# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2116 data_global #============================================================================== #Manuscript Number:B005101M _publ_contact_author_name 'Prof. Xiao-Zeng You' _publ_contact_author_address ; Prof. Xiao-Zeng You Coordination Chemistry Institue Nanjing University, Nanjing 210093, P. R. China ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_requested_journal 'JCS Dalton' _publ_section_title ; Highly stable copper(I)-olefin coordination polymer capable of co-existing with water and acid ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #========================================================================= data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 B Cu F4 N3 O2' _chemical_formula_weight 479.70 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 28.4958(1) _cell_length_b 10.2352(2) _cell_length_c 14.8060(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.203(1) _cell_angle_gamma 90.00 _cell_volume 3840.68(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6418 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 28.32 _exptl_crystal_description slab _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6860 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13400 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4709 _reflns_number_gt 2902 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.1749P)^2^+60.5520P] 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 4709 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.3357 _refine_ls_wR_factor_gt 0.3125 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 -0.16291(4) 1.45323(10) 0.32241(7) 0.0276(3) Uani 1 1 d . . . O1 O -0.2770(3) 1.3184(7) 0.2757(6) 0.0496(17) Uani 1 1 d . . . O2 O -0.2922(3) 1.5290(7) 0.2927(6) 0.0514(18) Uani 1 1 d . . . H2B H -0.3098 1.4985 0.3186 0.077 Uiso 1 1 calc R . . N1 N -0.1052(3) 1.3188(7) 0.3588(5) 0.0331(15) Uani 1 1 d . . . N2 N -0.1001(3) 1.5773(7) 0.3264(5) 0.0316(15) Uani 1 1 d . . . N3 N -0.1681(2) 1.5087(8) -0.0512(4) 0.0303(15) Uani 1 1 d . . . B1 B -0.1254(6) 1.0115(14) 0.5753(11) 0.058(3) Uani 1 1 d . . . F1 F -0.0894(6) 1.0957(15) 0.5926(9) 0.169(6) Uani 1 1 d . . . F2 F -0.1683(7) 1.073(2) 0.551(2) 0.293(14) Uani 1 1 d . . . F3 F -0.1224(9) 0.9432(18) 0.6493(10) 0.232(11) Uani 1 1 d . . . F4 F -0.1338(6) 0.9365(11) 0.4947(10) 0.137(5) Uani 1 1 d . . . C1 C -0.1081(4) 1.1924(9) 0.3738(7) 0.042(2) Uani 1 1 d . . . H1A H -0.1394 1.1594 0.3695 0.050 Uiso 1 1 calc R . . C2 C -0.0667(5) 1.1068(10) 0.3957(8) 0.056(3) Uani 1 1 d . . . H2A H -0.0704 1.0188 0.4070 0.067 Uiso 1 1 calc R . . C3 C -0.0202(5) 1.1519(11) 0.4009(8) 0.056(3) Uani 1 1 d . . . H3A H 0.0074 1.0946 0.4132 0.068 Uiso 1 1 calc R . . C4 C -0.0149(4) 1.2865(10) 0.3873(7) 0.045(2) Uani 1 1 d . . . C5 C 0.0319(4) 1.3441(13) 0.3936(8) 0.056(3) Uani 1 1 d . . . H5A H 0.0606 1.2912 0.4048 0.067 Uiso 1 1 calc R . . C6 C 0.0355(4) 1.4750(13) 0.3835(8) 0.055(3) Uani 1 1 d . . . H6A H 0.0669 1.5104 0.3899 0.066 Uiso 1 1 calc R . . C7 C -0.0082(4) 1.5596(10) 0.3631(7) 0.043(2) Uani 1 1 d . . . C8 C -0.0063(4) 1.6946(11) 0.3516(7) 0.052(3) Uani 1 1 d . . . H8A H 0.0251 1.7351 0.3626 0.063 Uiso 1 1 calc R . . C9 C -0.0514(5) 1.7668(10) 0.3238(8) 0.052(3) Uani 1 1 d . . . H9A H -0.0514 1.8561 0.3123 0.062 Uiso 1 1 calc R . . C10 C -0.0973(4) 1.7044(9) 0.3129(7) 0.043(2) Uani 1 1 d . . . H10A H -0.1274 1.7547 0.2954 0.051 Uiso 1 1 calc R . . C11 C -0.0561(3) 1.5043(9) 0.3522(6) 0.0306(16) Uani 1 1 d . . . C12 C -0.0591(3) 1.3663(9) 0.3634(6) 0.0330(17) Uani 1 1 d . . . C13 C -0.2715(3) 1.4332(9) 0.2633(6) 0.0338(18) Uani 1 1 d . . . C14 C -0.2389(3) 1.4848(9) 0.2152(6) 0.0330(18) Uani 1 1 d . . . H14A H -0.2474 1.5728 0.1861 0.040 Uiso 1 1 calc R . . C15 C -0.2164(3) 1.4022(9) 0.1742(6) 0.0328(17) Uani 1 1 d . . . H15A H -0.2292 1.3120 0.1672 0.039 Uiso 1 1 calc R . . C16 C -0.1977(3) 1.4384(8) 0.1008(6) 0.0316(17) Uani 1 1 d . . . C17 C -0.1862(4) 1.3430(9) 0.0479(6) 0.0385(19) Uani 1 1 d . . . H17A H -0.1877 1.2553 0.0629 0.046 Uiso 1 1 calc R . . C18 C -0.1725(4) 1.3768(9) -0.0267(6) 0.039(2) Uani 1 1 d . . . H18A H -0.1658 1.3107 -0.0625 0.047 Uiso 1 1 calc R . . C19 C -0.1797(4) 1.5945(9) -0.0007(6) 0.0356(19) Uani 1 1 d . . . H19A H -0.1785 1.6819 -0.0166 0.043 Uiso 1 1 calc R . . C20 C -0.1938(4) 1.5675(8) 0.0751(6) 0.038(2) Uani 1 1 d . . . H20A H -0.2007 1.6356 0.1089 0.045 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 Cu1 0.0247(5) 0.0391(6) 0.0233(5) 0.0001(4) 0.0146(4) 0.0011(4) O1 0.057(4) 0.043(4) 0.064(4) 0.000(3) 0.041(4) -0.009(3) O2 0.049(4) 0.058(5) 0.066(5) 0.005(3) 0.042(4) 0.008(3) N1 0.039(4) 0.030(4) 0.033(3) -0.003(3) 0.019(3) 0.000(3) N2 0.031(3) 0.033(4) 0.029(3) -0.005(3) 0.013(3) -0.001(3) N3 0.019(3) 0.069(5) 0.008(2) 0.004(3) 0.011(2) 0.018(3) B1 0.080(9) 0.052(7) 0.073(9) 0.000(6) 0.061(8) -0.006(7) F1 0.185(12) 0.227(14) 0.133(9) -0.082(9) 0.108(9) -0.152(12) F2 0.126(14) 0.24(2) 0.49(4) -0.03(2) 0.12(2) 0.055(14) F3 0.30(2) 0.259(19) 0.091(9) 0.045(10) 0.049(11) -0.144(18) F4 0.196(13) 0.118(8) 0.140(10) -0.054(7) 0.114(10) -0.064(8) C1 0.053(5) 0.033(5) 0.034(4) -0.001(4) 0.017(4) 0.001(4) C2 0.080(8) 0.036(5) 0.052(6) -0.001(4) 0.031(6) 0.013(5) C3 0.063(7) 0.053(6) 0.054(6) 0.014(5) 0.028(5) 0.028(5) C4 0.039(5) 0.054(6) 0.041(5) 0.004(4) 0.017(4) 0.014(4) C5 0.033(5) 0.081(8) 0.054(6) 0.002(6) 0.021(4) 0.021(5) C6 0.033(5) 0.087(9) 0.049(6) 0.000(6) 0.022(4) 0.001(5) C7 0.033(4) 0.065(7) 0.035(4) -0.006(4) 0.019(4) -0.011(4) C8 0.053(6) 0.067(7) 0.037(5) -0.005(5) 0.021(4) -0.021(5) C9 0.067(7) 0.038(5) 0.057(6) -0.003(5) 0.035(5) -0.015(5) C10 0.049(5) 0.037(5) 0.046(5) 0.005(4) 0.025(4) 0.001(4) C11 0.034(4) 0.039(4) 0.027(4) -0.001(3) 0.021(3) -0.001(3) C12 0.032(4) 0.039(5) 0.031(4) -0.001(3) 0.017(3) 0.005(3) C13 0.031(4) 0.048(5) 0.027(4) -0.001(3) 0.017(3) -0.001(4) C14 0.031(4) 0.036(4) 0.034(4) 0.004(3) 0.017(3) -0.003(3) C15 0.035(4) 0.034(4) 0.030(4) 0.003(3) 0.015(3) -0.001(3) C16 0.033(4) 0.037(5) 0.029(4) -0.002(3) 0.018(3) -0.006(3) C17 0.046(5) 0.042(5) 0.036(4) -0.002(4) 0.026(4) -0.004(4) C18 0.044(5) 0.048(5) 0.032(4) -0.002(4) 0.024(4) -0.002(4) C19 0.049(5) 0.036(4) 0.023(4) 0.007(3) 0.018(4) 0.002(4) C20 0.059(6) 0.028(4) 0.026(4) -0.002(3) 0.019(4) -0.007(4) _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 N3 1.981(6) 6_586 ? Cu1 N1 2.020(7) . ? Cu1 C14 2.041(8) . ? Cu1 C15 2.086(8) . ? Cu1 N2 2.173(7) . ? O1 C13 1.210(11) . ? O2 C13 1.316(11) . ? N1 C1 1.321(11) . ? N1 C12 1.372(11) . ? N2 C10 1.324(11) . ? N2 C11 1.356(11) . ? N3 C19 1.291(11) . ? N3 C18 1.419(12) . ? N3 Cu1 1.981(6) 6_585 ? B1 F3 1.270(17) . ? B1 F1 1.273(17) . ? B1 F2 1.27(2) . ? B1 F4 1.344(17) . ? C1 C2 1.383(14) . ? C2 C3 1.372(17) . ? C3 C4 1.410(16) . ? C4 C12 1.405(12) . ? C4 C5 1.422(15) . ? C5 C6 1.357(17) . ? C6 C7 1.432(15) . ? C7 C8 1.397(15) . ? C7 C11 1.416(12) . ? C8 C9 1.372(16) . ? C9 C10 1.397(14) . ? C11 C12 1.430(13) . ? C13 C14 1.503(11) . ? C14 C15 1.359(12) . ? C15 C16 1.461(11) . ? C16 C17 1.383(12) . ? C16 C20 1.393(11) . ? C17 C18 1.373(11) . ? C19 C20 1.382(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N1 106.6(3) 6_586 . ? N3 Cu1 C14 101.1(3) 6_586 . ? N1 Cu1 C14 139.4(3) . . ? N3 Cu1 C15 135.1(3) 6_586 . ? N1 Cu1 C15 103.0(3) . . ? C14 Cu1 C15 38.4(3) . . ? N3 Cu1 N2 106.0(3) 6_586 . ? N1 Cu1 N2 80.2(3) . . ? C14 Cu1 N2 119.7(3) . . ? C15 Cu1 N2 111.8(3) . . ? C1 N1 C12 118.1(8) . . ? C1 N1 Cu1 127.3(7) . . ? C12 N1 Cu1 114.6(5) . . ? C10 N2 C11 118.2(8) . . ? C10 N2 Cu1 132.5(6) . . ? C11 N2 Cu1 109.2(5) . . ? C19 N3 C18 115.0(7) . . ? C19 N3 Cu1 124.3(6) . 6_585 ? C18 N3 Cu1 118.8(5) . 6_585 ? F3 B1 F1 118.0(16) . . ? F3 B1 F2 100.9(19) . . ? F1 B1 F2 107.7(17) . . ? F3 B1 F4 111.5(15) . . ? F1 B1 F4 111.5(12) . . ? F2 B1 F4 105.9(19) . . ? N1 C1 C2 123.2(10) . . ? C3 C2 C1 119.8(10) . . ? C2 C3 C4 119.0(10) . . ? C12 C4 C3 117.5(9) . . ? C12 C4 C5 118.8(9) . . ? C3 C4 C5 123.7(10) . . ? C6 C5 C4 121.2(9) . . ? C5 C6 C7 121.2(10) . . ? C8 C7 C11 118.1(9) . . ? C8 C7 C6 123.1(10) . . ? C11 C7 C6 118.9(9) . . ? C9 C8 C7 119.1(9) . . ? C8 C9 C10 119.1(9) . . ? N2 C10 C9 123.4(10) . . ? N2 C11 C7 122.0(8) . . ? N2 C11 C12 118.7(7) . . ? C7 C11 C12 119.1(8) . . ? N1 C12 C4 122.3(8) . . ? N1 C12 C11 116.8(7) . . ? C4 C12 C11 120.6(8) . . ? O1 C13 O2 124.4(8) . . ? O1 C13 C14 124.3(8) . . ? O2 C13 C14 111.3(8) . . ? C15 C14 C13 120.9(8) . . ? C15 C14 Cu1 72.6(5) . . ? C13 C14 Cu1 104.0(5) . . ? C14 C15 C16 125.5(8) . . ? C14 C15 Cu1 69.0(5) . . ? C16 C15 Cu1 112.3(6) . . ? C17 C16 C20 116.5(8) . . ? C17 C16 C15 120.3(8) . . ? C20 C16 C15 123.1(8) . . ? C18 C17 C16 120.4(9) . . ? C17 C18 N3 122.4(8) . . ? N3 C19 C20 125.6(8) . . ? C19 C20 C16 120.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C1 76.6(8) 6_586 . . . ? C14 Cu1 N1 C1 -54.6(9) . . . . ? C15 Cu1 N1 C1 -69.2(8) . . . . ? N2 Cu1 N1 C1 -179.5(8) . . . . ? N3 Cu1 N1 C12 -106.5(6) 6_586 . . . ? C14 Cu1 N1 C12 122.4(6) . . . . ? C15 Cu1 N1 C12 107.8(6) . . . . ? N2 Cu1 N1 C12 -2.6(6) . . . . ? N3 Cu1 N2 C10 -73.5(8) 6_586 . . . ? N1 Cu1 N2 C10 -178.1(8) . . . . ? C14 Cu1 N2 C10 39.7(9) . . . . ? C15 Cu1 N2 C10 81.7(9) . . . . ? N3 Cu1 N2 C11 103.4(5) 6_586 . . . ? N1 Cu1 N2 C11 -1.2(5) . . . . ? C14 Cu1 N2 C11 -143.4(5) . . . . ? C15 Cu1 N2 C11 -101.4(6) . . . . ? C12 N1 C1 C2 1.2(13) . . . . ? Cu1 N1 C1 C2 178.1(7) . . . . ? N1 C1 C2 C3 -1.2(16) . . . . ? C1 C2 C3 C4 2.3(16) . . . . ? C2 C3 C4 C12 -3.5(15) . . . . ? C2 C3 C4 C5 178.4(10) . . . . ? C12 C4 C5 C6 4.3(15) . . . . ? C3 C4 C5 C6 -177.6(11) . . . . ? C4 C5 C6 C7 -1.9(16) . . . . ? C5 C6 C7 C8 -179.6(10) . . . . ? C5 C6 C7 C11 -0.8(15) . . . . ? C11 C7 C8 C9 -4.3(14) . . . . ? C6 C7 C8 C9 174.6(10) . . . . ? C7 C8 C9 C10 3.3(15) . . . . ? C11 N2 C10 C9 0.1(14) . . . . ? Cu1 N2 C10 C9 176.8(7) . . . . ? C8 C9 C10 N2 -1.2(16) . . . . ? C10 N2 C11 C7 -1.1(12) . . . . ? Cu1 N2 C11 C7 -178.5(6) . . . . ? C10 N2 C11 C12 -177.8(8) . . . . ? Cu1 N2 C11 C12 4.8(9) . . . . ? C8 C7 C11 N2 3.2(13) . . . . ? C6 C7 C11 N2 -175.7(8) . . . . ? C8 C7 C11 C12 179.8(8) . . . . ? C6 C7 C11 C12 1.0(12) . . . . ? C1 N1 C12 C4 -2.5(12) . . . . ? Cu1 N1 C12 C4 -179.8(7) . . . . ? C1 N1 C12 C11 -176.7(7) . . . . ? Cu1 N1 C12 C11 6.0(9) . . . . ? C3 C4 C12 N1 3.6(14) . . . . ? C5 C4 C12 N1 -178.1(8) . . . . ? C3 C4 C12 C11 177.7(9) . . . . ? C5 C4 C12 C11 -4.1(13) . . . . ? N2 C11 C12 N1 -7.4(11) . . . . ? C7 C11 C12 N1 175.8(7) . . . . ? N2 C11 C12 C4 178.2(8) . . . . ? C7 C11 C12 C4 1.5(12) . . . . ? O1 C13 C14 C15 5.6(13) . . . . ? O2 C13 C14 C15 -176.2(8) . . . . ? O1 C13 C14 Cu1 -72.3(10) . . . . ? O2 C13 C14 Cu1 106.0(7) . . . . ? N3 Cu1 C14 C15 -156.0(5) 6_586 . . . ? N1 Cu1 C14 C15 -23.3(7) . . . . ? N2 Cu1 C14 C15 88.2(6) . . . . ? N3 Cu1 C14 C13 -37.5(6) 6_586 . . . ? N1 Cu1 C14 C13 95.1(7) . . . . ? C15 Cu1 C14 C13 118.4(8) . . . . ? N2 Cu1 C14 C13 -153.3(5) . . . . ? C13 C14 C15 C16 160.8(8) . . . . ? Cu1 C14 C15 C16 -103.0(8) . . . . ? C13 C14 C15 Cu1 -96.2(7) . . . . ? N3 Cu1 C15 C14 34.5(7) 6_586 . . . ? N1 Cu1 C15 C14 164.7(5) . . . . ? N2 Cu1 C15 C14 -110.8(5) . . . . ? N3 Cu1 C15 C16 155.5(6) 6_586 . . . ? N1 Cu1 C15 C16 -74.3(6) . . . . ? C14 Cu1 C15 C16 121.0(9) . . . . ? N2 Cu1 C15 C16 10.2(7) . . . . ? C14 C15 C16 C17 -165.9(9) . . . . ? Cu1 C15 C16 C17 114.7(8) . . . . ? C14 C15 C16 C20 9.6(14) . . . . ? Cu1 C15 C16 C20 -69.8(10) . . . . ? C20 C16 C17 C18 -0.8(13) . . . . ? C15 C16 C17 C18 175.0(8) . . . . ? C16 C17 C18 N3 1.6(14) . . . . ? C19 N3 C18 C17 -2.3(12) . . . . ? Cu1 N3 C18 C17 -167.4(7) 6_585 . . . ? C18 N3 C19 C20 2.2(12) . . . . ? Cu1 N3 C19 C20 166.4(7) 6_585 . . . ? N3 C19 C20 C16 -1.6(15) . . . . ? C17 C16 C20 C19 0.7(13) . . . . ? C15 C16 C20 C19 -174.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.073 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.201 #==========================================================================END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 B Cu F4 N3 O3' _chemical_formula_weight 473.70 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.0050(3) _cell_length_b 19.8147(8) _cell_length_c 27.2050(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3776.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7177 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 28.34 _exptl_crystal_description slab _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7260 _exptl_absorpt_correction_T_max 0.8285 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25221 _diffrn_reflns_av_R_equivalents 0.1267 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4678 _reflns_number_gt 2797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0696P)^2^+0.6654P] 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 4678 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.41607(6) 0.04353(2) 0.616476(17) 0.02422(16) Uani 1 1 d . . . O1 O 0.5884(4) 0.10110(14) 0.50276(11) 0.0384(7) Uani 1 1 d . . . H1B H 0.6652 0.1322 0.5006 0.058 Uiso 1 1 calc R . . O2 O 0.4224(5) 0.17590(14) 0.54619(12) 0.0456(8) Uani 1 1 d . . . N1 N 0.3404(4) -0.00606(15) 0.68014(12) 0.0262(7) Uani 1 1 d . . . N2 N 0.4526(5) 0.12109(16) 0.66926(12) 0.0297(8) Uani 1 1 d . . . N3 N 0.6799(4) 0.00686(16) 0.60195(11) 0.0248(7) Uani 1 1 d . . . C1 C 0.2957(6) -0.0721(2) 0.68370(16) 0.0346(10) Uani 1 1 d . . . H1A H 0.2821 -0.0971 0.6549 0.042 Uiso 1 1 calc R . . C2 C 0.2694(6) -0.1041(2) 0.72789(18) 0.0424(11) Uani 1 1 d . . . H2A H 0.2405 -0.1515 0.7291 0.051 Uiso 1 1 d R . . C3 C 0.2864(7) -0.0676(3) 0.77050(18) 0.0469(12) Uani 1 1 d . . . H3A H 0.2649 -0.0887 0.8018 0.056 Uiso 1 1 d R . . C4 C 0.3336(6) 0.0000(2) 0.76765(15) 0.0383(11) Uani 1 1 d . . . H4A H 0.3485 0.0265 0.7969 0.046 Uiso 1 1 d R . . C5 C 0.3606(5) 0.0298(2) 0.72192(15) 0.0285(9) Uani 1 1 d . . . C6 C 0.4163(5) 0.1014(2) 0.71593(15) 0.0286(9) Uani 1 1 d . . . C7 C 0.4277(6) 0.1465(2) 0.75466(17) 0.0414(11) Uani 1 1 d . . . H7A H 0.4004 0.1317 0.7875 0.050 Uiso 1 1 d R . . C8 C 0.4787(7) 0.2118(2) 0.74555(19) 0.0479(13) Uani 1 1 d . . . H8A H 0.4891 0.2435 0.7721 0.057 Uiso 1 1 d R . . C9 C 0.5160(7) 0.2324(2) 0.6983(2) 0.0474(13) Uani 1 1 d . . . H9A H 0.5514 0.2783 0.6915 0.057 Uiso 1 1 d R . . C10 C 0.5032(7) 0.1851(2) 0.66103(18) 0.0407(11) Uani 1 1 d . . . H10A H 0.5297 0.1992 0.6280 0.049 Uiso 1 1 d R . . C11 C 0.6982(6) -0.05866(19) 0.59106(15) 0.0282(9) Uani 1 1 d . . . H11A H 0.5883 -0.0873 0.5942 0.034 Uiso 1 1 d R . . C12 C 0.8673(6) -0.0861(2) 0.57603(17) 0.0365(11) Uani 1 1 d . . . H12A H 0.8750 -0.1333 0.5685 0.044 Uiso 1 1 d R . . C13 C 1.0251(6) -0.0457(2) 0.57096(17) 0.0372(11) Uani 1 1 d . . . H13A H 1.1443 -0.0646 0.5604 0.045 Uiso 1 1 d R . . C14 C 1.0122(5) 0.02268(19) 0.58181(14) 0.0256(9) Uani 1 1 d . . . C15 C 0.8341(5) 0.04620(19) 0.59742(14) 0.0246(8) Uani 1 1 d . . . H15A H 0.8218 0.0932 0.6055 0.030 Uiso 1 1 d R . . C16 C 0.3257(6) 0.06118(19) 0.54608(14) 0.0263(9) Uani 1 1 d . . . H16A H 0.3208 0.0235 0.5240 0.032 Uiso 1 1 d R . . C17 C 0.4470(6) 0.1190(2) 0.53187(14) 0.0277(9) Uani 1 1 d . . . C18 C 0.1694(5) 0.07138(19) 0.57560(14) 0.0260(9) Uani 1 1 d . . . H18A H 0.1622 0.1118 0.5929 0.031 Uiso 1 1 calc R . . F4 F 0.3970(5) 0.19224(14) 0.34625(11) 0.0712(10) Uani 1 1 d . . . F3 F 0.6659(7) 0.2054(2) 0.38865(17) 0.1213(17) Uani 1 1 d . . . F2 F 0.3956(7) 0.2281(2) 0.42342(16) 0.1339(19) Uani 1 1 d . . . O1W O 0.8514(5) 0.19237(15) 0.49087(13) 0.0590(10) Uani 1 1 d . . . H1W1 H 0.7121 0.1981 0.4886 0.088 Uiso 1 1 d R . . H2W1 H 0.8872 0.2236 0.5172 0.088 Uiso 1 1 d R . . F1 F 0.5003(7) 0.29643(16) 0.36534(15) 0.1087(15) Uani 1 1 d . . . B1 B 0.4869(10) 0.2317(3) 0.3806(2) 0.0469(14) 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 0.0175(2) 0.0301(3) 0.0251(3) -0.0008(2) 0.0028(2) 0.0004(2) O1 0.0342(17) 0.0384(16) 0.0427(18) -0.0008(14) 0.0151(15) -0.0057(14) O2 0.061(2) 0.0290(16) 0.047(2) 0.0023(14) 0.0153(17) 0.0012(16) N1 0.0204(17) 0.0283(18) 0.0300(19) -0.0007(15) 0.0027(14) -0.0003(15) N2 0.029(2) 0.0291(18) 0.0312(19) -0.0035(15) 0.0021(15) 0.0016(15) N3 0.0158(16) 0.0322(19) 0.0262(17) 0.0007(14) 0.0003(13) 0.0020(14) C1 0.030(2) 0.037(2) 0.038(3) 0.000(2) 0.0017(19) -0.001(2) C2 0.033(3) 0.039(3) 0.056(3) 0.011(2) 0.006(2) 0.001(2) C3 0.033(3) 0.064(3) 0.044(3) 0.020(3) 0.011(2) 0.005(2) C4 0.034(2) 0.056(3) 0.025(2) 0.000(2) 0.0035(19) 0.005(2) C5 0.0168(19) 0.041(3) 0.027(2) 0.0031(19) 0.0039(16) 0.0043(17) C6 0.0195(19) 0.035(2) 0.031(2) -0.0062(18) -0.0004(18) 0.0041(18) C7 0.036(3) 0.056(3) 0.033(2) -0.010(2) 0.005(2) -0.001(2) C8 0.042(3) 0.050(3) 0.052(3) -0.026(3) -0.002(2) 0.001(2) C9 0.040(3) 0.035(3) 0.067(4) -0.019(2) -0.004(3) 0.000(2) C10 0.047(3) 0.031(2) 0.044(3) -0.002(2) -0.003(2) -0.004(2) C11 0.022(2) 0.029(2) 0.033(2) 0.0023(18) 0.0011(18) -0.0050(17) C12 0.028(2) 0.030(2) 0.051(3) -0.007(2) 0.003(2) 0.0038(19) C13 0.023(2) 0.036(2) 0.052(3) -0.009(2) 0.009(2) 0.008(2) C14 0.0173(19) 0.032(2) 0.028(2) -0.0022(17) 0.0006(17) 0.0000(17) C15 0.0205(19) 0.029(2) 0.0240(19) 0.0012(17) 0.0010(16) -0.0024(18) C16 0.023(2) 0.031(2) 0.025(2) -0.0042(17) -0.0008(17) 0.0016(17) C17 0.026(2) 0.033(2) 0.024(2) 0.0040(17) 0.0006(17) -0.0016(18) C18 0.021(2) 0.029(2) 0.028(2) -0.0054(17) -0.0046(17) 0.0015(18) F4 0.103(3) 0.0470(17) 0.063(2) 0.0011(15) -0.0285(19) -0.0165(16) F3 0.095(3) 0.105(3) 0.164(5) -0.052(3) -0.046(3) 0.029(3) F2 0.182(5) 0.146(4) 0.074(3) -0.029(3) 0.050(3) -0.042(3) O1W 0.054(2) 0.0423(19) 0.080(3) 0.0042(18) 0.018(2) -0.0144(17) F1 0.183(4) 0.0455(19) 0.098(3) 0.0070(19) -0.057(3) -0.030(2) B1 0.063(4) 0.037(3) 0.040(3) -0.002(3) 0.000(3) -0.004(3) _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 N3 2.025(3) . ? Cu1 C16 2.047(4) . ? Cu1 N1 2.060(3) . ? Cu1 N2 2.119(3) . ? Cu1 C18 2.128(4) . ? O1 C17 1.317(5) . ? O1 H1B 0.8200 . ? O2 C17 1.205(5) . ? N1 C5 1.348(5) . ? N1 C1 1.350(5) . ? N2 C10 1.336(5) . ? N2 C6 1.352(5) . ? N3 C11 1.338(5) . ? N3 C15 1.338(5) . ? C1 C2 1.371(6) . ? C1 H1A 0.9300 . ? C2 C3 1.371(6) . ? C2 H2A 0.9599 . ? C3 C4 1.382(7) . ? C3 H3A 0.9596 . ? C4 C5 1.391(6) . ? C4 H4A 0.9597 . ? C5 C6 1.481(5) . ? C6 C7 1.383(6) . ? C7 C8 1.366(6) . ? C7 H7A 0.9598 . ? C8 C9 1.373(7) . ? C8 H8A 0.9598 . ? C9 C10 1.384(6) . ? C9 H9A 0.9598 . ? C10 H10A 0.9596 . ? C11 C12 1.366(5) . ? C11 H11A 0.9596 . ? C12 C13 1.372(6) . ? C12 H12A 0.9599 . ? C13 C14 1.389(5) . ? C13 H13A 0.9596 . ? C14 C15 1.398(5) . ? C14 C18 1.474(5) 1_655 ? C15 H15A 0.9598 . ? C16 C18 1.373(5) . ? C16 C17 1.478(5) . ? C16 H16A 0.9599 . ? C18 C14 1.474(5) 1_455 ? C18 H18A 0.9300 . ? F4 B1 1.371(6) . ? F3 B1 1.375(8) . ? F2 B1 1.330(7) . ? O1W H1W1 0.9843 . ? O1W H2W1 0.9798 . ? F1 B1 1.352(6) . ? 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 N3 Cu1 C16 99.26(14) . . ? N3 Cu1 N1 103.17(12) . . ? C16 Cu1 N1 142.02(14) . . ? N3 Cu1 N2 106.41(13) . . ? C16 Cu1 N2 123.19(14) . . ? N1 Cu1 N2 78.89(13) . . ? N3 Cu1 C18 137.09(14) . . ? C16 Cu1 C18 38.35(15) . . ? N1 Cu1 C18 110.73(14) . . ? N2 Cu1 C18 105.31(14) . . ? C17 O1 H1B 109.5 . . ? C5 N1 C1 118.4(3) . . ? C5 N1 Cu1 115.5(2) . . ? C1 N1 Cu1 125.6(3) . . ? C10 N2 C6 118.7(4) . . ? C10 N2 Cu1 127.4(3) . . ? C6 N2 Cu1 113.9(3) . . ? C11 N3 C15 117.9(3) . . ? C11 N3 Cu1 118.6(3) . . ? C15 N3 Cu1 123.1(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 119.6 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C7 121.2(4) . . ? N2 C6 C5 115.4(3) . . ? C7 C6 C5 123.3(4) . . ? C8 C7 C6 119.2(4) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 119.7 . . ? C8 C9 C10 118.2(4) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 121.1 . . ? N2 C10 C9 122.5(4) . . ? N2 C10 H10A 118.9 . . ? C9 C10 H10A 118.6 . . ? N3 C11 C12 122.4(4) . . ? N3 C11 H11A 118.5 . . ? C12 C11 H11A 119.2 . . ? C11 C12 C13 119.8(4) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.2 . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.1 . . ? C13 C14 C15 116.6(4) . . ? C13 C14 C18 124.4(4) . 1_655 ? C15 C14 C18 118.9(3) . 1_655 ? N3 C15 C14 123.7(3) . . ? N3 C15 H15A 118.1 . . ? C14 C15 H15A 118.2 . . ? C18 C16 C17 119.8(4) . . ? C18 C16 Cu1 74.0(2) . . ? C17 C16 Cu1 101.5(3) . . ? C18 C16 H16A 116.9 . . ? C17 C16 H16A 117.4 . . ? Cu1 C16 H16A 117.7 . . ? O2 C17 O1 123.6(4) . . ? O2 C17 C16 124.0(4) . . ? O1 C17 C16 112.4(3) . . ? C16 C18 C14 124.5(4) . 1_455 ? C16 C18 Cu1 67.6(2) . . ? C14 C18 Cu1 112.1(3) 1_455 . ? C16 C18 H18A 117.7 . . ? C14 C18 H18A 117.7 1_455 . ? Cu1 C18 H18A 90.2 . . ? H1W1 O1W H2W1 103.1 . . ? F2 B1 F1 110.7(5) . . ? F2 B1 F4 110.2(5) . . ? F1 B1 F4 111.3(5) . . ? F2 B1 F3 106.2(5) . . ? F1 B1 F3 110.2(5) . . ? F4 B1 F3 108.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C5 100.5(3) . . . . ? C16 Cu1 N1 C5 -134.9(3) . . . . ? N2 Cu1 N1 C5 -4.0(3) . . . . ? C18 Cu1 N1 C5 -106.3(3) . . . . ? N3 Cu1 N1 C1 -71.2(3) . . . . ? C16 Cu1 N1 C1 53.4(4) . . . . ? N2 Cu1 N1 C1 -175.7(3) . . . . ? C18 Cu1 N1 C1 82.0(3) . . . . ? N3 Cu1 N2 C10 82.0(4) . . . . ? C16 Cu1 N2 C10 -31.1(4) . . . . ? N1 Cu1 N2 C10 -177.4(4) . . . . ? C18 Cu1 N2 C10 -68.7(4) . . . . ? N3 Cu1 N2 C6 -99.0(3) . . . . ? C16 Cu1 N2 C6 147.9(3) . . . . ? N1 Cu1 N2 C6 1.6(3) . . . . ? C18 Cu1 N2 C6 110.3(3) . . . . ? C16 Cu1 N3 C11 -84.1(3) . . . . ? N1 Cu1 N3 C11 65.0(3) . . . . ? N2 Cu1 N3 C11 147.1(3) . . . . ? C18 Cu1 N3 C11 -76.8(3) . . . . ? C16 Cu1 N3 C15 88.3(3) . . . . ? N1 Cu1 N3 C15 -122.5(3) . . . . ? N2 Cu1 N3 C15 -40.4(3) . . . . ? C18 Cu1 N3 C15 95.7(3) . . . . ? C5 N1 C1 C2 0.2(6) . . . . ? Cu1 N1 C1 C2 171.7(3) . . . . ? N1 C1 C2 C3 0.9(7) . . . . ? C1 C2 C3 C4 -1.4(7) . . . . ? C2 C3 C4 C5 0.8(6) . . . . ? C1 N1 C5 C4 -0.9(6) . . . . ? Cu1 N1 C5 C4 -173.2(3) . . . . ? C1 N1 C5 C6 177.9(3) . . . . ? Cu1 N1 C5 C6 5.6(4) . . . . ? C3 C4 C5 N1 0.4(6) . . . . ? C3 C4 C5 C6 -178.4(4) . . . . ? C10 N2 C6 C7 1.1(6) . . . . ? Cu1 N2 C6 C7 -178.0(3) . . . . ? C10 N2 C6 C5 179.8(4) . . . . ? Cu1 N2 C6 C5 0.8(4) . . . . ? N1 C5 C6 N2 -4.2(5) . . . . ? C4 C5 C6 N2 174.6(4) . . . . ? N1 C5 C6 C7 174.5(4) . . . . ? C4 C5 C6 C7 -6.7(6) . . . . ? N2 C6 C7 C8 -0.7(6) . . . . ? C5 C6 C7 C8 -179.4(4) . . . . ? C6 C7 C8 C9 0.7(7) . . . . ? C7 C8 C9 C10 -1.0(7) . . . . ? C6 N2 C10 C9 -1.4(6) . . . . ? Cu1 N2 C10 C9 177.6(3) . . . . ? C8 C9 C10 N2 1.3(7) . . . . ? C15 N3 C11 C12 0.4(6) . . . . ? Cu1 N3 C11 C12 173.3(3) . . . . ? N3 C11 C12 C13 -1.0(7) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 -0.2(6) . . . . ? C12 C13 C14 C18 -177.1(4) . . . 1_655 ? C11 N3 C15 C14 0.3(6) . . . . ? Cu1 N3 C15 C14 -172.2(3) . . . . ? C13 C14 C15 N3 -0.4(6) . . . . ? C18 C14 C15 N3 176.7(4) 1_655 . . . ? N3 Cu1 C16 C18 171.9(2) . . . . ? N1 Cu1 C16 C18 46.2(3) . . . . ? N2 Cu1 C16 C18 -71.4(3) . . . . ? N3 Cu1 C16 C17 -70.1(3) . . . . ? N1 Cu1 C16 C17 164.2(2) . . . . ? N2 Cu1 C16 C17 46.6(3) . . . . ? C18 Cu1 C16 C17 118.0(4) . . . . ? C18 C16 C17 O2 3.0(6) . . . . ? Cu1 C16 C17 O2 -75.0(4) . . . . ? C18 C16 C17 O1 -178.7(4) . . . . ? Cu1 C16 C17 O1 103.3(3) . . . . ? C17 C16 C18 C14 163.4(4) . . . 1_455 ? Cu1 C16 C18 C14 -102.2(4) . . . 1_455 ? C17 C16 C18 Cu1 -94.3(3) . . . . ? N3 Cu1 C18 C16 -11.8(3) . . . . ? N1 Cu1 C18 C16 -151.7(2) . . . . ? N2 Cu1 C18 C16 124.7(2) . . . . ? N3 Cu1 C18 C14 107.8(3) . . . 1_455 ? C16 Cu1 C18 C14 119.6(4) . . . 1_455 ? N1 Cu1 C18 C14 -32.1(3) . . . 1_455 ? N2 Cu1 C18 C14 -115.7(3) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.553 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.097 #==================================================================END