# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Hayley J. Clayton' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; 'Lindsay P. Harding' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; 'John P. Irvine' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; 'John C. Jeffery' ; School of Chemistry University of Bristol Cantocks Close Bristol BS8 1TS, UK ; ; T.Riis-Johannessen ; ; School of Chemistry University of Bristol Cantocks Close Bristol BS8 1TS, UK ; 'Andrew P. Laws' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; 'Craig R. Rice' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; 'Martina Whitehead' ; Department of Chemical and Biological Sciences University of Huddersfield Huddersfield HD1 3DH, UK ; _publ_contact_author_email C.R.RICE@HUD.AC.UK _publ_contact_author_name 'Craig Rice' _publ_section_title ;Metal-Specific Allosteric Activation and Deactivation of a Diamine ; data_craig25m _database_code_depnum_ccdc_archive 'CCDC 606008' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 Cd Cl2 N6 O8 S2' _chemical_formula_weight 731.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 '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 8.9198(3) _cell_length_b 11.5523(4) _cell_length_c 13.7786(5) _cell_angle_alpha 96.685(2) _cell_angle_beta 104.617(2) _cell_angle_gamma 105.987(2) _cell_volume 1294.07(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3756 _cell_measurement_theta_min 6.766 _cell_measurement_theta_max 139.708 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 10.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.498833 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9914 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 70.21 _reflns_number_total 4397 _reflns_number_gt 3826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0537P)^2^+0.6937P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4397 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Cd1 Cd 0.54352(3) 0.76254(2) 0.75540(2) 0.02458(10) Uani 1 1 d . . . N11 N 0.3473(4) 0.5943(3) 0.6516(3) 0.0258(7) Uani 1 1 d . . . C12 C 0.2497(5) 0.5304(3) 0.6972(3) 0.0261(9) Uani 1 1 d . . . S13 S 0.09794(12) 0.40589(9) 0.61569(8) 0.0304(2) Uani 1 1 d . . . C14 C 0.1735(6) 0.4432(4) 0.5167(3) 0.0317(10) Uani 1 1 d . . . C15 C 0.3045(5) 0.5450(4) 0.5482(3) 0.0292(9) Uani 1 1 d . . . C16 C 0.4006(6) 0.6091(4) 0.4853(4) 0.0345(10) Uani 1 1 d . . . N21 N 0.3868(4) 0.6706(3) 0.8545(3) 0.0231(7) Uani 1 1 d . . . C22 C 0.4157(5) 0.7186(3) 0.9544(3) 0.0242(8) Uani 1 1 d . . . C23 C 0.3182(5) 0.6546(3) 1.0102(3) 0.0256(9) Uani 1 1 d . . . N23 N 0.3201(4) 0.6978(3) 1.1073(3) 0.0297(8) Uani 1 1 d . . . C24 C 0.2036(5) 0.5387(4) 0.9590(4) 0.0284(9) Uani 1 1 d . . . C25 C 0.1773(5) 0.4942(4) 0.8591(3) 0.0265(9) Uani 1 1 d . . . C26 C 0.2702(5) 0.5649(3) 0.8068(3) 0.0241(8) Uani 1 1 d . . . C1 C 0.4656(5) 0.7717(3) 1.1894(3) 0.0268(9) Uani 1 1 d . . . C2 C 0.4148(6) 0.7923(4) 1.2861(3) 0.0343(10) Uani 1 1 d . . . C3 C 0.5947(6) 0.7059(4) 1.2051(4) 0.0359(11) Uani 1 1 d . . . N31 N 0.6274(4) 0.8744(3) 0.9234(3) 0.0233(7) Uani 1 1 d . . . C32 C 0.5510(5) 0.8386(3) 0.9928(3) 0.0233(8) Uani 1 1 d . . . C33 C 0.5995(5) 0.9148(3) 1.0903(3) 0.0242(8) Uani 1 1 d . . . N33 N 0.5289(5) 0.8922(3) 1.1659(3) 0.0293(8) Uani 1 1 d . . . C34 C 0.7249(5) 1.0291(4) 1.1088(3) 0.0260(9) Uani 1 1 d . . . C35 C 0.7979(5) 1.0625(4) 1.0359(3) 0.0267(9) Uani 1 1 d . . . C36 C 0.7469(5) 0.9814(3) 0.9421(3) 0.0254(9) Uani 1 1 d . . . N41 N 0.7600(4) 0.9283(3) 0.7692(3) 0.0248(7) Uani 1 1 d . . . C42 C 0.8149(5) 1.0051(3) 0.8576(3) 0.0245(8) Uani 1 1 d . . . S43 S 0.97282(12) 1.13336(9) 0.86297(8) 0.0303(2) Uani 1 1 d . . . C44 C 0.9607(5) 1.0780(4) 0.7394(4) 0.0331(10) Uani 1 1 d . . . C45 C 0.8417(5) 0.9682(4) 0.6995(3) 0.0284(9) Uani 1 1 d . . . C46 C 0.7938(6) 0.8917(4) 0.5957(4) 0.0341(10) Uani 1 1 d . . . Cl1 Cl 0.84393(11) 0.63171(8) 0.79600(7) 0.0276(2) Uani 1 1 d . . . O1A O 0.7050(4) 0.6393(3) 0.7184(3) 0.0501(9) Uani 1 1 d . . . O1B O 0.9899(4) 0.6965(3) 0.7751(3) 0.0458(9) Uani 1 1 d . . . O1C O 0.8312(4) 0.5041(2) 0.7901(3) 0.0363(7) Uani 1 1 d . . . O1D O 0.8418(5) 0.6851(3) 0.8944(3) 0.0469(9) Uani 1 1 d . . . Cl2 Cl 0.25237(12) 0.87420(8) 0.59127(8) 0.0309(2) Uani 1 1 d . . . O2A O 0.4053(4) 0.8879(3) 0.6666(3) 0.0416(8) Uani 1 1 d . . . O2B O 0.1367(4) 0.7639(3) 0.5925(4) 0.0763(15) Uani 1 1 d . . . O2C O 0.2764(8) 0.8686(5) 0.4938(3) 0.0898(18) Uani 1 1 d . . . O2D O 0.2022(4) 0.9786(3) 0.6170(2) 0.0358(7) Uani 1 1 d . . . H1 H 0.561(5) 0.950(4) 1.215(4) 0.024(11) Uiso 1 1 d . . . H2 H 0.151(4) 0.504(3) 0.994(3) 0.006(9) Uiso 1 1 d . . . H3 H 0.105(5) 0.423(4) 0.827(3) 0.020(10) Uiso 1 1 d . . . H4 H 0.683(7) 0.882(4) 0.565(4) 0.045(14) Uiso 1 1 d . . . H5 H 0.396(6) 0.698(5) 0.480(4) 0.044(14) Uiso 1 1 d . . . H6 H 0.359(6) 0.712(5) 1.300(4) 0.044(14) Uiso 1 1 d . . . H7 H 0.518(6) 0.624(4) 0.518(4) 0.031(12) Uiso 1 1 d . . . H8 H 0.864(6) 0.928(4) 0.560(4) 0.036(13) Uiso 1 1 d . . . H9 H 0.372(6) 0.571(4) 0.423(4) 0.036(13) Uiso 1 1 d . . . H10 H 0.757(5) 1.077(4) 1.173(3) 0.017(10) Uiso 1 1 d . . . H11 H 0.123(7) 0.394(5) 0.457(4) 0.050(15) Uiso 1 1 d . . . H12 H 0.328(6) 0.834(4) 1.275(4) 0.039(13) Uiso 1 1 d . . . H13 H 0.879(6) 1.138(5) 1.051(4) 0.040(13) Uiso 1 1 d . . . H14 H 1.027(7) 1.119(5) 0.707(4) 0.056(17) Uiso 1 1 d . . . H15 H 0.628(5) 0.695(4) 1.147(4) 0.023(11) Uiso 1 1 d . . . H16 H 0.701(7) 0.757(5) 1.264(5) 0.061(17) Uiso 1 1 d . . . H17 H 0.551(6) 0.629(4) 1.223(4) 0.036(12) Uiso 1 1 d . . . H18 H 0.506(7) 0.833(5) 1.343(4) 0.043(14) Uiso 1 1 d . . . H19 H 0.266(6) 0.649(5) 1.128(4) 0.041(15) Uiso 1 1 d . . . H20 H 0.810(6) 0.827(5) 0.602(4) 0.045(15) Uiso 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 Cd1 0.02761(16) 0.01906(15) 0.02358(15) 0.00103(10) 0.00509(12) 0.00556(11) N11 0.0323(18) 0.0170(15) 0.0256(17) -0.0010(13) 0.0044(16) 0.0101(14) C12 0.0260(19) 0.0187(18) 0.030(2) 0.0031(16) 0.0026(19) 0.0070(15) S13 0.0278(5) 0.0233(5) 0.0307(5) -0.0012(4) -0.0012(5) 0.0050(4) C14 0.036(2) 0.027(2) 0.028(2) -0.0019(18) 0.002(2) 0.0122(18) C15 0.035(2) 0.0228(19) 0.026(2) -0.0011(16) 0.0012(19) 0.0129(17) C16 0.046(3) 0.029(2) 0.024(2) 0.0020(18) 0.005(2) 0.010(2) N21 0.0240(16) 0.0169(15) 0.0256(17) 0.0013(13) 0.0049(15) 0.0058(13) C22 0.0235(19) 0.0235(19) 0.026(2) 0.0040(16) 0.0055(18) 0.0104(16) C23 0.0232(19) 0.0242(19) 0.028(2) 0.0032(17) 0.0043(18) 0.0093(16) N23 0.0281(18) 0.0280(18) 0.0286(19) 0.0034(16) 0.0077(17) 0.0037(15) C24 0.0223(19) 0.028(2) 0.036(2) 0.0107(19) 0.011(2) 0.0057(16) C25 0.0237(19) 0.0198(19) 0.032(2) 0.0007(17) 0.0049(19) 0.0059(17) C26 0.0228(18) 0.0219(19) 0.027(2) 0.0034(16) 0.0051(18) 0.0092(15) C1 0.031(2) 0.0208(18) 0.026(2) 0.0048(16) 0.0043(19) 0.0071(16) C2 0.043(3) 0.030(2) 0.025(2) 0.0062(18) 0.009(2) 0.004(2) C3 0.036(2) 0.035(2) 0.040(3) 0.016(2) 0.009(2) 0.016(2) N31 0.0241(16) 0.0214(15) 0.0250(17) 0.0042(14) 0.0057(15) 0.0095(13) C32 0.0234(19) 0.0212(19) 0.0234(19) 0.0032(16) 0.0027(17) 0.0085(15) C33 0.0255(19) 0.0233(18) 0.0252(19) 0.0081(16) 0.0050(18) 0.0107(16) N33 0.043(2) 0.0191(17) 0.0229(17) 0.0015(14) 0.0111(17) 0.0052(15) C34 0.029(2) 0.0214(19) 0.0212(19) -0.0015(16) 0.0021(18) 0.0063(16) C35 0.029(2) 0.0204(19) 0.027(2) 0.0024(16) 0.0039(19) 0.0077(17) C36 0.026(2) 0.0194(18) 0.028(2) 0.0027(16) 0.0033(18) 0.0068(16) N41 0.0229(16) 0.0227(16) 0.0276(17) 0.0059(14) 0.0065(15) 0.0060(13) C42 0.0204(18) 0.0229(19) 0.028(2) 0.0048(16) 0.0049(17) 0.0052(15) S43 0.0273(5) 0.0260(5) 0.0321(5) 0.0027(4) 0.0076(5) 0.0021(4) C44 0.033(2) 0.031(2) 0.034(2) 0.0073(19) 0.011(2) 0.0070(18) C45 0.028(2) 0.030(2) 0.031(2) 0.0071(18) 0.0104(19) 0.0131(17) C46 0.039(3) 0.032(2) 0.032(2) 0.006(2) 0.013(2) 0.010(2) Cl1 0.0275(5) 0.0221(4) 0.0281(5) 0.0007(4) 0.0024(4) 0.0068(4) O1A 0.050(2) 0.0426(18) 0.046(2) -0.0116(15) -0.0119(17) 0.0297(17) O1B 0.0402(18) 0.0312(16) 0.067(2) 0.0090(16) 0.0239(18) 0.0063(14) O1C 0.0370(16) 0.0231(14) 0.0461(19) 0.0056(13) 0.0092(15) 0.0088(12) O1D 0.062(2) 0.0389(18) 0.0350(18) -0.0011(14) 0.0189(18) 0.0085(16) Cl2 0.0336(5) 0.0273(5) 0.0277(5) 0.0013(4) 0.0019(4) 0.0117(4) O2A 0.0359(17) 0.0240(14) 0.052(2) 0.0038(14) -0.0070(16) 0.0085(13) O2B 0.0343(19) 0.036(2) 0.136(4) 0.013(2) -0.001(2) 0.0012(16) O2C 0.181(5) 0.102(3) 0.041(2) 0.029(2) 0.049(3) 0.110(4) O2D 0.0377(16) 0.0344(16) 0.0353(16) 0.0026(13) 0.0053(14) 0.0183(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N11 2.259(3) . ? Cd1 N41 2.264(3) . ? Cd1 N21 2.330(3) . ? Cd1 N31 2.342(3) . ? Cd1 O1A 2.386(3) . ? Cd1 O2A 2.398(3) . ? N11 C12 1.314(5) . ? N11 C15 1.385(5) . ? C12 C26 1.467(6) . ? C12 S13 1.716(4) . ? S13 C14 1.715(5) . ? C14 C15 1.344(6) . ? C14 H11 0.88(6) . ? C15 C16 1.485(7) . ? C16 H5 1.04(5) . ? C16 H7 0.98(5) . ? C16 H9 0.86(5) . ? N21 C26 1.331(5) . ? N21 C22 1.354(5) . ? C22 C23 1.418(6) . ? C22 C32 1.498(5) . ? C23 N23 1.367(6) . ? C23 C24 1.414(6) . ? N23 C1 1.455(5) . ? N23 H19 0.77(5) . ? C24 C25 1.349(6) . ? C24 H2 0.82(4) . ? C25 C26 1.392(6) . ? C25 H3 0.88(4) . ? C1 N33 1.459(5) . ? C1 C2 1.525(6) . ? C1 C3 1.531(6) . ? C2 H6 0.99(5) . ? C2 H12 1.00(5) . ? C2 H18 0.94(6) . ? C3 H15 0.93(5) . ? C3 H16 1.05(6) . ? C3 H17 0.95(5) . ? N31 C36 1.338(5) . ? N31 C32 1.348(5) . ? C32 C33 1.410(6) . ? C33 N33 1.362(5) . ? C33 C34 1.423(5) . ? N33 H1 0.82(5) . ? C34 C35 1.364(6) . ? C34 H10 0.92(4) . ? C35 C36 1.394(6) . ? C35 H13 0.93(5) . ? C36 C42 1.462(6) . ? N41 C42 1.312(5) . ? N41 C45 1.391(5) . ? C42 S43 1.720(4) . ? S43 C44 1.713(5) . ? C44 C45 1.356(6) . ? C44 H14 0.90(6) . ? C45 C46 1.483(6) . ? C46 H4 0.94(5) . ? C46 H8 0.93(5) . ? C46 H20 0.81(5) . ? Cl1 O1B 1.428(3) . ? Cl1 O1D 1.429(4) . ? Cl1 O1C 1.437(3) . ? Cl1 O1A 1.449(3) . ? Cl2 O2B 1.406(4) . ? Cl2 O2C 1.409(4) . ? Cl2 O2D 1.435(3) . ? Cl2 O2A 1.447(3) . ? 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 N11 Cd1 N41 146.69(13) . . ? N11 Cd1 N21 73.12(12) . . ? N41 Cd1 N21 140.18(12) . . ? N11 Cd1 N31 140.42(12) . . ? N41 Cd1 N31 72.80(12) . . ? N21 Cd1 N31 67.40(11) . . ? N11 Cd1 O1A 79.27(12) . . ? N41 Cd1 O1A 87.04(13) . . ? N21 Cd1 O1A 109.27(12) . . ? N31 Cd1 O1A 115.95(11) . . ? N11 Cd1 O2A 88.84(10) . . ? N41 Cd1 O2A 80.06(11) . . ? N21 Cd1 O2A 107.47(11) . . ? N31 Cd1 O2A 100.24(11) . . ? O1A Cd1 O2A 135.83(13) . . ? C12 N11 C15 112.3(3) . . ? C12 N11 Cd1 114.3(3) . . ? C15 N11 Cd1 133.4(3) . . ? N11 C12 C26 122.3(4) . . ? N11 C12 S13 113.3(3) . . ? C26 C12 S13 124.4(3) . . ? C14 S13 C12 89.6(2) . . ? C15 C14 S13 111.4(4) . . ? C15 C14 H11 132(4) . . ? S13 C14 H11 116(4) . . ? C14 C15 N11 113.4(4) . . ? C14 C15 C16 127.9(4) . . ? N11 C15 C16 118.7(4) . . ? C15 C16 H5 116(3) . . ? C15 C16 H7 110(3) . . ? H5 C16 H7 102(4) . . ? C15 C16 H9 114(3) . . ? H5 C16 H9 105(4) . . ? H7 C16 H9 110(4) . . ? C26 N21 C22 122.3(4) . . ? C26 N21 Cd1 115.1(3) . . ? C22 N21 Cd1 122.6(2) . . ? N21 C22 C23 119.0(4) . . ? N21 C22 C32 113.7(3) . . ? C23 C22 C32 127.2(4) . . ? N23 C23 C24 117.3(4) . . ? N23 C23 C22 125.7(4) . . ? C24 C23 C22 117.0(4) . . ? C23 N23 C1 124.9(4) . . ? C23 N23 H19 112(4) . . ? C1 N23 H19 110(4) . . ? C25 C24 C23 122.1(4) . . ? C25 C24 H2 124(3) . . ? C23 C24 H2 114(3) . . ? C24 C25 C26 118.0(4) . . ? C24 C25 H3 122(3) . . ? C26 C25 H3 120(3) . . ? N21 C26 C25 121.3(4) . . ? N21 C26 C12 114.9(3) . . ? C25 C26 C12 123.8(4) . . ? N23 C1 N33 109.7(3) . . ? N23 C1 C2 107.7(4) . . ? N33 C1 C2 107.1(3) . . ? N23 C1 C3 110.3(4) . . ? N33 C1 C3 111.0(4) . . ? C2 C1 C3 111.0(4) . . ? C1 C2 H6 110(3) . . ? C1 C2 H12 111(3) . . ? H6 C2 H12 103(4) . . ? C1 C2 H18 111(3) . . ? H6 C2 H18 108(4) . . ? H12 C2 H18 114(4) . . ? C1 C3 H15 112(3) . . ? C1 C3 H16 112(3) . . ? H15 C3 H16 105(4) . . ? C1 C3 H17 109(3) . . ? H15 C3 H17 111(4) . . ? H16 C3 H17 108(4) . . ? C36 N31 C32 122.8(4) . . ? C36 N31 Cd1 114.8(3) . . ? C32 N31 Cd1 122.2(2) . . ? N31 C32 C33 119.4(3) . . ? N31 C32 C22 114.0(4) . . ? C33 C32 C22 126.6(4) . . ? N33 C33 C32 125.5(4) . . ? N33 C33 C34 117.1(4) . . ? C32 C33 C34 117.3(4) . . ? C33 N33 C1 125.5(4) . . ? C33 N33 H1 114(3) . . ? C1 N33 H1 115(3) . . ? C35 C34 C33 121.4(4) . . ? C35 C34 H10 122(3) . . ? C33 C34 H10 116(3) . . ? C34 C35 C36 118.3(4) . . ? C34 C35 H13 119(3) . . ? C36 C35 H13 123(3) . . ? N31 C36 C35 120.8(4) . . ? N31 C36 C42 115.1(4) . . ? C35 C36 C42 124.1(3) . . ? C42 N41 C45 113.1(3) . . ? C42 N41 Cd1 114.6(3) . . ? C45 N41 Cd1 132.2(3) . . ? N41 C42 C36 122.3(3) . . ? N41 C42 S43 113.2(3) . . ? C36 C42 S43 124.4(3) . . ? C44 S43 C42 89.5(2) . . ? C45 C44 S43 112.1(4) . . ? C45 C44 H14 126(4) . . ? S43 C44 H14 122(4) . . ? C44 C45 N41 112.1(4) . . ? C44 C45 C46 128.2(4) . . ? N41 C45 C46 119.7(4) . . ? C45 C46 H4 107(3) . . ? C45 C46 H8 109(3) . . ? H4 C46 H8 114(4) . . ? C45 C46 H20 108(4) . . ? H4 C46 H20 113(5) . . ? H8 C46 H20 105(5) . . ? O1B Cl1 O1D 110.5(2) . . ? O1B Cl1 O1C 109.93(19) . . ? O1D Cl1 O1C 110.7(2) . . ? O1B Cl1 O1A 108.6(2) . . ? O1D Cl1 O1A 109.1(2) . . ? O1C Cl1 O1A 107.88(18) . . ? Cl1 O1A Cd1 121.9(2) . . ? O2B Cl2 O2C 109.3(3) . . ? O2B Cl2 O2D 111.5(2) . . ? O2C Cl2 O2D 110.5(2) . . ? O2B Cl2 O2A 108.6(2) . . ? O2C Cl2 O2A 108.8(3) . . ? O2D Cl2 O2A 108.01(18) . . ? Cl2 O2A Cd1 139.10(17) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 70.21 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.248 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.098 # Attachment 'CCDC606009.cif' data_craigum _database_code_depnum_ccdc_archive 'CCDC 606009' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H44 Cd2 Cl4 N16 O16 S4' _chemical_formula_weight 1547.79 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' S S 0.1246 0.1234 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.217(4) _cell_length_b 11.429(2) _cell_length_c 23.837(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.17(3) _cell_angle_gamma 90.00 _cell_volume 5605.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21560 _cell_measurement_theta_min 4.773 _cell_measurement_theta_max 54.990 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.883604 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'frames each covering 0.3\% in\w' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31695 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0125 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6443 _reflns_number_gt 6209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0272P)^2^+9.0361P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6443 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.005 _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 Cd1 Cd 0.520563(5) 0.669246(10) 0.855233(5) 0.01455(4) Uani 1 1 d . . . Cl1 Cl 0.61243(2) 0.44643(4) 0.956459(19) 0.02462(9) Uani 1 1 d . . . O1A O 0.56891(7) 0.54631(12) 0.94228(6) 0.0294(3) Uani 1 1 d . . . O1B O 0.67736(7) 0.48646(16) 0.96990(9) 0.0512(5) Uani 1 1 d . . . O1C O 0.59361(8) 0.36963(14) 0.90507(7) 0.0408(4) Uani 1 1 d . . . O1D O 0.60803(8) 0.38699(13) 1.00734(6) 0.0374(3) Uani 1 1 d . . . N51 N 0.50002(7) 0.77927(13) 0.93063(7) 0.0235(3) Uani 1 1 d . . . C52 C 0.47896(8) 0.81909(15) 0.96301(8) 0.0201(3) Uani 1 1 d . . . C53 C 0.45181(9) 0.87180(18) 1.00400(8) 0.0240(3) Uani 1 1 d . . . N11 N 0.62722(6) 0.72905(12) 0.88237(6) 0.0167(3) Uani 1 1 d . . . C12 C 0.66028(7) 0.65801(15) 0.86136(7) 0.0175(3) Uani 1 1 d . . . S13 S 0.741975(19) 0.68809(4) 0.88725(2) 0.02258(9) Uani 1 1 d . . . C14 C 0.73045(8) 0.80269(17) 0.92845(8) 0.0230(3) Uani 1 1 d . . . C15 C 0.66703(8) 0.81184(15) 0.92132(7) 0.0195(3) Uani 1 1 d . . . C16 C 0.64032(9) 0.89765(17) 0.95309(8) 0.0250(4) Uani 1 1 d . . . N21 N 0.56600(6) 0.55147(12) 0.79965(6) 0.0154(3) Uani 1 1 d . . . C22 C 0.63128(7) 0.56015(14) 0.82063(7) 0.0166(3) Uani 1 1 d . . . C23 C 0.66885(8) 0.47793(16) 0.80498(7) 0.0199(3) Uani 1 1 d . . . C24 C 0.63917(8) 0.38567(15) 0.76850(8) 0.0207(3) Uani 1 1 d . . . C25 C 0.57100(8) 0.37541(15) 0.74557(7) 0.0193(3) Uani 1 1 d . . . C26 C 0.53617(7) 0.46314(14) 0.76212(7) 0.0158(3) Uani 1 1 d . . . N27 N 0.54026(9) 0.28507(14) 0.70905(8) 0.0253(3) Uani 1 1 d . . . N31 N 0.41577(6) 0.60598(12) 0.83980(6) 0.0171(3) Uani 1 1 d . . . C32 C 0.37237(7) 0.68189(14) 0.80657(7) 0.0169(3) Uani 1 1 d . . . S33 S 0.29512(2) 0.65526(4) 0.80352(2) 0.02363(9) Uani 1 1 d . . . C34 C 0.32366(9) 0.53665(17) 0.84973(8) 0.0248(4) Uani 1 1 d . . . C35 C 0.38856(8) 0.52278(15) 0.86529(7) 0.0206(3) Uani 1 1 d . . . C36 C 0.42911(10) 0.43096(17) 0.90681(9) 0.0265(4) Uani 1 1 d . . . N41 N 0.44921(6) 0.78804(12) 0.77850(6) 0.0144(2) Uani 1 1 d . . . C42 C 0.38736(7) 0.77955(14) 0.77439(7) 0.0157(3) Uani 1 1 d . . . C43 C 0.34030(8) 0.86007(16) 0.74034(7) 0.0188(3) Uani 1 1 d . . . C44 C 0.35709(8) 0.94855(15) 0.71072(7) 0.0187(3) Uani 1 1 d . . . C45 C 0.42129(7) 0.95756(14) 0.71308(7) 0.0167(3) Uani 1 1 d . . . C46 C 0.46581(7) 0.87284(14) 0.74800(7) 0.0144(3) Uani 1 1 d . . . N47 N 0.43930(8) 1.04362(14) 0.68361(7) 0.0212(3) Uani 1 1 d . . . Cl2 Cl 0.380961(18) 0.07322(3) 0.860760(17) 0.01762(8) Uani 1 1 d . . . O2A O 0.44137(6) 0.03513(12) 0.85685(6) 0.0266(3) Uani 1 1 d . . . O2B O 0.39459(6) 0.13039(12) 0.91814(6) 0.0267(3) Uani 1 1 d . . . O2C O 0.34937(7) 0.15368(12) 0.81215(6) 0.0304(3) Uani 1 1 d . . . O2D O 0.33946(6) -0.02603(12) 0.85583(6) 0.0276(3) Uani 1 1 d . . . N61 N 0.31107(9) 0.16013(17) 0.60688(9) 0.0384(4) Uani 1 1 d . . . C62 C 0.27194(9) 0.22806(16) 0.58695(8) 0.0241(3) Uani 1 1 d . . . C63 C 0.22174(10) 0.31546(18) 0.56110(9) 0.0288(4) Uani 1 1 d . . . H1 H 0.4749(13) 1.042(2) 0.6826(11) 0.036(7) Uiso 1 1 d . . . H2 H 0.4331(12) 0.811(2) 1.0194(11) 0.037(6) Uiso 1 1 d . . . H3 H 0.7655(11) 0.850(2) 0.9513(10) 0.027(6) Uiso 1 1 d . . . H4 H 0.2980(10) 0.8531(18) 0.7403(9) 0.020(5) Uiso 1 1 d . . . H5 H 0.7128(11) 0.4859(19) 0.8197(10) 0.026(5) Uiso 1 1 d . . . H6 H 0.6013(12) 0.928(2) 0.9271(10) 0.029(6) Uiso 1 1 d . . . H7 H 0.4111(12) 1.083(2) 0.6612(11) 0.030(6) Uiso 1 1 d . . . H8 H 0.4207(12) 0.930(2) 0.9838(11) 0.039(6) Uiso 1 1 d . . . H9 H 0.3291(11) 1.003(2) 0.6892(11) 0.033(6) Uiso 1 1 d . . . H10 H 0.6323(11) 0.863(2) 0.9840(11) 0.033(6) Uiso 1 1 d . . . H11 H 0.2977(12) 0.491(2) 0.8633(11) 0.042(7) Uiso 1 1 d . . . H12 H 0.6621(11) 0.3309(19) 0.7580(10) 0.027(6) Uiso 1 1 d . . . H13 H 0.4589(12) 0.396(2) 0.8905(11) 0.037(6) Uiso 1 1 d . . . H14 H 0.4854(12) 0.909(2) 1.0364(11) 0.035(6) Uiso 1 1 d . . . H15 H 0.4551(12) 0.466(2) 0.9443(11) 0.038(6) Uiso 1 1 d . . . H16 H 0.6722(12) 0.959(2) 0.9706(11) 0.039(7) Uiso 1 1 d . . . H17 H 0.2434(15) 0.388(3) 0.5571(14) 0.070(10) Uiso 1 1 d . . . H18 H 0.4028(13) 0.373(2) 0.9134(11) 0.043(7) Uiso 1 1 d . . . H19 H 0.1993(16) 0.335(3) 0.5870(15) 0.069(10) Uiso 1 1 d . . . H20 H 0.5632(13) 0.237(2) 0.7017(11) 0.039(7) Uiso 1 1 d . . . H21 H 0.5037(15) 0.291(3) 0.6900(14) 0.056(9) Uiso 1 1 d . . . H22 H 0.1939(14) 0.293(3) 0.5231(14) 0.057(8) Uiso 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 Cd1 0.01044(6) 0.01740(7) 0.01575(6) 0.00003(4) 0.00486(4) 0.00044(4) Cl1 0.0237(2) 0.0260(2) 0.0239(2) 0.00717(16) 0.00865(16) 0.00571(16) O1A 0.0304(7) 0.0298(7) 0.0298(7) 0.0113(5) 0.0135(6) 0.0095(6) O1B 0.0212(7) 0.0531(11) 0.0688(12) 0.0140(9) 0.0050(7) 0.0011(7) O1C 0.0550(10) 0.0385(8) 0.0300(7) -0.0021(6) 0.0172(7) 0.0087(7) O1D 0.0619(10) 0.0266(7) 0.0273(7) 0.0106(6) 0.0208(7) 0.0115(7) N51 0.0206(7) 0.0241(7) 0.0244(7) -0.0046(6) 0.0070(6) -0.0010(6) C52 0.0151(7) 0.0218(8) 0.0208(8) -0.0029(6) 0.0039(6) -0.0018(6) C53 0.0195(8) 0.0289(9) 0.0244(8) -0.0064(7) 0.0090(7) -0.0010(7) N11 0.0142(6) 0.0193(7) 0.0150(6) 0.0022(5) 0.0038(5) -0.0006(5) C12 0.0113(7) 0.0237(8) 0.0164(7) 0.0049(6) 0.0041(6) 0.0006(6) S13 0.01064(17) 0.0323(2) 0.0231(2) 0.00128(16) 0.00446(15) -0.00046(15) C14 0.0177(8) 0.0301(9) 0.0191(8) 0.0008(7) 0.0044(6) -0.0046(7) C15 0.0180(8) 0.0235(8) 0.0149(7) 0.0013(6) 0.0039(6) -0.0040(6) C16 0.0243(9) 0.0282(9) 0.0218(8) -0.0054(7) 0.0080(7) -0.0055(7) N21 0.0133(6) 0.0173(6) 0.0165(6) 0.0035(5) 0.0067(5) 0.0019(5) C22 0.0135(7) 0.0201(8) 0.0164(7) 0.0043(6) 0.0058(6) 0.0015(6) C23 0.0137(7) 0.0273(9) 0.0190(7) 0.0046(6) 0.0066(6) 0.0045(6) C24 0.0199(8) 0.0225(8) 0.0234(8) 0.0049(6) 0.0123(6) 0.0077(6) C25 0.0211(8) 0.0184(8) 0.0211(8) 0.0017(6) 0.0112(6) 0.0019(6) C26 0.0153(8) 0.0167(7) 0.0178(7) 0.0026(6) 0.0090(6) 0.0004(6) N27 0.0234(8) 0.0225(8) 0.0348(9) -0.0076(6) 0.0166(7) 0.0005(6) N31 0.0157(6) 0.0199(7) 0.0167(6) -0.0026(5) 0.0074(5) -0.0024(5) C32 0.0116(7) 0.0237(8) 0.0159(7) -0.0047(6) 0.0058(6) -0.0027(6) S33 0.01196(18) 0.0353(2) 0.0249(2) 0.00269(17) 0.00838(16) -0.00246(16) C34 0.0200(8) 0.0318(9) 0.0244(8) 0.0019(7) 0.0104(7) -0.0053(7) C35 0.0203(8) 0.0251(8) 0.0182(7) -0.0021(6) 0.0093(6) -0.0059(6) C36 0.0275(9) 0.0251(9) 0.0290(9) 0.0051(7) 0.0131(8) -0.0016(7) N41 0.0110(6) 0.0173(6) 0.0147(6) -0.0028(5) 0.0046(5) -0.0002(5) C42 0.0112(7) 0.0206(8) 0.0151(7) -0.0039(6) 0.0047(5) -0.0009(6) C43 0.0109(7) 0.0271(8) 0.0178(7) -0.0033(6) 0.0048(6) 0.0015(6) C44 0.0127(7) 0.0232(8) 0.0179(7) -0.0005(6) 0.0033(6) 0.0044(6) C45 0.0143(7) 0.0189(7) 0.0153(7) -0.0022(6) 0.0036(6) 0.0017(6) C46 0.0109(7) 0.0171(7) 0.0143(7) -0.0022(5) 0.0038(5) -0.0004(5) N47 0.0142(7) 0.0238(7) 0.0234(7) 0.0065(6) 0.0044(6) 0.0038(6) Cl2 0.01473(17) 0.02151(19) 0.01776(17) 0.00089(14) 0.00743(14) -0.00156(14) O2A 0.0179(6) 0.0380(7) 0.0272(6) -0.0038(5) 0.0121(5) 0.0008(5) O2B 0.0218(6) 0.0357(7) 0.0231(6) -0.0078(5) 0.0092(5) -0.0008(5) O2C 0.0257(7) 0.0344(7) 0.0282(7) 0.0129(6) 0.0067(5) 0.0012(6) O2D 0.0276(7) 0.0256(7) 0.0342(7) -0.0020(5) 0.0169(6) -0.0087(5) N61 0.0322(9) 0.0407(10) 0.0414(10) 0.0144(8) 0.0129(8) 0.0126(8) C62 0.0231(8) 0.0274(9) 0.0225(8) 0.0029(7) 0.0095(7) -0.0002(7) C63 0.0262(9) 0.0299(10) 0.0270(9) 0.0001(8) 0.0062(8) 0.0071(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 Cd1 N11 2.3116(14) . ? Cd1 N31 2.3307(14) . ? Cd1 N41 2.3481(15) . ? Cd1 N21 2.3656(14) . ? Cd1 N51 2.3747(15) . ? Cd1 O1A 2.3982(14) . ? Cl1 O1D 1.4255(14) . ? Cl1 O1B 1.4297(16) . ? Cl1 O1C 1.4351(16) . ? Cl1 O1A 1.4511(14) . ? N51 C52 1.138(2) . ? C52 C53 1.458(2) . ? C53 H2 0.95(3) . ? C53 H8 0.95(3) . ? C53 H14 0.95(2) . ? N11 C12 1.314(2) . ? N11 C15 1.386(2) . ? C12 C22 1.462(2) . ? C12 S13 1.7171(17) . ? S13 C14 1.713(2) . ? C14 C15 1.358(2) . ? C14 H3 0.94(2) . ? C15 C16 1.492(3) . ? C16 H6 0.92(2) . ? C16 H10 0.91(3) . ? C16 H16 0.97(3) . ? N21 C26 1.346(2) . ? N21 C22 1.347(2) . ? C22 C23 1.398(2) . ? C23 C24 1.368(3) . ? C23 H5 0.91(2) . ? C24 C25 1.408(2) . ? C24 H12 0.90(2) . ? C25 N27 1.357(2) . ? C25 C26 1.411(2) . ? C26 C26 1.489(3) 2_656 ? N27 H20 0.81(3) . ? N27 H21 0.77(3) . ? N31 C32 1.317(2) . ? N31 C35 1.384(2) . ? C32 C42 1.462(2) . ? C32 S33 1.7172(16) . ? S33 C34 1.711(2) . ? C34 C35 1.356(2) . ? C34 H11 0.92(3) . ? C35 C36 1.490(3) . ? C36 H13 0.97(3) . ? C36 H15 0.95(3) . ? C36 H18 0.94(3) . ? N41 C42 1.3437(19) . ? N41 C46 1.344(2) . ? C42 C43 1.399(2) . ? C43 C44 1.364(2) . ? C43 H4 0.94(2) . ? C44 C45 1.410(2) . ? C44 H9 0.89(2) . ? C45 N47 1.354(2) . ? C45 C46 1.410(2) . ? C46 C46 1.486(3) 2_656 ? N47 H1 0.80(3) . ? N47 H7 0.79(2) . ? Cl2 O2C 1.4377(14) . ? Cl2 O2D 1.4384(13) . ? Cl2 O2B 1.4411(13) . ? Cl2 O2A 1.4471(13) . ? N61 C62 1.128(3) . ? C62 C63 1.450(3) . ? C63 H17 0.98(4) . ? C63 H19 0.95(3) . ? C63 H22 0.92(3) . ? 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 N11 Cd1 N31 173.37(5) . . ? N11 Cd1 N41 111.50(5) . . ? N31 Cd1 N41 73.49(5) . . ? N11 Cd1 N21 73.50(5) . . ? N31 Cd1 N21 110.31(5) . . ? N41 Cd1 N21 101.43(5) . . ? N11 Cd1 N51 95.80(5) . . ? N31 Cd1 N51 79.51(5) . . ? N41 Cd1 N51 90.99(5) . . ? N21 Cd1 N51 165.88(5) . . ? N11 Cd1 O1A 81.60(5) . . ? N31 Cd1 O1A 92.83(5) . . ? N41 Cd1 O1A 164.37(5) . . ? N21 Cd1 O1A 90.27(5) . . ? N51 Cd1 O1A 78.85(5) . . ? O1D Cl1 O1B 110.44(11) . . ? O1D Cl1 O1C 110.08(10) . . ? O1B Cl1 O1C 109.36(12) . . ? O1D Cl1 O1A 108.63(9) . . ? O1B Cl1 O1A 109.14(10) . . ? O1C Cl1 O1A 109.18(9) . . ? Cl1 O1A Cd1 134.74(8) . . ? C52 N51 Cd1 166.18(14) . . ? N51 C52 C53 179.1(2) . . ? C52 C53 H2 107.9(15) . . ? C52 C53 H8 110.9(15) . . ? H2 C53 H8 111(2) . . ? C52 C53 H14 109.5(14) . . ? H2 C53 H14 110(2) . . ? H8 C53 H14 107(2) . . ? C12 N11 C15 111.72(14) . . ? C12 N11 Cd1 111.83(11) . . ? C15 N11 Cd1 135.82(11) . . ? N11 C12 C22 123.80(14) . . ? N11 C12 S13 113.97(12) . . ? C22 C12 S13 122.22(12) . . ? C14 S13 C12 89.59(9) . . ? C15 C14 S13 111.07(14) . . ? C15 C14 H3 128.6(14) . . ? S13 C14 H3 120.3(14) . . ? C14 C15 N11 113.65(16) . . ? C14 C15 C16 125.42(16) . . ? N11 C15 C16 120.89(15) . . ? C15 C16 H6 111.1(14) . . ? C15 C16 H10 111.0(16) . . ? H6 C16 H10 107(2) . . ? C15 C16 H16 109.2(15) . . ? H6 C16 H16 111(2) . . ? H10 C16 H16 107(2) . . ? C26 N21 C22 119.54(14) . . ? C26 N21 Cd1 126.29(10) . . ? C22 N21 Cd1 112.16(10) . . ? N21 C22 C23 121.26(15) . . ? N21 C22 C12 116.47(14) . . ? C23 C22 C12 122.26(15) . . ? C24 C23 C22 119.66(15) . . ? C24 C23 H5 120.8(14) . . ? C22 C23 H5 119.5(14) . . ? C23 C24 C25 120.08(16) . . ? C23 C24 H12 121.7(14) . . ? C25 C24 H12 118.2(14) . . ? N27 C25 C24 121.31(16) . . ? N27 C25 C26 121.59(15) . . ? C24 C25 C26 117.10(15) . . ? N21 C26 C25 122.31(14) . . ? N21 C26 C26 116.53(12) . 2_656 ? C25 C26 C26 121.15(13) . 2_656 ? C25 N27 H20 116.5(18) . . ? C25 N27 H21 118(2) . . ? H20 N27 H21 123(3) . . ? C32 N31 C35 112.01(14) . . ? C32 N31 Cd1 110.59(11) . . ? C35 N31 Cd1 136.03(11) . . ? N31 C32 C42 123.96(14) . . ? N31 C32 S33 113.70(12) . . ? C42 C32 S33 122.33(12) . . ? C34 S33 C32 89.52(9) . . ? C35 C34 S33 111.49(14) . . ? C35 C34 H11 125.5(16) . . ? S33 C34 H11 123.0(16) . . ? C34 C35 N31 113.28(16) . . ? C34 C35 C36 125.33(16) . . ? N31 C35 C36 121.37(15) . . ? C35 C36 H13 110.8(14) . . ? C35 C36 H15 109.4(15) . . ? H13 C36 H15 106(2) . . ? C35 C36 H18 110.7(16) . . ? H13 C36 H18 110(2) . . ? H15 C36 H18 110(2) . . ? C42 N41 C46 119.63(13) . . ? C42 N41 Cd1 112.73(10) . . ? C46 N41 Cd1 126.58(10) . . ? N41 C42 C43 120.96(15) . . ? N41 C42 C32 116.48(14) . . ? C43 C42 C32 122.55(14) . . ? C44 C43 C42 119.84(15) . . ? C44 C43 H4 122.0(13) . . ? C42 C43 H4 118.1(13) . . ? C43 C44 C45 120.26(15) . . ? C43 C44 H9 123.0(16) . . ? C45 C44 H9 116.7(16) . . ? N47 C45 C46 121.77(15) . . ? N47 C45 C44 121.67(15) . . ? C46 C45 C44 116.56(15) . . ? N41 C46 C45 122.69(14) . . ? N41 C46 C46 116.61(12) . 2_656 ? C45 C46 C46 120.70(13) . 2_656 ? C45 N47 H1 119.3(18) . . ? C45 N47 H7 116.7(17) . . ? H1 N47 H7 122(2) . . ? O2C Cl2 O2D 109.61(9) . . ? O2C Cl2 O2B 109.80(9) . . ? O2D Cl2 O2B 109.50(8) . . ? O2C Cl2 O2A 108.85(8) . . ? O2D Cl2 O2A 109.81(8) . . ? O2B Cl2 O2A 109.25(8) . . ? N61 C62 C63 179.7(2) . . ? C62 C63 H17 107.2(19) . . ? C62 C63 H19 113.2(19) . . ? H17 C63 H19 105(3) . . ? C62 C63 H22 110.3(19) . . ? H17 C63 H22 108(3) . . ? H19 C63 H22 112(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.796 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.065 # Attachment 'CCDC660889.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 660889' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cu2(l)2)(PF6)2.3MeCN _chemical_melting_point ? _chemical_formula_moiety '[Cu2(l)2][PF6]2.3MeCN' _chemical_formula_sum 'C42 H41 Cu2 F12 N15 P2 S4' _chemical_formula_weight 1301.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1593(2) _cell_length_b 36.2844(7) _cell_length_c 12.3673(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.1370(10) _cell_angle_gamma 90.00 _cell_volume 5313.57(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6143 _cell_measurement_theta_min 4.871 _cell_measurement_theta_max 138.262 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 3.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.445475 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; The scattering contributions from two severely disordered acetonitrile molecules wew removed using the SQUEEZE function in PLATON (A. L. Spek, Acta. Cryst., 1990, A46, C-34; PLATON, A Multipurpose Crystallographic Tool; Utrecht University, Utrecht, The Netherlands, A. L. Spek, 2003). The additional 2 acetonitrile molecules expressed in the complex formula [Cu2(L)2][PF6]2.3MeCN are based on the residual electron count of 162 electrons per unit cell (ie. ca 8*MeCN). ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30844 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 70.26 _reflns_number_total 8480 _reflns_number_gt 6374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0561P)^2^+0.4941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8480 _refine_ls_number_parameters 713 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.62136(3) 0.189062(12) 0.03412(4) 0.03820(14) Uani 1 1 d . . . Cu2 Cu 0.64625(4) 0.085785(12) 0.02037(4) 0.04079(14) Uani 1 1 d . . . N11 N 0.5596(2) 0.20013(7) 0.1680(2) 0.0398(6) Uani 1 1 d . . . C12 C 0.6163(3) 0.18354(9) 0.2581(3) 0.0406(8) Uani 1 1 d . . . S13 S 0.55777(8) 0.18911(3) 0.37147(8) 0.0583(3) Uani 1 1 d . . . C14 C 0.4531(3) 0.21532(11) 0.2926(3) 0.0609(11) Uani 1 1 d . . . H1 H 0.3949 0.2261 0.3190 0.073 Uiso 1 1 calc R . . C15 C 0.4653(3) 0.21854(10) 0.1865(3) 0.0487(9) Uani 1 1 d . . . C16 C 0.3937(3) 0.23956(11) 0.0932(4) 0.0621(11) Uani 1 1 d . . . H2A H 0.3313 0.2504 0.1174 0.093 Uiso 1 1 calc R . . H3B H 0.3657 0.2232 0.0322 0.093 Uiso 1 1 calc R . . H4C H 0.4379 0.2587 0.0700 0.093 Uiso 1 1 calc R . . N21 N 0.74173(19) 0.16107(6) 0.1554(2) 0.0338(6) Uani 1 1 d . . . C22 C 0.8369(2) 0.14447(7) 0.1432(3) 0.0351(7) Uani 1 1 d . . . C23 C 0.9166(3) 0.12995(8) 0.2328(3) 0.0442(8) Uani 1 1 d . . . C24 C 0.8918(3) 0.13217(9) 0.3370(3) 0.0505(9) Uani 1 1 d . . . H5 H 0.9418 0.1223 0.3984 0.061 Uiso 1 1 calc R . . C25 C 0.7944(3) 0.14878(9) 0.3500(3) 0.0468(8) Uani 1 1 d . . . H6 H 0.7777 0.1501 0.4196 0.056 Uiso 1 1 calc R . . C26 C 0.7209(3) 0.16365(8) 0.2570(3) 0.0393(7) Uani 1 1 d . . . N27 N 1.0149(3) 0.11456(10) 0.2171(5) 0.0592(11) Uani 1 1 d . . . N31 N 0.76789(19) 0.11714(6) -0.0340(2) 0.0350(6) Uani 1 1 d . . . C32 C 0.8450(2) 0.13980(7) 0.0255(3) 0.0345(7) Uani 1 1 d . . . C33 C 0.9229(2) 0.15900(8) -0.0216(3) 0.0400(8) Uani 1 1 d . . . C34 C 0.9150(3) 0.15506(9) -0.1343(3) 0.0502(9) Uani 1 1 d . . . H7 H 0.9632 0.1682 -0.1687 0.060 Uiso 1 1 calc R . . C35 C 0.8355(3) 0.13158(9) -0.1956(3) 0.0497(9) Uani 1 1 d . . . H8 H 0.8299 0.1285 -0.2714 0.060 Uiso 1 1 calc R . . C36 C 0.7637(3) 0.11250(8) -0.1420(3) 0.0414(8) Uani 1 1 d . . . N37 N 1.0057(2) 0.18083(8) 0.0423(3) 0.0489(8) Uani 1 1 d . . . N41 N 0.6176(2) 0.06775(7) -0.1390(2) 0.0418(6) Uani 1 1 d . . . C42 C 0.6788(3) 0.08589(9) -0.1967(3) 0.0434(8) Uani 1 1 d . . . S43 S 0.64943(9) 0.07476(3) -0.33537(9) 0.0676(3) Uani 1 1 d . . . C44 C 0.5492(4) 0.04442(12) -0.3131(4) 0.0685(12) Uani 1 1 d . . . H9 H 0.5044 0.0301 -0.3684 0.082 Uiso 1 1 calc R . . C45 C 0.5431(3) 0.04378(10) -0.2063(3) 0.0538(9) Uani 1 1 d . . . C46 C 0.4681(4) 0.02038(12) -0.1543(4) 0.0721(12) Uani 1 1 d . . . H10A H 0.4049 0.0121 -0.2105 0.108 Uiso 1 1 calc R . . H11B H 0.4414 0.0346 -0.0999 0.108 Uiso 1 1 calc R . . H12C H 0.5097 -0.0005 -0.1190 0.108 Uiso 1 1 calc R . . N51 N 0.6797(2) 0.06546(7) 0.1765(2) 0.0423(6) Uani 1 1 d . . . C52 C 0.6029(3) 0.07510(9) 0.2311(3) 0.0482(9) Uani 1 1 d . . . S53 S 0.63236(11) 0.06082(3) 0.36632(9) 0.0705(3) Uani 1 1 d . . . C54 C 0.7536(4) 0.04105(11) 0.3478(4) 0.0689(12) Uani 1 1 d . . . H13 H 0.8044 0.0285 0.4031 0.083 Uiso 1 1 calc R . . C55 C 0.7672(3) 0.04574(9) 0.2429(3) 0.0549(10) Uani 1 1 d . . . C56 C 0.8604(3) 0.03182(11) 0.1946(4) 0.0706(12) Uani 1 1 d . . . H14A H 0.9260 0.0274 0.2531 0.106 Uiso 1 1 calc R . . H15B H 0.8779 0.0498 0.1441 0.106 Uiso 1 1 calc R . . H16C H 0.8376 0.0092 0.1555 0.106 Uiso 1 1 calc R . . N61 N 0.5062(2) 0.10712(7) 0.0719(2) 0.0388(6) Uani 1 1 d . . . C62 C 0.4198(3) 0.12643(8) 0.0125(3) 0.0424(8) Uani 1 1 d . . . C63 C 0.3250(3) 0.13596(10) 0.0544(4) 0.0559(10) Uani 1 1 d . . . C64 C 0.3253(3) 0.12494(11) 0.1621(4) 0.0645(12) Uani 1 1 d . . . H17 H 0.2646 0.1309 0.1929 0.077 Uiso 1 1 calc R . . C65 C 0.4141(3) 0.10542(10) 0.2231(3) 0.0562(10) Uani 1 1 d . . . H18 H 0.4142 0.0982 0.2953 0.067 Uiso 1 1 calc R . . C66 C 0.5043(3) 0.09644(9) 0.1763(3) 0.0440(8) Uani 1 1 d . . . N67 N 0.2364(3) 0.15482(12) -0.0096(5) 0.0780(13) Uani 1 1 d . . . N71 N 0.51487(19) 0.16222(6) -0.1000(2) 0.0366(6) Uani 1 1 d . . . C72 C 0.4321(2) 0.13761(8) -0.1000(3) 0.0403(8) Uani 1 1 d . . . C73 C 0.3687(3) 0.12194(10) -0.1983(3) 0.0535(9) Uani 1 1 d . . . C74 C 0.3949(4) 0.13215(10) -0.2978(4) 0.0613(11) Uani 1 1 d . . . H19 H 0.3558 0.1218 -0.3642 0.074 Uiso 1 1 calc R . . C75 C 0.4784(3) 0.15747(10) -0.2978(3) 0.0543(9) Uani 1 1 d . . . H20 H 0.4956 0.1647 -0.3642 0.065 Uiso 1 1 calc R . . C76 C 0.5367(3) 0.17214(9) -0.1984(3) 0.0413(8) Uani 1 1 d . . . N77 N 0.2846(4) 0.09711(12) -0.1959(5) 0.0759(12) Uani 1 1 d . . . N81 N 0.6781(2) 0.21290(6) -0.0910(2) 0.0356(6) Uani 1 1 d . . . C82 C 0.6290(3) 0.19866(8) -0.1874(3) 0.0387(7) Uani 1 1 d . . . S83 S 0.68521(8) 0.21328(2) -0.29589(8) 0.0511(2) Uani 1 1 d . . . C84 C 0.7798(3) 0.23958(9) -0.2054(3) 0.0469(9) Uani 1 1 d . . . H21 H 0.8346 0.2542 -0.2257 0.056 Uiso 1 1 calc R . . C85 C 0.7655(2) 0.23665(8) -0.1003(3) 0.0387(8) Uani 1 1 d . . . C86 C 0.8301(3) 0.25605(9) -0.0008(3) 0.0464(8) Uani 1 1 d . . . H22A H 0.8986 0.2658 -0.0159 0.070 Uiso 1 1 calc R . . H23B H 0.8483 0.2391 0.0603 0.070 Uiso 1 1 calc R . . H24C H 0.7855 0.2759 0.0178 0.070 Uiso 1 1 calc R . . P1 P 0.12306(7) 0.25288(3) 0.80034(9) 0.0515(2) Uani 1 1 d . . . F1A F 0.0903(2) 0.24024(7) 0.9122(2) 0.0813(7) Uani 1 1 d . . . F1B F 0.1528(2) 0.26480(7) 0.6873(2) 0.0828(8) Uani 1 1 d . . . F1C F 0.2162(2) 0.22117(7) 0.8140(2) 0.0828(8) Uani 1 1 d . . . F1D F 0.02885(19) 0.28434(6) 0.7858(2) 0.0758(7) Uani 1 1 d . . . F1E F 0.21461(19) 0.28000(7) 0.8682(2) 0.0841(8) Uani 1 1 d . . . F1F F 0.0303(2) 0.22534(7) 0.7341(2) 0.0866(8) Uani 1 1 d . . . P2 P 0.22529(10) 0.05405(3) 0.45536(10) 0.0668(3) Uani 1 1 d . . . F2A F 0.2504(3) 0.05010(8) 0.5860(2) 0.1003(9) Uani 1 1 d . A . F2B F 0.2043(3) 0.05970(9) 0.3250(3) 0.1125(11) Uani 1 1 d . A . F2C F 0.1099(11) 0.0368(5) 0.4454(14) 0.209(8) Uani 0.60 1 d P A 1 F2D F 0.2729(16) 0.0146(3) 0.4455(11) 0.143(6) Uani 0.60 1 d P A 1 F2E F 0.3426(9) 0.0732(4) 0.4683(13) 0.138(7) Uani 0.60 1 d P A 1 F2F F 0.1696(14) 0.0908(2) 0.4752(11) 0.150(6) Uani 0.60 1 d P A 1 F2G F 0.126(2) 0.0810(8) 0.4516(14) 0.204(14) Uani 0.40 1 d P A 2 F2H F 0.1441(19) 0.0207(5) 0.4370(11) 0.133(8) Uani 0.40 1 d P A 2 F2I F 0.3244(16) 0.0292(5) 0.4500(18) 0.140(8) Uani 0.40 1 d P A 2 F2J F 0.304(3) 0.0880(7) 0.4629(18) 0.184(13) Uani 0.40 1 d P A 2 N100 N -0.0310(5) 0.14381(15) 0.6131(4) 0.132(2) Uani 1 1 d . . . C101 C 0.0434(5) 0.15816(13) 0.5926(4) 0.0752(13) Uani 1 1 d . . . C102 C 0.1342(4) 0.17692(14) 0.5596(4) 0.0830(14) Uani 1 1 d . . . H10B H 0.1632 0.1617 0.5089 0.124 Uiso 1 1 calc R . . H10C H 0.1933 0.1819 0.6239 0.124 Uiso 1 1 calc R . . H10D H 0.1070 0.1997 0.5238 0.124 Uiso 1 1 calc R . . H66 H 1.005(3) 0.1844(9) 0.109(3) 0.035(10) Uiso 1 1 d . . . H65 H 1.052(4) 0.1070(13) 0.263(4) 0.070(17) Uiso 1 1 d . . . H67 H 1.025(3) 0.1988(11) 0.005(3) 0.061(12) Uiso 1 1 d . . . H61 H 0.237(4) 0.1683(13) -0.068(4) 0.085(17) Uiso 1 1 d . . . H62 H 0.272(5) 0.0911(15) -0.131(5) 0.11(2) Uiso 1 1 d . . . H64 H 1.009(4) 0.1077(12) 0.154(4) 0.065(17) Uiso 1 1 d . . . H63 H 0.264(4) 0.0870(11) -0.256(4) 0.063(14) Uiso 1 1 d . . . H60 H 0.191(4) 0.1602(13) 0.020(4) 0.081(15) Uiso 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 0.0339(2) 0.0535(3) 0.0303(3) 0.00308(19) 0.0136(2) 0.00245(17) Cu2 0.0372(2) 0.0512(3) 0.0354(4) 0.00405(19) 0.0113(2) -0.00291(18) N11 0.0345(13) 0.0533(15) 0.035(2) -0.0028(12) 0.0156(13) -0.0026(10) C12 0.0372(17) 0.0560(19) 0.032(2) -0.0037(14) 0.0149(16) -0.0118(13) S13 0.0546(5) 0.0909(7) 0.0372(7) -0.0075(4) 0.0267(5) -0.0141(4) C14 0.044(2) 0.090(3) 0.057(3) -0.016(2) 0.028(2) -0.0060(17) C15 0.0326(17) 0.068(2) 0.051(3) -0.0107(17) 0.0217(17) -0.0039(14) C16 0.0379(19) 0.082(3) 0.069(3) -0.002(2) 0.018(2) 0.0107(17) N21 0.0316(12) 0.0404(13) 0.0314(18) 0.0007(10) 0.0109(12) -0.0044(9) C22 0.0288(15) 0.0379(16) 0.037(2) 0.0032(12) 0.0051(14) -0.0013(10) C23 0.0381(17) 0.0443(18) 0.046(3) 0.0024(14) 0.0015(17) -0.0016(12) C24 0.053(2) 0.052(2) 0.037(3) 0.0104(15) -0.0087(18) -0.0006(15) C25 0.058(2) 0.053(2) 0.029(2) 0.0042(14) 0.0098(18) -0.0099(15) C26 0.0374(16) 0.0476(18) 0.033(2) 0.0008(13) 0.0083(16) -0.0076(12) N27 0.0408(19) 0.065(2) 0.065(4) 0.012(2) -0.002(2) 0.0160(14) N31 0.0319(13) 0.0410(14) 0.0340(19) 0.0020(10) 0.0113(12) 0.0032(9) C32 0.0264(14) 0.0378(16) 0.040(2) 0.0041(12) 0.0097(14) 0.0058(10) C33 0.0337(16) 0.0371(16) 0.054(3) 0.0015(13) 0.0188(16) 0.0040(11) C34 0.0463(19) 0.050(2) 0.064(3) 0.0023(16) 0.0325(19) -0.0024(14) C35 0.053(2) 0.060(2) 0.044(3) 0.0000(15) 0.0260(19) -0.0002(15) C36 0.0399(17) 0.0473(18) 0.041(3) 0.0015(14) 0.0173(16) 0.0034(12) N37 0.0421(16) 0.0482(18) 0.062(3) -0.0037(15) 0.0248(17) -0.0064(11) N41 0.0389(14) 0.0512(16) 0.0341(19) -0.0008(11) 0.0059(13) -0.0025(11) C42 0.0426(18) 0.057(2) 0.032(2) 0.0012(14) 0.0109(16) 0.0040(13) S43 0.0734(7) 0.0929(7) 0.0391(7) -0.0109(5) 0.0181(5) -0.0113(5) C44 0.070(3) 0.081(3) 0.051(3) -0.019(2) 0.006(2) -0.017(2) C45 0.052(2) 0.059(2) 0.046(3) -0.0068(16) 0.0007(19) -0.0055(15) C46 0.067(3) 0.074(3) 0.072(3) -0.007(2) 0.008(2) -0.030(2) N51 0.0477(16) 0.0408(15) 0.0346(19) 0.0071(11) 0.0014(14) -0.0051(11) C52 0.057(2) 0.0470(19) 0.039(3) 0.0034(14) 0.0086(18) -0.0166(14) S53 0.0941(8) 0.0804(7) 0.0359(7) 0.0134(5) 0.0122(6) -0.0159(6) C54 0.077(3) 0.061(2) 0.055(3) 0.0196(19) -0.012(2) -0.0083(19) C55 0.061(2) 0.0456(19) 0.049(3) 0.0105(16) -0.006(2) -0.0079(15) C56 0.059(2) 0.064(2) 0.078(4) 0.005(2) -0.006(2) 0.0126(18) N61 0.0388(14) 0.0425(14) 0.0367(19) 0.0016(11) 0.0120(13) -0.0072(10) C62 0.0364(17) 0.0456(18) 0.047(3) 0.0048(14) 0.0126(16) -0.0063(12) C63 0.0400(19) 0.058(2) 0.075(3) 0.0028(18) 0.025(2) -0.0042(14) C64 0.054(2) 0.074(3) 0.078(4) -0.004(2) 0.043(2) -0.0084(18) C65 0.061(2) 0.067(2) 0.049(3) 0.0024(17) 0.029(2) -0.0170(17) C66 0.0446(18) 0.0482(18) 0.042(2) 0.0013(14) 0.0150(17) -0.0117(13) N67 0.0438(19) 0.094(3) 0.104(4) 0.021(3) 0.032(2) 0.0197(18) N71 0.0297(12) 0.0411(14) 0.0390(19) 0.0021(11) 0.0076(12) 0.0034(9) C72 0.0298(15) 0.0471(18) 0.041(2) 0.0066(14) 0.0026(15) 0.0022(12) C73 0.0443(19) 0.054(2) 0.055(3) 0.0054(17) -0.0029(19) -0.0055(15) C74 0.069(3) 0.063(2) 0.042(3) -0.0011(17) -0.010(2) -0.0045(18) C75 0.061(2) 0.060(2) 0.037(3) 0.0080(16) 0.0034(19) 0.0039(16) C76 0.0414(18) 0.0487(18) 0.033(2) 0.0063(14) 0.0070(16) 0.0076(13) N77 0.076(3) 0.083(3) 0.059(4) 0.000(2) -0.006(2) -0.0317(19) N81 0.0331(13) 0.0440(14) 0.0334(19) 0.0060(11) 0.0154(12) 0.0040(10) C82 0.0400(17) 0.0464(17) 0.032(2) 0.0053(13) 0.0123(16) 0.0065(12) S83 0.0607(5) 0.0630(5) 0.0349(6) 0.0075(4) 0.0219(5) 0.0011(4) C84 0.0495(19) 0.051(2) 0.047(3) 0.0079(15) 0.0260(18) 0.0022(14) C85 0.0380(16) 0.0388(17) 0.044(2) 0.0052(13) 0.0200(16) 0.0053(11) C86 0.0422(18) 0.0508(19) 0.051(3) -0.0027(15) 0.0219(18) -0.0018(13) P1 0.0438(5) 0.0659(6) 0.0496(7) 0.0060(4) 0.0205(5) -0.0005(4) F1A 0.0913(18) 0.0989(18) 0.0665(19) 0.0163(13) 0.0446(15) -0.0105(13) F1B 0.0829(17) 0.1132(19) 0.0650(19) 0.0238(14) 0.0434(15) 0.0206(14) F1C 0.0808(17) 0.0948(18) 0.075(2) 0.0062(13) 0.0220(15) 0.0316(13) F1D 0.0624(14) 0.0812(16) 0.092(2) 0.0076(13) 0.0357(14) 0.0154(11) F1E 0.0575(14) 0.1078(19) 0.095(2) -0.0253(15) 0.0336(14) -0.0255(12) F1F 0.0673(15) 0.1019(19) 0.094(2) -0.0278(15) 0.0250(15) -0.0153(13) P2 0.0763(7) 0.0641(6) 0.0519(9) 0.0008(5) -0.0026(6) 0.0111(5) F2A 0.133(3) 0.110(2) 0.053(2) 0.0054(14) 0.0122(18) -0.0023(18) F2B 0.146(3) 0.122(2) 0.059(2) 0.0131(16) 0.002(2) 0.019(2) F2C 0.091(6) 0.235(16) 0.296(16) -0.114(11) 0.036(7) -0.070(8) F2D 0.280(19) 0.074(5) 0.085(6) 0.016(4) 0.063(10) 0.063(7) F2E 0.083(4) 0.234(19) 0.097(7) 0.027(9) 0.018(4) -0.048(6) F2F 0.193(12) 0.070(4) 0.172(11) -0.014(5) 0.012(8) 0.054(5) F2G 0.22(2) 0.34(3) 0.070(9) 0.091(14) 0.064(11) 0.22(2) F2H 0.187(19) 0.110(10) 0.078(8) 0.019(7) -0.022(9) -0.070(10) F2I 0.119(10) 0.151(18) 0.132(11) -0.017(12) -0.011(8) 0.078(11) F2J 0.34(3) 0.154(15) 0.067(11) -0.039(10) 0.074(18) -0.149(19) N100 0.194(6) 0.153(5) 0.074(4) -0.036(3) 0.082(4) -0.086(4) C101 0.114(4) 0.080(3) 0.036(3) -0.004(2) 0.025(3) -0.013(3) C102 0.074(3) 0.086(3) 0.093(4) -0.004(3) 0.028(3) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.009(3) . ? Cu1 N81 2.025(2) . ? Cu1 N71 2.098(3) . ? Cu1 N21 2.103(3) . ? Cu2 N51 2.020(3) . ? Cu2 N41 2.031(3) . ? Cu2 N31 2.094(2) . ? Cu2 N61 2.097(2) . ? N11 C12 1.315(4) . ? N11 C15 1.390(4) . ? C12 C26 1.465(4) . ? C12 S13 1.723(3) . ? S13 C14 1.706(4) . ? C14 C15 1.359(5) . ? C14 H1 0.9300 . ? C15 C16 1.487(5) . ? C16 H2A 0.9600 . ? C16 H3B 0.9600 . ? C16 H4C 0.9600 . ? N21 C26 1.341(4) . ? N21 C22 1.343(4) . ? C22 C23 1.399(5) . ? C22 C32 1.491(5) . ? C23 N27 1.372(5) . ? C23 C24 1.391(5) . ? C24 C25 1.370(5) . ? C24 H5 0.9300 . ? C25 C26 1.395(5) . ? C25 H6 0.9300 . ? N27 H65 0.69(5) . ? N27 H64 0.80(5) . ? N31 C36 1.335(4) . ? N31 C32 1.336(4) . ? C32 C33 1.405(4) . ? C33 N37 1.379(4) . ? C33 C34 1.383(5) . ? C34 C35 1.379(5) . ? C34 H7 0.9300 . ? C35 C36 1.395(4) . ? C35 H8 0.9300 . ? C36 C42 1.462(5) . ? N37 H66 0.84(4) . ? N37 H67 0.86(4) . ? N41 C42 1.318(4) . ? N41 C45 1.388(4) . ? C42 S43 1.719(4) . ? S43 C44 1.710(4) . ? C44 C45 1.340(6) . ? C44 H9 0.9300 . ? C45 C46 1.495(5) . ? C46 H10A 0.9600 . ? C46 H11B 0.9600 . ? C46 H12C 0.9600 . ? N51 C52 1.318(4) . ? N51 C55 1.386(4) . ? C52 C66 1.459(5) . ? C52 S53 1.709(4) . ? S53 C54 1.701(5) . ? C54 C55 1.355(6) . ? C54 H13 0.9300 . ? C55 C56 1.485(6) . ? C56 H14A 0.9600 . ? C56 H15B 0.9600 . ? C56 H16C 0.9600 . ? N61 C62 1.336(4) . ? N61 C66 1.353(4) . ? C62 C63 1.409(4) . ? C62 C72 1.490(5) . ? C63 N67 1.367(5) . ? C63 C64 1.390(6) . ? C64 C65 1.366(6) . ? C64 H17 0.9300 . ? C65 C66 1.390(5) . ? C65 H18 0.9300 . ? N67 H61 0.87(5) . ? N67 H60 0.76(5) . ? N71 C72 1.345(4) . ? N71 C76 1.351(4) . ? C72 C73 1.403(5) . ? C73 N77 1.368(5) . ? C73 C74 1.390(6) . ? C74 C75 1.369(5) . ? C74 H19 0.9300 . ? C75 C76 1.380(5) . ? C75 H20 0.9300 . ? C76 C82 1.461(4) . ? N77 H62 0.87(6) . ? N77 H63 0.82(5) . ? N81 C82 1.312(4) . ? N81 C85 1.394(4) . ? C82 S83 1.722(3) . ? S83 C84 1.703(4) . ? C84 C85 1.354(5) . ? C84 H21 0.9300 . ? C85 C86 1.479(5) . ? C86 H22A 0.9600 . ? C86 H23B 0.9600 . ? C86 H24C 0.9600 . ? P1 F1E 1.577(3) . ? P1 F1B 1.581(2) . ? P1 F1F 1.588(3) . ? P1 F1A 1.592(2) . ? P1 F1C 1.596(2) . ? P1 F1D 1.598(2) . ? P2 F2C 1.515(11) . ? P2 F2I 1.518(15) . ? P2 F2F 1.539(9) . ? P2 F2G 1.542(15) . ? P2 F2H 1.546(14) . ? P2 F2J 1.547(18) . ? P2 F2D 1.559(10) . ? P2 F2E 1.561(10) . ? P2 F2A 1.581(3) . ? P2 F2B 1.588(3) . ? N100 C101 1.122(6) . ? C101 C102 1.433(6) . ? C102 H10B 0.9600 . ? C102 H10C 0.9600 . ? C102 H10D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cu1 N81 143.19(10) . . ? N11 Cu1 N71 117.75(10) . . ? N81 Cu1 N71 81.38(10) . . ? N11 Cu1 N21 80.73(10) . . ? N81 Cu1 N21 116.62(9) . . ? N71 Cu1 N21 122.95(9) . . ? N51 Cu2 N41 139.75(11) . . ? N51 Cu2 N31 120.11(11) . . ? N41 Cu2 N31 80.85(10) . . ? N51 Cu2 N61 81.10(11) . . ? N41 Cu2 N61 116.24(11) . . ? N31 Cu2 N61 125.35(9) . . ? C12 N11 C15 112.0(3) . . ? C12 N11 Cu1 112.6(2) . . ? C15 N11 Cu1 135.1(3) . . ? N11 C12 C26 120.5(3) . . ? N11 C12 S13 113.6(2) . . ? C26 C12 S13 125.8(3) . . ? C14 S13 C12 89.56(17) . . ? C15 C14 S13 111.7(3) . . ? C15 C14 H1 124.2 . . ? S13 C14 H1 124.2 . . ? C14 C15 N11 113.1(3) . . ? C14 C15 C16 128.3(3) . . ? N11 C15 C16 118.6(3) . . ? C15 C16 H2A 109.5 . . ? C15 C16 H3B 109.5 . . ? H2A C16 H3B 109.5 . . ? C15 C16 H4C 109.5 . . ? H2A C16 H4C 109.5 . . ? H3B C16 H4C 109.5 . . ? C26 N21 C22 119.2(3) . . ? C26 N21 Cu1 112.67(19) . . ? C22 N21 Cu1 127.9(2) . . ? N21 C22 C23 122.7(3) . . ? N21 C22 C32 114.2(3) . . ? C23 C22 C32 122.9(3) . . ? N27 C23 C24 122.3(4) . . ? N27 C23 C22 120.7(4) . . ? C24 C23 C22 117.1(3) . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H5 119.7 . . ? C23 C24 H5 119.7 . . ? C24 C25 C26 118.8(3) . . ? C24 C25 H6 120.6 . . ? C26 C25 H6 120.6 . . ? N21 C26 C25 121.6(3) . . ? N21 C26 C12 113.1(3) . . ? C25 C26 C12 125.3(3) . . ? C23 N27 H65 118(4) . . ? C23 N27 H64 112(3) . . ? H65 N27 H64 125(5) . . ? C36 N31 C32 119.4(3) . . ? C36 N31 Cu2 112.6(2) . . ? C32 N31 Cu2 128.0(2) . . ? N31 C32 C33 122.1(3) . . ? N31 C32 C22 114.5(2) . . ? C33 C32 C22 123.3(3) . . ? N37 C33 C34 120.8(3) . . ? N37 C33 C32 121.3(3) . . ? C34 C33 C32 117.9(3) . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H7 120.1 . . ? C33 C34 H7 120.1 . . ? C34 C35 C36 118.8(3) . . ? C34 C35 H8 120.6 . . ? C36 C35 H8 120.6 . . ? N31 C36 C35 121.9(3) . . ? N31 C36 C42 114.1(3) . . ? C35 C36 C42 124.1(3) . . ? C33 N37 H66 119(2) . . ? C33 N37 H67 113(3) . . ? H66 N37 H67 118(4) . . ? C42 N41 C45 111.1(3) . . ? C42 N41 Cu2 111.8(2) . . ? C45 N41 Cu2 136.7(2) . . ? N41 C42 C36 120.4(3) . . ? N41 C42 S43 114.0(3) . . ? C36 C42 S43 125.6(3) . . ? C44 S43 C42 89.13(19) . . ? C45 C44 S43 111.8(3) . . ? C45 C44 H9 124.1 . . ? S43 C44 H9 124.1 . . ? C44 C45 N41 113.9(3) . . ? C44 C45 C46 127.6(4) . . ? N41 C45 C46 118.5(4) . . ? C45 C46 H10A 109.5 . . ? C45 C46 H11B 109.5 . . ? H10A C46 H11B 109.5 . . ? C45 C46 H12C 109.5 . . ? H10A C46 H12C 109.5 . . ? H11B C46 H12C 109.5 . . ? C52 N51 C55 111.8(3) . . ? C52 N51 Cu2 112.4(2) . . ? C55 N51 Cu2 135.7(3) . . ? N51 C52 C66 120.4(3) . . ? N51 C52 S53 113.9(3) . . ? C66 C52 S53 125.7(3) . . ? C54 S53 C52 89.5(2) . . ? C55 C54 S53 112.0(3) . . ? C55 C54 H13 124.0 . . ? S53 C54 H13 124.0 . . ? C54 C55 N51 112.8(4) . . ? C54 C55 C56 127.8(4) . . ? N51 C55 C56 119.4(4) . . ? C55 C56 H14A 109.5 . . ? C55 C56 H15B 109.5 . . ? H14A C56 H15B 109.5 . . ? C55 C56 H16C 109.5 . . ? H14A C56 H16C 109.5 . . ? H15B C56 H16C 109.5 . . ? C62 N61 C66 119.5(3) . . ? C62 N61 Cu2 128.2(2) . . ? C66 N61 Cu2 112.1(2) . . ? N61 C62 C63 122.2(3) . . ? N61 C62 C72 115.0(3) . . ? C63 C62 C72 122.8(3) . . ? N67 C63 C64 121.9(4) . . ? N67 C63 C62 120.9(4) . . ? C64 C63 C62 117.2(3) . . ? C65 C64 C63 120.5(3) . . ? C65 C64 H17 119.8 . . ? C63 C64 H17 119.8 . . ? C64 C65 C66 119.4(4) . . ? C64 C65 H18 120.3 . . ? C66 C65 H18 120.3 . . ? N61 C66 C65 121.1(3) . . ? N61 C66 C52 113.9(3) . . ? C65 C66 C52 125.0(3) . . ? C63 N67 H61 128(3) . . ? C63 N67 H60 115(4) . . ? H61 N67 H60 113(5) . . ? C72 N71 C76 118.5(3) . . ? C72 N71 Cu1 129.4(2) . . ? C76 N71 Cu1 112.1(2) . . ? N71 C72 C73 122.2(3) . . ? N71 C72 C62 114.5(3) . . ? C73 C72 C62 123.1(3) . . ? N77 C73 C74 121.2(4) . . ? N77 C73 C72 120.9(4) . . ? C74 C73 C72 117.9(3) . . ? C75 C74 C73 119.9(4) . . ? C75 C74 H19 120.1 . . ? C73 C74 H19 120.1 . . ? C74 C75 C76 119.3(4) . . ? C74 C75 H20 120.3 . . ? C76 C75 H20 120.3 . . ? N71 C76 C75 122.2(3) . . ? N71 C76 C82 113.3(3) . . ? C75 C76 C82 124.4(3) . . ? C73 N77 H62 118(4) . . ? C73 N77 H63 110(3) . . ? H62 N77 H63 130(5) . . ? C82 N81 C85 111.5(3) . . ? C82 N81 Cu1 111.3(2) . . ? C85 N81 Cu1 136.5(2) . . ? N81 C82 C76 121.6(3) . . ? N81 C82 S83 114.1(2) . . ? C76 C82 S83 124.3(3) . . ? C84 S83 C82 89.37(16) . . ? C85 C84 S83 111.8(2) . . ? C85 C84 H21 124.1 . . ? S83 C84 H21 124.1 . . ? C84 C85 N81 113.2(3) . . ? C84 C85 C86 127.0(3) . . ? N81 C85 C86 119.8(3) . . ? C85 C86 H22A 109.5 . . ? C85 C86 H23B 109.5 . . ? H22A C86 H23B 109.5 . . ? C85 C86 H24C 109.5 . . ? H22A C86 H24C 109.5 . . ? H23B C86 H24C 109.5 . . ? F1E P1 F1B 91.37(15) . . ? F1E P1 F1F 178.97(16) . . ? F1B P1 F1F 89.66(16) . . ? F1E P1 F1A 90.19(15) . . ? F1B P1 F1A 178.43(17) . . ? F1F P1 F1A 88.78(15) . . ? F1E P1 F1C 89.73(15) . . ? F1B P1 F1C 89.53(14) . . ? F1F P1 F1C 90.28(15) . . ? F1A P1 F1C 90.69(14) . . ? F1E P1 F1D 90.88(14) . . ? F1B P1 F1D 90.42(13) . . ? F1F P1 F1D 89.12(14) . . ? F1A P1 F1D 89.35(14) . . ? F1C P1 F1D 179.39(17) . . ? F2C P2 F2I 118.8(9) . . ? F2C P2 F2F 86.4(8) . . ? F2I P2 F2F 154.5(10) . . ? F2C P2 F2G 63.8(11) . . ? F2I P2 F2G 175.0(11) . . ? F2F P2 F2G 24.2(14) . . ? F2C P2 F2H 27.9(10) . . ? F2I P2 F2H 90.9(9) . . ? F2F P2 F2H 114.3(11) . . ? F2G P2 F2H 91.4(13) . . ? F2C P2 F2J 151.6(13) . . ? F2I P2 F2J 89.5(12) . . ? F2F P2 F2J 65.7(11) . . ? F2G P2 F2J 87.8(15) . . ? F2H P2 F2J 175.1(10) . . ? F2C P2 F2D 88.2(7) . . ? F2I P2 F2D 30.6(8) . . ? F2F P2 F2D 172.6(8) . . ? F2G P2 F2D 151.7(13) . . ? F2H P2 F2D 60.4(8) . . ? F2J P2 F2D 120.1(13) . . ? F2C P2 F2E 177.7(9) . . ? F2I P2 F2E 63.4(9) . . ? F2F P2 F2E 91.4(8) . . ? F2G P2 F2E 114.2(14) . . ? F2H P2 F2E 154.3(11) . . ? F2J P2 F2E 26.4(14) . . ? F2D P2 F2E 94.0(8) . . ? F2C P2 F2A 90.3(7) . . ? F2I P2 F2A 91.1(8) . . ? F2F P2 F2A 84.6(5) . . ? F2G P2 F2A 93.2(6) . . ? F2H P2 F2A 92.7(5) . . ? F2J P2 F2A 92.1(8) . . ? F2D P2 F2A 90.4(5) . . ? F2E P2 F2A 88.6(6) . . ? F2C P2 F2B 92.2(7) . . ? F2I P2 F2B 88.8(8) . . ? F2F P2 F2B 94.3(5) . . ? F2G P2 F2B 86.8(6) . . ? F2H P2 F2B 90.1(5) . . ? F2J P2 F2B 85.0(8) . . ? F2D P2 F2B 90.9(5) . . ? F2E P2 F2B 88.8(6) . . ? F2A P2 F2B 177.2(2) . . ? N100 C101 C102 176.4(6) . . ? C101 C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10B C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 70.26 _diffrn_measured_fraction_theta_full 0.837 _refine_diff_density_max 0.407 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.055