Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Kay Severin' _publ_contact_author_address ; Institut des Sciences et Ingenierie Chimiques Ecole Polytechnique Federale de Lausanne(EPFL) 1015 Lausanne Switzerland ; _publ_contact_author_email kay.severin@epfl.ch _publ_contact_author_fax '+41 21 693 9305' _publ_contact_author_phone '+41 21 693 9302' _publ_section_title ; Enhanced Hydrolytic Activity of Cu(II) and Zn(II) Complexes in Highly Cross-Linked Polymers ; loop_ _publ_author_name _publ_author_address A.Schiller ; Institut des Sciences et Ingenierie Chimiques Ecole Polytechnique Federale de Lausanne(EPFL) 1015 Lausanne Switzerland ; R.Scopelliti ; Institut des Sciences et Ingenierie Chimiques Ecole Polytechnique Federale de Lausanne(EPFL) 1015 Lausanne Switzerland ; K.Severin ; Institut des Sciences et Ingenierie Chimiques Ecole Polytechnique Federale de Lausanne(EPFL) 1015 Lausanne Switzerland ; #===END data_ligand5 _database_code_depnum_ccdc_archive 'CCDC 604874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris[(1-vinylimidazol-2-yl)methyl]amine ; _chemical_name_common Tris((1-vinylimidazol-2-yl)methyl)amine _chemical_melting_point ? _chemical_formula_moiety 'C18 H21 N7, 2(H2 O)' _chemical_formula_sum 'C18 H25 N7 O2' _chemical_formula_weight 371.45 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' _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 8.7133(17) _cell_length_b 10.2885(18) _cell_length_c 12.011(2) _cell_angle_alpha 94.105(15) _cell_angle_beta 94.136(17) _cell_angle_gamma 103.709(16) _cell_volume 1038.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 2798 _cell_measurement_theta_min 2.03695 _cell_measurement_theta_max 24.8236 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6178 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3200 _reflns_number_gt 2248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction, CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction, CrysAlis RED' _computing_data_reduction 'Oxford Diffraction, CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0846P)^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 SHELXL _refine_ls_extinction_coef 0.001(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3200 _refine_ls_number_parameters 257 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 N1 N 0.0616(2) 0.31693(16) 0.20434(14) 0.0300(5) Uani 1 1 d . . . N2 N 0.2267(3) 0.13171(19) 0.02765(17) 0.0432(6) Uani 1 1 d . . . N3 N 0.2978(2) 0.12187(17) 0.21059(16) 0.0338(5) Uani 1 1 d . . . N4 N -0.0915(2) 0.18649(18) 0.43622(16) 0.0386(5) Uani 1 1 d . . . N5 N 0.1040(2) 0.37412(17) 0.47094(15) 0.0342(5) Uani 1 1 d . . . N6 N 0.1218(2) 0.65319(18) 0.17521(17) 0.0437(6) Uani 1 1 d . . . N7 N 0.3409(2) 0.57331(19) 0.17308(17) 0.0432(5) Uani 1 1 d . . . C1 C 0.0287(3) 0.1721(2) 0.16133(19) 0.0341(6) Uani 1 1 d . . . H1A H -0.0487 0.1541 0.0942 0.041 Uiso 1 1 calc R . . H1B H -0.0176 0.1150 0.2193 0.041 Uiso 1 1 calc R . . C2 C 0.1813(3) 0.1389(2) 0.1317(2) 0.0344(6) Uani 1 1 d . . . C3 C 0.3798(3) 0.1088(2) 0.0414(2) 0.0478(7) Uani 1 1 d . . . H3 H 0.4433 0.0993 -0.0183 0.057 Uiso 1 1 calc R . . C4 C 0.4252(3) 0.1018(2) 0.1516(2) 0.0421(6) Uani 1 1 d . . . H4 H 0.5224 0.0866 0.1821 0.051 Uiso 1 1 calc R . . C5 C 0.2892(3) 0.1254(2) 0.3297(2) 0.0362(6) Uani 1 1 d . . . H5 H 0.2035 0.1550 0.3588 0.043 Uiso 1 1 calc R . . C6 C 0.3905(3) 0.0909(2) 0.4023(2) 0.0442(6) Uani 1 1 d . . . H6A H 0.4779 0.0607 0.3768 0.053 Uiso 1 1 calc R . . H6B H 0.3759 0.0963 0.4800 0.053 Uiso 1 1 calc R . . C7 C -0.0569(3) 0.3422(2) 0.28163(19) 0.0327(6) Uani 1 1 d . . . H7A H -0.1644 0.2909 0.2510 0.039 Uiso 1 1 calc R . . H7B H -0.0558 0.4389 0.2875 0.039 Uiso 1 1 calc R . . C8 C -0.0196(3) 0.3010(2) 0.39570(19) 0.0315(5) Uani 1 1 d . . . C9 C -0.0120(3) 0.1868(2) 0.5414(2) 0.0433(6) Uani 1 1 d . . . H9 H -0.0376 0.1178 0.5903 0.052 Uiso 1 1 calc R . . C10 C 0.1089(3) 0.3014(2) 0.5642(2) 0.0422(6) Uani 1 1 d . . . H10 H 0.1807 0.3258 0.6299 0.051 Uiso 1 1 calc R . . C11 C 0.2083(3) 0.5011(2) 0.4542(2) 0.0391(6) Uani 1 1 d . . . H11 H 0.1839 0.5440 0.3901 0.047 Uiso 1 1 calc R . . C12 C 0.3360(3) 0.5625(3) 0.5218(2) 0.0541(7) Uani 1 1 d . . . H12A H 0.3641 0.5226 0.5867 0.065 Uiso 1 1 calc R . . H12B H 0.3993 0.6463 0.5053 0.065 Uiso 1 1 calc R . . C13 C 0.0750(3) 0.4066(2) 0.11145(18) 0.0315(5) Uani 1 1 d . . . H13A H -0.0321 0.4135 0.0832 0.038 Uiso 1 1 calc R . . H13B H 0.1228 0.3676 0.0489 0.038 Uiso 1 1 calc R . . C14 C 0.1763(3) 0.5450(2) 0.15180(19) 0.0353(6) Uani 1 1 d . . . C15 C 0.2563(4) 0.7554(3) 0.2145(2) 0.0600(8) Uani 1 1 d . . . H15 H 0.2543 0.8450 0.2384 0.072 Uiso 1 1 calc R . . C16 C 0.3886(4) 0.7093(3) 0.2137(2) 0.0572(8) Uani 1 1 d . . . H16 H 0.4940 0.7593 0.2364 0.069 Uiso 1 1 calc R . . C17 C 0.4365(3) 0.4804(3) 0.1576(2) 0.0509(7) Uani 1 1 d . . . H17 H 0.3846 0.3875 0.1482 0.061 Uiso 1 1 calc R . . C18 C 0.5929(4) 0.5135(4) 0.1554(3) 0.0710(9) Uani 1 1 d . . . H18A H 0.6490 0.6054 0.1645 0.085 Uiso 1 1 calc R . . H18B H 0.6488 0.4454 0.1446 0.085 Uiso 1 1 calc R . . O1 O -0.3026(2) -0.03609(18) 0.30037(15) 0.0495(5) Uani 1 1 d D . . H1C H -0.237(3) 0.035(2) 0.352(2) 0.074 Uiso 1 1 d D . . H1D H -0.236(3) -0.092(2) 0.275(2) 0.074 Uiso 1 1 d D . . O2 O 0.1083(3) 0.17940(19) -0.18665(15) 0.0596(6) Uani 1 1 d D . . H2C H 0.047(3) 0.244(3) -0.183(3) 0.089 Uiso 1 1 d D . . H2D H 0.147(4) 0.169(3) -0.1102(17) 0.089 Uiso 1 1 d 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 N1 0.0318(11) 0.0280(9) 0.0293(10) 0.0017(7) 0.0053(9) 0.0053(8) N2 0.0565(15) 0.0426(11) 0.0365(12) 0.0037(9) 0.0114(11) 0.0215(10) N3 0.0379(12) 0.0335(10) 0.0322(11) 0.0057(8) 0.0074(10) 0.0108(8) N4 0.0405(12) 0.0363(11) 0.0369(12) 0.0028(8) 0.0095(10) 0.0037(9) N5 0.0356(11) 0.0358(10) 0.0303(11) 0.0010(8) 0.0028(9) 0.0075(8) N6 0.0516(14) 0.0314(10) 0.0462(13) 0.0031(9) 0.0056(11) 0.0061(9) N7 0.0392(14) 0.0384(11) 0.0461(13) 0.0101(9) 0.0011(10) -0.0034(9) C1 0.0372(14) 0.0289(11) 0.0332(13) -0.0007(9) 0.0040(11) 0.0027(9) C2 0.0425(15) 0.0263(11) 0.0343(13) 0.0021(9) 0.0065(12) 0.0077(9) C3 0.0570(18) 0.0540(15) 0.0444(17) 0.0127(12) 0.0204(14) 0.0304(13) C4 0.0435(16) 0.0457(14) 0.0452(16) 0.0118(11) 0.0170(13) 0.0205(11) C5 0.0373(14) 0.0391(13) 0.0345(14) 0.0059(10) 0.0094(12) 0.0116(10) C6 0.0408(16) 0.0538(15) 0.0382(15) 0.0058(11) 0.0048(13) 0.0114(12) C7 0.0285(13) 0.0334(12) 0.0356(13) 0.0008(9) 0.0044(10) 0.0065(9) C8 0.0294(13) 0.0338(11) 0.0308(13) -0.0015(9) 0.0060(10) 0.0068(9) C9 0.0514(17) 0.0424(14) 0.0359(15) 0.0083(10) 0.0069(13) 0.0089(12) C10 0.0486(16) 0.0472(14) 0.0298(14) 0.0034(10) 0.0015(12) 0.0103(12) C11 0.0395(15) 0.0363(13) 0.0381(14) 0.0018(10) 0.0065(12) 0.0020(10) C12 0.0427(16) 0.0578(16) 0.0519(17) 0.0027(13) -0.0023(14) -0.0046(12) C13 0.0307(13) 0.0338(12) 0.0284(12) 0.0034(9) -0.0009(10) 0.0059(9) C14 0.0394(15) 0.0333(12) 0.0306(13) 0.0063(9) 0.0036(11) 0.0025(10) C15 0.078(2) 0.0299(13) 0.062(2) -0.0009(12) 0.0094(17) -0.0047(14) C16 0.058(2) 0.0446(15) 0.0528(18) 0.0064(12) 0.0005(15) -0.0179(14) C17 0.0359(17) 0.0539(16) 0.0616(19) 0.0199(13) 0.0014(14) 0.0049(12) C18 0.040(2) 0.099(2) 0.070(2) 0.0225(18) 0.0015(16) 0.0065(16) O1 0.0334(10) 0.0544(11) 0.0542(12) -0.0034(9) 0.0027(9) 0.0010(8) O2 0.0851(16) 0.0686(13) 0.0357(11) 0.0045(9) 0.0064(11) 0.0394(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C13 1.492(3) . ? N1 C7 1.492(3) . ? N1 C1 1.495(3) . ? N2 C2 1.340(3) . ? N2 C3 1.409(3) . ? N3 C2 1.389(3) . ? N3 C4 1.406(3) . ? N3 C5 1.437(3) . ? N4 C8 1.339(3) . ? N4 C9 1.395(3) . ? N5 C8 1.386(3) . ? N5 C10 1.395(3) . ? N5 C11 1.440(3) . ? N6 C14 1.330(3) . ? N6 C15 1.403(3) . ? N7 C14 1.395(3) . ? N7 C16 1.402(3) . ? N7 C17 1.420(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.366(4) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.322(3) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.499(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.377(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.326(3) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.512(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.347(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.327(4) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? O1 H1C 0.967(17) . ? O1 H1D 0.955(16) . ? O2 H2C 0.946(17) . ? O2 H2D 0.976(17) . ? 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 C13 N1 C7 111.89(16) . . ? C13 N1 C1 111.88(16) . . ? C7 N1 C1 111.82(15) . . ? C2 N2 C3 104.7(2) . . ? C2 N3 C4 106.95(19) . . ? C2 N3 C5 126.18(19) . . ? C4 N3 C5 126.9(2) . . ? C8 N4 C9 105.85(19) . . ? C8 N5 C10 107.37(18) . . ? C8 N5 C11 125.8(2) . . ? C10 N5 C11 126.8(2) . . ? C14 N6 C15 105.2(2) . . ? C14 N7 C16 105.7(2) . . ? C14 N7 C17 125.9(2) . . ? C16 N7 C17 128.4(2) . . ? N1 C1 C2 109.42(17) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 N3 111.5(2) . . ? N2 C2 C1 124.7(2) . . ? N3 C2 C1 123.71(19) . . ? C4 C3 N2 111.3(2) . . ? C4 C3 H3 124.3 . . ? N2 C3 H3 124.3 . . ? C3 C4 N3 105.6(2) . . ? C3 C4 H4 127.2 . . ? N3 C4 H4 127.2 . . ? C6 C5 N3 125.5(2) . . ? C6 C5 H5 117.3 . . ? N3 C5 H5 117.3 . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? N1 C7 C8 110.59(18) . . ? N1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N4 C8 N5 110.7(2) . . ? N4 C8 C7 125.7(2) . . ? N5 C8 C7 123.45(19) . . ? C10 C9 N4 110.4(2) . . ? C10 C9 H9 124.8 . . ? N4 C9 H9 124.8 . . ? C9 C10 N5 105.7(2) . . ? C9 C10 H10 127.1 . . ? N5 C10 H10 127.1 . . ? C12 C11 N5 124.8(2) . . ? C12 C11 H11 117.6 . . ? N5 C11 H11 117.6 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? N1 C13 C14 110.57(18) . . ? N1 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N6 C14 N7 111.40(19) . . ? N6 C14 C13 125.3(2) . . ? N7 C14 C13 123.3(2) . . ? C16 C15 N6 110.8(2) . . ? C16 C15 H15 124.6 . . ? N6 C15 H15 124.6 . . ? C15 C16 N7 106.9(2) . . ? C15 C16 H16 126.6 . . ? N7 C16 H16 126.6 . . ? C18 C17 N7 124.9(3) . . ? C18 C17 H17 117.6 . . ? N7 C17 H17 117.6 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? H1C O1 H1D 107(2) . . ? H2C O2 H2D 107.9(19) . . ? 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 C13 N1 C1 C2 80.0(2) . . . . ? C7 N1 C1 C2 -153.58(19) . . . . ? C3 N2 C2 N3 0.1(2) . . . . ? C3 N2 C2 C1 175.6(2) . . . . ? C4 N3 C2 N2 -0.3(2) . . . . ? C5 N3 C2 N2 179.18(18) . . . . ? C4 N3 C2 C1 -175.89(19) . . . . ? C5 N3 C2 C1 3.6(3) . . . . ? N1 C1 C2 N2 -99.3(2) . . . . ? N1 C1 C2 N3 75.6(2) . . . . ? C2 N2 C3 C4 0.2(3) . . . . ? N2 C3 C4 N3 -0.4(3) . . . . ? C2 N3 C4 C3 0.5(2) . . . . ? C5 N3 C4 C3 -179.1(2) . . . . ? C2 N3 C5 C6 170.1(2) . . . . ? C4 N3 C5 C6 -10.5(3) . . . . ? C13 N1 C7 C8 -154.85(17) . . . . ? C1 N1 C7 C8 78.7(2) . . . . ? C9 N4 C8 N5 0.5(2) . . . . ? C9 N4 C8 C7 176.1(2) . . . . ? C10 N5 C8 N4 -0.4(2) . . . . ? C11 N5 C8 N4 178.99(19) . . . . ? C10 N5 C8 C7 -176.14(19) . . . . ? C11 N5 C8 C7 3.3(3) . . . . ? N1 C7 C8 N4 -100.6(2) . . . . ? N1 C7 C8 N5 74.5(2) . . . . ? C8 N4 C9 C10 -0.4(3) . . . . ? N4 C9 C10 N5 0.2(3) . . . . ? C8 N5 C10 C9 0.2(2) . . . . ? C11 N5 C10 C9 -179.3(2) . . . . ? C8 N5 C11 C12 -172.5(2) . . . . ? C10 N5 C11 C12 6.8(4) . . . . ? C7 N1 C13 C14 79.1(2) . . . . ? C1 N1 C13 C14 -154.57(18) . . . . ? C15 N6 C14 N7 -0.7(3) . . . . ? C15 N6 C14 C13 177.1(2) . . . . ? C16 N7 C14 N6 0.7(3) . . . . ? C17 N7 C14 N6 179.7(2) . . . . ? C16 N7 C14 C13 -177.2(2) . . . . ? C17 N7 C14 C13 1.8(4) . . . . ? N1 C13 C14 N6 -103.7(3) . . . . ? N1 C13 C14 N7 73.9(3) . . . . ? C14 N6 C15 C16 0.5(3) . . . . ? N6 C15 C16 N7 -0.1(3) . . . . ? C14 N7 C16 C15 -0.4(3) . . . . ? C17 N7 C16 C15 -179.3(3) . . . . ? C14 N7 C17 C18 165.1(3) . . . . ? C16 N7 C17 C18 -16.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1C N4 0.967(17) 1.926(18) 2.885(3) 171(3) . O2 H2D N2 0.976(17) 1.852(17) 2.823(3) 173(2) . O1 H1D O2 0.955(16) 1.922(18) 2.852(3) 164(3) 2 O2 H2C N6 0.946(17) 2.008(18) 2.940(3) 168(3) 2_565 _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.176 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.052 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 604875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H21 Cl N7 Zn, P F6' _chemical_formula_sum 'C18 H21 Cl F6 N7 P Zn' _chemical_formula_weight 581.21 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 13.8886(4) _cell_length_b 24.7471(11) _cell_length_c 14.5306(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.775(4) _cell_angle_gamma 90.00 _cell_volume 4728.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 8621 _cell_measurement_theta_min 2.4584 _cell_measurement_theta_max 29.19725 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7120 _exptl_absorpt_correction_T_max 0.8662 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13843 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3773 _reflns_number_gt 3215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction, CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction, CrysAlis RED' _computing_data_reduction 'Oxford Diffraction, CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0511P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3773 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Zn1 Zn -0.128937(18) -0.038830(9) 0.208287(17) 0.02013(10) Uani 1 1 d . . . Cl1 Cl -0.13155(4) 0.042262(19) 0.13561(4) 0.02595(14) Uani 1 1 d . . . N1 N -0.11686(13) -0.13448(6) 0.27958(12) 0.0203(4) Uani 1 1 d . . . N2 N 0.00153(13) -0.07266(7) 0.20267(12) 0.0230(4) Uani 1 1 d . . . N3 N 0.10321(14) -0.13822(8) 0.18990(14) 0.0295(4) Uani 1 1 d . B . N4 N -0.12590(13) -0.03037(7) 0.34765(13) 0.0236(4) Uani 1 1 d . . . N5 N -0.10115(14) -0.05568(8) 0.49872(13) 0.0291(4) Uani 1 1 d . . . N6 N -0.26058(13) -0.07721(6) 0.13629(12) 0.0201(4) Uani 1 1 d . . . N7 N -0.38526(13) -0.13547(7) 0.11673(13) 0.0228(4) Uani 1 1 d . . . C1 C -0.05541(16) -0.16447(8) 0.23176(17) 0.0258(5) Uani 1 1 d . . . H1A H -0.0999 -0.1814 0.1712 0.031 Uiso 1 1 calc R . . H1B H -0.0168 -0.1934 0.2752 0.031 Uiso 1 1 calc R . . C2 C 0.01666(16) -0.12549(8) 0.20875(15) 0.0229(5) Uani 1 1 d . . . C3 C 0.08177(18) -0.05060(9) 0.17958(16) 0.0284(5) Uani 1 1 d . . . H3 H 0.0908 -0.0132 0.1702 0.034 Uiso 1 1 calc R . . C4 C 0.14551(19) -0.09009(10) 0.17236(17) 0.0338(6) Uani 1 1 d . . . H4 H 0.2072 -0.0859 0.1581 0.041 Uiso 1 1 calc R . . C5 C 0.1424(2) -0.19103(10) 0.1840(2) 0.0445(7) Uani 1 1 d . . . H5 H 0.2144 -0.1935 0.2083 0.053 Uiso 1 1 calc R A 1 C6A C 0.0981(4) -0.2348(2) 0.1524(4) 0.0537(14) Uani 0.55 1 d P B 1 H6A1 H 0.1232 -0.2574 0.1125 0.064 Uiso 0.55 1 calc PR B 1 H6A2 H 0.0396 -0.2452 0.1684 0.064 Uiso 0.55 1 calc PR B 1 C6B C 0.2083(5) -0.1995(3) 0.1413(5) 0.0536(17) Uani 0.45 1 d P B 2 H6B1 H 0.2049 -0.2314 0.1041 0.064 Uiso 0.45 1 calc PR B 2 H6B2 H 0.2608 -0.1738 0.1468 0.064 Uiso 0.45 1 calc PR B 2 C7 C -0.06693(17) -0.12542(8) 0.38389(15) 0.0267(5) Uani 1 1 d . . . H7A H 0.0079 -0.1265 0.3992 0.032 Uiso 1 1 calc R . . H7B H -0.0867 -0.1541 0.4218 0.032 Uiso 1 1 calc R . . C8 C -0.09893(16) -0.07135(9) 0.41007(15) 0.0241(5) Uani 1 1 d . . . C9 C -0.14589(17) 0.01276(9) 0.39909(17) 0.0296(5) Uani 1 1 d . . . H9 H -0.1670 0.0476 0.3730 0.036 Uiso 1 1 calc R . . C10 C -0.13102(18) -0.00206(10) 0.49118(17) 0.0330(6) Uani 1 1 d . . . H10 H -0.1393 0.0200 0.5416 0.040 Uiso 1 1 calc R . . C11 C -0.07314(19) -0.08823(11) 0.58453(17) 0.0400(6) Uani 1 1 d . . . H11 H -0.0434 -0.1225 0.5820 0.048 Uiso 1 1 calc R . . C12 C -0.0859(2) -0.07375(13) 0.66580(19) 0.0542(8) Uani 1 1 d . . . H12A H -0.1154 -0.0397 0.6706 0.065 Uiso 1 1 calc R . . H12B H -0.0657 -0.0972 0.7204 0.065 Uiso 1 1 calc R . . C13 C -0.22202(16) -0.15330(8) 0.25513(16) 0.0240(5) Uani 1 1 d . . . H13A H -0.2468 -0.1475 0.3111 0.029 Uiso 1 1 calc R . . H13B H -0.2255 -0.1924 0.2404 0.029 Uiso 1 1 calc R . . C14 C -0.28749(15) -0.12269(8) 0.16856(15) 0.0202(5) Uani 1 1 d . . . C15 C -0.34389(16) -0.06003(8) 0.05983(15) 0.0231(5) Uani 1 1 d . . . H15 H -0.3461 -0.0284 0.0222 0.028 Uiso 1 1 calc R . . C16 C -0.42088(17) -0.09513(8) 0.04725(15) 0.0259(5) Uani 1 1 d . . . H16 H -0.4866 -0.0929 0.0002 0.031 Uiso 1 1 calc R . . C17 C -0.44087(18) -0.18107(9) 0.13121(19) 0.0330(6) Uani 1 1 d . . . H17 H -0.4034 -0.2119 0.1620 0.040 Uiso 1 1 calc R . . C18 C -0.53904(19) -0.18349(10) 0.1053(2) 0.0452(7) Uani 1 1 d . . . H18A H -0.5789 -0.1534 0.0744 0.054 Uiso 1 1 calc R . . H18B H -0.5713 -0.2153 0.1173 0.054 Uiso 1 1 calc R . . P1 P -0.2500 -0.26121(3) 0.0000 0.0321(2) Uani 1 2 d S . . F1 F -0.2500 -0.19676(8) 0.0000 0.0575(6) Uani 1 2 d S C . F2 F -0.2500 -0.32558(8) 0.0000 0.0506(6) Uani 1 2 d S C . F3A F -0.2572(4) -0.25708(19) -0.1111(4) 0.0543(13) Uani 0.60 1 d P C 1 F4A F -0.1307(4) -0.2572(2) 0.0302(4) 0.0671(15) Uani 0.60 1 d P C 1 F3B F -0.3098(6) -0.2674(3) -0.1143(6) 0.070(3) Uani 0.40 1 d P C 2 F4B F -0.1453(7) -0.2671(3) -0.0210(6) 0.077(3) Uani 0.40 1 d P C 2 P2 P -0.2500 0.15387(3) 0.5000 0.0311(2) Uani 1 2 d S . . F5 F -0.31171(11) 0.10793(6) 0.42694(11) 0.0469(4) Uani 1 1 d . . . F6 F -0.16608(12) 0.15276(7) 0.44629(13) 0.0591(5) Uani 1 1 d . . . F7 F -0.31319(13) 0.19849(6) 0.42699(13) 0.0657(5) 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 Zn1 0.02119(16) 0.02008(14) 0.01902(15) 0.00061(9) 0.00631(11) -0.00176(9) Cl1 0.0282(3) 0.0205(3) 0.0306(3) 0.0026(2) 0.0116(2) -0.0011(2) N1 0.0195(10) 0.0235(9) 0.0187(9) 0.0013(7) 0.0074(7) 0.0004(7) N2 0.0220(10) 0.0254(9) 0.0215(10) -0.0003(7) 0.0070(8) -0.0028(7) N3 0.0245(11) 0.0349(10) 0.0302(11) -0.0041(8) 0.0103(9) 0.0008(8) N4 0.0227(10) 0.0263(9) 0.0209(10) -0.0024(7) 0.0060(8) -0.0014(7) N5 0.0242(11) 0.0429(11) 0.0209(10) -0.0038(8) 0.0083(8) -0.0054(8) N6 0.0218(9) 0.0223(9) 0.0170(9) -0.0003(7) 0.0074(7) -0.0017(7) N7 0.0214(10) 0.0239(9) 0.0238(10) -0.0045(7) 0.0082(8) -0.0027(7) C1 0.0260(12) 0.0231(11) 0.0304(13) 0.0014(9) 0.0119(10) 0.0016(8) C2 0.0185(12) 0.0291(12) 0.0200(11) -0.0006(8) 0.0049(9) 0.0014(8) C3 0.0277(13) 0.0335(12) 0.0255(12) -0.0019(9) 0.0107(10) -0.0097(9) C4 0.0261(13) 0.0461(15) 0.0329(14) -0.0063(11) 0.0146(11) -0.0088(11) C5 0.0370(16) 0.0432(16) 0.0605(19) -0.0057(13) 0.0259(14) 0.0083(12) C6A 0.057(4) 0.050(3) 0.063(4) -0.008(3) 0.031(3) 0.009(3) C6B 0.055(4) 0.058(4) 0.058(4) -0.004(3) 0.032(3) 0.023(3) C7 0.0249(12) 0.0323(12) 0.0219(11) 0.0058(9) 0.0061(9) 0.0020(9) C8 0.0205(11) 0.0347(12) 0.0165(11) 0.0009(9) 0.0051(9) -0.0039(9) C9 0.0258(13) 0.0307(12) 0.0322(13) -0.0104(10) 0.0090(10) -0.0038(9) C10 0.0303(14) 0.0414(14) 0.0286(13) -0.0128(10) 0.0114(11) -0.0082(10) C11 0.0401(15) 0.0582(16) 0.0197(13) 0.0048(11) 0.0068(11) -0.0076(12) C12 0.071(2) 0.0672(19) 0.0261(15) -0.0057(13) 0.0186(15) -0.0297(16) C13 0.0249(12) 0.0224(11) 0.0270(12) 0.0044(8) 0.0115(10) -0.0009(9) C14 0.0211(12) 0.0202(10) 0.0209(11) -0.0037(8) 0.0092(9) -0.0015(8) C15 0.0261(12) 0.0253(11) 0.0185(11) 0.0013(8) 0.0080(9) 0.0023(9) C16 0.0239(12) 0.0316(12) 0.0202(11) -0.0044(9) 0.0043(9) 0.0007(9) C17 0.0296(14) 0.0226(11) 0.0475(15) -0.0019(10) 0.0133(11) -0.0051(9) C18 0.0315(16) 0.0326(13) 0.072(2) 0.0017(12) 0.0179(14) -0.0085(11) P1 0.0408(6) 0.0316(5) 0.0281(5) 0.000 0.0170(4) 0.000 F1 0.1033(19) 0.0312(11) 0.0475(14) 0.000 0.0375(14) 0.000 F2 0.0610(14) 0.0317(11) 0.0552(14) 0.000 0.0132(12) 0.000 F3A 0.102(4) 0.038(2) 0.032(2) -0.0088(14) 0.035(3) 0.001(2) F4A 0.0410(19) 0.069(3) 0.092(4) -0.007(2) 0.022(3) -0.0066(17) F3B 0.108(6) 0.040(4) 0.038(3) -0.001(2) -0.012(4) 0.021(4) F4B 0.074(6) 0.047(3) 0.143(8) 0.001(5) 0.082(7) -0.005(3) P2 0.0274(5) 0.0250(4) 0.0357(5) 0.000 0.0031(4) 0.000 F5 0.0428(9) 0.0411(8) 0.0482(9) -0.0145(7) 0.0025(7) -0.0032(7) F6 0.0479(10) 0.0728(12) 0.0631(11) 0.0170(9) 0.0272(9) -0.0030(8) F7 0.0765(12) 0.0388(9) 0.0653(12) 0.0116(8) 0.0000(9) 0.0228(8) _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 Zn1 N2 2.0214(18) . ? Zn1 N4 2.0227(18) . ? Zn1 N6 2.0269(16) . ? Zn1 Cl1 2.2625(5) . ? N1 C13 1.464(3) . ? N1 C1 1.464(3) . ? N1 C7 1.467(3) . ? N2 C2 1.323(3) . ? N2 C3 1.376(3) . ? N3 C2 1.353(3) . ? N3 C4 1.388(3) . ? N3 C5 1.429(3) . ? N4 C8 1.331(3) . ? N4 C9 1.382(3) . ? N5 C8 1.355(3) . ? N5 C10 1.384(3) . ? N5 C11 1.429(3) . ? N6 C14 1.319(3) . ? N6 C15 1.388(3) . ? N7 C14 1.361(3) . ? N7 C16 1.393(3) . ? N7 C17 1.421(3) . ? C1 C2 1.503(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.345(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6A 1.256(6) . ? C5 C6B 1.278(7) . ? C5 H5 0.9500 . ? C6A H6A1 0.9500 . ? C6A H6A2 0.9500 . ? C6B H6B1 0.9500 . ? C6B H6B2 0.9500 . ? C7 C8 1.497(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.338(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.300(4) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.499(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.344(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.294(3) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? P1 F4A 1.574(6) . ? P1 F4A 1.574(6) 2_455 ? P1 F4B 1.586(8) . ? P1 F4B 1.586(8) 2_455 ? P1 F3A 1.589(5) . ? P1 F3A 1.589(5) 2_455 ? P1 F2 1.593(2) . ? P1 F1 1.595(2) . ? P1 F3B 1.608(8) . ? P1 F3B 1.608(8) 2_455 ? P2 F7 1.5861(15) 2_456 ? P2 F7 1.5861(15) . ? P2 F6 1.5980(16) 2_456 ? P2 F6 1.5980(16) . ? P2 F5 1.6025(14) . ? P2 F5 1.6025(14) 2_456 ? 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 N2 Zn1 N4 110.68(7) . . ? N2 Zn1 N6 117.16(7) . . ? N4 Zn1 N6 106.85(7) . . ? N2 Zn1 Cl1 103.21(5) . . ? N4 Zn1 Cl1 111.56(5) . . ? N6 Zn1 Cl1 107.36(5) . . ? C13 N1 C1 114.33(16) . . ? C13 N1 C7 113.72(18) . . ? C1 N1 C7 114.45(16) . . ? C2 N2 C3 106.54(18) . . ? C2 N2 Zn1 122.14(14) . . ? C3 N2 Zn1 130.73(14) . . ? C2 N3 C4 107.07(19) . . ? C2 N3 C5 127.2(2) . . ? C4 N3 C5 125.6(2) . . ? C8 N4 C9 106.34(19) . . ? C8 N4 Zn1 120.92(15) . . ? C9 N4 Zn1 132.73(15) . . ? C8 N5 C10 107.29(18) . . ? C8 N5 C11 125.8(2) . . ? C10 N5 C11 126.9(2) . . ? C14 N6 C15 106.71(17) . . ? C14 N6 Zn1 121.88(13) . . ? C15 N6 Zn1 130.59(13) . . ? C14 N7 C16 107.03(17) . . ? C14 N7 C17 126.55(18) . . ? C16 N7 C17 126.41(18) . . ? N1 C1 C2 108.16(17) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 110.43(19) . . ? N2 C2 C1 123.12(18) . . ? N3 C2 C1 126.45(19) . . ? C4 C3 N2 109.6(2) . . ? C4 C3 H3 125.2 . . ? N2 C3 H3 125.2 . . ? C3 C4 N3 106.3(2) . . ? C3 C4 H4 126.8 . . ? N3 C4 H4 126.8 . . ? C6A C5 C6B 91.4(4) . . ? C6A C5 N3 131.3(3) . . ? C6B C5 N3 121.7(4) . . ? C6A C5 H5 114.4 . . ? C6B C5 H5 48.3 . . ? N3 C5 H5 114.4 . . ? C5 C6A H6A1 120.0 . . ? C5 C6A H6A2 120.0 . . ? H6A1 C6A H6A2 120.0 . . ? C5 C6B H6B1 120.0 . . ? C5 C6B H6B2 120.0 . . ? H6B1 C6B H6B2 120.0 . . ? N1 C7 C8 108.59(16) . . ? N1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? N1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? N4 C8 N5 110.00(19) . . ? N4 C8 C7 123.3(2) . . ? N5 C8 C7 126.64(19) . . ? C10 C9 N4 109.6(2) . . ? C10 C9 H9 125.2 . . ? N4 C9 H9 125.2 . . ? C9 C10 N5 106.7(2) . . ? C9 C10 H10 126.6 . . ? N5 C10 H10 126.6 . . ? C12 C11 N5 124.0(3) . . ? C12 C11 H11 118.0 . . ? N5 C11 H11 118.0 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? N1 C13 C14 109.34(17) . . ? N1 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N1 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N6 C14 N7 110.36(17) . . ? N6 C14 C13 124.40(18) . . ? N7 C14 C13 125.07(18) . . ? C16 C15 N6 109.43(18) . . ? C16 C15 H15 125.3 . . ? N6 C15 H15 125.3 . . ? C15 C16 N7 106.46(18) . . ? C15 C16 H16 126.8 . . ? N7 C16 H16 126.8 . . ? C18 C17 N7 124.5(2) . . ? C18 C17 H17 117.8 . . ? N7 C17 H17 117.8 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? F4A P1 F4A 172.8(4) . 2_455 ? F4A P1 F4B 27.3(3) . . ? F4A P1 F4B 154.1(4) 2_455 . ? F4A P1 F4B 154.1(4) . 2_455 ? F4A P1 F4B 27.3(3) 2_455 2_455 ? F4B P1 F4B 169.4(6) . 2_455 ? F4A P1 F3A 89.7(3) . . ? F4A P1 F3A 89.8(3) 2_455 . ? F4B P1 F3A 64.6(4) . . ? F4B P1 F3A 116.1(3) 2_455 . ? F4A P1 F3A 89.8(3) . 2_455 ? F4A P1 F3A 89.7(3) 2_455 2_455 ? F4B P1 F3A 116.1(3) . 2_455 ? F4B P1 F3A 64.6(4) 2_455 2_455 ? F3A P1 F3A 172.6(3) . 2_455 ? F4A P1 F2 93.6(2) . . ? F4A P1 F2 93.6(2) 2_455 . ? F4B P1 F2 84.7(3) . . ? F4B P1 F2 84.7(3) 2_455 . ? F3A P1 F2 93.69(17) . . ? F3A P1 F2 93.69(17) 2_455 . ? F4A P1 F1 86.4(2) . . ? F4A P1 F1 86.4(2) 2_455 . ? F4B P1 F1 95.3(3) . . ? F4B P1 F1 95.3(3) 2_455 . ? F3A P1 F1 86.31(17) . . ? F3A P1 F1 86.31(17) 2_455 . ? F2 P1 F1 180.0 . . ? F4A P1 F3B 116.2(4) . . ? F4A P1 F3B 64.6(4) 2_455 . ? F4B P1 F3B 89.6(4) . . ? F4B P1 F3B 89.4(4) 2_455 . ? F3A P1 F3B 27.6(3) . . ? F3A P1 F3B 154.0(3) 2_455 . ? F2 P1 F3B 84.5(3) . . ? F1 P1 F3B 95.5(3) . . ? F4A P1 F3B 64.6(4) . 2_455 ? F4A P1 F3B 116.2(4) 2_455 2_455 ? F4B P1 F3B 89.4(4) . 2_455 ? F4B P1 F3B 89.6(4) 2_455 2_455 ? F3A P1 F3B 154.0(3) . 2_455 ? F3A P1 F3B 27.6(3) 2_455 2_455 ? F2 P1 F3B 84.5(3) . 2_455 ? F1 P1 F3B 95.5(3) . 2_455 ? F3B P1 F3B 169.0(5) . 2_455 ? F7 P2 F7 91.75(13) 2_456 . ? F7 P2 F6 91.08(9) 2_456 2_456 ? F7 P2 F6 90.28(10) . 2_456 ? F7 P2 F6 90.28(10) 2_456 . ? F7 P2 F6 91.08(9) . . ? F6 P2 F6 178.04(14) 2_456 . ? F7 P2 F5 178.74(9) 2_456 . ? F7 P2 F5 89.31(8) . . ? F6 P2 F5 89.58(8) 2_456 . ? F6 P2 F5 89.03(9) . . ? F7 P2 F5 89.31(8) 2_456 2_456 ? F7 P2 F5 178.74(9) . 2_456 ? F6 P2 F5 89.03(9) 2_456 2_456 ? F6 P2 F5 89.58(8) . 2_456 ? F5 P2 F5 89.64(11) . 2_456 ? 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 N4 Zn1 N2 C2 82.45(16) . . . . ? N6 Zn1 N2 C2 -40.37(18) . . . . ? Cl1 Zn1 N2 C2 -158.07(15) . . . . ? N4 Zn1 N2 C3 -107.67(18) . . . . ? N6 Zn1 N2 C3 129.52(17) . . . . ? Cl1 Zn1 N2 C3 11.81(19) . . . . ? N2 Zn1 N4 C8 -48.79(17) . . . . ? N6 Zn1 N4 C8 79.83(17) . . . . ? Cl1 Zn1 N4 C8 -163.10(14) . . . . ? N2 Zn1 N4 C9 129.92(19) . . . . ? N6 Zn1 N4 C9 -101.5(2) . . . . ? Cl1 Zn1 N4 C9 15.6(2) . . . . ? N2 Zn1 N6 C14 73.08(18) . . . . ? N4 Zn1 N6 C14 -51.68(18) . . . . ? Cl1 Zn1 N6 C14 -171.49(15) . . . . ? N2 Zn1 N6 C15 -118.74(18) . . . . ? N4 Zn1 N6 C15 116.51(18) . . . . ? Cl1 Zn1 N6 C15 -3.30(19) . . . . ? C13 N1 C1 C2 144.59(17) . . . . ? C7 N1 C1 C2 -81.7(2) . . . . ? C3 N2 C2 N3 -0.4(2) . . . . ? Zn1 N2 C2 N3 171.66(13) . . . . ? C3 N2 C2 C1 -179.30(19) . . . . ? Zn1 N2 C2 C1 -7.3(3) . . . . ? C4 N3 C2 N2 0.9(2) . . . . ? C5 N3 C2 N2 -176.2(2) . . . . ? C4 N3 C2 C1 179.8(2) . . . . ? C5 N3 C2 C1 2.7(4) . . . . ? N1 C1 C2 N2 -20.8(3) . . . . ? N1 C1 C2 N3 160.46(19) . . . . ? C2 N2 C3 C4 -0.4(2) . . . . ? Zn1 N2 C3 C4 -171.46(15) . . . . ? N2 C3 C4 N3 0.9(3) . . . . ? C2 N3 C4 C3 -1.1(2) . . . . ? C5 N3 C4 C3 176.1(2) . . . . ? C2 N3 C5 C6A 35.7(6) . . . . ? C4 N3 C5 C6A -140.9(4) . . . . ? C2 N3 C5 C6B 161.0(4) . . . . ? C4 N3 C5 C6B -15.6(5) . . . . ? C13 N1 C7 C8 -80.9(2) . . . . ? C1 N1 C7 C8 145.10(18) . . . . ? C9 N4 C8 N5 0.0(2) . . . . ? Zn1 N4 C8 N5 179.00(13) . . . . ? C9 N4 C8 C7 -177.5(2) . . . . ? Zn1 N4 C8 C7 1.5(3) . . . . ? C10 N5 C8 N4 -0.1(2) . . . . ? C11 N5 C8 N4 -177.47(19) . . . . ? C10 N5 C8 C7 177.4(2) . . . . ? C11 N5 C8 C7 0.0(4) . . . . ? N1 C7 C8 N4 -28.2(3) . . . . ? N1 C7 C8 N5 154.7(2) . . . . ? C8 N4 C9 C10 0.1(2) . . . . ? Zn1 N4 C9 C10 -178.78(15) . . . . ? N4 C9 C10 N5 -0.1(3) . . . . ? C8 N5 C10 C9 0.1(2) . . . . ? C11 N5 C10 C9 177.5(2) . . . . ? C8 N5 C11 C12 -172.8(2) . . . . ? C10 N5 C11 C12 10.3(4) . . . . ? C1 N1 C13 C14 -90.7(2) . . . . ? C7 N1 C13 C14 135.30(18) . . . . ? C15 N6 C14 N7 -0.6(2) . . . . ? Zn1 N6 C14 N7 170.09(13) . . . . ? C15 N6 C14 C13 -176.07(19) . . . . ? Zn1 N6 C14 C13 -5.4(3) . . . . ? C16 N7 C14 N6 0.3(2) . . . . ? C17 N7 C14 N6 -179.2(2) . . . . ? C16 N7 C14 C13 175.8(2) . . . . ? C17 N7 C14 C13 -3.7(3) . . . . ? N1 C13 C14 N6 -16.3(3) . . . . ? N1 C13 C14 N7 168.87(19) . . . . ? C14 N6 C15 C16 0.6(2) . . . . ? Zn1 N6 C15 C16 -168.94(16) . . . . ? N6 C15 C16 N7 -0.4(2) . . . . ? C14 N7 C16 C15 0.0(2) . . . . ? C17 N7 C16 C15 179.5(2) . . . . ? C14 N7 C17 C18 155.9(3) . . . . ? C16 N7 C17 C18 -23.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.320 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.052 #===END data_complex7 _database_code_depnum_ccdc_archive 'CCDC 604876' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H21 Cl Cu N7, P F6' _chemical_formula_sum 'C18 H21 Cl Cu F6 N7 P' _chemical_formula_weight 579.38 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 13.5389(9) _cell_length_b 24.865(2) _cell_length_c 14.5342(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.009(6) _cell_angle_gamma 90.00 _cell_volume 4653.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 4881 _cell_measurement_theta_min 2.4414 _cell_measurement_theta_max 24.96165 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 1.1042 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13536 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3895 _reflns_number_gt 2752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0645P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3895 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _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 -0.12919(4) -0.049129(18) 0.20820(3) 0.02666(16) Uani 1 1 d . . . Cl1 Cl -0.12921(8) 0.03139(4) 0.13958(7) 0.0334(3) Uani 1 1 d . . . N1 N -0.1238(2) -0.12952(12) 0.26878(19) 0.0258(7) Uani 1 1 d . . . N2 N 0.0116(3) -0.07353(13) 0.2080(2) 0.0293(8) Uani 1 1 d . . . N3 N 0.1123(3) -0.14089(14) 0.1952(2) 0.0341(8) Uani 1 1 d . . . N4 N -0.1303(2) -0.03205(13) 0.3506(2) 0.0298(8) Uani 1 1 d . . . N5 N -0.0974(2) -0.06024(14) 0.5003(2) 0.0300(8) Uani 1 1 d . . . N6 N -0.2709(3) -0.07529(13) 0.1327(2) 0.0280(7) Uani 1 1 d . . . N7 N -0.3990(2) -0.13330(13) 0.1120(2) 0.0285(7) Uani 1 1 d . . . C1 C -0.0631(3) -0.16196(16) 0.2204(3) 0.0300(9) Uani 1 1 d . . . H1A H -0.1081 -0.1746 0.1567 0.036 Uiso 1 1 calc R . . H1B H -0.0331 -0.1938 0.2603 0.036 Uiso 1 1 calc R . . C2 C 0.0221(3) -0.12659(16) 0.2081(2) 0.0294(9) Uani 1 1 d . . . C3 C 0.1001(3) -0.05295(18) 0.1942(3) 0.0345(10) Uani 1 1 d . . . H3 H 0.1147 -0.0158 0.1904 0.041 Uiso 1 1 calc R . . C4 C 0.1634(4) -0.0938(2) 0.1868(3) 0.0427(11) Uani 1 1 d . . . H4 H 0.2297 -0.0907 0.1777 0.051 Uiso 1 1 calc R . . C5 C 0.1515(4) -0.1933(2) 0.1864(3) 0.0527(13) Uani 1 1 d . . . H5 H 0.2246 -0.1980 0.2114 0.063 Uiso 1 1 calc R . . C6 C 0.0980(5) -0.2346(3) 0.1483(4) 0.0795(19) Uani 1 1 d . . . H6A H 0.0246 -0.2320 0.1223 0.095 Uiso 1 1 calc R . . H6B H 0.1316 -0.2679 0.1460 0.095 Uiso 1 1 calc R . . C7 C -0.0694(3) -0.12541(16) 0.3750(2) 0.0287(9) Uani 1 1 d . . . H7A H -0.0894 -0.1558 0.4094 0.034 Uiso 1 1 calc R . . H7B H 0.0068 -0.1265 0.3878 0.034 Uiso 1 1 calc R . . C8 C -0.1004(3) -0.07353(16) 0.4090(2) 0.0276(9) Uani 1 1 d . . . C9 C -0.1470(3) 0.00955(17) 0.4064(3) 0.0327(10) Uani 1 1 d . . . H9 H -0.1695 0.0446 0.3835 0.039 Uiso 1 1 calc R . . C10 C -0.1269(3) -0.00700(18) 0.4980(3) 0.0349(10) Uani 1 1 d . . . H10 H -0.1319 0.0139 0.5511 0.042 Uiso 1 1 calc R . . C11 C -0.0654(3) -0.09510(19) 0.5824(3) 0.0416(11) Uani 1 1 d . . . H11 H -0.0436 -0.1304 0.5729 0.050 Uiso 1 1 calc R . . C12 C -0.0642(4) -0.0817(2) 0.6686(3) 0.0623(16) Uani 1 1 d . . . H12A H -0.0855 -0.0467 0.6806 0.075 Uiso 1 1 calc R . . H12B H -0.0420 -0.1069 0.7201 0.075 Uiso 1 1 calc R . . C13 C -0.2308(3) -0.14984(16) 0.2500(3) 0.0322(10) Uani 1 1 d . . . H13A H -0.2544 -0.1435 0.3071 0.039 Uiso 1 1 calc R . . H13B H -0.2330 -0.1890 0.2372 0.039 Uiso 1 1 calc R . . C14 C -0.3002(3) -0.12074(16) 0.1637(2) 0.0275(9) Uani 1 1 d . . . C15 C -0.3541(3) -0.05794(16) 0.0566(2) 0.0304(9) Uani 1 1 d . . . H15 H -0.3551 -0.0264 0.0195 0.036 Uiso 1 1 calc R . . C16 C -0.4336(3) -0.09282(17) 0.0431(3) 0.0328(10) Uani 1 1 d . . . H16 H -0.5002 -0.0903 -0.0039 0.039 Uiso 1 1 calc R . . C17 C -0.4560(4) -0.17858(17) 0.1258(3) 0.0401(11) Uani 1 1 d . . . H17 H -0.4179 -0.2090 0.1574 0.048 Uiso 1 1 calc R . . C18 C -0.5562(4) -0.1815(2) 0.0985(4) 0.0572(14) Uani 1 1 d . . . H18A H -0.5967 -0.1518 0.0667 0.069 Uiso 1 1 calc R . . H18B H -0.5893 -0.2133 0.1103 0.069 Uiso 1 1 calc R . . P1 P -0.2500 -0.26234(6) 0.0000 0.0337(4) Uani 1 2 d S . . F1 F -0.2500 -0.19825(13) 0.0000 0.0548(10) Uani 1 2 d S A . F2 F -0.2500 -0.32662(13) 0.0000 0.0521(10) Uani 1 2 d S A . F3A F -0.3102(8) -0.2659(5) -0.1127(9) 0.055(3) Uani 0.50 1 d P A 1 F4A F -0.1418(13) -0.2671(6) -0.0206(9) 0.065(3) Uani 0.50 1 d P A 1 F3B F -0.2615(9) -0.2583(6) -0.1126(9) 0.068(4) Uani 0.50 1 d P A 2 F4B F -0.1286(13) -0.2577(7) 0.0233(11) 0.083(4) Uani 0.50 1 d P A 2 P2 P -0.2500 0.15294(6) 0.5000 0.0348(4) Uani 1 2 d S . . F5 F -0.31229(19) 0.10724(10) 0.42794(17) 0.0505(7) Uani 1 1 d . . . F6 F -0.1625(2) 0.15231(11) 0.4473(2) 0.0617(8) Uani 1 1 d . . . F7 F -0.3130(3) 0.19775(11) 0.4272(2) 0.0750(10) 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 0.0301(3) 0.0268(3) 0.0222(2) 0.00020(19) 0.00681(19) -0.0033(2) Cl1 0.0412(6) 0.0275(5) 0.0330(5) 0.0008(4) 0.0136(4) -0.0021(5) N1 0.032(2) 0.0259(17) 0.0207(15) -0.0005(12) 0.0093(13) -0.0034(14) N2 0.032(2) 0.030(2) 0.0251(16) 0.0005(13) 0.0083(14) -0.0067(15) N3 0.028(2) 0.041(2) 0.0323(18) -0.0019(15) 0.0071(15) 0.0028(17) N4 0.033(2) 0.0286(18) 0.0262(16) -0.0012(14) 0.0064(14) -0.0011(15) N5 0.0229(19) 0.046(2) 0.0222(16) -0.0022(14) 0.0077(13) -0.0053(16) N6 0.034(2) 0.0309(19) 0.0180(15) -0.0007(13) 0.0065(14) -0.0049(15) N7 0.0249(19) 0.0335(19) 0.0271(16) -0.0086(14) 0.0081(14) -0.0050(15) C1 0.029(2) 0.030(2) 0.031(2) 0.0011(16) 0.0095(17) -0.0011(18) C2 0.027(2) 0.038(3) 0.0212(18) -0.0002(16) 0.0039(16) 0.0010(19) C3 0.033(3) 0.040(3) 0.031(2) 0.0028(18) 0.0102(18) -0.011(2) C4 0.032(3) 0.062(3) 0.033(2) -0.004(2) 0.0089(19) -0.009(2) C5 0.056(3) 0.044(3) 0.056(3) -0.005(2) 0.015(2) 0.011(3) C6 0.067(4) 0.082(5) 0.081(4) -0.015(3) 0.010(3) 0.033(4) C7 0.027(2) 0.035(2) 0.0227(18) 0.0048(16) 0.0065(16) 0.0021(18) C8 0.023(2) 0.039(2) 0.0200(18) -0.0022(16) 0.0059(15) -0.0051(18) C9 0.030(2) 0.035(2) 0.035(2) -0.0064(18) 0.0117(18) -0.0039(19) C10 0.030(3) 0.048(3) 0.028(2) -0.0144(18) 0.0114(18) -0.008(2) C11 0.037(3) 0.060(3) 0.025(2) 0.0039(19) 0.0053(18) -0.013(2) C12 0.095(4) 0.064(4) 0.030(2) -0.005(2) 0.022(3) -0.035(3) C13 0.041(3) 0.024(2) 0.031(2) 0.0020(16) 0.0099(18) -0.0054(19) C14 0.029(2) 0.031(2) 0.0257(18) -0.0047(16) 0.0129(17) -0.0016(18) C15 0.030(2) 0.042(3) 0.0192(18) 0.0026(16) 0.0065(16) 0.0007(19) C16 0.025(2) 0.047(3) 0.0246(19) -0.0062(18) 0.0048(16) -0.001(2) C17 0.041(3) 0.033(3) 0.046(2) -0.0083(19) 0.014(2) -0.010(2) C18 0.044(4) 0.050(3) 0.076(4) -0.008(3) 0.016(3) -0.021(3) P1 0.0404(10) 0.0338(9) 0.0273(7) 0.000 0.0110(7) 0.000 F1 0.097(3) 0.028(2) 0.0373(19) 0.000 0.018(2) 0.000 F2 0.061(3) 0.028(2) 0.059(2) 0.000 0.0064(19) 0.000 F3A 0.075(7) 0.039(5) 0.033(4) -0.002(3) -0.010(5) 0.009(5) F4A 0.056(7) 0.050(6) 0.107(10) -0.008(6) 0.051(8) -0.011(4) F3B 0.131(12) 0.047(5) 0.035(5) -0.011(3) 0.039(8) 0.001(7) F4B 0.044(5) 0.062(7) 0.141(13) -0.003(8) 0.025(9) -0.005(5) P2 0.0372(9) 0.0294(9) 0.0339(8) 0.000 0.0052(7) 0.000 F5 0.0451(16) 0.0489(16) 0.0457(15) -0.0167(12) -0.0032(12) 0.0001(13) F6 0.0626(19) 0.064(2) 0.0700(18) 0.0148(15) 0.0369(15) 0.0001(16) F7 0.096(3) 0.0445(17) 0.073(2) 0.0199(15) 0.0105(17) 0.0325(17) _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 N2 2.001(3) . ? Cu1 N6 2.002(3) . ? Cu1 N4 2.118(3) . ? Cu1 N1 2.176(3) . ? Cu1 Cl1 2.2367(11) . ? N1 C1 1.476(5) . ? N1 C13 1.478(5) . ? N1 C7 1.494(4) . ? N2 C2 1.327(5) . ? N2 C3 1.374(5) . ? N3 C2 1.340(5) . ? N3 C4 1.385(6) . ? N3 C5 1.428(6) . ? N4 C8 1.317(5) . ? N4 C9 1.376(5) . ? N5 C8 1.356(4) . ? N5 C10 1.380(5) . ? N5 C11 1.429(5) . ? N6 C14 1.322(5) . ? N6 C15 1.381(5) . ? N7 C14 1.352(5) . ? N7 C16 1.394(5) . ? N7 C17 1.414(5) . ? C1 C2 1.504(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.353(6) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.280(7) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.488(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.338(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.292(6) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.500(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.349(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.293(6) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? P1 F4B 1.576(17) 2_455 ? P1 F4B 1.576(17) . ? P1 F4A 1.588(16) 2_455 ? P1 F4A 1.588(16) . ? P1 F3A 1.591(12) . ? P1 F3A 1.591(12) 2_455 ? P1 F1 1.594(4) . ? P1 F2 1.598(4) . ? P1 F3B 1.599(12) 2_455 ? P1 F3B 1.599(12) . ? P2 F7 1.591(3) 2_456 ? P2 F7 1.591(3) . ? P2 F6 1.598(3) 2_456 ? P2 F6 1.598(3) . ? P2 F5 1.598(2) . ? P2 F5 1.598(2) 2_456 ? 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 N2 Cu1 N6 130.76(13) . . ? N2 Cu1 N4 110.90(12) . . ? N6 Cu1 N4 107.79(12) . . ? N2 Cu1 N1 79.00(12) . . ? N6 Cu1 N1 80.20(12) . . ? N4 Cu1 N1 78.35(11) . . ? N2 Cu1 Cl1 98.03(10) . . ? N6 Cu1 Cl1 100.29(9) . . ? N4 Cu1 Cl1 104.91(9) . . ? N1 Cu1 Cl1 176.28(8) . . ? C1 N1 C13 112.6(3) . . ? C1 N1 C7 111.1(3) . . ? C13 N1 C7 110.9(3) . . ? C1 N1 Cu1 105.3(2) . . ? C13 N1 Cu1 109.3(2) . . ? C7 N1 Cu1 107.4(2) . . ? C2 N2 C3 105.8(3) . . ? C2 N2 Cu1 113.8(3) . . ? C3 N2 Cu1 139.6(3) . . ? C2 N3 C4 106.8(4) . . ? C2 N3 C5 129.4(4) . . ? C4 N3 C5 123.8(4) . . ? C8 N4 C9 106.4(3) . . ? C8 N4 Cu1 112.3(3) . . ? C9 N4 Cu1 141.2(3) . . ? C8 N5 C10 106.8(3) . . ? C8 N5 C11 125.4(4) . . ? C10 N5 C11 127.8(3) . . ? C14 N6 C15 106.5(3) . . ? C14 N6 Cu1 115.4(3) . . ? C15 N6 Cu1 138.0(3) . . ? C14 N7 C16 106.7(3) . . ? C14 N7 C17 126.4(3) . . ? C16 N7 C17 126.8(3) . . ? N1 C1 C2 107.3(3) . . ? N1 C1 H1A 110.3 . . ? C2 C1 H1A 110.3 . . ? N1 C1 H1B 110.3 . . ? C2 C1 H1B 110.3 . . ? H1A C1 H1B 108.5 . . ? N2 C2 N3 111.5(4) . . ? N2 C2 C1 119.7(3) . . ? N3 C2 C1 128.8(4) . . ? C4 C3 N2 109.6(4) . . ? C4 C3 H3 125.2 . . ? N2 C3 H3 125.2 . . ? C3 C4 N3 106.4(4) . . ? C3 C4 H4 126.8 . . ? N3 C4 H4 126.8 . . ? C6 C5 N3 126.5(5) . . ? C6 C5 H5 116.7 . . ? N3 C5 H5 116.7 . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? C8 C7 N1 107.6(3) . . ? C8 C7 H7A 110.2 . . ? N1 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? N1 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N4 C8 N5 110.5(3) . . ? N4 C8 C7 121.8(3) . . ? N5 C8 C7 127.6(3) . . ? C10 C9 N4 109.6(4) . . ? C10 C9 H9 125.2 . . ? N4 C9 H9 125.2 . . ? C9 C10 N5 106.7(3) . . ? C9 C10 H10 126.6 . . ? N5 C10 H10 126.6 . . ? C12 C11 N5 124.3(5) . . ? C12 C11 H11 117.9 . . ? N5 C11 H11 117.9 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? N1 C13 C14 108.3(3) . . ? N1 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? N1 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? N6 C14 N7 110.9(3) . . ? N6 C14 C13 121.4(3) . . ? N7 C14 C13 127.6(3) . . ? C16 C15 N6 109.4(3) . . ? C16 C15 H15 125.3 . . ? N6 C15 H15 125.3 . . ? C15 C16 N7 106.5(3) . . ? C15 C16 H16 126.8 . . ? N7 C16 H16 126.8 . . ? C18 C17 N7 124.6(5) . . ? C18 C17 H17 117.7 . . ? N7 C17 H17 117.7 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? F4B P1 F4B 171.6(13) 2_455 . ? F4B P1 F4A 23.7(6) 2_455 2_455 ? F4B P1 F4A 157.9(9) . 2_455 ? F4B P1 F4A 157.9(9) 2_455 . ? F4B P1 F4A 23.7(6) . . ? F4A P1 F4A 171.4(12) 2_455 . ? F4B P1 F3A 67.3(6) 2_455 . ? F4B P1 F3A 113.2(6) . . ? F4A P1 F3A 88.9(6) 2_455 . ? F4A P1 F3A 90.6(6) . . ? F4B P1 F3A 113.2(6) 2_455 2_455 ? F4B P1 F3A 67.3(6) . 2_455 ? F4A P1 F3A 90.6(6) 2_455 2_455 ? F4A P1 F3A 88.9(6) . 2_455 ? F3A P1 F3A 173.5(10) . 2_455 ? F4B P1 F1 85.8(6) 2_455 . ? F4B P1 F1 85.8(6) . . ? F4A P1 F1 94.3(6) 2_455 . ? F4A P1 F1 94.3(6) . . ? F3A P1 F1 93.2(5) . . ? F3A P1 F1 93.2(5) 2_455 . ? F4B P1 F2 94.2(6) 2_455 . ? F4B P1 F2 94.2(6) . . ? F4A P1 F2 85.7(6) 2_455 . ? F4A P1 F2 85.7(6) . . ? F3A P1 F2 86.8(5) . . ? F3A P1 F2 86.8(5) 2_455 . ? F1 P1 F2 180.0 . . ? F4B P1 F3B 88.9(7) 2_455 2_455 ? F4B P1 F3B 90.6(7) . 2_455 ? F4A P1 F3B 67.4(6) 2_455 2_455 ? F4A P1 F3B 113.2(6) . 2_455 ? F3A P1 F3B 156.1(6) . 2_455 ? F3A P1 F3B 24.8(5) 2_455 2_455 ? F1 P1 F3B 86.4(5) . 2_455 ? F2 P1 F3B 93.6(5) . 2_455 ? F4B P1 F3B 90.6(7) 2_455 . ? F4B P1 F3B 88.9(7) . . ? F4A P1 F3B 113.2(6) 2_455 . ? F4A P1 F3B 67.4(6) . . ? F3A P1 F3B 24.8(5) . . ? F3A P1 F3B 156.1(6) 2_455 . ? F1 P1 F3B 86.4(5) . . ? F2 P1 F3B 93.6(5) . . ? F3B P1 F3B 172.8(10) 2_455 . ? F7 P2 F7 91.1(2) 2_456 . ? F7 P2 F6 90.69(16) 2_456 2_456 ? F7 P2 F6 90.09(16) . 2_456 ? F7 P2 F6 90.09(16) 2_456 . ? F7 P2 F6 90.69(16) . . ? F6 P2 F6 178.9(2) 2_456 . ? F7 P2 F5 179.13(17) 2_456 . ? F7 P2 F5 89.78(14) . . ? F6 P2 F5 89.31(14) 2_456 . ? F6 P2 F5 89.90(15) . . ? F7 P2 F5 89.78(14) 2_456 2_456 ? F7 P2 F5 179.13(17) . 2_456 ? F6 P2 F5 89.90(15) 2_456 2_456 ? F6 P2 F5 89.31(14) . 2_456 ? F5 P2 F5 89.4(2) . 2_456 ? 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 N2 Cu1 N1 C1 -33.8(2) . . . . ? N6 Cu1 N1 C1 101.4(2) . . . . ? N4 Cu1 N1 C1 -148.0(2) . . . . ? Cl1 Cu1 N1 C1 3.5(14) . . . . ? N2 Cu1 N1 C13 -154.9(2) . . . . ? N6 Cu1 N1 C13 -19.8(2) . . . . ? N4 Cu1 N1 C13 90.8(2) . . . . ? Cl1 Cu1 N1 C13 -117.7(13) . . . . ? N2 Cu1 N1 C7 84.7(2) . . . . ? N6 Cu1 N1 C7 -140.2(2) . . . . ? N4 Cu1 N1 C7 -29.6(2) . . . . ? Cl1 Cu1 N1 C7 121.9(12) . . . . ? N6 Cu1 N2 C2 -43.6(3) . . . . ? N4 Cu1 N2 C2 95.9(3) . . . . ? N1 Cu1 N2 C2 23.0(2) . . . . ? Cl1 Cu1 N2 C2 -154.7(2) . . . . ? N6 Cu1 N2 C3 124.1(4) . . . . ? N4 Cu1 N2 C3 -96.3(4) . . . . ? N1 Cu1 N2 C3 -169.2(4) . . . . ? Cl1 Cu1 N2 C3 13.1(4) . . . . ? N2 Cu1 N4 C8 -56.7(3) . . . . ? N6 Cu1 N4 C8 92.2(3) . . . . ? N1 Cu1 N4 C8 16.6(3) . . . . ? Cl1 Cu1 N4 C8 -161.6(2) . . . . ? N2 Cu1 N4 C9 118.8(4) . . . . ? N6 Cu1 N4 C9 -92.3(4) . . . . ? N1 Cu1 N4 C9 -167.9(4) . . . . ? Cl1 Cu1 N4 C9 13.9(4) . . . . ? N2 Cu1 N6 C14 77.1(3) . . . . ? N4 Cu1 N6 C14 -63.3(3) . . . . ? N1 Cu1 N6 C14 11.0(3) . . . . ? Cl1 Cu1 N6 C14 -172.8(2) . . . . ? N2 Cu1 N6 C15 -107.1(4) . . . . ? N4 Cu1 N6 C15 112.4(4) . . . . ? N1 Cu1 N6 C15 -173.3(4) . . . . ? Cl1 Cu1 N6 C15 3.0(4) . . . . ? C13 N1 C1 C2 156.3(3) . . . . ? C7 N1 C1 C2 -78.7(4) . . . . ? Cu1 N1 C1 C2 37.3(3) . . . . ? C3 N2 C2 N3 0.1(4) . . . . ? Cu1 N2 C2 N3 171.9(2) . . . . ? C3 N2 C2 C1 -179.2(3) . . . . ? Cu1 N2 C2 C1 -7.4(4) . . . . ? C4 N3 C2 N2 0.3(4) . . . . ? C5 N3 C2 N2 -176.9(4) . . . . ? C4 N3 C2 C1 179.5(3) . . . . ? C5 N3 C2 C1 2.3(6) . . . . ? N1 C1 C2 N2 -22.5(4) . . . . ? N1 C1 C2 N3 158.3(3) . . . . ? C2 N2 C3 C4 -0.5(4) . . . . ? Cu1 N2 C3 C4 -168.8(3) . . . . ? N2 C3 C4 N3 0.7(4) . . . . ? C2 N3 C4 C3 -0.6(4) . . . . ? C5 N3 C4 C3 176.8(4) . . . . ? C2 N3 C5 C6 32.7(8) . . . . ? C4 N3 C5 C6 -144.1(6) . . . . ? C1 N1 C7 C8 151.2(3) . . . . ? C13 N1 C7 C8 -82.8(4) . . . . ? Cu1 N1 C7 C8 36.6(3) . . . . ? C9 N4 C8 N5 0.0(4) . . . . ? Cu1 N4 C8 N5 177.1(2) . . . . ? C9 N4 C8 C7 -176.5(3) . . . . ? Cu1 N4 C8 C7 0.5(5) . . . . ? C10 N5 C8 N4 -0.3(4) . . . . ? C11 N5 C8 N4 -178.1(3) . . . . ? C10 N5 C8 C7 176.0(4) . . . . ? C11 N5 C8 C7 -1.8(6) . . . . ? N1 C7 C8 N4 -26.2(5) . . . . ? N1 C7 C8 N5 157.8(4) . . . . ? C8 N4 C9 C10 0.2(4) . . . . ? Cu1 N4 C9 C10 -175.4(3) . . . . ? N4 C9 C10 N5 -0.4(4) . . . . ? C8 N5 C10 C9 0.4(4) . . . . ? C11 N5 C10 C9 178.1(4) . . . . ? C8 N5 C11 C12 -179.2(4) . . . . ? C10 N5 C11 C12 3.4(7) . . . . ? C1 N1 C13 C14 -92.8(4) . . . . ? C7 N1 C13 C14 142.1(3) . . . . ? Cu1 N1 C13 C14 23.8(3) . . . . ? C15 N6 C14 N7 -0.8(4) . . . . ? Cu1 N6 C14 N7 176.3(2) . . . . ? C15 N6 C14 C13 -176.8(3) . . . . ? Cu1 N6 C14 C13 0.3(4) . . . . ? C16 N7 C14 N6 0.4(4) . . . . ? C17 N7 C14 N6 -179.1(3) . . . . ? C16 N7 C14 C13 176.1(4) . . . . ? C17 N7 C14 C13 -3.4(6) . . . . ? N1 C13 C14 N6 -17.4(5) . . . . ? N1 C13 C14 N7 167.3(3) . . . . ? C14 N6 C15 C16 0.8(4) . . . . ? Cu1 N6 C15 C16 -175.2(3) . . . . ? N6 C15 C16 N7 -0.6(4) . . . . ? C14 N7 C16 C15 0.1(4) . . . . ? C17 N7 C16 C15 179.7(3) . . . . ? C14 N7 C17 C18 157.0(4) . . . . ? C16 N7 C17 C18 -22.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.871 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.086 #===END data_complex8 _database_code_depnum_ccdc_archive 'CCDC 604877' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 Cu N9 O8 P, F6 P, 0.5(C4 H10 O), ' _chemical_formula_sum 'C32 H34 Cu F6 N9 O8.50 P2' _chemical_formula_weight 920.16 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' P P 0.1023 0.0942 '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 8.5886(16) _cell_length_b 13.3393(19) _cell_length_c 17.721(3) _cell_angle_alpha 101.074(12) _cell_angle_beta 96.831(14) _cell_angle_gamma 92.850(13) _cell_volume 1972.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 3074 _cell_measurement_theta_min 1.8169 _cell_measurement_theta_max 22.24 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11660 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.1645 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6067 _reflns_number_gt 3288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction, CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction, CrysAlis RED' _computing_data_reduction 'Oxford Diffraction, CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0211P)^2^+40.7065P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6067 _refine_ls_number_parameters 458 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.1884 _refine_ls_R_factor_gt 0.1356 _refine_ls_wR_factor_ref 0.3275 _refine_ls_wR_factor_gt 0.3044 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.109 _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 0.3160(2) 0.26957(12) 0.18449(11) 0.0373(5) Uani 1 1 d U . . P1 P 0.6514(5) 0.1950(3) 0.2445(3) 0.0524(13) Uani 1 1 d U . . O1 O 0.4785(11) 0.2042(8) 0.2381(8) 0.068(3) Uani 1 1 d U . . O2 O 0.7461(12) 0.2277(7) 0.1900(6) 0.048(2) Uani 1 1 d U . . O3 O 0.7149(12) 0.2528(10) 0.3326(7) 0.068(4) Uani 1 1 d U A . N1 N 0.1245(12) 0.3324(6) 0.1322(6) 0.0224(19) Uani 1 1 d U . . N2 N 0.4064(12) 0.2955(7) 0.0852(7) 0.032(2) Uani 1 1 d U . . N3 N 0.3781(13) 0.3710(8) -0.0164(6) 0.031(2) Uani 1 1 d U . . N4 N 0.1586(13) 0.1450(7) 0.1617(8) 0.043(3) Uani 1 1 d U . . N5 N -0.0557(13) 0.0636(7) 0.0911(7) 0.039(3) Uani 1 1 d U . . N6 N 0.3011(15) 0.3963(10) 0.2679(7) 0.047(3) Uani 1 1 d U . . N7 N 0.1562(17) 0.5153(12) 0.3152(9) 0.072(4) Uani 1 1 d U . . C1 C 0.1852(14) 0.4053(8) 0.0854(8) 0.027(3) Uani 1 1 d U . . H1A H 0.1014 0.4157 0.0447 0.032 Uiso 1 1 calc R . . H1B H 0.2207 0.4726 0.1193 0.032 Uiso 1 1 calc R . . C2 C 0.3187(15) 0.3586(9) 0.0495(8) 0.028(2) Uani 1 1 d U . . C3 C 0.5224(17) 0.2664(9) 0.0382(10) 0.044(3) Uani 1 1 d U . . H3 H 0.6013 0.2213 0.0477 0.052 Uiso 1 1 calc R . . C4 C 0.5038(16) 0.3127(10) -0.0226(9) 0.040(3) Uani 1 1 d U . . H4 H 0.5676 0.3061 -0.0633 0.048 Uiso 1 1 calc R . . C5 C 0.3198(16) 0.4390(11) -0.0646(9) 0.039(3) Uani 1 1 d U . . H5 H 0.2315 0.4756 -0.0516 0.047 Uiso 1 1 calc R . . C6 C 0.3837(16) 0.4534(11) -0.1269(9) 0.041(4) Uani 1 1 d U . . H6A H 0.4720 0.4176 -0.1411 0.050 Uiso 1 1 calc R . . H6B H 0.3408 0.4994 -0.1572 0.050 Uiso 1 1 calc R . . C7 C 0.0164(15) 0.2478(8) 0.0796(8) 0.030(3) Uani 1 1 d U . . H7A H -0.0943 0.2655 0.0787 0.036 Uiso 1 1 calc R . . H7B H 0.0435 0.2376 0.0260 0.036 Uiso 1 1 calc R . . C8 C 0.0384(15) 0.1528(8) 0.1114(9) 0.035(3) Uani 1 1 d U . . C9 C 0.1466(17) 0.0455(9) 0.1773(10) 0.051(5) Uani 1 1 d U . . H9 H 0.2166 0.0180 0.2124 0.061 Uiso 1 1 calc R . . C10 C 0.0143(17) -0.0037(9) 0.1320(10) 0.047(4) Uani 1 1 d U . . H10 H -0.0230 -0.0727 0.1293 0.057 Uiso 1 1 calc R . . C11 C -0.1921(16) 0.0446(10) 0.0360(9) 0.042(4) Uani 1 1 d U . . H11 H -0.2180 0.0962 0.0074 0.050 Uiso 1 1 calc R . . C12 C -0.286(2) -0.0402(11) 0.0214(10) 0.059(5) Uani 1 1 d U . . H12A H -0.2636 -0.0934 0.0489 0.071 Uiso 1 1 calc R . . H12B H -0.3761 -0.0480 -0.0166 0.071 Uiso 1 1 calc R . . C13 C 0.0403(14) 0.3889(8) 0.1927(7) 0.027(2) Uani 1 1 d U . . H13A H -0.0379 0.3423 0.2081 0.032 Uiso 1 1 calc R . . H13B H -0.0149 0.4444 0.1736 0.032 Uiso 1 1 calc R . . C14 C 0.1653(17) 0.4332(11) 0.2611(8) 0.036(3) Uani 1 1 d U . . C15 C 0.393(2) 0.4556(19) 0.3303(10) 0.088(7) Uani 1 1 d U . . H15 H 0.5001 0.4478 0.3474 0.105 Uiso 1 1 calc R . . C16 C 0.303(2) 0.527(2) 0.3631(12) 0.115(9) Uani 1 1 d U . . H16 H 0.3327 0.5768 0.4095 0.138 Uiso 1 1 calc R . . C17 C 0.033(2) 0.5744(16) 0.3331(11) 0.088(7) Uani 1 1 d U . . H17 H 0.0599 0.6435 0.3587 0.105 Uiso 1 1 calc R . . C18 C -0.120(2) 0.5446(15) 0.3183(10) 0.070(6) Uani 1 1 d U . . H18A H -0.1530 0.4762 0.2928 0.084 Uiso 1 1 calc R . . H18B H -0.1951 0.5917 0.3332 0.084 Uiso 1 1 calc R . . C19A C 0.8700(15) 0.2455(13) 0.3601(9) 0.021(5) Uiso 0.50 1 d PGU A 1 C20A C 0.8998(16) 0.3066(12) 0.4339(9) 0.033(6) Uiso 0.50 1 d PGU A 1 H20A H 0.8164 0.3386 0.4575 0.039 Uiso 0.50 1 calc PR A 1 C21A C 1.0517(19) 0.3210(12) 0.4732(8) 0.036(6) Uiso 0.50 1 d PGU A 1 H21A H 1.0721 0.3628 0.5237 0.043 Uiso 0.50 1 calc PR A 1 C22A C 1.1738(15) 0.2742(13) 0.4388(10) 0.026(6) Uiso 0.50 1 d PGU A 1 C23A C 1.1439(17) 0.2131(13) 0.3649(10) 0.039(7) Uiso 0.50 1 d PGU A 1 H23A H 1.2273 0.1811 0.3414 0.047 Uiso 0.50 1 calc PR A 1 C24A C 0.992(2) 0.1987(13) 0.3256(8) 0.035(7) Uiso 0.50 1 d PGU A 1 H24A H 0.9716 0.1569 0.2751 0.043 Uiso 0.50 1 calc PR A 1 N8A N 1.331(4) 0.290(2) 0.4802(17) 0.056(7) Uiso 0.50 1 d PU A 1 O5A O 1.430(3) 0.2404(19) 0.4571(15) 0.070(7) Uiso 0.50 1 d PU A 1 O6A O 1.360(3) 0.355(2) 0.5402(18) 0.089(9) Uiso 0.50 1 d PU A 1 C19B C 0.8617(15) 0.2942(13) 0.3723(10) 0.029(6) Uiso 0.50 1 d PGU A 2 C20B C 0.8952(16) 0.3812(12) 0.4307(10) 0.031(6) Uiso 0.50 1 d PGU A 2 H20B H 0.8129 0.4219 0.4468 0.037 Uiso 0.50 1 calc PR A 2 C21B C 1.0491(19) 0.4085(11) 0.4654(9) 0.041(7) Uiso 0.50 1 d PGU A 2 H21B H 1.0720 0.4679 0.5053 0.050 Uiso 0.50 1 calc PR A 2 C22B C 1.1695(15) 0.3489(13) 0.4419(10) 0.021(5) Uiso 0.50 1 d PGU A 2 C23B C 1.1360(18) 0.2620(12) 0.3835(11) 0.056(9) Uiso 0.50 1 d PGU A 2 H23B H 1.2182 0.2213 0.3674 0.067 Uiso 0.50 1 calc PR A 2 C24B C 0.982(2) 0.2347(11) 0.3487(10) 0.040(7) Uiso 0.50 1 d PGU A 2 H24B H 0.9592 0.1753 0.3088 0.048 Uiso 0.50 1 calc PR A 2 N8B N 1.333(3) 0.3815(16) 0.4795(13) 0.032(5) Uiso 0.50 1 d PU A 2 O5B O 1.444(3) 0.3255(16) 0.4601(12) 0.047(5) Uiso 0.50 1 d PU A 2 O6B O 1.355(3) 0.4672(16) 0.5242(13) 0.058(6) Uiso 0.50 1 d PU A 2 C25A C 0.5713(19) 0.0401(12) 0.3189(9) 0.028(6) Uiso 0.50 1 d PGU B 3 C26A C 0.541(2) 0.0893(9) 0.3916(10) 0.038(7) Uiso 0.50 1 d PGU B 3 H26A H 0.5817 0.1580 0.4119 0.045 Uiso 0.50 1 calc PR B 3 C27A C 0.451(2) 0.0381(12) 0.4347(8) 0.048(8) Uiso 0.50 1 d PGU B 3 H27A H 0.4305 0.0717 0.4844 0.057 Uiso 0.50 1 calc PR B 3 C28A C 0.392(2) -0.0624(12) 0.4050(10) 0.036(6) Uiso 0.50 1 d PGU B 3 C29A C 0.422(2) -0.1117(10) 0.3322(10) 0.039(7) Uiso 0.50 1 d PGU B 3 H29A H 0.3813 -0.1804 0.3119 0.047 Uiso 0.50 1 calc PR B 3 C30A C 0.512(2) -0.0604(12) 0.2892(8) 0.033(6) Uiso 0.50 1 d PGU B 3 H30A H 0.5325 -0.0941 0.2395 0.040 Uiso 0.50 1 calc PR B 3 O4A O 0.660(2) 0.0853(12) 0.2707(11) 0.029(4) Uiso 0.50 1 d PU B 3 N9A N 0.309(3) -0.1196(18) 0.4535(15) 0.044(6) Uiso 0.50 1 d PU B 3 O7A O 0.287(3) -0.0729(17) 0.5191(15) 0.065(7) Uiso 0.50 1 d PU B 3 O8A O 0.247(2) -0.2059(14) 0.4213(12) 0.043(5) Uiso 0.50 1 d PU B 3 C25B C 0.636(2) -0.0047(11) 0.2543(10) 0.021(5) Uiso 0.50 1 d PGU B 4 C26B C 0.522(2) 0.0112(10) 0.3039(10) 0.034(7) Uiso 0.50 1 d PGU B 4 H26B H 0.4811 0.0764 0.3155 0.041 Uiso 0.50 1 calc PR B 4 C27B C 0.468(2) -0.0684(13) 0.3367(10) 0.040(7) Uiso 0.50 1 d PGU B 4 H27B H 0.3900 -0.0575 0.3706 0.048 Uiso 0.50 1 calc PR B 4 C28B C 0.528(2) -0.1639(11) 0.3198(11) 0.029(6) Uiso 0.50 1 d PGU B 4 C29B C 0.642(2) -0.1798(10) 0.2702(11) 0.056(9) Uiso 0.50 1 d PGU B 4 H29B H 0.6828 -0.2451 0.2586 0.067 Uiso 0.50 1 calc PR B 4 C30B C 0.6960(19) -0.1002(13) 0.2374(10) 0.045(7) Uiso 0.50 1 d PGU B 4 H30B H 0.7739 -0.1111 0.2035 0.053 Uiso 0.50 1 calc PR B 4 O4B O 0.704(2) 0.0703(13) 0.2192(11) 0.034(4) Uiso 0.50 1 d PU B 4 N9B N 0.472(4) -0.251(2) 0.3498(17) 0.060(8) Uiso 0.50 1 d PU B 4 O7B O 0.371(3) -0.2389(16) 0.3904(14) 0.059(6) Uiso 0.50 1 d PU B 4 O8B O 0.543(4) -0.330(2) 0.3394(17) 0.091(9) Uiso 0.50 1 d PU B 4 P2 P 0.1144(5) -0.2899(3) 0.1386(3) 0.0408(10) Uani 1 1 d U . . F1 F 0.0246(11) -0.3744(7) 0.1730(7) 0.073(3) Uani 1 1 d U . . F2 F 0.2794(10) -0.3284(6) 0.1710(5) 0.051(2) Uani 1 1 d U . . F3 F 0.1180(11) -0.3713(5) 0.0578(5) 0.058(2) Uani 1 1 d U . . F4 F 0.2061(10) -0.2060(5) 0.1030(5) 0.048(2) Uani 1 1 d U . . F5 F -0.0498(9) -0.2526(5) 0.1041(5) 0.047(2) Uani 1 1 d U . . F6 F 0.1132(11) -0.2081(7) 0.2166(5) 0.060(2) Uani 1 1 d U . . O9 O 0.047(3) -0.0181(18) 0.5468(16) 0.084(8) Uiso 0.50 1 d PDU C -1 C31 C 0.086(6) 0.101(3) 0.662(2) 0.099(15) Uiso 0.50 1 d PDU C -1 H31A H 0.1318 0.1689 0.6895 0.080 Uiso 0.50 1 calc PR C -1 H31B H 0.1337 0.0485 0.6871 0.080 Uiso 0.50 1 calc PR C -1 H31C H -0.0280 0.0970 0.6647 0.080 Uiso 0.50 1 calc PR C -1 C32 C 0.115(4) 0.084(2) 0.5783(18) 0.060(9) Uiso 0.50 1 d PDU C -1 H32A H 0.0634 0.1341 0.5512 0.080 Uiso 0.50 1 calc PR C -1 H32B H 0.2293 0.0891 0.5744 0.080 Uiso 0.50 1 calc PR C -1 C33 C 0.064(6) -0.052(3) 0.465(2) 0.103(15) Uiso 0.50 1 d PDU C -1 H33A H 0.1753 -0.0622 0.4590 0.080 Uiso 0.50 1 calc PR C -1 H33B H 0.0289 0.0011 0.4356 0.080 Uiso 0.50 1 calc PR C -1 C34 C -0.038(6) -0.152(3) 0.434(3) 0.114(17) Uiso 0.50 1 d PDU C -1 H34A H -0.0165 -0.1814 0.3820 0.080 Uiso 0.50 1 calc PR C -1 H34B H -0.1491 -0.1386 0.4333 0.080 Uiso 0.50 1 calc PR C -1 H34C H -0.0128 -0.2003 0.4686 0.080 Uiso 0.50 1 calc PR C -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 0.0304(10) 0.0242(8) 0.0542(12) 0.0120(8) -0.0104(8) -0.0085(7) P1 0.034(2) 0.0299(19) 0.090(4) 0.024(2) -0.020(2) -0.0100(16) O1 0.027(5) 0.068(6) 0.117(10) 0.062(7) -0.018(5) -0.014(4) O2 0.034(6) 0.049(6) 0.051(6) -0.013(5) 0.003(5) 0.006(5) O3 0.031(6) 0.122(10) 0.055(6) 0.042(7) -0.002(5) -0.019(6) N1 0.029(5) 0.008(4) 0.025(5) -0.005(3) 0.002(4) -0.002(3) N2 0.020(5) 0.019(5) 0.051(6) -0.003(4) -0.006(4) 0.000(4) N3 0.024(6) 0.031(5) 0.035(6) -0.004(4) 0.010(5) -0.006(4) N4 0.029(6) 0.020(4) 0.080(9) 0.020(5) -0.011(5) -0.004(4) N5 0.034(7) 0.011(4) 0.065(9) -0.005(5) 0.000(5) -0.003(4) N6 0.031(6) 0.072(7) 0.031(6) -0.002(5) 0.001(5) -0.021(5) N7 0.041(7) 0.090(10) 0.060(9) -0.042(7) 0.021(7) -0.034(6) C1 0.026(7) 0.020(6) 0.033(7) 0.002(5) 0.008(5) 0.001(4) C2 0.023(6) 0.022(6) 0.037(7) -0.004(5) 0.009(5) -0.001(4) C3 0.032(8) 0.020(6) 0.074(10) -0.003(6) 0.009(6) 0.004(5) C4 0.027(7) 0.030(7) 0.054(8) -0.013(6) 0.008(6) -0.003(5) C5 0.022(8) 0.048(8) 0.049(9) 0.011(7) 0.010(6) -0.003(6) C6 0.024(8) 0.057(9) 0.043(8) 0.002(7) 0.018(7) -0.002(7) C7 0.028(7) 0.012(5) 0.041(8) -0.006(4) -0.013(6) -0.002(4) C8 0.026(7) 0.011(5) 0.063(10) 0.000(5) 0.000(6) 0.000(4) C9 0.039(9) 0.015(6) 0.096(13) 0.018(7) -0.012(8) -0.005(5) C10 0.035(9) 0.011(5) 0.090(13) 0.001(6) -0.001(7) -0.001(5) C11 0.029(8) 0.031(7) 0.060(10) -0.005(7) 0.004(6) -0.003(5) C12 0.061(11) 0.040(8) 0.060(11) -0.019(8) 0.000(9) -0.022(7) C13 0.021(6) 0.019(5) 0.038(7) 0.001(5) 0.005(4) -0.008(4) C14 0.031(7) 0.050(7) 0.021(6) -0.003(5) 0.011(5) -0.023(5) C15 0.025(8) 0.176(19) 0.036(10) -0.036(10) 0.011(7) -0.032(8) C16 0.043(10) 0.20(2) 0.055(13) -0.081(14) 0.019(8) -0.041(10) C17 0.061(9) 0.101(14) 0.073(14) -0.064(11) 0.044(10) -0.031(7) C18 0.053(8) 0.093(13) 0.046(11) -0.039(10) 0.033(9) -0.011(9) P2 0.041(2) 0.0227(17) 0.056(3) 0.0102(17) -0.006(2) -0.0034(15) F1 0.057(6) 0.057(5) 0.116(8) 0.057(5) -0.004(6) -0.011(5) F2 0.041(4) 0.048(5) 0.057(6) 0.005(4) -0.009(4) 0.008(4) F3 0.076(6) 0.019(3) 0.065(5) -0.011(3) -0.019(4) 0.017(4) F4 0.050(5) 0.030(4) 0.065(6) 0.009(4) 0.018(4) -0.006(4) F5 0.037(4) 0.028(4) 0.076(6) 0.016(4) -0.003(4) 0.002(3) F6 0.060(6) 0.062(5) 0.047(5) -0.013(4) 0.005(4) 0.005(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 O1 1.932(10) . ? Cu1 N4 2.035(10) . ? Cu1 N6 2.041(13) . ? Cu1 N1 2.083(10) . ? Cu1 N2 2.086(12) . ? P1 O2 1.449(12) . ? P1 O1 1.489(11) . ? P1 O3 1.619(13) . ? P1 O4A 1.619(16) . ? P1 O4B 1.734(18) . ? O3 C19A 1.378(16) . ? O3 C19B 1.400(15) . ? N1 C13 1.472(16) . ? N1 C1 1.507(14) . ? N1 C7 1.513(13) . ? N2 C2 1.354(16) . ? N2 C3 1.396(18) . ? N3 C2 1.363(16) . ? N3 C4 1.364(16) . ? N3 C5 1.430(17) . ? N4 C8 1.303(16) . ? N4 C9 1.408(15) . ? N5 C8 1.367(14) . ? N5 C10 1.376(17) . ? N5 C11 1.412(17) . ? N6 C14 1.290(19) . ? N6 C15 1.368(19) . ? N7 C14 1.322(19) . ? N7 C17 1.38(2) . ? N7 C16 1.42(2) . ? C1 C2 1.483(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.34(2) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.331(19) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.495(16) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.368(18) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.321(18) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.525(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.35(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.33(2) . ? C17 H17 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19A C20A 1.3900 . ? C19A C24A 1.3900 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A C22A 1.3900 . ? C21A H21A 0.9500 . ? C22A C23A 1.3900 . ? C22A N8A 1.45(3) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? N8A O5A 1.17(3) . ? N8A O6A 1.22(4) . ? C19B C20B 1.3900 . ? C19B C24B 1.3900 . ? C20B C21B 1.3900 . ? C20B H20B 0.9500 . ? C21B C22B 1.3900 . ? C21B H21B 0.9500 . ? C22B C23B 1.3900 . ? C22B N8B 1.49(2) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? N8B O6B 1.25(3) . ? N8B O5B 1.27(3) . ? C25A C26A 1.3900 . ? C25A C30A 1.3900 . ? C25A O4A 1.41(2) . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A N9A 1.47(3) . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? N9A O8A 1.24(3) . ? N9A O7A 1.25(3) . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C25B O4B 1.41(2) . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B C29B 1.3900 . ? C28B N9B 1.45(3) . ? C29B C30B 1.3900 . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? N9B O7B 1.19(3) . ? N9B O8B 1.23(4) . ? P2 F1 1.590(9) . ? P2 F6 1.590(9) . ? P2 F4 1.604(8) . ? P2 F5 1.609(8) . ? P2 F2 1.611(8) . ? P2 F3 1.627(9) . ? O9 C32 1.433(18) . ? O9 C33 1.458(19) . ? C31 C32 1.516(19) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.531(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 Cu1 N4 94.5(4) . . ? O1 Cu1 N6 99.7(6) . . ? N4 Cu1 N6 123.6(5) . . ? O1 Cu1 N1 174.2(4) . . ? N4 Cu1 N1 81.0(4) . . ? N6 Cu1 N1 80.0(4) . . ? O1 Cu1 N2 104.8(5) . . ? N4 Cu1 N2 112.2(5) . . ? N6 Cu1 N2 116.0(4) . . ? N1 Cu1 N2 80.4(4) . . ? O2 P1 O1 122.0(7) . . ? O2 P1 O3 111.1(6) . . ? O1 P1 O3 103.8(8) . . ? O2 P1 O4A 124.2(8) . . ? O1 P1 O4A 99.8(7) . . ? O3 P1 O4A 90.1(8) . . ? O2 P1 O4B 91.1(8) . . ? O1 P1 O4B 113.9(8) . . ? O3 P1 O4B 115.3(8) . . ? O4A P1 O4B 35.1(7) . . ? P1 O1 Cu1 140.4(7) . . ? C19A O3 C19B 27.3(9) . . ? C19A O3 P1 117.8(12) . . ? C19B O3 P1 134.9(12) . . ? C13 N1 C1 109.4(8) . . ? C13 N1 C7 110.5(9) . . ? C1 N1 C7 109.8(9) . . ? C13 N1 Cu1 109.2(7) . . ? C1 N1 Cu1 108.3(7) . . ? C7 N1 Cu1 109.6(6) . . ? C2 N2 C3 105.9(12) . . ? C2 N2 Cu1 111.3(9) . . ? C3 N2 Cu1 142.6(9) . . ? C2 N3 C4 107.1(12) . . ? C2 N3 C5 123.9(12) . . ? C4 N3 C5 128.9(13) . . ? C8 N4 C9 107.6(10) . . ? C8 N4 Cu1 113.0(8) . . ? C9 N4 Cu1 138.9(9) . . ? C8 N5 C10 106.0(11) . . ? C8 N5 C11 126.1(11) . . ? C10 N5 C11 127.9(10) . . ? C14 N6 C15 108.5(15) . . ? C14 N6 Cu1 112.5(9) . . ? C15 N6 Cu1 139.0(14) . . ? C14 N7 C17 132.0(15) . . ? C14 N7 C16 104.8(17) . . ? C17 N7 C16 122.8(16) . . ? C2 C1 N1 107.0(9) . . ? C2 C1 H1A 110.3 . . ? N1 C1 H1A 110.3 . . ? C2 C1 H1B 110.3 . . ? N1 C1 H1B 110.3 . . ? H1A C1 H1B 108.6 . . ? N2 C2 N3 109.7(12) . . ? N2 C2 C1 119.9(12) . . ? N3 C2 C1 130.3(12) . . ? C4 C3 N2 108.6(13) . . ? C4 C3 H3 125.7 . . ? N2 C3 H3 125.7 . . ? C3 C4 N3 108.7(14) . . ? C3 C4 H4 125.7 . . ? N3 C4 H4 125.7 . . ? C6 C5 N3 123.0(15) . . ? C6 C5 H5 118.5 . . ? N3 C5 H5 118.5 . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? C8 C7 N1 107.0(9) . . ? C8 C7 H7A 110.3 . . ? N1 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? N1 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? N4 C8 N5 111.3(11) . . ? N4 C8 C7 122.1(10) . . ? N5 C8 C7 126.5(12) . . ? C10 C9 N4 106.4(12) . . ? C10 C9 H9 126.8 . . ? N4 C9 H9 126.8 . . ? C9 C10 N5 108.6(11) . . ? C9 C10 H10 125.7 . . ? N5 C10 H10 125.7 . . ? C12 C11 N5 124.4(15) . . ? C12 C11 H11 117.8 . . ? N5 C11 H11 117.8 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? N1 C13 C14 106.1(10) . . ? N1 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? N1 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? N6 C14 N7 112.3(14) . . ? N6 C14 C13 121.1(13) . . ? N7 C14 C13 126.3(15) . . ? C16 C15 N6 106.9(17) . . ? C16 C15 H15 126.5 . . ? N6 C15 H15 126.5 . . ? C15 C16 N7 107.2(15) . . ? C15 C16 H16 126.4 . . ? N7 C16 H16 126.4 . . ? C18 C17 N7 126.8(17) . . ? C18 C17 H17 116.6 . . ? N7 C17 H17 116.6 . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? O3 C19A C20A 107.4(12) . . ? O3 C19A C24A 132.3(12) . . ? C20A C19A C24A 120.0 . . ? C21A C20A C19A 120.0 . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C20A C21A C22A 120.0 . . ? C20A C21A H21A 120.0 . . ? C22A C21A H21A 120.0 . . ? C23A C22A C21A 120.0 . . ? C23A C22A N8A 120.5(17) . . ? C21A C22A N8A 119.5(17) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C23A C24A C19A 120.0 . . ? C23A C24A H24A 120.0 . . ? C19A C24A H24A 120.0 . . ? O5A N8A O6A 120(3) . . ? O5A N8A C22A 120(3) . . ? O6A N8A C22A 120(3) . . ? C20B C19B C24B 120.0 . . ? C20B C19B O3 128.3(13) . . ? C24B C19B O3 111.7(13) . . ? C21B C20B C19B 120.0 . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C22B 120.0 . . ? C20B C21B H21B 120.0 . . ? C22B C21B H21B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B N8B 118.5(14) . . ? C23B C22B N8B 121.5(14) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C19B 120.0 . . ? C23B C24B H24B 120.0 . . ? C19B C24B H24B 120.0 . . ? O6B N8B O5B 124(2) . . ? O6B N8B C22B 117(2) . . ? O5B N8B C22B 118.9(19) . . ? C26A C25A C30A 120.0 . . ? C26A C25A O4A 124.4(13) . . ? C30A C25A O4A 115.6(13) . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C29A C28A C27A 120.0 . . ? C29A C28A N9A 119.9(15) . . ? C27A C28A N9A 119.8(15) . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30A 120.0 . . ? C25A C30A H30A 120.0 . . ? C25A O4A P1 131.2(15) . . ? O8A N9A O7A 125(3) . . ? O8A N9A C28A 116(2) . . ? O7A N9A C28A 118(2) . . ? C26B C25B C30B 120.0 . . ? C26B C25B O4B 125.5(14) . . ? C30B C25B O4B 114.5(14) . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C26B C27B C28B 120.0 . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B N9B 117.3(18) . . ? C27B C28B N9B 122.7(17) . . ? C28B C29B C30B 120.0 . . ? C28B C29B H29B 120.0 . . ? C30B C29B H29B 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30B 120.0 . . ? C25B C30B H30B 120.0 . . ? C25B O4B P1 118.0(15) . . ? O7B N9B O8B 123(3) . . ? O7B N9B C28B 118(3) . . ? O8B N9B C28B 119(3) . . ? F1 P2 F6 90.9(6) . . ? F1 P2 F4 179.1(6) . . ? F6 P2 F4 89.9(5) . . ? F1 P2 F5 91.1(5) . . ? F6 P2 F5 89.7(5) . . ? F4 P2 F5 89.3(4) . . ? F1 P2 F2 89.3(5) . . ? F6 P2 F2 91.6(5) . . ? F4 P2 F2 90.3(5) . . ? F5 P2 F2 178.6(6) . . ? F1 P2 F3 90.6(6) . . ? F6 P2 F3 178.5(6) . . ? F4 P2 F3 88.6(5) . . ? F5 P2 F3 90.3(5) . . ? F2 P2 F3 88.4(5) . . ? C32 O9 C33 113(3) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O9 C32 C31 103(3) . . ? O9 C32 H32A 111.1 . . ? C31 C32 H32A 111.1 . . ? O9 C32 H32B 111.1 . . ? C31 C32 H32B 111.1 . . ? H32A C32 H32B 109.0 . . ? O9 C33 C34 108(3) . . ? O9 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? O9 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 O2 P1 O1 Cu1 -13.0(17) . . . . ? O3 P1 O1 Cu1 113.3(13) . . . . ? O4A P1 O1 Cu1 -154.3(13) . . . . ? O4B P1 O1 Cu1 -120.6(13) . . . . ? N4 Cu1 O1 P1 138.1(14) . . . . ? N6 Cu1 O1 P1 -96.7(14) . . . . ? N1 Cu1 O1 P1 177(4) . . . . ? N2 Cu1 O1 P1 23.7(15) . . . . ? O2 P1 O3 C19A -55.7(13) . . . . ? O1 P1 O3 C19A 171.4(11) . . . . ? O4A P1 O3 C19A 71.3(13) . . . . ? O4B P1 O3 C19A 46.1(14) . . . . ? O2 P1 O3 C19B -29.0(17) . . . . ? O1 P1 O3 C19B -161.8(15) . . . . ? O4A P1 O3 C19B 98.1(17) . . . . ? O4B P1 O3 C19B 72.9(17) . . . . ? O1 Cu1 N1 C13 58(5) . . . . ? N4 Cu1 N1 C13 96.9(7) . . . . ? N6 Cu1 N1 C13 -29.8(7) . . . . ? N2 Cu1 N1 C13 -148.6(7) . . . . ? O1 Cu1 N1 C1 177(5) . . . . ? N4 Cu1 N1 C1 -144.0(8) . . . . ? N6 Cu1 N1 C1 89.3(7) . . . . ? N2 Cu1 N1 C1 -29.5(7) . . . . ? O1 Cu1 N1 C7 -64(5) . . . . ? N4 Cu1 N1 C7 -24.2(9) . . . . ? N6 Cu1 N1 C7 -150.9(9) . . . . ? N2 Cu1 N1 C7 90.3(8) . . . . ? O1 Cu1 N2 C2 -168.0(8) . . . . ? N4 Cu1 N2 C2 90.7(8) . . . . ? N6 Cu1 N2 C2 -59.2(9) . . . . ? N1 Cu1 N2 C2 14.6(8) . . . . ? O1 Cu1 N2 C3 17.2(14) . . . . ? N4 Cu1 N2 C3 -84.1(13) . . . . ? N6 Cu1 N2 C3 126.1(13) . . . . ? N1 Cu1 N2 C3 -160.2(13) . . . . ? O1 Cu1 N4 C8 -167.5(12) . . . . ? N6 Cu1 N4 C8 87.7(13) . . . . ? N1 Cu1 N4 C8 16.2(11) . . . . ? N2 Cu1 N4 C8 -59.5(12) . . . . ? O1 Cu1 N4 C9 3.3(18) . . . . ? N6 Cu1 N4 C9 -101.5(18) . . . . ? N1 Cu1 N4 C9 -173.0(18) . . . . ? N2 Cu1 N4 C9 111.3(17) . . . . ? O1 Cu1 N6 C14 -154.8(10) . . . . ? N4 Cu1 N6 C14 -52.7(12) . . . . ? N1 Cu1 N6 C14 19.3(9) . . . . ? N2 Cu1 N6 C14 93.3(10) . . . . ? O1 Cu1 N6 C15 25.2(19) . . . . ? N4 Cu1 N6 C15 127.3(17) . . . . ? N1 Cu1 N6 C15 -160.7(18) . . . . ? N2 Cu1 N6 C15 -86.7(19) . . . . ? C13 N1 C1 C2 157.0(10) . . . . ? C7 N1 C1 C2 -81.6(12) . . . . ? Cu1 N1 C1 C2 38.1(10) . . . . ? C3 N2 C2 N3 -1.2(12) . . . . ? Cu1 N2 C2 N3 -177.9(7) . . . . ? C3 N2 C2 C1 -178.9(10) . . . . ? Cu1 N2 C2 C1 4.3(13) . . . . ? C4 N3 C2 N2 1.1(13) . . . . ? C5 N3 C2 N2 -175.2(10) . . . . ? C4 N3 C2 C1 178.5(12) . . . . ? C5 N3 C2 C1 2.2(19) . . . . ? N1 C1 C2 N2 -28.8(14) . . . . ? N1 C1 C2 N3 154.0(11) . . . . ? C2 N2 C3 C4 0.9(13) . . . . ? Cu1 N2 C3 C4 175.8(10) . . . . ? N2 C3 C4 N3 -0.2(14) . . . . ? C2 N3 C4 C3 -0.5(14) . . . . ? C5 N3 C4 C3 175.5(12) . . . . ? C2 N3 C5 C6 177.0(12) . . . . ? C4 N3 C5 C6 2(2) . . . . ? C13 N1 C7 C8 -93.2(12) . . . . ? C1 N1 C7 C8 146.0(11) . . . . ? Cu1 N1 C7 C8 27.1(13) . . . . ? C9 N4 C8 N5 -0.4(18) . . . . ? Cu1 N4 C8 N5 173.3(10) . . . . ? C9 N4 C8 C7 -177.9(14) . . . . ? Cu1 N4 C8 C7 -4.2(19) . . . . ? C10 N5 C8 N4 -0.5(18) . . . . ? C11 N5 C8 N4 -177.5(14) . . . . ? C10 N5 C8 C7 176.9(15) . . . . ? C11 N5 C8 C7 0(2) . . . . ? N1 C7 C8 N4 -16.0(19) . . . . ? N1 C7 C8 N5 166.9(14) . . . . ? C8 N4 C9 C10 1.1(19) . . . . ? Cu1 N4 C9 C10 -170.0(13) . . . . ? N4 C9 C10 N5 -1.4(19) . . . . ? C8 N5 C10 C9 1.2(18) . . . . ? C11 N5 C10 C9 178.1(15) . . . . ? C8 N5 C11 C12 -175.3(16) . . . . ? C10 N5 C11 C12 8(3) . . . . ? C1 N1 C13 C14 -85.3(11) . . . . ? C7 N1 C13 C14 153.7(9) . . . . ? Cu1 N1 C13 C14 33.1(10) . . . . ? C15 N6 C14 N7 0.1(19) . . . . ? Cu1 N6 C14 N7 -179.9(10) . . . . ? C15 N6 C14 C13 174.9(13) . . . . ? Cu1 N6 C14 C13 -5.1(15) . . . . ? C17 N7 C14 N6 -175.0(19) . . . . ? C16 N7 C14 N6 -2.8(19) . . . . ? C17 N7 C14 C13 10(3) . . . . ? C16 N7 C14 C13 -177.3(15) . . . . ? N1 C13 C14 N6 -19.5(15) . . . . ? N1 C13 C14 N7 154.5(13) . . . . ? C14 N6 C15 C16 3(2) . . . . ? Cu1 N6 C15 C16 -177.1(15) . . . . ? N6 C15 C16 N7 -4(3) . . . . ? C14 N7 C16 C15 4(2) . . . . ? C17 N7 C16 C15 177.6(19) . . . . ? C14 N7 C17 C18 25(4) . . . . ? C16 N7 C17 C18 -146(2) . . . . ? C19B O3 C19A C20A 40(2) . . . . ? P1 O3 C19A C20A 175.8(8) . . . . ? C19B O3 C19A C24A -134(3) . . . . ? P1 O3 C19A C24A 2.3(18) . . . . ? O3 C19A C20A C21A -174.4(13) . . . . ? C24A C19A C20A C21A 0.0 . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C23A 0.0 . . . . ? C20A C21A C22A N8A 179.8(18) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? N8A C22A C23A C24A -179.8(18) . . . . ? C22A C23A C24A C19A 0.0 . . . . ? O3 C19A C24A C23A 172.8(17) . . . . ? C20A C19A C24A C23A 0.0 . . . . ? C23A C22A N8A O5A -11(3) . . . . ? C21A C22A N8A O5A 169(2) . . . . ? C23A C22A N8A O6A 170(2) . . . . ? C21A C22A N8A O6A -10(3) . . . . ? C19A O3 C19B C20B -155(3) . . . . ? P1 O3 C19B C20B 144.5(13) . . . . ? C19A O3 C19B C24B 23(2) . . . . ? P1 O3 C19B C24B -37.7(18) . . . . ? C24B C19B C20B C21B 0.0 . . . . ? O3 C19B C20B C21B 177.7(17) . . . . ? C19B C20B C21B C22B 0.0 . . . . ? C20B C21B C22B C23B 0.0 . . . . ? C20B C21B C22B N8B 179.0(16) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? N8B C22B C23B C24B -178.9(17) . . . . ? C22B C23B C24B C19B 0.0 . . . . ? C20B C19B C24B C23B 0.0 . . . . ? O3 C19B C24B C23B -178.0(14) . . . . ? C21B C22B N8B O6B -8(3) . . . . ? C23B C22B N8B O6B 171.2(18) . . . . ? C21B C22B N8B O5B 177.6(17) . . . . ? C23B C22B N8B O5B -3(3) . . . . ? C30A C25A C26A C27A 0.0 . . . . ? O4A C25A C26A C27A 179.6(18) . . . . ? C25A C26A C27A C28A 0.0 . . . . ? C26A C27A C28A C29A 0.0 . . . . ? C26A C27A C28A N9A 174.5(19) . . . . ? C27A C28A C29A C30A 0.0 . . . . ? N9A C28A C29A C30A -174.5(18) . . . . ? C28A C29A C30A C25A 0.0 . . . . ? C26A C25A C30A C29A 0.0 . . . . ? O4A C25A C30A C29A -179.6(16) . . . . ? C26A C25A O4A P1 -48(2) . . . . ? C30A C25A O4A P1 131.5(15) . . . . ? O2 P1 O4A C25A -176.1(15) . . . . ? O1 P1 O4A C25A -36.0(19) . . . . ? O3 P1 O4A C25A 68.0(18) . . . . ? O4B P1 O4A C25A -154(3) . . . . ? C29A C28A N9A O8A -11(3) . . . . ? C27A C28A N9A O8A 174.3(18) . . . . ? C29A C28A N9A O7A 178.3(19) . . . . ? C27A C28A N9A O7A 4(3) . . . . ? C30B C25B C26B C27B 0.0 . . . . ? O4B C25B C26B C27B -178.1(18) . . . . ? C25B C26B C27B C28B 0.0 . . . . ? C26B C27B C28B C29B 0.0 . . . . ? C26B C27B C28B N9B -178(2) . . . . ? C27B C28B C29B C30B 0.0 . . . . ? N9B C28B C29B C30B 177.8(19) . . . . ? C28B C29B C30B C25B 0.0 . . . . ? C26B C25B C30B C29B 0.0 . . . . ? O4B C25B C30B C29B 178.3(16) . . . . ? C26B C25B O4B P1 5(2) . . . . ? C30B C25B O4B P1 -173.6(10) . . . . ? O2 P1 O4B C25B -177.2(14) . . . . ? O1 P1 O4B C25B -51.2(17) . . . . ? O3 P1 O4B C25B 68.7(16) . . . . ? O4A P1 O4B C25B 20.8(14) . . . . ? C29B C28B N9B O7B -178(2) . . . . ? C27B C28B N9B O7B 0(3) . . . . ? C29B C28B N9B O8B 10(3) . . . . ? C27B C28B N9B O8B -172(2) . . . . ? C33 O9 C32 C31 -180(4) . . . . ? C32 O9 C33 C34 -170(3) . . . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 0.736 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.126 #===END