# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email M.A.Halcrow@leeds.ac.uk _publ_contact_author_name 'Malcolm A.Halcrow' loop_ _publ_author_name 'Rebecca Docherty' 'Floriana Tuna' 'Colin Kilner' 'Eric McInnes' 'Malcolm A.Halcrow' data_mh400rt _database_code_depnum_ccdc_archive 'CCDC 866481' #TrackingRef '- MCu Chem Comm..CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)copper(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Cu N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Cu F8 N6' _chemical_formula_weight 703.70 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' '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' F F 0.0171 0.0103 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 'C 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' _cell_length_a 12.7056(10) _cell_length_b 12.6356(11) _cell_length_c 19.7176(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.378(4) _cell_angle_gamma 90.00 _cell_volume 3151.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 23962 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 28.04 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 1.114 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23962 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.04 _reflns_number_total 6565 _reflns_number_gt 5356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'local program' _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. The crystal used was a racemic twin. Both BF~4~^-^ ions are disordered. Anion B38--F42 was modelled over two equally occupied sites labelled 'A' and 'B', sharing a common wholly occupied B atom B38. Anion B43--F47 was refined over three equally occupied orientations 'A', 'B' and 'C', with orientations A and B sharing the same B atom B43A which therefore has occupancy 0.67. The refined restraints B---F = 1.39(2) and F...F = 2.27(2)\%A were applied to these groups. All wholly occupied non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. There are two residual Fourier peaks of +1.3-1.4 e.\%A^-3^, both of them 1.0\%A from Cu1. ; _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^)+(0.1036P)^2^+7.2514P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(2) _refine_ls_number_reflns 6565 _refine_ls_number_parameters 433 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.106 _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 0.74928(6) 0.72972(5) 0.74991(4) 0.0492(2) Uani 1 1 d . . . N2 N 0.7443(5) 0.7348(4) 0.6452(2) 0.0386(13) Uani 1 1 d . . . C3 C 0.6524(5) 0.7045(5) 0.6090(3) 0.0518(14) Uani 1 1 d . . . C4 C 0.6459(7) 0.7069(7) 0.5378(4) 0.0713(19) Uani 1 1 d . . . H4 H 0.5859 0.6834 0.5113 0.086 Uiso 1 1 calc R . . C5 C 0.7360(11) 0.7474(8) 0.5075(5) 0.081(3) Uani 1 1 d . . . H5 H 0.7328 0.7536 0.4603 0.098 Uiso 1 1 calc R . . C6 C 0.8238(8) 0.7762(7) 0.5446(5) 0.078(3) Uani 1 1 d . . . H6 H 0.8827 0.7984 0.5237 0.094 Uiso 1 1 calc R . . C7 C 0.8265(6) 0.7727(5) 0.6162(3) 0.0521(14) Uani 1 1 d . . . C8 C 0.5639(5) 0.6666(5) 0.6504(3) 0.0507(13) Uani 1 1 d . . . N9 N 0.5892(4) 0.6653(4) 0.7182(3) 0.0495(11) Uani 1 1 d . . . C10 C 0.5155(6) 0.6313(5) 0.7600(4) 0.0581(16) Uani 1 1 d . . . H10 H 0.5331 0.6299 0.8069 0.070 Uiso 1 1 calc R . . C11 C 0.4142(6) 0.5985(6) 0.7337(5) 0.067(2) Uani 1 1 d . . . H11 H 0.3652 0.5750 0.7625 0.080 Uiso 1 1 calc R . . C12 C 0.3897(7) 0.6020(6) 0.6657(5) 0.068(2) Uani 1 1 d . . . H12 H 0.3223 0.5823 0.6475 0.082 Uiso 1 1 calc R . . C13 C 0.4660(6) 0.6356(6) 0.6209(5) 0.0706(19) Uani 1 1 d . . . H13 H 0.4500 0.6364 0.5739 0.085 Uiso 1 1 calc R . . C14 C 0.9195(5) 0.8028(5) 0.6645(4) 0.0527(15) Uani 1 1 d . . . N15 N 0.9061(4) 0.7981(4) 0.7315(3) 0.0529(12) Uani 1 1 d . . . C16 C 0.9853(6) 0.8298(6) 0.7779(4) 0.0648(18) Uani 1 1 d . . . H16 H 0.9744 0.8286 0.8239 0.078 Uiso 1 1 calc R . . C17 C 1.0832(7) 0.8643(7) 0.7588(6) 0.076(3) Uani 1 1 d . . . H17 H 1.1371 0.8865 0.7908 0.092 Uiso 1 1 calc R . . C18 C 1.0956(7) 0.8636(8) 0.6891(6) 0.080(3) Uani 1 1 d . . . H18 H 1.1606 0.8830 0.6748 0.096 Uiso 1 1 calc R . . C19 C 1.0163(6) 0.8356(7) 0.6417(5) 0.074(2) Uani 1 1 d . . . H19 H 1.0254 0.8380 0.5955 0.089 Uiso 1 1 calc R . . N20 N 0.7556(5) 0.7224(4) 0.8501(4) 0.058(2) Uani 1 1 d . . . C21 C 0.7205(5) 0.8057(6) 0.8894(4) 0.0527(14) Uani 1 1 d . . . C22 C 0.7200(7) 0.8026(6) 0.9595(4) 0.0609(17) Uani 1 1 d . . . H22 H 0.6955 0.8597 0.9834 0.073 Uiso 1 1 calc R . . C23 C 0.7583(9) 0.7092(7) 0.9938(4) 0.070(2) Uani 1 1 d . . . H23 H 0.7616 0.7054 1.0411 0.084 Uiso 1 1 calc R . . C24 C 0.7911(7) 0.6228(6) 0.9562(3) 0.0636(18) Uani 1 1 d . . . H24 H 0.8143 0.5608 0.9782 0.076 Uiso 1 1 calc R . . C25 C 0.7886(5) 0.6311(5) 0.8857(3) 0.0522(14) Uani 1 1 d . . . C26 C 0.6878(5) 0.8994(5) 0.8446(3) 0.0495(13) Uani 1 1 d . . . N27 N 0.6886(4) 0.8858(4) 0.7780(3) 0.0510(12) Uani 1 1 d . . . C28 C 0.6541(6) 0.9671(6) 0.7343(4) 0.0605(16) Uani 1 1 d . . . H28 H 0.6515 0.9559 0.6876 0.073 Uiso 1 1 calc R . . C29 C 0.6228(6) 1.0662(6) 0.7583(5) 0.069(2) Uani 1 1 d . . . H29 H 0.6017 1.1212 0.7288 0.082 Uiso 1 1 calc R . . C30 C 0.6254(7) 1.0769(6) 0.8287(5) 0.075(2) Uani 1 1 d . . . H30 H 0.6060 1.1415 0.8464 0.090 Uiso 1 1 calc R . . C31 C 0.6556(7) 0.9958(6) 0.8736(4) 0.071(2) Uani 1 1 d . . . H31 H 0.6549 1.0039 0.9204 0.085 Uiso 1 1 calc R . . C32 C 0.8235(5) 0.5463(5) 0.8397(3) 0.0462(12) Uani 1 1 d . . . N33 N 0.8192(4) 0.5711(4) 0.7733(3) 0.0522(12) Uani 1 1 d . . . C34 C 0.8537(6) 0.4985(5) 0.7279(4) 0.0573(15) Uani 1 1 d . . . H34 H 0.8518 0.5168 0.6821 0.069 Uiso 1 1 calc R . . C35 C 0.8911(7) 0.3990(6) 0.7485(5) 0.073(2) Uani 1 1 d . . . H35 H 0.9146 0.3508 0.7176 0.088 Uiso 1 1 calc R . . C36 C 0.8916(8) 0.3753(7) 0.8171(5) 0.076(3) Uani 1 1 d . . . H36 H 0.9141 0.3084 0.8320 0.092 Uiso 1 1 calc R . . C37 C 0.8605(6) 0.4460(6) 0.8639(4) 0.0654(18) Uani 1 1 d . . . H37 H 0.8635 0.4289 0.9100 0.078 Uiso 1 1 calc R . . B38 B 0.9953(9) 1.0183(8) 0.9398(5) 0.106(5) Uani 1 1 d D . . F39A F 1.0166(16) 1.0447(15) 1.0035(7) 0.131(7) Uiso 0.50 1 d PD A 1 F40A F 0.9242(11) 1.0899(11) 0.9032(7) 0.109(4) Uiso 0.50 1 d PD A 1 F41A F 1.0819(8) 1.0033(10) 0.9016(5) 0.082(3) Uiso 0.50 1 d PD A 1 F42A F 0.9418(10) 0.9178(9) 0.9374(6) 0.104(4) Uiso 0.50 1 d PD A 1 F39B F 1.0565(13) 1.0288(12) 1.0085(5) 0.105(4) Uiso 0.50 1 d PD A 2 F40B F 0.9764(12) 1.1241(10) 0.9235(7) 0.121(4) Uiso 0.50 1 d PD A 2 F41B F 1.0647(12) 0.9652(12) 0.9044(7) 0.113(5) Uiso 0.50 1 d PD A 2 F42B F 0.9086(14) 0.9645(17) 0.9544(12) 0.208(12) Uiso 0.50 1 d PD A 2 B43A B 1.0283(10) 0.4976(11) 1.0603(7) 0.092(6) Uiso 0.67 1 d PD . . F44A F 1.0072(14) 0.4746(17) 0.9941(6) 0.092(5) Uiso 0.34 1 d PD B 1 F45A F 0.9870(17) 0.5857(14) 1.0860(11) 0.105(8) Uiso 0.34 1 d PD B 1 F46A F 1.1434(9) 0.5065(13) 1.0672(7) 0.071(3) Uiso 0.34 1 d PD B 1 F47A F 1.0060(19) 0.4118(16) 1.1048(10) 0.140(8) Uiso 0.34 1 d PD B 1 F44B F 1.0281(13) 0.5481(13) 0.9938(6) 0.087(4) Uiso 0.33 1 d PD B 2 F45B F 0.9431(13) 0.4276(14) 1.0519(10) 0.117(6) Uiso 0.33 1 d PD B 2 F46B F 1.1241(12) 0.4547(16) 1.0793(8) 0.094(5) Uiso 0.33 1 d PD B 2 F47B F 1.0021(15) 0.5763(13) 1.1049(9) 0.088(6) Uiso 0.33 1 d PD B 2 B43C B 1.0307(16) 0.4659(18) 1.0601(10) 0.066(7) Uiso 0.33 1 d PD B 3 F44C F 0.951(2) 0.505(2) 1.0964(13) 0.177(12) Uiso 0.33 1 d PD B 3 F45C F 0.9867(13) 0.4116(14) 1.0038(7) 0.088(4) Uiso 0.33 1 d PD B 3 F46C F 1.092(2) 0.394(2) 1.1004(12) 0.151(9) Uiso 0.33 1 d PD B 3 F47C F 1.095(3) 0.547(2) 1.0416(17) 0.221(18) Uiso 0.33 1 d PD B 3 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 0.0426(3) 0.0424(3) 0.0631(4) -0.0022(4) 0.0081(3) -0.0013(4) N2 0.049(3) 0.043(3) 0.024(2) 0.0011(17) 0.001(2) -0.005(2) C3 0.052(4) 0.045(3) 0.058(3) -0.002(2) 0.005(3) 0.003(3) C4 0.070(5) 0.079(5) 0.064(4) -0.003(4) 0.001(4) -0.003(4) C5 0.096(8) 0.090(6) 0.060(5) 0.003(4) 0.017(5) 0.005(5) C6 0.075(6) 0.085(6) 0.078(5) 0.014(4) 0.029(5) 0.021(4) C7 0.056(4) 0.051(3) 0.051(3) 0.004(3) 0.014(3) 0.009(3) C8 0.053(4) 0.042(3) 0.057(3) -0.006(2) 0.004(3) 0.002(3) N9 0.047(3) 0.042(2) 0.059(3) -0.004(2) 0.003(2) 0.002(2) C10 0.057(4) 0.052(3) 0.065(4) 0.004(3) 0.004(3) 0.002(3) C11 0.050(4) 0.051(4) 0.101(6) 0.002(4) 0.017(4) -0.007(3) C12 0.051(4) 0.051(4) 0.103(6) -0.009(4) 0.007(4) -0.018(3) C13 0.057(4) 0.064(4) 0.088(5) -0.004(4) -0.007(4) -0.002(3) C14 0.044(3) 0.034(2) 0.082(4) 0.004(3) 0.016(3) -0.001(2) N15 0.045(3) 0.040(2) 0.074(3) -0.002(2) 0.011(3) 0.004(2) C16 0.068(5) 0.051(4) 0.074(4) -0.006(3) -0.001(4) 0.003(3) C17 0.048(4) 0.056(5) 0.123(7) -0.018(4) -0.002(4) -0.008(3) C18 0.044(4) 0.068(5) 0.131(8) -0.007(5) 0.025(5) -0.019(4) C19 0.056(5) 0.078(5) 0.090(5) 0.007(4) 0.026(4) -0.008(4) N20 0.026(3) 0.024(3) 0.124(6) -0.009(3) 0.009(3) -0.0045(18) C21 0.044(4) 0.052(3) 0.063(4) 0.001(3) 0.008(3) -0.004(3) C22 0.067(5) 0.059(4) 0.059(4) -0.009(3) 0.016(3) -0.006(4) C23 0.104(7) 0.064(5) 0.043(4) 0.006(3) 0.012(4) 0.006(4) C24 0.074(5) 0.059(4) 0.057(4) 0.007(3) -0.001(3) -0.002(3) C25 0.043(3) 0.042(3) 0.071(4) -0.001(3) 0.003(3) -0.006(2) C26 0.042(3) 0.050(3) 0.056(3) -0.004(2) 0.004(2) 0.005(3) N27 0.046(3) 0.047(3) 0.061(3) -0.004(2) 0.007(2) -0.003(2) C28 0.055(4) 0.056(4) 0.069(4) 0.011(3) -0.001(3) -0.009(3) C29 0.054(4) 0.046(4) 0.103(6) 0.006(4) -0.006(4) 0.009(3) C30 0.077(6) 0.033(3) 0.112(7) -0.012(4) -0.003(5) 0.017(3) C31 0.083(6) 0.058(4) 0.073(4) -0.017(3) 0.013(4) 0.013(4) C32 0.037(3) 0.043(3) 0.058(3) 0.000(2) 0.001(2) -0.003(2) N33 0.042(3) 0.049(3) 0.065(3) -0.001(2) 0.006(2) 0.000(2) C34 0.048(4) 0.059(4) 0.065(4) -0.001(3) 0.009(3) -0.002(3) C35 0.062(5) 0.044(4) 0.115(7) -0.012(4) 0.018(4) 0.000(3) C36 0.075(6) 0.047(4) 0.105(7) -0.004(4) -0.005(5) 0.010(4) C37 0.059(4) 0.056(4) 0.080(5) 0.011(3) -0.001(3) 0.005(3) B38 0.170(14) 0.084(7) 0.072(6) 0.002(5) 0.054(8) -0.029(9) _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 N20 1.971(9) . ? Cu1 N2 2.061(5) . ? Cu1 N27 2.207(5) . ? Cu1 N33 2.224(5) . ? Cu1 N9 2.225(6) . ? Cu1 N15 2.232(6) . ? N2 C7 1.327(9) . ? N2 C3 1.365(9) . ? C3 C4 1.399(10) . ? C3 C8 1.526(9) . ? C4 C5 1.435(15) . ? C5 C6 1.326(16) . ? C6 C7 1.409(11) . ? C7 C14 1.495(11) . ? C8 N9 1.345(8) . ? C8 C13 1.380(10) . ? N9 C10 1.374(9) . ? C10 C11 1.404(11) . ? C11 C12 1.349(13) . ? C12 C13 1.435(12) . ? C14 N15 1.350(9) . ? C14 C19 1.410(9) . ? N15 C16 1.356(10) . ? C16 C17 1.402(12) . ? C17 C18 1.398(14) . ? C18 C19 1.356(14) . ? N20 C25 1.395(9) . ? N20 C21 1.404(9) . ? C21 C22 1.384(10) . ? C21 C26 1.511(10) . ? C22 C23 1.424(12) . ? C23 C24 1.405(11) . ? C24 C25 1.391(10) . ? C25 C32 1.498(9) . ? C26 N27 1.326(8) . ? C26 C31 1.422(9) . ? N27 C28 1.385(9) . ? C28 C29 1.408(11) . ? C29 C30 1.393(13) . ? C30 C31 1.385(12) . ? C32 N33 1.343(8) . ? C32 C37 1.419(9) . ? N33 C34 1.380(8) . ? C34 C35 1.391(11) . ? C35 C36 1.385(14) . ? C36 C37 1.370(12) . ? B38 F39A 1.302(13) . ? B38 F41A 1.404(13) . ? B38 F40A 1.426(13) . ? B38 F42A 1.439(13) . ? B38 F42B 1.349(14) . ? B38 F41B 1.353(13) . ? B38 F40B 1.391(13) . ? B38 F39B 1.503(14) . ? B43A F44A 1.341(14) . ? B43A F45A 1.350(15) . ? B43A F47A 1.440(15) . ? B43A F46A 1.460(15) . ? B43A F46B 1.354(15) . ? B43A F47B 1.388(15) . ? B43A F45B 1.396(15) . ? B43A F44B 1.459(15) . ? B43C F45C 1.378(17) . ? B43C F44C 1.383(17) . ? B43C F47C 1.383(18) . ? B43C F46C 1.398(18) . ? 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 N20 Cu1 N2 178.9(2) . . ? N20 Cu1 N27 76.9(2) . . ? N2 Cu1 N27 104.2(2) . . ? N20 Cu1 N33 76.8(2) . . ? N2 Cu1 N33 102.1(2) . . ? N27 Cu1 N33 153.6(2) . . ? N20 Cu1 N9 102.4(2) . . ? N2 Cu1 N9 77.8(2) . . ? N27 Cu1 N9 93.77(19) . . ? N33 Cu1 N9 93.77(19) . . ? N20 Cu1 N15 103.2(2) . . ? N2 Cu1 N15 76.7(2) . . ? N27 Cu1 N15 91.89(19) . . ? N33 Cu1 N15 92.1(2) . . ? N9 Cu1 N15 154.4(2) . . ? C7 N2 C3 123.1(6) . . ? C7 N2 Cu1 119.5(5) . . ? C3 N2 Cu1 117.3(4) . . ? N2 C3 C4 119.0(6) . . ? N2 C3 C8 116.4(5) . . ? C4 C3 C8 124.5(6) . . ? C3 C4 C5 116.8(8) . . ? C6 C5 C4 122.1(9) . . ? C5 C6 C7 119.0(9) . . ? N2 C7 C6 119.8(8) . . ? N2 C7 C14 115.1(6) . . ? C6 C7 C14 125.0(7) . . ? N9 C8 C13 122.4(6) . . ? N9 C8 C3 114.6(6) . . ? C13 C8 C3 123.0(6) . . ? C8 N9 C10 119.2(6) . . ? C8 N9 Cu1 113.7(4) . . ? C10 N9 Cu1 127.0(4) . . ? N9 C10 C11 121.6(6) . . ? C12 C11 C10 118.4(7) . . ? C11 C12 C13 121.0(8) . . ? C8 C13 C12 117.4(8) . . ? N15 C14 C19 121.2(7) . . ? N15 C14 C7 116.6(5) . . ? C19 C14 C7 122.1(7) . . ? C14 N15 C16 119.6(6) . . ? C14 N15 Cu1 111.9(4) . . ? C16 N15 Cu1 128.5(5) . . ? N15 C16 C17 122.2(8) . . ? C18 C17 C16 116.5(8) . . ? C19 C18 C17 122.3(7) . . ? C18 C19 C14 118.2(8) . . ? C25 N20 C21 115.9(8) . . ? C25 N20 Cu1 121.7(5) . . ? C21 N20 Cu1 122.2(5) . . ? C22 C21 N20 124.2(7) . . ? C22 C21 C26 125.4(6) . . ? N20 C21 C26 110.4(6) . . ? C21 C22 C23 117.7(7) . . ? C24 C23 C22 119.9(7) . . ? C25 C24 C23 119.3(7) . . ? C24 C25 N20 123.0(6) . . ? C24 C25 C32 124.8(6) . . ? N20 C25 C32 112.2(6) . . ? N27 C26 C31 122.5(6) . . ? N27 C26 C21 116.8(5) . . ? C31 C26 C21 120.7(6) . . ? C26 N27 C28 119.2(6) . . ? C26 N27 Cu1 113.5(4) . . ? C28 N27 Cu1 127.3(5) . . ? N27 C28 C29 122.3(7) . . ? C30 C29 C28 116.1(7) . . ? C31 C30 C29 122.9(6) . . ? C30 C31 C26 116.8(7) . . ? N33 C32 C37 121.2(6) . . ? N33 C32 C25 115.9(5) . . ? C37 C32 C25 122.9(6) . . ? C32 N33 C34 119.4(5) . . ? C32 N33 Cu1 113.0(4) . . ? C34 N33 Cu1 127.5(4) . . ? N33 C34 C35 122.2(7) . . ? C36 C35 C34 116.8(7) . . ? C37 C36 C35 122.8(8) . . ? C36 C37 C32 117.6(8) . . ? F39A B38 F41A 116.7(12) . . ? F39A B38 F40A 113.0(12) . . ? F41A B38 F40A 107.7(9) . . ? F39A B38 F42A 108.2(11) . . ? F41A B38 F42A 104.7(9) . . ? F40A B38 F42A 105.6(11) . . ? F42B B38 F41B 116.4(13) . . ? F42B B38 F40B 114.1(13) . . ? F41B B38 F40B 117.6(10) . . ? F42B B38 F39B 102.5(11) . . ? F41B B38 F39B 101.6(11) . . ? F40B B38 F39B 100.8(10) . . ? F44A B43A F45A 119.8(14) . . ? F44A B43A F47A 113.4(14) . . ? F45A B43A F47A 106.6(13) . . ? F44A B43A F46A 102.4(11) . . ? F45A B43A F46A 108.9(13) . . ? F47A B43A F46A 104.7(12) . . ? F46B B43A F47B 112.0(12) . . ? F46B B43A F45B 116.5(14) . . ? F47B B43A F45B 107.5(13) . . ? F46B B43A F44B 110.4(12) . . ? F47B B43A F44B 106.0(13) . . ? F45B B43A F44B 103.5(12) . . ? F45C B43C F44C 109.4(16) . . ? F45C B43C F47C 111.3(16) . . ? F44C B43C F47C 110.5(17) . . ? F45C B43C F46C 107.3(16) . . ? F44C B43C F46C 109.4(16) . . ? F47C B43C F46C 108.9(16) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.415 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.099 #=END data_mh400lt _database_code_depnum_ccdc_archive 'CCDC 866482' #TrackingRef '- MCu Chem Comm..CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2,2':6',2''-terpyridine)copper(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Cu N6, 2[B F4]' _chemical_formula_sum 'C30 H22 B2 Cu F8 N6' _chemical_formula_weight 703.70 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' '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' F F 0.0171 0.0103 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 'C 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' _cell_length_a 12.6690(10) _cell_length_b 12.5211(10) _cell_length_c 19.4354(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.776(4) _cell_angle_gamma 90.00 _cell_volume 3067.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33789 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 28.21 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33789 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.21 _reflns_number_total 7025 _reflns_number_gt 6372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'local program' _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. The crystal used was a racemic twin. Anion B43--F47 was disordered over two sites labelled 'A' and 'B', with a refined occupancy ration of 0.57:0.43. The refined restraints B---F = 1.40(2) and F...F = 2.29(2)\%A were applied to these groups. All wholly occupied non-H atoms were refined anisotropically, while H atoms were placed in calculated positions and refined using a riding model. There are two residual Fourier peaks of +2.2-2.4 e.\%A^-3^, both of them 1.0\%A from Cu1. ; _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^)+(0.1270P)^2^+8.1077P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.207(18) _refine_ls_number_reflns 7025 _refine_ls_number_parameters 422 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1970 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _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 Cu1 Cu 0.75001(4) 0.72170(4) 0.75001(3) 0.03204(17) Uani 1 1 d . . . N2 N 0.7417(4) 0.7298(3) 0.6428(2) 0.0264(9) Uani 1 1 d . . . C3 C 0.6490(4) 0.7012(4) 0.6067(3) 0.0334(10) Uani 1 1 d . . . C4 C 0.6399(5) 0.7101(5) 0.5345(3) 0.0420(12) Uani 1 1 d . . . H4 H 0.5762 0.6897 0.5077 0.050 Uiso 1 1 calc R . . C5 C 0.7285(5) 0.7509(6) 0.5016(3) 0.0433(12) Uani 1 1 d . . . H5 H 0.7237 0.7581 0.4528 0.052 Uiso 1 1 calc R . . C6 C 0.8211(6) 0.7795(5) 0.5417(4) 0.0431(15) Uani 1 1 d . . . H6 H 0.8800 0.8065 0.5205 0.052 Uiso 1 1 calc R . . C7 C 0.8264(5) 0.7680(4) 0.6140(3) 0.0317(10) Uani 1 1 d . . . C8 C 0.5632(5) 0.6630(4) 0.6474(3) 0.0344(10) Uani 1 1 d . . . N9 N 0.5904(4) 0.6583(3) 0.7172(2) 0.0334(9) Uani 1 1 d . . . C10 C 0.5171(5) 0.6217(4) 0.7588(3) 0.0367(11) Uani 1 1 d . . . H10 H 0.5364 0.6170 0.8072 0.044 Uiso 1 1 calc R . . C11 C 0.4140(5) 0.5908(5) 0.7322(3) 0.0422(13) Uani 1 1 d . . . H11 H 0.3644 0.5660 0.7621 0.051 Uiso 1 1 calc R . . C12 C 0.3862(5) 0.5977(5) 0.6608(3) 0.0434(13) Uani 1 1 d . . . H12 H 0.3168 0.5781 0.6419 0.052 Uiso 1 1 calc R . . C13 C 0.4605(4) 0.6333(5) 0.6170(3) 0.0381(11) Uani 1 1 d . . . H13 H 0.4427 0.6375 0.5684 0.046 Uiso 1 1 calc R . . C14 C 0.9203(4) 0.7977(3) 0.6631(3) 0.0301(9) Uani 1 1 d . . . N15 N 0.9067(4) 0.7927(3) 0.7315(2) 0.0333(9) Uani 1 1 d . . . C16 C 0.9875(5) 0.8225(4) 0.7789(3) 0.0375(11) Uani 1 1 d . . . H16 H 0.9770 0.8195 0.8266 0.045 Uiso 1 1 calc R . . C17 C 1.0861(5) 0.8578(5) 0.7600(4) 0.0459(14) Uani 1 1 d . . . H17 H 1.1413 0.8792 0.7939 0.055 Uiso 1 1 calc R . . C18 C 1.0996(6) 0.8600(5) 0.6902(4) 0.0498(16) Uani 1 1 d . . . H18 H 1.1658 0.8820 0.6760 0.060 Uiso 1 1 calc R . . C19 C 1.0176(5) 0.8305(5) 0.6403(3) 0.0396(11) Uani 1 1 d . . . H19 H 1.0271 0.8324 0.5924 0.048 Uiso 1 1 calc R . . N20 N 0.7525(4) 0.7145(3) 0.8517(4) 0.0438(16) Uani 1 1 d . . . C21 C 0.7173(4) 0.7987(4) 0.8898(3) 0.0322(10) Uani 1 1 d . . . C22 C 0.7123(6) 0.7944(5) 0.9614(3) 0.0405(13) Uani 1 1 d . . . H22 H 0.6893 0.8545 0.9857 0.049 Uiso 1 1 calc R . . C23 C 0.7423(6) 0.6989(5) 0.9968(3) 0.0462(14) Uani 1 1 d . . . H23 H 0.7365 0.6930 1.0450 0.055 Uiso 1 1 calc R . . C24 C 0.7808(5) 0.6125(5) 0.9603(3) 0.0418(12) Uani 1 1 d . . . H24 H 0.8042 0.5488 0.9836 0.050 Uiso 1 1 calc R . . C25 C 0.7839(4) 0.6226(4) 0.8878(3) 0.0338(10) Uani 1 1 d . . . C26 C 0.6854(4) 0.8938(4) 0.8448(3) 0.0316(10) Uani 1 1 d . . . N27 N 0.6886(4) 0.8797(3) 0.7763(2) 0.0328(9) Uani 1 1 d . . . C28 C 0.6577(5) 0.9603(4) 0.7316(3) 0.0398(12) Uani 1 1 d . . . H28 H 0.6590 0.9489 0.6833 0.048 Uiso 1 1 calc R . . C29 C 0.6235(5) 1.0613(5) 0.7551(4) 0.0437(13) Uani 1 1 d . . . H29 H 0.6017 1.1167 0.7235 0.052 Uiso 1 1 calc R . . C30 C 0.6233(5) 1.0757(5) 0.8255(4) 0.0502(16) Uani 1 1 d . . . H30 H 0.6015 1.1422 0.8428 0.060 Uiso 1 1 calc R . . C31 C 0.6552(5) 0.9922(4) 0.8723(3) 0.0431(13) Uani 1 1 d . . . H31 H 0.6563 1.0021 0.9208 0.052 Uiso 1 1 calc R . . C32 C 0.8228(4) 0.5386(4) 0.8419(3) 0.0332(10) Uani 1 1 d . . . N33 N 0.8217(4) 0.5619(3) 0.7743(2) 0.0324(8) Uani 1 1 d . . . C34 C 0.8575(5) 0.4902(4) 0.7294(3) 0.0392(11) Uani 1 1 d . . . H34 H 0.8560 0.5090 0.6819 0.047 Uiso 1 1 calc R . . C35 C 0.8966(5) 0.3892(5) 0.7508(3) 0.0441(13) Uani 1 1 d . . . H35 H 0.9231 0.3412 0.7188 0.053 Uiso 1 1 calc R . . C36 C 0.8957(6) 0.3609(5) 0.8207(4) 0.0446(14) Uani 1 1 d . . . H36 H 0.9179 0.2917 0.8361 0.054 Uiso 1 1 calc R . . C37 C 0.8614(5) 0.4364(4) 0.8680(3) 0.0391(11) Uani 1 1 d . . . H37 H 0.8637 0.4200 0.9159 0.047 Uiso 1 1 calc R . . B38 B 0.9945(8) 1.0112(7) 0.9401(4) 0.055(2) Uani 1 1 d . . . F39 F 1.0336(5) 1.0362(4) 1.0077(2) 0.0712(14) Uani 1 1 d . . . F40 F 0.9394(6) 1.1004(5) 0.9083(3) 0.095(2) Uani 1 1 d . . . F41 F 1.0767(3) 0.9829(3) 0.90029(19) 0.0526(9) Uani 1 1 d . . . F42 F 0.9253(4) 0.9230(4) 0.9409(3) 0.0730(13) Uani 1 1 d . . . B43A B 1.0242(11) 0.5172(11) 1.0486(7) 0.054(4) Uiso 0.57 1 d PD A 1 F44A F 1.0137(7) 0.5728(7) 0.9857(4) 0.0564(18) Uiso 0.57 1 d PD A 1 F45A F 0.9826(9) 0.5755(9) 1.1009(5) 0.068(3) Uiso 0.57 1 d PD A 1 F46A F 1.1309(6) 0.4914(7) 1.0658(4) 0.0598(18) Uiso 0.57 1 d PD A 1 F47A F 0.9594(9) 0.4246(8) 1.0385(6) 0.085(3) Uiso 0.57 1 d PD A 1 B43B B 1.0190(12) 0.4988(12) 1.0622(8) 0.048(5) Uiso 0.43 1 d PD B 2 F44B F 1.0249(12) 0.5314(13) 0.9926(6) 0.089(4) Uiso 0.43 1 d PD B 2 F45B F 1.0015(9) 0.5956(8) 1.1000(5) 0.041(2) Uiso 0.43 1 d PD B 2 F46B F 1.1108(9) 0.4480(9) 1.0840(6) 0.066(3) Uiso 0.43 1 d PD B 2 F47B F 0.9282(9) 0.4361(9) 1.0616(6) 0.069(3) Uiso 0.43 1 d PD B 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 Cu1 0.0263(3) 0.0259(2) 0.0441(3) -0.0010(2) 0.0047(2) -0.0007(2) N2 0.029(3) 0.026(2) 0.0223(17) 0.0006(13) -0.0036(16) -0.0030(15) C3 0.028(3) 0.029(2) 0.044(3) -0.0016(18) 0.008(2) 0.0027(18) C4 0.033(3) 0.047(3) 0.046(3) -0.002(2) 0.004(2) 0.001(2) C5 0.042(3) 0.053(3) 0.036(3) 0.003(2) 0.009(2) -0.003(3) C6 0.036(4) 0.046(3) 0.049(3) 0.002(2) 0.012(3) 0.006(2) C7 0.026(3) 0.029(2) 0.041(2) 0.0032(18) 0.005(2) 0.0064(18) C8 0.038(3) 0.029(2) 0.037(2) -0.0038(17) 0.006(2) 0.0035(19) N9 0.033(2) 0.0264(18) 0.041(2) -0.0016(15) 0.0023(17) 0.0021(16) C10 0.041(3) 0.029(2) 0.040(2) 0.0028(18) 0.005(2) 0.005(2) C11 0.033(3) 0.036(3) 0.060(3) 0.002(2) 0.015(2) -0.007(2) C12 0.031(3) 0.045(3) 0.054(3) -0.001(3) 0.005(2) -0.013(2) C13 0.028(3) 0.042(3) 0.044(3) -0.003(2) 0.000(2) -0.002(2) C14 0.028(3) 0.0211(18) 0.042(2) -0.0004(16) 0.0071(19) -0.0008(17) N15 0.033(2) 0.0222(16) 0.046(2) -0.0011(15) 0.0102(18) 0.0009(15) C16 0.036(3) 0.034(2) 0.042(3) -0.0023(19) 0.003(2) 0.005(2) C17 0.033(3) 0.035(3) 0.068(4) -0.003(3) -0.002(3) -0.008(2) C18 0.029(3) 0.041(3) 0.080(5) 0.005(3) 0.008(3) -0.009(2) C19 0.027(3) 0.043(3) 0.049(3) 0.007(2) 0.007(2) -0.004(2) N20 0.011(2) 0.0156(18) 0.104(5) -0.010(2) 0.001(2) -0.0036(14) C21 0.027(3) 0.028(2) 0.041(3) 0.0007(19) 0.000(2) -0.0021(19) C22 0.042(4) 0.038(3) 0.043(3) -0.011(2) 0.011(2) -0.004(2) C23 0.057(4) 0.043(3) 0.038(3) -0.003(2) 0.005(3) -0.005(3) C24 0.044(3) 0.040(3) 0.041(3) 0.003(2) 0.002(2) -0.007(2) C25 0.027(3) 0.031(2) 0.043(3) 0.0017(19) 0.004(2) -0.0043(19) C26 0.029(3) 0.024(2) 0.042(2) -0.0046(17) 0.0068(19) 0.0000(17) N27 0.031(2) 0.0283(18) 0.039(2) -0.0006(15) 0.0054(17) -0.0011(16) C28 0.039(3) 0.036(2) 0.043(3) 0.008(2) 0.000(2) -0.003(2) C29 0.027(3) 0.034(3) 0.069(4) 0.003(2) -0.002(2) 0.001(2) C30 0.037(3) 0.032(3) 0.081(5) -0.002(3) 0.004(3) 0.009(2) C31 0.046(4) 0.034(3) 0.050(3) -0.009(2) 0.007(2) 0.014(2) C32 0.029(3) 0.028(2) 0.043(2) 0.0004(18) 0.0035(19) -0.0038(18) N33 0.032(2) 0.0234(18) 0.042(2) 0.0054(15) 0.0012(17) -0.0004(16) C34 0.032(3) 0.037(3) 0.049(3) -0.005(2) 0.003(2) -0.006(2) C35 0.038(3) 0.036(3) 0.058(3) -0.009(2) 0.003(3) 0.002(2) C36 0.043(4) 0.035(3) 0.054(3) 0.008(2) -0.001(3) 0.005(2) C37 0.038(3) 0.031(2) 0.048(3) 0.004(2) -0.002(2) -0.002(2) B38 0.067(6) 0.051(4) 0.049(4) 0.003(3) 0.022(4) -0.005(4) F39 0.102(4) 0.066(3) 0.049(2) -0.0152(18) 0.024(2) -0.027(3) F40 0.134(5) 0.082(3) 0.079(3) 0.031(3) 0.053(3) 0.054(4) F41 0.052(2) 0.059(2) 0.0492(19) -0.0083(16) 0.0146(16) -0.0083(17) F42 0.060(3) 0.083(3) 0.074(3) 0.014(2) -0.001(2) -0.024(2) _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 N20 1.976(8) . ? Cu1 N2 2.079(4) . ? Cu1 N27 2.205(4) . ? Cu1 N9 2.206(5) . ? Cu1 N33 2.228(4) . ? Cu1 N15 2.237(5) . ? N2 C7 1.346(8) . ? N2 C3 1.354(8) . ? C3 C4 1.402(8) . ? C3 C8 1.485(7) . ? C4 C5 1.440(9) . ? C5 C6 1.387(10) . ? C6 C7 1.409(9) . ? C7 C14 1.494(8) . ? C8 N9 1.368(7) . ? C8 C13 1.423(8) . ? N9 C10 1.369(7) . ? C10 C11 1.410(9) . ? C11 C12 1.399(9) . ? C12 C13 1.404(8) . ? C14 N15 1.361(7) . ? C14 C19 1.413(7) . ? N15 C16 1.357(8) . ? C16 C17 1.408(9) . ? C17 C18 1.385(11) . ? C18 C19 1.397(10) . ? N20 C25 1.385(7) . ? N20 C21 1.387(7) . ? C21 C22 1.401(8) . ? C21 C26 1.508(7) . ? C22 C23 1.411(9) . ? C23 C24 1.408(9) . ? C24 C25 1.419(8) . ? C25 C32 1.494(7) . ? C26 N27 1.347(7) . ? C26 C31 1.411(7) . ? N27 C28 1.364(7) . ? C28 C29 1.426(9) . ? C29 C30 1.380(10) . ? C30 C31 1.418(9) . ? C32 N33 1.346(7) . ? C32 C37 1.444(7) . ? N33 C34 1.362(7) . ? C34 C35 1.406(8) . ? C35 C36 1.404(9) . ? C36 C37 1.417(9) . ? B38 F39 1.391(10) . ? B38 F41 1.405(9) . ? B38 F42 1.411(10) . ? B38 F40 1.425(10) . ? B43A F46A 1.397(13) . ? B43A F45A 1.398(14) . ? B43A F44A 1.402(15) . ? B43A F47A 1.423(14) . ? B43B F46B 1.356(15) . ? B43B F44B 1.422(16) . ? B43B F47B 1.392(16) . ? B43B F45B 1.447(14) . ? 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 N20 Cu1 N2 178.0(3) . . ? N20 Cu1 N27 77.26(17) . . ? N2 Cu1 N27 101.86(16) . . ? N20 Cu1 N9 101.19(19) . . ? N2 Cu1 N9 77.04(18) . . ? N27 Cu1 N9 93.18(16) . . ? N20 Cu1 N33 77.42(17) . . ? N2 Cu1 N33 103.54(16) . . ? N27 Cu1 N33 154.50(16) . . ? N9 Cu1 N33 94.60(16) . . ? N20 Cu1 N15 104.71(19) . . ? N2 Cu1 N15 77.04(19) . . ? N27 Cu1 N15 91.13(16) . . ? N9 Cu1 N15 154.07(17) . . ? N33 Cu1 N15 92.39(16) . . ? C7 N2 C3 124.4(5) . . ? C7 N2 Cu1 118.1(4) . . ? C3 N2 Cu1 117.4(4) . . ? N2 C3 C4 118.5(5) . . ? N2 C3 C8 117.0(5) . . ? C4 C3 C8 124.5(5) . . ? C3 C4 C5 118.9(6) . . ? C6 C5 C4 119.7(6) . . ? C5 C6 C7 119.1(6) . . ? N2 C7 C6 119.4(6) . . ? N2 C7 C14 116.1(5) . . ? C6 C7 C14 124.5(5) . . ? N9 C8 C13 121.9(5) . . ? N9 C8 C3 114.6(5) . . ? C13 C8 C3 123.5(5) . . ? C8 N9 C10 118.8(5) . . ? C8 N9 Cu1 113.8(4) . . ? C10 N9 Cu1 127.3(4) . . ? N9 C10 C11 122.3(5) . . ? C12 C11 C10 118.5(5) . . ? C11 C12 C13 120.3(6) . . ? C12 C13 C8 118.2(5) . . ? N15 C14 C19 121.3(5) . . ? N15 C14 C7 116.2(4) . . ? C19 C14 C7 122.5(5) . . ? C16 N15 C14 119.3(5) . . ? C16 N15 Cu1 128.4(4) . . ? C14 N15 Cu1 112.1(3) . . ? N15 C16 C17 122.6(5) . . ? C18 C17 C16 117.4(6) . . ? C17 C18 C19 121.3(6) . . ? C18 C19 C14 118.1(6) . . ? C25 N20 C21 117.0(6) . . ? C25 N20 Cu1 121.3(4) . . ? C21 N20 Cu1 121.7(4) . . ? N20 C21 C22 123.3(5) . . ? N20 C21 C26 111.9(5) . . ? C22 C21 C26 124.8(5) . . ? C21 C22 C23 118.7(5) . . ? C24 C23 C22 119.7(5) . . ? C23 C24 C25 118.5(5) . . ? N20 C25 C24 122.8(5) . . ? N20 C25 C32 112.2(5) . . ? C24 C25 C32 125.0(5) . . ? N27 C26 C31 121.7(5) . . ? N27 C26 C21 115.9(4) . . ? C31 C26 C21 122.4(5) . . ? C26 N27 C28 119.9(4) . . ? C26 N27 Cu1 113.1(3) . . ? C28 N27 Cu1 127.0(4) . . ? N27 C28 C29 121.9(5) . . ? C30 C29 C28 117.7(6) . . ? C29 C30 C31 120.7(5) . . ? C26 C31 C30 118.1(5) . . ? N33 C32 C37 120.4(5) . . ? N33 C32 C25 117.3(4) . . ? C37 C32 C25 122.3(5) . . ? C32 N33 C34 120.8(4) . . ? C32 N33 Cu1 111.5(3) . . ? C34 N33 Cu1 127.7(4) . . ? N33 C34 C35 122.2(5) . . ? C36 C35 C34 118.5(6) . . ? C35 C36 C37 119.5(5) . . ? C36 C37 C32 118.5(5) . . ? F39 B38 F41 111.3(8) . . ? F39 B38 F42 109.2(6) . . ? F41 B38 F42 107.7(6) . . ? F39 B38 F40 110.2(6) . . ? F41 B38 F40 108.5(6) . . ? F42 B38 F40 109.9(8) . . ? F46A B43A F45A 111.9(10) . . ? F46A B43A F44A 109.2(10) . . ? F45A B43A F44A 111.4(11) . . ? F46A B43A F47A 112.1(11) . . ? F45A B43A F47A 105.8(11) . . ? F44A B43A F47A 106.3(10) . . ? F46B B43B F47B 114.9(13) . . ? F46B B43B F44B 107.9(12) . . ? F47B B43B F44B 106.0(12) . . ? F46B B43B F45B 113.9(12) . . ? F47B B43B F45B 107.9(11) . . ? F44B B43B F45B 105.5(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.445 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.135