . C12 C -0.0989(9) 0.1355(5) 0.1167(7) 0.041(3) Uani 1 d . . . N13 N -0.0969(7) 0.1884(4) 0.0721(5) 0.039(2) Uani 1 d . . . C14 C 0.0101(10) 0.2055(5) 0.0706(7) 0.054(3) Uani 1 d . . . H14A H 0.0176 0.2426 0.0418 0.065 Uiso 1 calc R . . C15 C 0.1078(10) 0.1716(5) 0.1086(8) 0.056(3) Uani 1 d . . . H15A H 0.1826 0.1848 0.1057 0.067 Uiso 1 calc R . . C16 C 0.0999(10) 0.1190(5) 0.1510(7) 0.050(3) Uani 1 d . . . H16A H 0.1692 0.0952 0.1778 0.060 Uiso 1 calc R . . N17 N -0.2057(8) 0.1170(4) 0.1194(6) 0.063(3) Uani 1 d . . . H17A H -0.2119 0.0824 0.1461 0.076 Uiso 1 calc R . . H17B H -0.2692 0.1393 0.0944 0.076 Uiso 1 calc R . . N21 N -0.2501(7) -0.1121(4) 0.1158(5) 0.033(2) Uani 1 d . . . C22 C -0.2511(9) -0.1653(5) 0.0724(7) 0.036(3) Uani 1 d . . . N23 N -0.3328(8) -0.1777(4) -0.0027(5) 0.036(2) Uani 1 d . . . C24 C -0.4130(9) -0.1341(5) -0.0341(7) 0.042(3) Uani 1 d . . . H24A H -0.4715 -0.1420 -0.0870 0.051 Uiso 1 calc R . . C25 C -0.4176(9) -0.0779(5) 0.0049(7) 0.042(3) Uani 1 d . . . H25A H -0.4760 -0.0472 -0.0196 0.051 Uiso 1 calc R . . C26 C -0.3332(10) -0.0697(5) 0.0806(7) 0.045(3) Uani 1 d . . . H26A H -0.3331 -0.0318 0.1101 0.054 Uiso 1 calc R . . N27 N -0.1687(7) -0.2066(4) 0.1039(5) 0.041(2) Uani 1 d . . . H27A H -0.1675 -0.2414 0.0762 0.049 Uiso 1 calc R . . H27B H -0.1141 -0.1998 0.1529 0.049 Uiso 1 calc R . . N31 N -0.2891(7) -0.1735(4) 0.3953(5) 0.043(2) Uani 1 d . . . C32 C -0.2252(9) -0.1622(5) 0.3402(7) 0.040(3) Uani 1 d . . . N33 N -0.2310(7) -0.1104(4) 0.2970(5) 0.040(2) Uani 1 d . . . C34 C -0.3079(9) -0.0654(5) 0.3038(7) 0.046(3) Uani 1 d . . . H34A H -0.3121 -0.0273 0.2740 0.055 Uiso 1 calc R . . C35 C -0.3791(9) -0.0742(5) 0.3525(7) 0.050(3) Uani 1 d . . . H35A H -0.4352 -0.0438 0.3563 0.060 Uiso 1 calc R . . C36 C -0.3650(9) -0.1292(5) 0.3955(7) 0.048(3) Uani 1 d . . . H36A H -0.4151 -0.1361 0.4289 0.058 Uiso 1 calc R . . N37 N -0.1510(8) -0.2072(4) 0.3359(6) 0.052(3) Uani 1 d . . . H37A H -0.1054 -0.2025 0.3041 0.062 Uiso 1 calc R . . H37B H -0.1474 -0.2418 0.3650 0.062 Uiso 1 calc R . . O1 O -0.0070(6) -0.0607(3) 0.1773(4) 0.0345(16) Uani 1 d . . . C1 C -0.0151(10) -0.0589(5) 0.0918(7) 0.051(3) Uani 1 d . . . H1A H -0.0175 -0.1015 0.0702 0.076 Uiso 1 calc R . . H1B H 0.0541 -0.0371 0.0857 0.076 Uiso 1 calc R . . H1C H -0.0875 -0.0367 0.0597 0.076 Uiso 1 calc R . . F1 F -0.1662(4) 0.0171(2) 0.2205(3) 0.0369(14) Uani 1 d . . . F2 F 0.0000 -0.1804(3) 0.2500 0.0311(18) Uani 1 d S . . F3 F -0.1461(4) -0.2919(2) 0.4560(3) 0.0376(14) Uani 1 d . . . B1 B 0.4722(13) 0.0860(4) 0.2449(9) 0.13(3) Uani 0.50 d PG A -1 F11 F 0.466(2) 0.0553(9) 0.3145(9) 0.104(10) Uani 0.50 d PG A -1 F12 F 0.5583(12) 0.0597(14) 0.2183(16) 0.145(15) Uani 0.50 d PG A -1 F13 F 0.499(3) 0.1470(5) 0.2641(16) 0.203(14) Uani 0.50 d PG A -1 F14 F 0.3660(11) 0.0818(8) 0.1824(8) 0.081(5) Uani 0.50 d PG A -1 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 0.0356(11) 0.0234(10) 0.0526(12) 0.000 0.0260(9) 0.000 Cu2 0.0372(7) 0.0295(7) 0.0413(7) -0.0026(6) 0.0245(6) -0.0055(6) Cu3 0.0381(10) 0.0326(10) 0.0508(12) -0.0001(9) 0.0320(9) 0.0003(8) N11 0.043(5) 0.026(5) 0.084(7) 0.011(5) 0.039(5) 0.006(4) C12 0.045(7) 0.027(6) 0.054(7) -0.011(6) 0.018(6) 0.005(5) N13 0.039(5) 0.036(5) 0.052(6) -0.003(5) 0.030(5) -0.009(4) C14 0.058(8) 0.042(7) 0.071(9) 0.025(7) 0.033(7) 0.014(6) C15 0.051(8) 0.053(8) 0.074(9) 0.018(7) 0.035(7) 0.000(6) C16 0.048(7) 0.049(7) 0.064(8) 0.001(7) 0.033(7) 0.007(6) N17 0.047(6) 0.042(6) 0.107(9) 0.037(6) 0.034(6) 0.009(5) N21 0.034(5) 0.033(5) 0.039(5) 0.005(4) 0.021(4) 0.002(4) C22 0.042(7) 0.028(6) 0.046(7) -0.001(5) 0.027(6) -0.002(5) N23 0.048(6) 0.032(5) 0.032(5) -0.003(4) 0.015(4) 0.002(4) C24 0.043(7) 0.050(7) 0.041(6) 0.017(6) 0.021(5) 0.004(6) C25 0.051(7) 0.025(6) 0.055(7) 0.006(6) 0.022(6) 0.015(5) C26 0.058(8) 0.034(6) 0.053(8) -0.001(6) 0.033(7) 0.001(6) N27 0.044(5) 0.042(5) 0.034(5) -0.009(4) 0.008(4) 0.007(4) N31 0.046(6) 0.039(5) 0.058(6) 0.003(5) 0.036(5) 0.003(4) C32 0.043(7) 0.041(7) 0.048(7) 0.003(6) 0.030(6) 0.003(5) N33 0.035(5) 0.040(6) 0.055(6) -0.003(5) 0.029(5) 0.000(4) C34 0.042(7) 0.048(7) 0.054(7) 0.015(6) 0.024(6) 0.008(5) C35 0.049(7) 0.055(8) 0.058(7) 0.010(6) 0.035(6) 0.015(6) C36 0.038(7) 0.048(7) 0.074(9) 0.015(7) 0.041(6) 0.005(6) N37 0.069(7) 0.031(5) 0.081(7) 0.018(5) 0.059(6) 0.009(5) O1 0.034(4) 0.033(4) 0.041(4) 0.005(3) 0.018(3) -0.004(3) C1 0.054(8) 0.046(7) 0.057(8) 0.022(6) 0.025(6) 0.000(6) F1 0.037(3) 0.026(3) 0.054(4) -0.008(3) 0.024(3) -0.007(2) F2 0.039(5) 0.021(4) 0.046(5) 0.000 0.032(4) 0.000 F3 0.035(3) 0.038(3) 0.052(4) -0.003(3) 0.031(3) 0.004(3) B1 0.27(10) 0.06(3) 0.10(3) 0.03(5) 0.10(5) -0.02(5) F11 0.21(3) 0.029(10) 0.031(9) 0.020(8) -0.018(12) -0.021(13) F12 0.025(10) 0.17(3) 0.19(3) 0.10(2) -0.035(17) 0.003(13) F13 0.41(3) 0.064(12) 0.09(2) -0.019(16) 0.03(2) -0.08(3) F14 0.061(10) 0.119(15) 0.065(10) -0.005(11) 0.025(8) -0.003(10) _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 F1 1.894(5) . ? Cu1 F1 1.894(5) 2 ? Cu1 N11 2.181(9) . ? Cu1 N11 2.181(9) 2 ? Cu1 O1 2.252(7) 2 ? Cu1 O1 2.252(7) . ? Cu1 Cu2 2.912(2) . ? Cu1 Cu2 2.912(2) 2 ? Cu2 O1 1.972(7) 2 ? Cu2 O1 1.978(6) . ? Cu2 N33 1.999(8) . ? Cu2 N21 2.016(8) . ? Cu2 F1 2.322(5) . ? Cu2 Cu2 2.899(3) 2 ? Cu3 F3 1.860(5) 7_446 ? Cu3 F3 1.860(5) . ? Cu3 N13 2.262(9) 6_556 ? Cu3 N13 2.262(9) 4_445 ? Cu3 N31 2.335(8) . ? Cu3 N31 2.335(8) 7_446 ? N11 C12 1.322(13) . ? N11 C16 1.364(12) . ? C12 N17 1.346(12) . ? C12 N13 1.360(13) . ? N13 C14 1.333(12) . ? N13 Cu3 2.262(9) 4_455 ? C14 C15 1.345(14) . ? C14 H14A 0.9500 . ? C15 C16 1.352(14) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N17 H17A 0.8800 . ? N17 H17B 0.8800 . ? N21 C26 1.333(12) . ? N21 C22 1.349(12) . ? C22 N27 1.302(12) . ? C22 N23 1.347(12) . ? N23 C24 1.318(12) . ? C24 C25 1.379(14) . ? C24 H24A 0.9500 . ? C25 C26 1.353(14) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? N27 H27A 0.8800 . ? N27 H27B 0.8800 . ? N31 C36 1.312(12) . ? N31 C32 1.390(11) . ? C32 N33 1.315(12) . ? C32 N37 1.325(12) . ? N33 C34 1.358(12) . ? C34 C35 1.364(13) . ? C34 H34A 0.9500 . ? C35 C36 1.362(14) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N37 H37A 0.8800 . ? N37 H37B 0.8800 . ? O1 C1 1.403(11) . ? O1 Cu2 1.972(7) 2 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? B1 F11 1.3603 . ? B1 F14 1.3605 . ? B1 F13 1.3607 . ? B1 F12 1.3607 . ? 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 F1 Cu1 F1 165.2(3) . 2 ? F1 Cu1 N11 96.1(3) . . ? F1 Cu1 N11 94.3(3) 2 . ? F1 Cu1 N11 94.3(3) . 2 ? F1 Cu1 N11 96.1(3) 2 2 ? N11 Cu1 N11 91.0(5) . 2 ? F1 Cu1 O1 83.5(2) . 2 ? F1 Cu1 O1 84.0(2) 2 2 ? N11 Cu1 O1 166.5(3) . 2 ? N11 Cu1 O1 102.5(3) 2 2 ? F1 Cu1 O1 84.0(2) . . ? F1 Cu1 O1 83.5(2) 2 . ? N11 Cu1 O1 102.5(3) . . ? N11 Cu1 O1 166.5(3) 2 . ? O1 Cu1 O1 63.9(3) 2 . ? F1 Cu1 Cu2 52.76(16) . . ? F1 Cu1 Cu2 112.47(17) 2 . ? N11 Cu1 Cu2 127.9(3) . . ? N11 Cu1 Cu2 127.0(2) 2 . ? O1 Cu1 Cu2 42.56(17) 2 . ? O1 Cu1 Cu2 42.70(15) . . ? F1 Cu1 Cu2 112.47(17) . 2 ? F1 Cu1 Cu2 52.76(16) 2 2 ? N11 Cu1 Cu2 127.0(2) . 2 ? N11 Cu1 Cu2 127.9(3) 2 2 ? O1 Cu1 Cu2 42.70(15) 2 2 ? O1 Cu1 Cu2 42.56(17) . 2 ? Cu2 Cu1 Cu2 59.71(7) . 2 ? O1 Cu2 O1 74.3(3) 2 . ? O1 Cu2 N33 94.9(3) 2 . ? O1 Cu2 N33 169.0(3) . . ? O1 Cu2 N21 169.6(3) 2 . ? O1 Cu2 N21 95.5(3) . . ? N33 Cu2 N21 95.3(3) . . ? O1 Cu2 F1 80.0(2) 2 . ? O1 Cu2 F1 80.4(2) . . ? N33 Cu2 F1 95.8(3) . . ? N21 Cu2 F1 97.1(3) . . ? O1 Cu2 Cu2 42.86(17) 2 2 ? O1 Cu2 Cu2 42.71(19) . 2 ? N33 Cu2 Cu2 129.2(3) . 2 ? N21 Cu2 Cu2 129.2(2) . 2 ? F1 Cu2 Cu2 100.65(12) . 2 ? O1 Cu2 Cu1 50.55(18) 2 . ? O1 Cu2 Cu1 50.54(18) . . ? N33 Cu2 Cu1 120.7(2) . . ? N21 Cu2 Cu1 121.6(2) . . ? F1 Cu2 Cu1 40.50(12) . . ? Cu2 Cu2 Cu1 60.14(3) 2 . ? F3 Cu3 F3 180.0 7_446 . ? F3 Cu3 N13 91.8(3) 7_446 6_556 ? F3 Cu3 N13 88.2(3) . 6_556 ? F3 Cu3 N13 88.2(3) 7_446 4_445 ? F3 Cu3 N13 91.8(3) . 4_445 ? N13 Cu3 N13 180.0 6_556 4_445 ? F3 Cu3 N31 87.7(2) 7_446 . ? F3 Cu3 N31 92.3(2) . . ? N13 Cu3 N31 85.6(3) 6_556 . ? N13 Cu3 N31 94.4(3) 4_445 . ? F3 Cu3 N31 92.3(2) 7_446 7_446 ? F3 Cu3 N31 87.7(2) . 7_446 ? N13 Cu3 N31 94.4(3) 6_556 7_446 ? N13 Cu3 N31 85.6(3) 4_445 7_446 ? N31 Cu3 N31 180.000(1) . 7_446 ? C12 N11 C16 115.9(9) . . ? C12 N11 Cu1 126.7(7) . . ? C16 N11 Cu1 115.5(7) . . ? N11 C12 N17 116.8(10) . . ? N11 C12 N13 126.6(10) . . ? N17 C12 N13 116.6(10) . . ? C14 N13 C12 115.1(9) . . ? C14 N13 Cu3 116.1(7) . 4_455 ? C12 N13 Cu3 128.8(7) . 4_455 ? N13 C14 C15 121.9(10) . . ? N13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C14 C15 C16 120.3(11) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 N11 120.2(11) . . ? C15 C16 H16A 119.9 . . ? N11 C16 H16A 119.9 . . ? C12 N17 H17A 120.0 . . ? C12 N17 H17B 120.0 . . ? H17A N17 H17B 120.0 . . ? C26 N21 C22 117.4(9) . . ? C26 N21 Cu2 117.1(7) . . ? C22 N21 Cu2 125.4(7) . . ? N27 C22 N23 118.0(9) . . ? N27 C22 N21 118.8(10) . . ? N23 C22 N21 123.2(10) . . ? C24 N23 C22 116.5(9) . . ? N23 C24 C25 124.3(11) . . ? N23 C24 H24A 117.9 . . ? C25 C24 H24A 117.9 . . ? C26 C25 C24 115.2(10) . . ? C26 C25 H25A 122.4 . . ? C24 C25 H25A 122.4 . . ? N21 C26 C25 123.3(10) . . ? N21 C26 H26A 118.4 . . ? C25 C26 H26A 118.4 . . ? C22 N27 H27A 120.0 . . ? C22 N27 H27B 120.0 . . ? H27A N27 H27B 120.0 . . ? C36 N31 C32 113.5(9) . . ? C36 N31 Cu3 118.6(7) . . ? C32 N31 Cu3 126.8(7) . . ? N33 C32 N37 120.3(9) . . ? N33 C32 N31 124.6(9) . . ? N37 C32 N31 115.1(9) . . ? C32 N33 C34 118.2(8) . . ? C32 N33 Cu2 125.4(7) . . ? C34 N33 Cu2 116.3(7) . . ? N33 C34 C35 121.0(10) . . ? N33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C36 C35 C34 116.1(10) . . ? C36 C35 H35A 121.9 . . ? C34 C35 H35A 121.9 . . ? N31 C36 C35 126.4(9) . . ? N31 C36 H36A 116.8 . . ? C35 C36 H36A 116.8 . . ? C32 N37 H37A 120.0 . . ? C32 N37 H37B 120.0 . . ? H37A N37 H37B 120.0 . . ? C1 O1 Cu2 127.6(6) . 2 ? C1 O1 Cu2 127.9(6) . . ? Cu2 O1 Cu2 94.4(3) 2 . ? C1 O1 Cu1 120.4(6) . . ? Cu2 O1 Cu1 86.9(2) 2 . ? Cu2 O1 Cu1 86.8(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Cu1 F1 Cu2 86.7(2) . . ? F11 B1 F14 109.5 . . ? F11 B1 F13 109.5 . . ? F14 B1 F13 109.5 . . ? F11 B1 F12 109.5 . . ? F14 B1 F12 109.5 . . ? F13 B1 F12 109.5 . . ? _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.866 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.130