Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Dr. Malcolm A. Halcrow' _publ_contact_author_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 3436506' _publ_contact_author_fax '+44 (0)113 3436565' _publ_contact_author_email malcolmh@leeds.ac.uk _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Copper(II) complexes of thioether-substituted salcyen and salcyan derivatives and their silver(I) adducts ; loop_ _publ_author_name _publ_author_address 'Isabelle Sylvestre' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Joanna Wolowska' ; CW EPR Service Centre. Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Eric J.L. McInnes' ; CW EPR Service Centre. Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #================================================================= data_islh _database_code_depnum_ccdc_archive 'CCDC 270588' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-bis(2-hydroxy-5-tert-butylbenzylidene)-trans- 1,2-dicyclohexylamino]copper(II) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H36 Cu N2 O2, H2 O' _chemical_formula_sum 'C28 H38 Cu N2 O3' _chemical_formula_weight 514.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.4650(1) _cell_length_b 11.0662(2) _cell_length_c 11.2949(2) _cell_angle_alpha 91.5998(8) _cell_angle_beta 98.6155(8) _cell_angle_gamma 97.9804(6) _cell_volume 1279.17(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26629 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.43 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26629 _diffrn_reflns_av_R_equivalents 0.1593 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5804 _reflns_number_gt 5166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. No disorder was detected during refinement. All non-H atoms were refined anisotropically, while all C-bound H atoms were placed in calculated positions and refined using a riding model. The water H atoms H34A and H34B were located in the difference map, and refined with a comnmon thermal parameter subject to the refined restraints O-H = 0.72(1)\%A and H...H = 1.18(2)\%A. The highest residual electron peak (0.9 e.\%A^-3^) and hole (-1.0 e.\%A^-3^) both lie <=1.0 \%A from Cu1. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.2969P] 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 5804 _refine_ls_number_parameters 321 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.26245(2) 0.48448(2) 0.01171(2) 0.02808(13) Uani 1 1 d . . . H34A H 0.240(4) 0.190(4) 0.090(3) 0.086(11) Uiso 1 1 d D . . H34B H 0.330(4) 0.218(3) 0.166(4) 0.086(11) Uiso 1 1 d D . . C2 C 0.1784(2) 0.69159(19) -0.0993(2) 0.0296(4) Uani 1 1 d . . . H2 H 0.1634 0.7298 -0.0223 0.036 Uiso 1 1 calc R . . C3 C 0.1081(2) 0.7570(2) -0.2010(2) 0.0376(5) Uani 1 1 d . . . H3A H 0.0138 0.7481 -0.1956 0.045 Uiso 1 1 calc R . . H3B H 0.1183 0.7195 -0.2791 0.045 Uiso 1 1 calc R . . C4 C 0.1647(2) 0.8924(2) -0.1933(3) 0.0427(6) Uani 1 1 d . . . H4A H 0.1218 0.9329 -0.2623 0.051 Uiso 1 1 calc R . . H4B H 0.1463 0.9314 -0.1189 0.051 Uiso 1 1 calc R . . C5 C 0.3117(2) 0.9098(2) -0.1937(2) 0.0430(6) Uani 1 1 d . . . H5A H 0.3459 0.9981 -0.1858 0.052 Uiso 1 1 calc R . . H5B H 0.3295 0.8771 -0.2711 0.052 Uiso 1 1 calc R . . C6 C 0.3826(2) 0.8447(2) -0.0908(2) 0.0373(5) Uani 1 1 d . . . H6A H 0.4772 0.8545 -0.0954 0.045 Uiso 1 1 calc R . . H6B H 0.3714 0.8819 -0.0129 0.045 Uiso 1 1 calc R . . C7 C 0.3269(2) 0.7085(2) -0.0991(2) 0.0308(4) Uani 1 1 d . . . H7 H 0.3441 0.6714 -0.1759 0.037 Uiso 1 1 calc R . . N8 N 0.13721(17) 0.55895(16) -0.09633(17) 0.0287(4) Uani 1 1 d . . . C9 C 0.0288(2) 0.50448(19) -0.15602(19) 0.0287(4) Uani 1 1 d . . . H9 H -0.0254 0.5530 -0.2030 0.034 Uiso 1 1 calc R . . C10 C -0.0163(2) 0.3749(2) -0.1566(2) 0.0285(4) Uani 1 1 d . . . C11 C 0.0512(2) 0.2934(2) -0.08523(19) 0.0291(4) Uani 1 1 d . . . C12 C -0.0021(2) 0.1689(2) -0.0981(2) 0.0305(4) Uani 1 1 d . . . H12 H 0.0398 0.1121 -0.0504 0.037 Uiso 1 1 calc R . . C13 C -0.1141(2) 0.1270(2) -0.1784(2) 0.0303(4) Uani 1 1 d . . . H13 H -0.1465 0.0421 -0.1847 0.036 Uiso 1 1 calc R . . C14 C -0.18131(19) 0.2068(2) -0.25126(19) 0.0289(4) Uani 1 1 d . . . C15 C -0.1317(2) 0.3294(2) -0.2365(2) 0.0292(4) Uani 1 1 d . . . H15 H -0.1769 0.3857 -0.2819 0.035 Uiso 1 1 calc R . . O16 O 0.15809(15) 0.32755(14) -0.00686(15) 0.0340(3) Uani 1 1 d . . . C17 C -0.2993(2) 0.1547(2) -0.3452(2) 0.0307(4) Uani 1 1 d . . . C18 C -0.4056(2) 0.0844(2) -0.2833(2) 0.0404(5) Uani 1 1 d . . . H18A H -0.4326 0.1395 -0.2253 0.061 Uiso 1 1 calc R . . H18B H -0.3712 0.0166 -0.2415 0.061 Uiso 1 1 calc R . . H18C H -0.4811 0.0523 -0.3435 0.061 Uiso 1 1 calc R . . C19 C -0.3573(2) 0.2541(2) -0.4173(2) 0.0386(5) Uani 1 1 d . . . H19A H -0.4302 0.2165 -0.4776 0.058 Uiso 1 1 calc R . . H19B H -0.2901 0.2996 -0.4572 0.058 Uiso 1 1 calc R . . H19C H -0.3889 0.3101 -0.3633 0.058 Uiso 1 1 calc R . . C20 C -0.2545(2) 0.0674(2) -0.4327(2) 0.0424(6) Uani 1 1 d . . . H20A H -0.3302 0.0280 -0.4890 0.064 Uiso 1 1 calc R . . H20B H -0.2127 0.0050 -0.3880 0.064 Uiso 1 1 calc R . . H20C H -0.1919 0.1134 -0.4772 0.064 Uiso 1 1 calc R . . N21 N 0.37827(17) 0.63615(17) 0.00084(17) 0.0295(4) Uani 1 1 d . . . C22 C 0.4876(2) 0.6714(2) 0.0692(2) 0.0298(4) Uani 1 1 d . . . H22 H 0.5397 0.7430 0.0492 0.036 Uiso 1 1 calc R . . C23 C 0.5373(2) 0.6104(2) 0.1740(2) 0.0283(4) Uani 1 1 d . . . C24 C 0.4735(2) 0.4982(2) 0.2087(2) 0.0296(4) Uani 1 1 d . . . C25 C 0.5263(2) 0.4559(2) 0.3199(2) 0.0319(4) Uani 1 1 d . . . H25 H 0.4881 0.3799 0.3451 0.038 Uiso 1 1 calc R . . C26 C 0.6317(2) 0.5221(2) 0.3927(2) 0.0316(4) Uani 1 1 d . . . H26 H 0.6625 0.4911 0.4676 0.038 Uiso 1 1 calc R . . C27 C 0.69565(19) 0.63416(19) 0.3599(2) 0.0285(4) Uani 1 1 d . . . C28 C 0.6480(2) 0.6743(2) 0.2501(2) 0.0290(4) Uani 1 1 d . . . H28 H 0.6910 0.7478 0.2240 0.035 Uiso 1 1 calc R . . O29 O 0.37006(15) 0.43189(14) 0.14580(15) 0.0339(3) Uani 1 1 d . . . C30 C 0.8104(2) 0.7038(2) 0.4471(2) 0.0300(4) Uani 1 1 d . . . C31 C 0.7652(2) 0.7299(2) 0.5675(2) 0.0357(5) Uani 1 1 d . . . H31A H 0.8376 0.7769 0.6223 0.054 Uiso 1 1 calc R . . H31B H 0.7370 0.6525 0.6025 0.054 Uiso 1 1 calc R . . H31C H 0.6920 0.7770 0.5543 0.054 Uiso 1 1 calc R . . C32 C 0.9201(2) 0.6251(2) 0.4682(2) 0.0382(5) Uani 1 1 d . . . H32A H 0.9452 0.6028 0.3912 0.057 Uiso 1 1 calc R . . H32B H 0.8897 0.5507 0.5071 0.057 Uiso 1 1 calc R . . H32C H 0.9958 0.6712 0.5198 0.057 Uiso 1 1 calc R . . C33 C 0.8633(2) 0.8253(2) 0.3986(2) 0.0366(5) Uani 1 1 d . . . H33A H 0.9306 0.8707 0.4597 0.055 Uiso 1 1 calc R . . H33B H 0.7919 0.8736 0.3787 0.055 Uiso 1 1 calc R . . H33C H 0.9013 0.8096 0.3265 0.055 Uiso 1 1 calc R . . O34 O 0.2814(3) 0.1679(2) 0.1394(3) 0.0638(7) Uani 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 Cu1 0.02768(17) 0.02282(17) 0.03180(19) 0.00593(11) -0.00137(11) 0.00245(11) C2 0.0305(10) 0.0227(10) 0.0345(11) 0.0067(8) 0.0006(8) 0.0039(7) C3 0.0325(11) 0.0304(11) 0.0462(13) 0.0113(10) -0.0058(9) 0.0025(8) C4 0.0389(12) 0.0293(12) 0.0574(16) 0.0171(11) -0.0023(11) 0.0031(9) C5 0.0390(12) 0.0364(13) 0.0507(15) 0.0199(11) 0.0012(10) -0.0018(9) C6 0.0324(11) 0.0349(12) 0.0419(13) 0.0139(10) 0.0002(9) -0.0016(9) C7 0.0304(10) 0.0305(11) 0.0314(11) 0.0083(8) 0.0025(8) 0.0050(8) N8 0.0291(8) 0.0228(9) 0.0325(9) 0.0041(7) 0.0003(7) 0.0028(6) C9 0.0294(10) 0.0251(10) 0.0314(11) 0.0048(8) 0.0014(8) 0.0062(8) C10 0.0281(10) 0.0243(10) 0.0319(11) 0.0025(8) 0.0015(8) 0.0028(8) C11 0.0275(9) 0.0274(10) 0.0318(11) 0.0044(8) 0.0023(8) 0.0038(8) C12 0.0308(10) 0.0249(10) 0.0356(11) 0.0056(8) 0.0013(8) 0.0065(8) C13 0.0311(10) 0.0236(10) 0.0350(11) 0.0033(8) 0.0027(8) 0.0020(8) C14 0.0266(9) 0.0276(10) 0.0313(11) 0.0019(8) 0.0016(8) 0.0025(7) C15 0.0281(10) 0.0264(10) 0.0326(11) 0.0065(8) 0.0004(8) 0.0054(8) O16 0.0346(8) 0.0257(8) 0.0374(9) 0.0062(6) -0.0061(6) 0.0018(6) C17 0.0293(10) 0.0245(10) 0.0357(11) 0.0032(8) -0.0022(8) 0.0020(8) C18 0.0310(11) 0.0398(13) 0.0467(14) 0.0103(10) -0.0012(10) -0.0020(9) C19 0.0376(12) 0.0320(12) 0.0423(13) 0.0076(10) -0.0062(10) 0.0042(9) C20 0.0383(12) 0.0402(13) 0.0451(14) -0.0073(11) -0.0052(10) 0.0077(10) N21 0.0302(9) 0.0268(9) 0.0304(9) 0.0057(7) 0.0004(7) 0.0041(7) C22 0.0294(10) 0.0272(10) 0.0325(11) 0.0058(8) 0.0037(8) 0.0032(8) C23 0.0266(9) 0.0273(10) 0.0309(10) 0.0061(8) 0.0010(8) 0.0061(8) C24 0.0274(9) 0.0266(10) 0.0340(11) 0.0038(8) 0.0013(8) 0.0047(8) C25 0.0325(10) 0.0250(10) 0.0371(11) 0.0079(9) 0.0013(9) 0.0036(8) C26 0.0316(10) 0.0304(11) 0.0321(11) 0.0067(9) -0.0009(8) 0.0077(8) C27 0.0244(9) 0.0275(10) 0.0336(11) 0.0027(8) 0.0010(8) 0.0069(7) C28 0.0258(9) 0.0267(10) 0.0338(11) 0.0050(8) 0.0033(8) 0.0024(8) O29 0.0328(8) 0.0248(7) 0.0397(9) 0.0089(6) -0.0065(6) 0.0004(6) C30 0.0265(9) 0.0299(11) 0.0321(11) 0.0045(8) -0.0002(8) 0.0033(8) C31 0.0352(11) 0.0370(12) 0.0342(12) 0.0016(9) 0.0030(9) 0.0052(9) C32 0.0309(10) 0.0451(13) 0.0378(12) 0.0046(10) -0.0018(9) 0.0102(9) C33 0.0333(11) 0.0356(12) 0.0378(12) 0.0039(10) 0.0003(9) -0.0010(9) O34 0.0697(15) 0.0348(11) 0.0767(17) 0.0179(10) -0.0210(12) 0.0033(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O29 1.9028(16) . ? Cu1 O16 1.9070(15) . ? Cu1 N8 1.9398(18) . ? Cu1 N21 1.9475(18) . ? C2 N8 1.474(3) . ? C2 C3 1.525(3) . ? C2 C7 1.539(3) . ? C3 C4 1.528(3) . ? C4 C5 1.524(3) . ? C5 C6 1.535(3) . ? C6 C7 1.534(3) . ? C7 N21 1.480(3) . ? N8 C9 1.290(3) . ? C9 C10 1.446(3) . ? C10 C15 1.416(3) . ? C10 C11 1.417(3) . ? C11 O16 1.321(3) . ? C11 C12 1.408(3) . ? C12 C13 1.385(3) . ? C13 C14 1.411(3) . ? C14 C15 1.380(3) . ? C14 C17 1.535(3) . ? C17 C19 1.526(3) . ? C17 C20 1.530(3) . ? C17 C18 1.535(3) . ? N21 C22 1.285(3) . ? C22 C23 1.444(3) . ? C23 C24 1.420(3) . ? C23 C28 1.422(3) . ? C24 O29 1.317(3) . ? C24 C25 1.413(3) . ? C25 C26 1.378(3) . ? C26 C27 1.412(3) . ? C27 C28 1.375(3) . ? C27 C30 1.533(3) . ? C30 C33 1.530(3) . ? C30 C32 1.530(3) . ? C30 C31 1.538(3) . ? O34 H34A 0.72(3) . ? O34 H34B 0.72(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 O29 Cu1 O16 90.01(7) . . ? O29 Cu1 N8 166.55(8) . . ? O16 Cu1 N8 93.57(7) . . ? O29 Cu1 N21 94.48(7) . . ? O16 Cu1 N21 168.88(7) . . ? N8 Cu1 N21 84.40(7) . . ? N8 C2 C3 116.68(18) . . ? N8 C2 C7 105.96(17) . . ? C3 C2 C7 111.89(18) . . ? C2 C3 C4 110.13(19) . . ? C5 C4 C3 111.2(2) . . ? C4 C5 C6 111.55(19) . . ? C7 C6 C5 109.86(19) . . ? N21 C7 C6 115.76(18) . . ? N21 C7 C2 104.73(16) . . ? C6 C7 C2 110.43(18) . . ? C9 N8 C2 122.41(18) . . ? C9 N8 Cu1 126.50(15) . . ? C2 N8 Cu1 111.04(13) . . ? N8 C9 C10 124.7(2) . . ? C15 C10 C11 119.82(19) . . ? C15 C10 C9 116.8(2) . . ? C11 C10 C9 123.4(2) . . ? O16 C11 C12 118.81(19) . . ? O16 C11 C10 124.15(19) . . ? C12 C11 C10 117.03(19) . . ? C13 C12 C11 121.8(2) . . ? C12 C13 C14 121.8(2) . . ? C15 C14 C13 116.66(19) . . ? C15 C14 C17 123.5(2) . . ? C13 C14 C17 119.78(19) . . ? C14 C15 C10 122.8(2) . . ? C11 O16 Cu1 126.86(14) . . ? C19 C17 C20 107.9(2) . . ? C19 C17 C18 108.82(19) . . ? C20 C17 C18 109.31(19) . . ? C19 C17 C14 112.39(18) . . ? C20 C17 C14 108.51(17) . . ? C18 C17 C14 109.84(19) . . ? C22 N21 C7 122.48(18) . . ? C22 N21 Cu1 125.69(16) . . ? C7 N21 Cu1 111.82(13) . . ? N21 C22 C23 125.0(2) . . ? C24 C23 C28 120.0(2) . . ? C24 C23 C22 123.0(2) . . ? C28 C23 C22 116.69(19) . . ? O29 C24 C25 118.29(19) . . ? O29 C24 C23 125.1(2) . . ? C25 C24 C23 116.58(19) . . ? C26 C25 C24 121.7(2) . . ? C25 C26 C27 122.4(2) . . ? C28 C27 C26 116.46(19) . . ? C28 C27 C30 124.29(19) . . ? C26 C27 C30 119.24(19) . . ? C27 C28 C23 122.8(2) . . ? C24 O29 Cu1 125.51(14) . . ? C33 C30 C32 108.97(18) . . ? C33 C30 C27 111.76(19) . . ? C32 C30 C27 109.20(18) . . ? C33 C30 C31 108.56(19) . . ? C32 C30 C31 108.86(19) . . ? C27 C30 C31 109.44(16) . . ? H34A O34 H34B 109(3) . . ? 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 O34 H34A O16 0.72(3) 2.10(3) 2.770(3) 154(4) . O34 H34B O29 0.72(3) 2.37(4) 2.936(3) 136(4) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.909 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.103 #=END data_c:\datasets\leeds\islhddq\islhddq _database_code_depnum_ccdc_archive 'CCDC 270589' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-bis(2-hydroxy-5-tert-butylbenzylidene)-trans- 1,2-dicyclohexylamino]copper(II) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H36 Cu N2 O2, C H2 Cl2' _chemical_formula_sum 'C29 H38 Cl2 Cu N2 O2' _chemical_formula_weight 581.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 8.2379(2) _cell_length_b 12.0392(2) _cell_length_c 14.8235(3) _cell_angle_alpha 99.3685(9) _cell_angle_beta 95.7750(7) _cell_angle_gamma 99.3788(10) _cell_volume 1418.90(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30377 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.50 _exptl_crystal_description Needle _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings The high value of R~int~ (0.107) probably reflects the high redundancy of the dataset collected, and the moderate quality of the crystal used which had a mosaicity of 0.57 (a strongly diffracting crystal would give a mosaicity of 0.35-0.40 under our conditions). ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30377 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6503 _reflns_number_gt 5250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. No disorder was detected during refinement (but see below). All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. Although the thermal parameters on the solvent atoms C34 and Cl35 are a little high, attempts to refine a disorder model involving these atoms afforded two orientations (with refined occupancies of 0.50 each) whose atoms had thermal ellipsoids slightly larger than those of the crystallographcially ordered solvent model. The residuals R1 and wR2 were also virtually identical in the two models. Therefore, an ordered CH~2~Cl~2~ molecule was included in the final least squares cycles, since the inclusion of a disorder model led to no improvement in the overall model. Presumably, the larger thermal parameters on Cl35 in particular reflect librational motion of this group in the crystal. ; _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^)+(0.0536P)^2^+0.4881P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6503 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.26545(3) 0.48339(2) 0.097859(17) 0.02578(10) Uani 1 1 d . . . C2 C 0.2559(3) 0.67048(17) 0.00384(15) 0.0273(4) Uani 1 1 d . . . H2 H 0.3646 0.7151 0.0370 0.033 Uiso 1 1 calc R . . C3 C 0.2135(3) 0.72340(18) -0.08016(16) 0.0326(5) Uani 1 1 d . . . H3A H 0.1059 0.6818 -0.1147 0.039 Uiso 1 1 calc R . . H3B H 0.2999 0.7177 -0.1217 0.039 Uiso 1 1 calc R . . C4 C 0.2035(3) 0.84957(19) -0.04777(17) 0.0358(5) Uani 1 1 d . . . H4A H 0.3143 0.8919 -0.0182 0.043 Uiso 1 1 calc R . . H4B H 0.1711 0.8835 -0.1018 0.043 Uiso 1 1 calc R . . C5 C 0.0789(3) 0.86257(19) 0.02015(16) 0.0331(5) Uani 1 1 d . . . H5A H -0.0338 0.8276 -0.0115 0.040 Uiso 1 1 calc R . . H5B H 0.0805 0.9450 0.0419 0.040 Uiso 1 1 calc R . . C6 C 0.1165(3) 0.80603(18) 0.10307(15) 0.0296(5) Uani 1 1 d . . . H6A H 0.2232 0.8467 0.1393 0.035 Uiso 1 1 calc R . . H6B H 0.0282 0.8112 0.1434 0.035 Uiso 1 1 calc R . . C7 C 0.1264(3) 0.68072(17) 0.07067(14) 0.0256(4) Uani 1 1 d . . . H7 H 0.0157 0.6405 0.0371 0.031 Uiso 1 1 calc R . . N8 N 0.2714(2) 0.54863(14) -0.01385(12) 0.0265(4) Uani 1 1 d . . . C9 C 0.2931(3) 0.49647(18) -0.09363(15) 0.0285(4) Uani 1 1 d . . . H9 H 0.2990 0.5396 -0.1419 0.034 Uiso 1 1 calc R . . C10 C 0.3091(3) 0.37840(18) -0.11533(15) 0.0268(4) Uani 1 1 d . . . C11 C 0.3141(2) 0.30617(18) -0.04868(15) 0.0259(4) Uani 1 1 d . . . C12 C 0.3220(3) 0.19028(18) -0.08172(15) 0.0279(4) Uani 1 1 d . . . H12 H 0.3263 0.1394 -0.0392 0.033 Uiso 1 1 calc R . . C13 C 0.3236(3) 0.14940(18) -0.17362(15) 0.0287(5) Uani 1 1 d . . . H13 H 0.3273 0.0707 -0.1926 0.034 Uiso 1 1 calc R . . C14 C 0.3199(3) 0.21987(18) -0.24106(15) 0.0277(4) Uani 1 1 d . . . C15 C 0.3146(3) 0.33258(19) -0.20971(15) 0.0293(5) Uani 1 1 d . . . H15 H 0.3147 0.3827 -0.2530 0.035 Uiso 1 1 calc R . . O16 O 0.31150(19) 0.34011(13) 0.04030(10) 0.0301(3) Uani 1 1 d . . . C17 C 0.3180(3) 0.16862(19) -0.34304(15) 0.0320(5) Uani 1 1 d . . . C18 C 0.3226(3) 0.2600(2) -0.40372(17) 0.0395(6) Uani 1 1 d . . . H18A H 0.2290 0.2998 -0.3953 0.059 Uiso 1 1 calc R . . H18B H 0.3148 0.2235 -0.4685 0.059 Uiso 1 1 calc R . . H18C H 0.4270 0.3151 -0.3862 0.059 Uiso 1 1 calc R . . C19 C 0.4702(3) 0.1103(2) -0.35432(18) 0.0409(6) Uani 1 1 d . . . H19A H 0.5721 0.1675 -0.3348 0.061 Uiso 1 1 calc R . . H19B H 0.4670 0.0754 -0.4191 0.061 Uiso 1 1 calc R . . H19C H 0.4683 0.0509 -0.3162 0.061 Uiso 1 1 calc R . . C20 C 0.1584(3) 0.0786(2) -0.37555(18) 0.0445(6) Uani 1 1 d . . . H20A H 0.1558 0.0182 -0.3384 0.067 Uiso 1 1 calc R . . H20B H 0.1563 0.0452 -0.4406 0.067 Uiso 1 1 calc R . . H20C H 0.0614 0.1153 -0.3683 0.067 Uiso 1 1 calc R . . N21 N 0.1733(2) 0.61714(15) 0.14392(12) 0.0270(4) Uani 1 1 d . . . C22 C 0.1532(3) 0.65121(18) 0.22866(15) 0.0293(5) Uani 1 1 d . . . H22 H 0.1034 0.7169 0.2417 0.035 Uiso 1 1 calc R . . C23 C 0.2000(3) 0.59773(18) 0.30458(15) 0.0283(4) Uani 1 1 d . . . C24 C 0.2679(3) 0.49611(18) 0.29368(15) 0.0301(5) Uani 1 1 d . . . C25 C 0.3115(3) 0.4560(2) 0.37555(16) 0.0366(5) Uani 1 1 d . . . H25 H 0.3551 0.3873 0.3714 0.044 Uiso 1 1 calc R . . C26 C 0.2930(3) 0.51305(19) 0.46122(16) 0.0347(5) Uani 1 1 d . . . H26 H 0.3259 0.4829 0.5142 0.042 Uiso 1 1 calc R . . C27 C 0.2273(3) 0.61435(18) 0.47305(15) 0.0296(5) Uani 1 1 d . . . C28 C 0.1814(3) 0.65297(18) 0.39354(15) 0.0297(5) Uani 1 1 d . . . H28 H 0.1346 0.7205 0.3988 0.036 Uiso 1 1 calc R . . O29 O 0.2914(2) 0.43798(13) 0.21409(11) 0.0361(4) Uani 1 1 d . . . C30 C 0.2174(3) 0.68186(19) 0.56894(15) 0.0325(5) Uani 1 1 d . . . C31 C 0.2120(4) 0.6049(2) 0.64218(18) 0.0493(7) Uani 1 1 d . . . H31A H 0.1197 0.5400 0.6228 0.074 Uiso 1 1 calc R . . H31B H 0.1963 0.6492 0.7012 0.074 Uiso 1 1 calc R . . H31C H 0.3166 0.5764 0.6492 0.074 Uiso 1 1 calc R . . C32 C 0.0622(3) 0.7368(2) 0.56872(18) 0.0444(6) Uani 1 1 d . . . H32A H -0.0369 0.6772 0.5485 0.067 Uiso 1 1 calc R . . H32B H 0.0676 0.7915 0.5264 0.067 Uiso 1 1 calc R . . H32C H 0.0565 0.7769 0.6311 0.067 Uiso 1 1 calc R . . C33 C 0.3703(3) 0.7778(2) 0.59552(17) 0.0416(6) Uani 1 1 d . . . H33A H 0.3680 0.8198 0.6577 0.062 Uiso 1 1 calc R . . H33B H 0.3695 0.8303 0.5515 0.062 Uiso 1 1 calc R . . H33C H 0.4712 0.7445 0.5944 0.062 Uiso 1 1 calc R . . C34 C 0.3053(4) 0.1780(2) 0.1934(2) 0.0541(7) Uani 1 1 d . . . H34A H 0.3729 0.2463 0.2349 0.065 Uiso 1 1 calc R . . H34B H 0.2468 0.2043 0.1414 0.065 Uiso 1 1 calc R . . Cl35 Cl 0.16105(15) 0.11035(10) 0.25312(10) 0.1076(4) Uani 1 1 d . . . Cl36 Cl 0.43623(8) 0.08647(5) 0.15072(4) 0.04239(16) 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 0.03226(16) 0.02359(15) 0.02179(15) 0.00182(10) 0.00321(10) 0.00850(11) C2 0.0306(11) 0.0238(10) 0.0271(11) 0.0024(8) 0.0047(8) 0.0055(8) C3 0.0448(13) 0.0264(11) 0.0287(12) 0.0054(9) 0.0097(10) 0.0090(10) C4 0.0494(14) 0.0265(11) 0.0351(13) 0.0104(10) 0.0091(11) 0.0106(10) C5 0.0398(12) 0.0294(11) 0.0343(12) 0.0090(10) 0.0057(10) 0.0144(10) C6 0.0337(11) 0.0291(11) 0.0281(11) 0.0047(9) 0.0048(9) 0.0120(9) C7 0.0269(10) 0.0259(10) 0.0240(10) 0.0033(8) 0.0014(8) 0.0071(8) N8 0.0296(9) 0.0221(8) 0.0273(9) 0.0013(7) 0.0042(7) 0.0057(7) C9 0.0335(11) 0.0257(10) 0.0275(11) 0.0055(9) 0.0071(9) 0.0065(9) C10 0.0284(10) 0.0244(10) 0.0271(11) 0.0015(9) 0.0048(8) 0.0059(8) C11 0.0256(10) 0.0258(10) 0.0260(11) 0.0022(9) 0.0027(8) 0.0069(8) C12 0.0321(11) 0.0258(10) 0.0273(11) 0.0052(9) 0.0047(9) 0.0086(9) C13 0.0293(11) 0.0243(10) 0.0325(12) 0.0008(9) 0.0057(9) 0.0083(8) C14 0.0283(10) 0.0274(10) 0.0269(11) 0.0015(9) 0.0063(8) 0.0050(8) C15 0.0347(11) 0.0271(11) 0.0263(11) 0.0033(9) 0.0071(9) 0.0060(9) O16 0.0404(8) 0.0285(8) 0.0229(8) 0.0036(6) 0.0046(6) 0.0116(7) C17 0.0416(12) 0.0274(11) 0.0254(11) -0.0008(9) 0.0075(9) 0.0053(9) C18 0.0549(15) 0.0379(13) 0.0267(12) 0.0030(10) 0.0100(10) 0.0112(11) C19 0.0546(15) 0.0351(12) 0.0358(13) 0.0016(10) 0.0174(11) 0.0145(11) C20 0.0512(15) 0.0409(14) 0.0336(13) -0.0030(11) 0.0012(11) -0.0019(12) N21 0.0325(9) 0.0265(9) 0.0234(9) 0.0051(7) 0.0027(7) 0.0095(7) C22 0.0327(11) 0.0266(10) 0.0292(12) 0.0029(9) 0.0033(9) 0.0102(9) C23 0.0343(11) 0.0263(10) 0.0238(11) 0.0016(9) 0.0039(9) 0.0072(9) C24 0.0399(12) 0.0259(11) 0.0251(11) 0.0030(9) 0.0047(9) 0.0089(9) C25 0.0549(14) 0.0290(11) 0.0294(12) 0.0061(10) 0.0052(10) 0.0172(11) C26 0.0511(14) 0.0307(11) 0.0236(11) 0.0051(9) 0.0035(10) 0.0115(10) C27 0.0370(12) 0.0266(10) 0.0242(11) 0.0021(9) 0.0056(9) 0.0047(9) C28 0.0377(12) 0.0248(10) 0.0267(11) 0.0011(9) 0.0064(9) 0.0086(9) O29 0.0579(10) 0.0301(8) 0.0238(8) 0.0018(7) 0.0059(7) 0.0205(8) C30 0.0434(13) 0.0302(11) 0.0234(11) 0.0018(9) 0.0074(9) 0.0068(10) C31 0.080(2) 0.0423(14) 0.0278(13) 0.0060(11) 0.0173(13) 0.0128(14) C32 0.0476(14) 0.0542(16) 0.0317(13) -0.0025(12) 0.0116(11) 0.0171(12) C33 0.0517(15) 0.0381(13) 0.0301(12) -0.0030(10) 0.0007(11) 0.0059(11) C34 0.084(2) 0.0472(15) 0.0395(15) 0.0054(13) 0.0114(14) 0.0372(15) Cl35 0.1056(8) 0.0985(8) 0.1299(10) 0.0042(7) 0.0830(8) 0.0271(6) Cl36 0.0467(3) 0.0423(3) 0.0396(3) 0.0054(3) 0.0101(3) 0.0115(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O29 1.8931(15) . ? Cu1 O16 1.9096(15) . ? Cu1 N21 1.9444(18) . ? Cu1 N8 1.9464(18) . ? C2 N8 1.476(3) . ? C2 C3 1.524(3) . ? C2 C7 1.533(3) . ? C3 C4 1.535(3) . ? C4 C5 1.517(3) . ? C5 C6 1.528(3) . ? C6 C7 1.525(3) . ? C7 N21 1.482(3) . ? N8 C9 1.289(3) . ? C9 C10 1.436(3) . ? C10 C11 1.420(3) . ? C10 C15 1.426(3) . ? C11 O16 1.319(3) . ? C11 C12 1.416(3) . ? C12 C13 1.373(3) . ? C13 C14 1.414(3) . ? C14 C15 1.370(3) . ? C14 C17 1.535(3) . ? C17 C18 1.528(3) . ? C17 C20 1.541(3) . ? C17 C19 1.544(3) . ? N21 C22 1.292(3) . ? C22 C23 1.435(3) . ? C23 C28 1.412(3) . ? C23 C24 1.418(3) . ? C24 O29 1.320(3) . ? C24 C25 1.412(3) . ? C25 C26 1.377(3) . ? C26 C27 1.406(3) . ? C27 C28 1.376(3) . ? C27 C30 1.535(3) . ? C30 C32 1.533(3) . ? C30 C33 1.534(3) . ? C30 C31 1.537(3) . ? C34 Cl35 1.729(3) . ? C34 Cl36 1.754(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 O29 Cu1 O16 89.86(6) . . ? O29 Cu1 N21 94.12(7) . . ? O16 Cu1 N21 168.39(7) . . ? O29 Cu1 N8 170.62(7) . . ? O16 Cu1 N8 93.81(7) . . ? N21 Cu1 N8 83.96(7) . . ? N8 C2 C3 116.76(17) . . ? N8 C2 C7 106.24(16) . . ? C3 C2 C7 111.10(17) . . ? C2 C3 C4 108.92(18) . . ? C5 C4 C3 111.64(19) . . ? C4 C5 C6 111.98(18) . . ? C7 C6 C5 110.09(18) . . ? N21 C7 C6 115.87(17) . . ? N21 C7 C2 105.52(16) . . ? C6 C7 C2 110.51(17) . . ? C9 N8 C2 122.42(18) . . ? C9 N8 Cu1 125.96(15) . . ? C2 N8 Cu1 111.56(13) . . ? N8 C9 C10 125.2(2) . . ? C11 C10 C15 119.55(19) . . ? C11 C10 C9 123.41(19) . . ? C15 C10 C9 117.00(19) . . ? O16 C11 C12 118.96(19) . . ? O16 C11 C10 124.42(19) . . ? C12 C11 C10 116.62(19) . . ? C13 C12 C11 121.8(2) . . ? C12 C13 C14 122.6(2) . . ? C15 C14 C13 116.2(2) . . ? C15 C14 C17 123.7(2) . . ? C13 C14 C17 120.14(19) . . ? C14 C15 C10 123.3(2) . . ? C11 O16 Cu1 126.39(13) . . ? C18 C17 C14 111.83(18) . . ? C18 C17 C20 108.7(2) . . ? C14 C17 C20 108.91(19) . . ? C18 C17 C19 108.62(19) . . ? C14 C17 C19 109.53(19) . . ? C20 C17 C19 109.2(2) . . ? C22 N21 C7 121.23(18) . . ? C22 N21 Cu1 125.82(15) . . ? C7 N21 Cu1 112.95(13) . . ? N21 C22 C23 125.2(2) . . ? C28 C23 C24 119.96(19) . . ? C28 C23 C22 117.04(19) . . ? C24 C23 C22 123.0(2) . . ? O29 C24 C25 119.00(19) . . ? O29 C24 C23 125.01(19) . . ? C25 C24 C23 116.0(2) . . ? C26 C25 C24 122.3(2) . . ? C25 C26 C27 122.3(2) . . ? C28 C27 C26 115.9(2) . . ? C28 C27 C30 121.94(19) . . ? C26 C27 C30 122.07(19) . . ? C27 C28 C23 123.6(2) . . ? C24 O29 Cu1 126.44(14) . . ? C32 C30 C33 108.2(2) . . ? C32 C30 C27 111.06(19) . . ? C33 C30 C27 108.53(19) . . ? C32 C30 C31 107.9(2) . . ? C33 C30 C31 109.3(2) . . ? C27 C30 C31 111.72(19) . . ? Cl35 C34 Cl36 111.47(16) . . ? 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 C34 H34B O16 0.99 2.42 3.224(3) 137.4 . C34 H34A O29 0.99 2.56 3.116(3) 115.3 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.630 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.089 #=END data_c:\datasets\leeds\is180\is180 _database_code_depnum_ccdc_archive 'CCDC 270590' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-bis(2-hydroxy-3-phenylsunlfanyl-5-tert-butylbenzylidene)-trans- 1,2-dicyclohexylamino]copper(II)silver(I) tetrafluoroborate acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H44 Ag B Cu F4 N2 O2 S2, B F4, 1.45[C2 H3 N]' _chemical_formula_sum 'C42.90 H48.35 Ag B Cu F4 N3.45 O2 S2' _chemical_formula_weight 966.64 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 8.4806(1) _cell_length_b 14.8652(2) _cell_length_c 17.4574(3) _cell_angle_alpha 89.8338(6) _cell_angle_beta 84.3792(6) _cell_angle_gamma 79.3241(8) _cell_volume 2152.03(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39767 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39767 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9801 _reflns_number_gt 8143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following moieties in the structure are disordered: i) The cyclohexyl ring C3-C8, which was modelled over two orientations with refined occupancies: C3A-C8A, occupancy 0.72 C3B-C8B, occupancy 0.28 All C-C bonds in this residue were restrained to 1.54(2)\%A, C-N bonds connecting to the ring to 1.47(1)\%A, and 1,3-C...C distances within a given disorder orientation to 2.51(2)\%A. ii) The tert-butyl group C38-C41 was modelled over three orientations with fixed occupancies: C38A-C41A, occupancy 0.40 C38B-C41B, occupancy 0.40 C38C-C41C, occupancy 0.20 All C-C bonds involving this residue were restrained to 1.54(2)\%A, and 1,3-C...C distances within a given disorder orientation to 2.51(2)\%A. iii) The BF~4~^-^ anion B49-F53 was modelled over three orientations with fixed occupancies: B49A-F53A, occupancy 0.50 B49A, F50B-F53B, occupancy 0.25 (so that B49A has a total occupancy of 0.75) B49C-F53C, occupancy 0.25 All B-F distances were restrained to 1.37(2)\%A, and F...F distances within a given disorder orientation to 2.24(2)\%A. iv) The disordered region of solvent was modelled using five partial MeCN molecules with fixed occupancies leading to a total stoichiometry of 1.45 MeCN molecules per asymmetric unit: C54A-N56A, occupancy 0.50 C54B-N56B, occupancy 0.25 C54C-N56C, occupancy 0.25 C54D-N56D, occupancy 0.25 C54E-N56E, occupancy 0.20 All C-C bonds within these molecules were restrained to 1.46(1)\%A, C-N distances to 1.16(1)\%A and 1,3-C...N distances to 2.62(1)\%A. The five residual Fourier peaks of 1.0-1.6 e.\%A^-3^ in the final model all lie within this disordered solvent region. All non-H atoms with occupancies >0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The torsions of the crystallographcially ordered methyl groups were allowed to refine freely, while the disordered methyl groups were fixed in staggered conformations. ; _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^)+(0.0880P)^2^+3.3485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9801 _refine_ls_number_parameters 596 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.038 _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 0.36312(5) 0.31519(3) 0.60578(3) 0.03353(14) Uani 1 1 d . . . Ag2 Ag 0.53325(3) 0.082796(18) 0.579060(16) 0.03626(12) Uani 1 1 d . . . C3A C 0.2483(7) 0.5003(3) 0.5916(3) 0.0363(11) Uani 0.72 1 d PD A 1 H3A H 0.3339 0.5153 0.6223 0.044 Uiso 0.72 1 calc PR A 1 C4A C 0.1761(16) 0.5868(5) 0.5496(5) 0.040(3) Uani 0.72 1 d PD A 1 H4A1 H 0.2613 0.6075 0.5149 0.048 Uiso 0.72 1 calc PR A 1 H4A2 H 0.0922 0.5732 0.5181 0.048 Uiso 0.72 1 calc PR A 1 C5A C 0.1025(8) 0.6615(4) 0.6084(4) 0.0476(14) Uani 0.72 1 d PD A 1 H5A1 H 0.0519 0.7164 0.5814 0.057 Uiso 0.72 1 calc PR A 1 H5A2 H 0.1890 0.6786 0.6364 0.057 Uiso 0.72 1 calc PR A 1 C6A C -0.0239(8) 0.6315(4) 0.6662(4) 0.0526(16) Uani 0.72 1 d PD A 1 H6A1 H -0.1166 0.6216 0.6391 0.063 Uiso 0.72 1 calc PR A 1 H6A2 H -0.0635 0.6809 0.7052 0.063 Uiso 0.72 1 calc PR A 1 C7A C 0.0441(17) 0.5434(7) 0.7067(5) 0.042(4) Uani 0.72 1 d PD A 1 H7A1 H -0.0433 0.5230 0.7402 0.051 Uiso 0.72 1 calc PR A 1 H7A2 H 0.1271 0.5552 0.7396 0.051 Uiso 0.72 1 calc PR A 1 C8A C 0.1194(6) 0.4676(3) 0.6468(3) 0.0386(11) Uani 0.72 1 d PD A 1 H8A H 0.0334 0.4517 0.6169 0.046 Uiso 0.72 1 calc PR A 1 C3B C 0.1731(14) 0.4868(7) 0.5754(7) 0.033(3) Uiso 0.28 1 d PD A 2 H3B H 0.0741 0.4618 0.5676 0.040 Uiso 0.28 1 calc PR A 2 C4B C 0.155(4) 0.5834(13) 0.5441(10) 0.040(10) Uiso 0.28 1 d PD A 2 H4B1 H 0.1305 0.5822 0.4898 0.048 Uiso 0.28 1 calc PR A 2 H4B2 H 0.2578 0.6051 0.5452 0.048 Uiso 0.28 1 calc PR A 2 C5B C 0.0207(19) 0.6507(9) 0.5900(7) 0.042(3) Uiso 0.28 1 d PD A 2 H5B1 H 0.0204 0.7134 0.5705 0.051 Uiso 0.28 1 calc PR A 2 H5B2 H -0.0851 0.6346 0.5829 0.051 Uiso 0.28 1 calc PR A 2 C6B C 0.045(2) 0.6489(9) 0.6755(7) 0.040(3) Uiso 0.28 1 d PD A 2 H6B1 H -0.0465 0.6899 0.7046 0.048 Uiso 0.28 1 calc PR A 2 H6B2 H 0.1451 0.6714 0.6834 0.048 Uiso 0.28 1 calc PR A 2 C7B C 0.056(5) 0.5509(15) 0.7058(12) 0.057(15) Uiso 0.28 1 d PD A 2 H7B1 H -0.0463 0.5299 0.7005 0.068 Uiso 0.28 1 calc PR A 2 H7B2 H 0.0730 0.5506 0.7612 0.068 Uiso 0.28 1 calc PR A 2 C8B C 0.1963(17) 0.4848(6) 0.6612(7) 0.033(3) Uiso 0.28 1 d PD A 2 H8B H 0.3009 0.5037 0.6692 0.040 Uiso 0.28 1 calc PR A 2 N9 N 0.3191(4) 0.4200(2) 0.5414(2) 0.0428(8) Uani 1 1 d D A . C10 C 0.3556(5) 0.4205(3) 0.4681(2) 0.0403(8) Uani 1 1 d . . . H10 H 0.3226 0.4761 0.4422 0.048 Uiso 1 1 calc R C . C11 C 0.4437(4) 0.3425(3) 0.4218(2) 0.0343(8) Uani 1 1 d . C . C12 C 0.5127(4) 0.2591(2) 0.4557(2) 0.0325(7) Uani 1 1 d . . . C13 C 0.5944(4) 0.1873(2) 0.4049(2) 0.0326(7) Uani 1 1 d . C . C14 C 0.6040(4) 0.1971(3) 0.3258(2) 0.0349(8) Uani 1 1 d . . . H14 H 0.6588 0.1473 0.2937 0.042 Uiso 1 1 calc R C . C15 C 0.5346(5) 0.2793(3) 0.2917(2) 0.0354(8) Uani 1 1 d . C . C16 C 0.4584(5) 0.3501(3) 0.3414(2) 0.0365(8) Uani 1 1 d . . . H16 H 0.4138 0.4068 0.3199 0.044 Uiso 1 1 calc R C . O17 O 0.5066(3) 0.24549(18) 0.52998(15) 0.0376(6) Uani 1 1 d . C . C18 C 0.5460(5) 0.2918(3) 0.2042(2) 0.0412(9) Uani 1 1 d . . . C19 C 0.6151(6) 0.2021(3) 0.1597(2) 0.0515(11) Uani 1 1 d . C . H19A H 0.7251 0.1791 0.1726 0.077 Uiso 1 1 calc R . . H19B H 0.6168 0.2132 0.1043 0.077 Uiso 1 1 calc R . . H19C H 0.5476 0.1566 0.1738 0.077 Uiso 1 1 calc R . . C20 C 0.6551(7) 0.3607(4) 0.1814(3) 0.0646(14) Uani 1 1 d . C . H20A H 0.7646 0.3365 0.1944 0.097 Uiso 1 1 calc R . . H20B H 0.6134 0.4187 0.2093 0.097 Uiso 1 1 calc R . . H20C H 0.6572 0.3712 0.1259 0.097 Uiso 1 1 calc R . . C21 C 0.3763(6) 0.3277(3) 0.1790(3) 0.0513(11) Uani 1 1 d . C . H21A H 0.3846 0.3380 0.1234 0.077 Uiso 1 1 calc R . . H21B H 0.3292 0.3854 0.2063 0.077 Uiso 1 1 calc R . . H21C H 0.3074 0.2825 0.1914 0.077 Uiso 1 1 calc R . . S22 S 0.68371(11) 0.08206(6) 0.44588(5) 0.0328(2) Uani 1 1 d . C . C23 C 0.8674(4) 0.1104(2) 0.4741(2) 0.0317(7) Uani 1 1 d . . . C24 C 0.8720(5) 0.1559(3) 0.5431(2) 0.0377(8) Uani 1 1 d . C . H24 H 0.7767 0.1728 0.5772 0.045 Uiso 1 1 calc R . . C25 C 1.0168(5) 0.1765(3) 0.5619(2) 0.0422(9) Uani 1 1 d . . . H25 H 1.0215 0.2065 0.6093 0.051 Uiso 1 1 calc R C . C26 C 1.1550(5) 0.1529(3) 0.5108(3) 0.0418(9) Uani 1 1 d . C . H26 H 1.2539 0.1675 0.5234 0.050 Uiso 1 1 calc R . . C27 C 1.1495(5) 0.1086(3) 0.4422(2) 0.0406(9) Uani 1 1 d . . . H27 H 1.2442 0.0937 0.4074 0.049 Uiso 1 1 calc R C . C28 C 1.0058(4) 0.0855(2) 0.4236(2) 0.0339(7) Uani 1 1 d . C . H28 H 1.0025 0.0532 0.3771 0.041 Uiso 1 1 calc R . . N29 N 0.2062(5) 0.3835(2) 0.6808(2) 0.0472(8) Uani 1 1 d D A . C30 C 0.1619(6) 0.3541(3) 0.7473(3) 0.0498(10) Uani 1 1 d . . . H30 H 0.0804 0.3936 0.7789 0.060 Uiso 1 1 calc R C . C31 C 0.2253(5) 0.2664(3) 0.7779(2) 0.0396(8) Uani 1 1 d . C . C32 C 0.3282(5) 0.1954(3) 0.7323(2) 0.0364(8) Uani 1 1 d . . . C33 C 0.3799(4) 0.1121(3) 0.7691(2) 0.0346(8) Uani 1 1 d . C . C34 C 0.3343(5) 0.0994(3) 0.8462(2) 0.0409(9) Uani 1 1 d . . . H34 H 0.3720 0.0422 0.8687 0.049 Uiso 1 1 calc R C . C35 C 0.2340(5) 0.1687(3) 0.8920(2) 0.0458(9) Uani 1 1 d D B . C36 C 0.1808(6) 0.2505(3) 0.8555(2) 0.0461(10) Uani 1 1 d . . . H36 H 0.1105 0.2981 0.8847 0.055 Uiso 1 1 calc R C . O37 O 0.3740(4) 0.20429(19) 0.65982(16) 0.0442(7) Uani 1 1 d . C . C38A C 0.2137(15) 0.1546(8) 0.9788(6) 0.042(3) Uiso 0.40 1 d PD B 1 C39A C 0.3705(16) 0.1326(10) 1.0161(8) 0.062(4) Uiso 0.40 1 d PD B 1 H39A H 0.4385 0.0779 0.9913 0.093 Uiso 0.40 1 calc PR B 1 H39B H 0.3470 0.1213 1.0710 0.093 Uiso 0.40 1 calc PR B 1 H39C H 0.4271 0.1844 1.0100 0.093 Uiso 0.40 1 calc PR B 1 C40A C 0.1270(17) 0.0720(8) 0.9894(7) 0.059(3) Uiso 0.40 1 d PD B 1 H40A H 0.1933 0.0183 0.9623 0.089 Uiso 0.40 1 calc PR B 1 H40B H 0.0225 0.0864 0.9683 0.089 Uiso 0.40 1 calc PR B 1 H40C H 0.1101 0.0589 1.0443 0.089 Uiso 0.40 1 calc PR B 1 C41A C 0.1144(16) 0.2407(8) 1.0219(7) 0.048(3) Uiso 0.40 1 d PD B 1 H41A H 0.1013 0.2286 1.0772 0.072 Uiso 0.40 1 calc PR B 1 H41B H 0.0080 0.2558 1.0027 0.072 Uiso 0.40 1 calc PR B 1 H41C H 0.1708 0.2922 1.0132 0.072 Uiso 0.40 1 calc PR B 1 C38B C 0.1679(15) 0.1442(9) 0.9745(6) 0.045(4) Uiso 0.40 1 d PD B 2 C39B C -0.0128(12) 0.1537(9) 0.9844(7) 0.064(3) Uiso 0.40 1 d PD B 2 H39D H -0.0454 0.1097 0.9503 0.095 Uiso 0.40 1 calc PR B 2 H39E H -0.0625 0.2160 0.9713 0.095 Uiso 0.40 1 calc PR B 2 H39F H -0.0480 0.1416 1.0380 0.095 Uiso 0.40 1 calc PR B 2 C40B C 0.2205(19) 0.2161(10) 1.0282(8) 0.076(4) Uiso 0.40 1 d PD B 2 H40D H 0.3381 0.2102 1.0214 0.114 Uiso 0.40 1 calc PR B 2 H40E H 0.1860 0.2048 1.0820 0.114 Uiso 0.40 1 calc PR B 2 H40F H 0.1701 0.2780 1.0146 0.114 Uiso 0.40 1 calc PR B 2 C41B C 0.2429(16) 0.0493(7) 1.0004(8) 0.064(3) Uiso 0.40 1 d PD B 2 H41D H 0.3605 0.0434 0.9964 0.096 Uiso 0.40 1 calc PR B 2 H41E H 0.2141 0.0028 0.9674 0.096 Uiso 0.40 1 calc PR B 2 H41F H 0.2025 0.0408 1.0539 0.096 Uiso 0.40 1 calc PR B 2 C38C C 0.169(2) 0.1645(14) 0.9785(9) 0.031(6) Uiso 0.20 1 d PD B 3 C39C C 0.316(3) 0.132(2) 1.0245(12) 0.067(8) Uiso 0.20 1 d PD B 3 H39G H 0.3738 0.0724 1.0045 0.101 Uiso 0.20 1 calc PR B 3 H39H H 0.2782 0.1270 1.0790 0.101 Uiso 0.20 1 calc PR B 3 H39I H 0.3879 0.1767 1.0192 0.101 Uiso 0.20 1 calc PR B 3 C40C C 0.061(3) 0.0916(15) 0.9845(12) 0.047(5) Uiso 0.20 1 d PD B 3 H40G H 0.1179 0.0355 0.9574 0.070 Uiso 0.20 1 calc PR B 3 H40H H -0.0389 0.1147 0.9611 0.070 Uiso 0.20 1 calc PR B 3 H40I H 0.0350 0.0782 1.0388 0.070 Uiso 0.20 1 calc PR B 3 C41C C 0.073(4) 0.2547(16) 1.0109(16) 0.097(15) Uiso 0.20 1 d PD B 3 H41G H 0.1447 0.2995 1.0117 0.145 Uiso 0.20 1 calc PR B 3 H41H H 0.0269 0.2459 1.0634 0.145 Uiso 0.20 1 calc PR B 3 H41I H -0.0132 0.2770 0.9785 0.145 Uiso 0.20 1 calc PR B 3 S42 S 0.49946(12) 0.01850(6) 0.71407(5) 0.0348(2) Uani 1 1 d . C . C43 C 0.6959(5) 0.0107(3) 0.7461(2) 0.0343(7) Uani 1 1 d . . . C44 C 0.7801(5) -0.0757(3) 0.7602(2) 0.0414(9) Uani 1 1 d . C . H44 H 0.7315 -0.1278 0.7553 0.050 Uiso 1 1 calc R . . C45 C 0.9350(5) -0.0860(3) 0.7814(3) 0.0482(10) Uani 1 1 d . . . H45 H 0.9933 -0.1453 0.7909 0.058 Uiso 1 1 calc R C . C46 C 1.0056(6) -0.0100(4) 0.7888(3) 0.0505(10) Uani 1 1 d . C . H46 H 1.1117 -0.0173 0.8040 0.061 Uiso 1 1 calc R . . C47 C 0.9220(6) 0.0766(3) 0.7740(3) 0.0512(11) Uani 1 1 d . . . H47 H 0.9714 0.1284 0.7784 0.061 Uiso 1 1 calc R C . C48 C 0.7659(5) 0.0875(3) 0.7529(3) 0.0452(9) Uani 1 1 d . C . H48 H 0.7076 0.1468 0.7433 0.054 Uiso 1 1 calc R . . B49A B 0.7136(11) 0.3756(5) 0.6921(5) 0.054(2) Uani 0.75 1 d PD . . F50A F 0.5594(13) 0.3720(10) 0.6887(8) 0.150(5) Uiso 0.50 1 d PD C 1 F51A F 0.7257(11) 0.4391(5) 0.7502(5) 0.078(2) Uiso 0.50 1 d PD C 1 F52A F 0.8108(10) 0.2956(5) 0.7171(5) 0.080(2) Uiso 0.50 1 d PD C 1 F53A F 0.7897(12) 0.3987(6) 0.6284(5) 0.083(2) Uiso 0.50 1 d PD C 1 F50B F 0.5948(11) 0.3914(7) 0.6375(6) 0.048(2) Uiso 0.25 1 d PD C 2 F51B F 0.669(2) 0.4472(8) 0.7431(7) 0.061(4) Uiso 0.25 1 d PD C 2 F52B F 0.7339(18) 0.2909(7) 0.7140(7) 0.068(3) Uiso 0.25 1 d PD C 2 F53B F 0.850(2) 0.3903(15) 0.6440(11) 0.126(9) Uiso 0.25 1 d PD C 2 B49C B 0.6884(17) 0.3718(10) 0.7095(9) 0.016(4) Uiso 0.25 1 d PD C 3 F50C F 0.6039(19) 0.3162(11) 0.6775(9) 0.093(5) Uiso 0.25 1 d PD C 3 F51C F 0.769(2) 0.4296(13) 0.6640(11) 0.118(7) Uiso 0.25 1 d PD C 3 F52C F 0.8003(18) 0.3218(11) 0.7513(10) 0.095(5) Uiso 0.25 1 d PD C 3 F53C F 0.5712(19) 0.4347(11) 0.7520(9) 0.101(5) Uiso 0.25 1 d PD C 3 C54A C -0.3099(13) 0.2689(8) 0.9334(7) 0.070(3) Uiso 0.50 1 d PD D 1 H54A H -0.2295 0.2691 0.9701 0.105 Uiso 0.50 1 calc PR D 1 H54B H -0.2586 0.2711 0.8808 0.105 Uiso 0.50 1 calc PR D 1 H54C H -0.3552 0.2129 0.9395 0.105 Uiso 0.50 1 calc PR D 1 C55A C -0.4425(16) 0.3511(9) 0.9486(9) 0.080(3) Uiso 0.50 1 d PD D 1 N56A N -0.5688(15) 0.3999(7) 0.9374(7) 0.069(3) Uiso 0.50 1 d PD D 1 C54B C -0.324(5) 0.414(4) 0.929(3) 0.17(2) Uiso 0.25 1 d PD E 2 H54D H -0.3507 0.3814 0.9763 0.261 Uiso 0.25 1 calc PR E 2 H54E H -0.3000 0.3702 0.8856 0.261 Uiso 0.25 1 calc PR E 2 H54F H -0.4165 0.4614 0.9196 0.261 Uiso 0.25 1 calc PR E 2 C55B C -0.183(2) 0.4559(15) 0.9378(13) 0.064(5) Uiso 0.25 1 d PD E 2 N56B N -0.0779(19) 0.4974(10) 0.9257(9) 0.035(3) Uiso 0.25 1 d PD E 2 C54C C -0.376(2) 0.3228(16) 0.9454(15) 0.065(6) Uiso 0.25 1 d PD F 3 H54G H -0.2789 0.3497 0.9448 0.098 Uiso 0.25 1 calc PR F 3 H54H H -0.3714 0.2868 0.8980 0.098 Uiso 0.25 1 calc PR F 3 H54I H -0.3824 0.2829 0.9899 0.098 Uiso 0.25 1 calc PR F 3 C55C C -0.519(3) 0.396(2) 0.950(3) 0.111(13) Uiso 0.25 1 d PD F 3 N56C N -0.657(2) 0.4285(12) 0.9524(11) 0.059(4) Uiso 0.25 1 d PD F 3 C54D C -0.232(4) 0.430(2) 0.974(2) 0.110(10) Uiso 0.25 1 d PD G 4 H54J H -0.3277 0.4696 0.9995 0.165 Uiso 0.25 1 calc PR G 4 H54K H -0.1818 0.3870 1.0108 0.165 Uiso 0.25 1 calc PR G 4 H54L H -0.2637 0.3958 0.9317 0.165 Uiso 0.25 1 calc PR G 4 C55D C -0.117(3) 0.486(2) 0.943(2) 0.092(10) Uiso 0.25 1 d PD G 4 N56D N -0.003(2) 0.5160(12) 0.9232(9) 0.053(4) Uiso 0.25 1 d PD G 4 C54E C -0.474(6) 0.3732(19) 0.893(3) 0.123(15) Uiso 0.20 1 d PD H 5 H54M H -0.5398 0.3742 0.8498 0.185 Uiso 0.20 1 calc PR H 5 H54N H -0.3905 0.4101 0.8804 0.185 Uiso 0.20 1 calc PR H 5 H54O H -0.5422 0.3984 0.9392 0.185 Uiso 0.20 1 calc PR H 5 C55E C -0.397(5) 0.2788(18) 0.907(2) 0.103(12) Uiso 0.20 1 d PD H 5 N56E N -0.317(2) 0.2146(13) 0.9322(11) 0.046(4) Uiso 0.20 1 d PD H 5 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 0.0354(3) 0.0306(2) 0.0339(2) 0.00392(17) -0.00486(18) -0.00351(18) Ag2 0.03975(19) 0.03345(17) 0.03509(18) 0.00553(11) -0.00548(12) -0.00470(12) C3A 0.037(3) 0.030(2) 0.043(3) 0.002(2) -0.012(2) -0.006(2) C4A 0.038(4) 0.028(4) 0.056(6) 0.006(2) -0.016(4) -0.003(3) C5A 0.046(3) 0.030(3) 0.068(4) 0.004(3) -0.011(3) -0.005(2) C6A 0.041(3) 0.040(3) 0.072(5) 0.001(3) -0.005(3) 0.002(3) C7A 0.040(5) 0.030(4) 0.052(6) 0.000(2) 0.003(3) 0.001(3) C8A 0.034(3) 0.035(3) 0.048(3) 0.003(2) -0.011(2) -0.006(2) N9 0.051(2) 0.0309(16) 0.0436(19) 0.0049(14) 0.0004(15) -0.0039(14) C10 0.045(2) 0.0315(18) 0.043(2) 0.0085(16) -0.0038(17) -0.0043(16) C11 0.0326(18) 0.0334(18) 0.0387(19) 0.0072(15) -0.0060(15) -0.0098(14) C12 0.0315(17) 0.0337(18) 0.0342(18) 0.0050(14) -0.0078(14) -0.0088(14) C13 0.0333(18) 0.0316(17) 0.0347(18) 0.0050(14) -0.0118(14) -0.0067(14) C14 0.0347(18) 0.0366(19) 0.0361(19) 0.0022(15) -0.0097(15) -0.0105(15) C15 0.0366(19) 0.0388(19) 0.0343(19) 0.0062(15) -0.0122(15) -0.0118(15) C16 0.0361(19) 0.0362(19) 0.039(2) 0.0091(15) -0.0132(15) -0.0074(15) O17 0.0425(15) 0.0359(13) 0.0327(13) 0.0067(10) -0.0045(11) -0.0023(11) C18 0.052(2) 0.043(2) 0.0320(19) 0.0079(16) -0.0139(17) -0.0116(18) C19 0.056(3) 0.063(3) 0.035(2) 0.0057(19) -0.0115(19) -0.005(2) C20 0.084(4) 0.079(4) 0.041(2) 0.009(2) -0.010(2) -0.041(3) C21 0.060(3) 0.053(3) 0.041(2) 0.0013(19) -0.022(2) -0.002(2) S22 0.0359(5) 0.0302(4) 0.0335(4) 0.0031(3) -0.0103(3) -0.0060(3) C23 0.0350(18) 0.0276(16) 0.0330(18) 0.0044(13) -0.0097(14) -0.0041(14) C24 0.038(2) 0.042(2) 0.0330(19) 0.0005(15) -0.0057(15) -0.0055(16) C25 0.049(2) 0.044(2) 0.037(2) -0.0027(16) -0.0143(17) -0.0113(18) C26 0.036(2) 0.0357(19) 0.056(2) 0.0052(17) -0.0161(17) -0.0064(16) C27 0.0360(19) 0.037(2) 0.046(2) 0.0043(16) -0.0025(16) -0.0001(15) C28 0.0390(19) 0.0309(17) 0.0304(18) 0.0029(14) -0.0055(14) -0.0018(14) N29 0.052(2) 0.0392(18) 0.044(2) 0.0050(15) 0.0004(16) 0.0044(15) C30 0.054(3) 0.045(2) 0.044(2) 0.0022(18) 0.0019(19) 0.0053(19) C31 0.043(2) 0.040(2) 0.0350(19) 0.0017(16) -0.0047(16) -0.0053(16) C32 0.040(2) 0.0352(19) 0.0353(19) 0.0048(15) -0.0054(15) -0.0090(15) C33 0.0355(18) 0.0349(18) 0.0348(19) 0.0035(14) -0.0075(15) -0.0083(15) C34 0.049(2) 0.041(2) 0.0347(19) 0.0073(16) -0.0105(17) -0.0104(17) C35 0.049(2) 0.054(2) 0.034(2) 0.0057(18) -0.0038(17) -0.0084(19) C36 0.052(2) 0.048(2) 0.036(2) 0.0007(17) -0.0015(18) -0.0035(19) O37 0.0601(18) 0.0333(14) 0.0342(14) 0.0062(11) 0.0039(12) -0.0001(12) S42 0.0412(5) 0.0313(4) 0.0341(5) 0.0034(3) -0.0093(4) -0.0096(4) C43 0.0400(19) 0.0365(18) 0.0286(17) 0.0048(14) -0.0065(14) -0.0114(15) C44 0.046(2) 0.039(2) 0.040(2) 0.0049(16) -0.0050(17) -0.0081(17) C45 0.044(2) 0.053(2) 0.045(2) 0.0130(19) -0.0077(18) -0.0015(19) C46 0.043(2) 0.069(3) 0.041(2) 0.001(2) -0.0132(18) -0.009(2) C47 0.054(3) 0.055(3) 0.051(3) -0.003(2) -0.014(2) -0.020(2) C48 0.050(2) 0.040(2) 0.048(2) 0.0016(17) -0.0125(19) -0.0122(18) B49A 0.076(6) 0.050(4) 0.039(4) 0.012(3) 0.000(4) -0.027(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 O17 1.879(3) . ? Cu1 O37 1.889(3) . ? Cu1 N9 1.919(3) . ? Cu1 N29 1.919(4) . ? Cu1 F50C 2.500(14) . ? Cu1 F50B 2.549(9) . ? Cu1 F50A 2.565(11) . ? Cu1 Ag2 3.5020(5) . ? Ag2 O37 2.411(3) . ? Ag2 S22 2.5392(10) . ? Ag2 O17 2.541(3) . ? Ag2 S42 2.5508(10) . ? C3A N9 1.481(5) . ? C3A C8A 1.532(7) . ? C3A C4A 1.536(8) . ? C4A C5A 1.517(9) . ? C5A C6A 1.526(8) . ? C6A C7A 1.531(9) . ? C7A C8A 1.543(9) . ? C8A N29 1.483(5) . ? C3B N9 1.508(8) . ? C3B C4B 1.521(17) . ? C3B C8B 1.530(14) . ? C4B C5B 1.529(17) . ? C5B C6B 1.526(15) . ? C6B C7B 1.537(18) . ? C7B C8B 1.541(18) . ? C8B N29 1.531(8) . ? N9 C10 1.288(5) . ? C10 C11 1.457(5) . ? C11 C16 1.402(5) . ? C11 C12 1.424(5) . ? C12 O17 1.310(4) . ? C12 C13 1.419(5) . ? C13 C14 1.383(5) . ? C13 S22 1.788(4) . ? C14 C15 1.411(5) . ? C15 C16 1.387(6) . ? C15 C18 1.534(5) . ? C18 C20 1.530(6) . ? C18 C19 1.534(6) . ? C18 C21 1.545(6) . ? S22 C23 1.801(4) . ? C23 C28 1.389(5) . ? C23 C24 1.391(5) . ? C24 C25 1.388(6) . ? C25 C26 1.391(6) . ? C26 C27 1.378(6) . ? C27 C28 1.394(6) . ? N29 C30 1.286(6) . ? C30 C31 1.438(6) . ? C31 C36 1.402(6) . ? C31 C32 1.426(6) . ? C32 O37 1.300(5) . ? C32 C33 1.410(5) . ? C33 C34 1.385(5) . ? C33 S42 1.784(4) . ? C34 C35 1.404(6) . ? C35 C36 1.391(6) . ? C35 C38A 1.527(11) . ? C35 C38B 1.561(12) . ? C35 C38C 1.561(15) . ? C38A C39A 1.518(14) . ? C38A C40A 1.546(13) . ? C38A C41A 1.548(13) . ? C38B C39B 1.505(14) . ? C38B C41B 1.522(14) . ? C38B C40B 1.576(14) . ? C38C C41C 1.512(17) . ? C38C C40C 1.543(17) . ? C38C C39C 1.546(17) . ? S42 C43 1.792(4) . ? C43 C44 1.383(6) . ? C43 C48 1.392(6) . ? C44 C45 1.381(6) . ? C45 C46 1.384(7) . ? C46 C47 1.386(7) . ? C47 C48 1.389(6) . ? B49A F53A 1.307(10) . ? B49A F50A 1.326(11) . ? B49A F52A 1.411(10) . ? B49A F51A 1.411(10) . ? B49A F52B 1.301(11) . ? B49A F51B 1.364(12) . ? B49A F53B 1.414(14) . ? B49A F50B 1.441(11) . ? B49C F50C 1.346(15) . ? B49C F52C 1.363(15) . ? B49C F53C 1.389(15) . ? B49C F51C 1.393(15) . ? C54A C55A 1.504(8) . ? C55A N56A 1.210(8) . ? C54B C55B 1.472(9) . ? C55B N56B 1.179(9) . ? C54C C55C 1.472(10) . ? C55C N56C 1.174(10) . ? C54D C55D 1.463(9) . ? C55D N56D 1.160(9) . ? C54E C55E 1.462(9) . ? C55E N56E 1.176(9) . ? 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 O17 Cu1 O37 85.37(12) . . ? O17 Cu1 N9 93.92(13) . . ? O37 Cu1 N9 168.79(15) . . ? O17 Cu1 N29 176.55(15) . . ? O37 Cu1 N29 93.99(14) . . ? N9 Cu1 N29 86.05(14) . . ? O17 Cu1 F50C 86.3(4) . . ? O37 Cu1 F50C 78.8(4) . . ? N9 Cu1 F50C 112.3(4) . . ? N29 Cu1 F50C 96.9(4) . . ? O17 Cu1 F50B 88.0(2) . . ? O37 Cu1 F50B 108.9(2) . . ? N9 Cu1 F50B 82.2(2) . . ? N29 Cu1 F50B 95.4(3) . . ? F50C Cu1 F50B 30.1(4) . . ? O17 Cu1 F50A 101.3(3) . . ? O37 Cu1 F50A 92.4(3) . . ? N9 Cu1 F50A 98.7(3) . . ? N29 Cu1 F50A 82.1(3) . . ? F50C Cu1 F50A 19.5(4) . . ? F50B Cu1 F50A 22.0(3) . . ? O37 Ag2 S22 132.30(7) . . ? O37 Ag2 O17 62.04(9) . . ? S22 Ag2 O17 70.28(6) . . ? O37 Ag2 S42 73.14(7) . . ? S22 Ag2 S42 151.53(3) . . ? O17 Ag2 S42 132.31(6) . . ? N9 C3A C8A 104.9(4) . . ? N9 C3A C4A 115.4(5) . . ? C8A C3A C4A 111.0(6) . . ? C5A C4A C3A 109.2(6) . . ? C4A C5A C6A 112.2(6) . . ? C5A C6A C7A 111.9(6) . . ? C6A C7A C8A 110.2(6) . . ? N29 C8A C3A 104.4(4) . . ? N29 C8A C7A 113.7(5) . . ? C3A C8A C7A 110.2(6) . . ? N9 C3B C4B 115.8(11) . . ? N9 C3B C8B 102.3(8) . . ? C4B C3B C8B 111.9(11) . . ? C3B C4B C5B 112.7(13) . . ? C6B C5B C4B 110.9(12) . . ? C5B C6B C7B 110.3(13) . . ? C6B C7B C8B 111.1(15) . . ? C3B C8B N29 103.1(8) . . ? C3B C8B C7B 109.6(13) . . ? N29 C8B C7B 115.2(12) . . ? C10 N9 C3A 126.4(4) . . ? C10 N9 C3B 117.9(5) . . ? C10 N9 Cu1 125.4(3) . . ? C3A N9 Cu1 108.0(3) . . ? C3B N9 Cu1 110.9(5) . . ? N9 C10 C11 125.0(4) . . ? C16 C11 C12 119.5(3) . . ? C16 C11 C10 118.6(3) . . ? C12 C11 C10 122.0(3) . . ? O17 C12 C13 118.9(3) . . ? O17 C12 C11 124.0(3) . . ? C13 C12 C11 117.1(3) . . ? C14 C13 C12 121.7(3) . . ? C14 C13 S22 120.3(3) . . ? C12 C13 S22 118.0(3) . . ? C13 C14 C15 121.6(4) . . ? C16 C15 C14 116.6(3) . . ? C16 C15 C18 121.0(3) . . ? C14 C15 C18 122.4(4) . . ? C15 C16 C11 123.5(3) . . ? C12 O17 Cu1 126.1(2) . . ? C12 O17 Ag2 119.1(2) . . ? Cu1 O17 Ag2 103.79(11) . . ? C20 C18 C15 109.7(3) . . ? C20 C18 C19 108.0(4) . . ? C15 C18 C19 112.5(3) . . ? C20 C18 C21 109.2(4) . . ? C15 C18 C21 109.7(4) . . ? C19 C18 C21 107.6(3) . . ? C13 S22 C23 101.19(16) . . ? C13 S22 Ag2 104.34(13) . . ? C23 S22 Ag2 98.03(12) . . ? C28 C23 C24 120.9(3) . . ? C28 C23 S22 117.2(3) . . ? C24 C23 S22 122.0(3) . . ? C25 C24 C23 119.6(4) . . ? C24 C25 C26 119.7(4) . . ? C27 C26 C25 120.5(4) . . ? C26 C27 C28 120.4(4) . . ? C23 C28 C27 119.0(3) . . ? C30 N29 C8A 123.2(4) . . ? C30 N29 C8B 124.4(5) . . ? C30 N29 Cu1 125.0(3) . . ? C8A N29 Cu1 110.8(3) . . ? C8B N29 Cu1 106.7(5) . . ? N29 C30 C31 125.4(4) . . ? C36 C31 C32 119.4(4) . . ? C36 C31 C30 117.9(4) . . ? C32 C31 C30 122.7(4) . . ? O37 C32 C33 119.7(3) . . ? O37 C32 C31 123.2(3) . . ? C33 C32 C31 117.0(3) . . ? C34 C33 C32 121.8(4) . . ? C34 C33 S42 118.9(3) . . ? C32 C33 S42 119.2(3) . . ? C33 C34 C35 121.9(4) . . ? C36 C35 C34 116.4(4) . . ? C36 C35 C38A 124.9(6) . . ? C34 C35 C38A 118.0(6) . . ? C36 C35 C38B 124.4(6) . . ? C34 C35 C38B 118.4(6) . . ? C38A C35 C38B 17.0(6) . . ? C36 C35 C38C 115.5(8) . . ? C34 C35 C38C 128.0(8) . . ? C38A C35 C38C 14.1(8) . . ? C38B C35 C38C 11.5(9) . . ? C35 C36 C31 123.5(4) . . ? C32 O37 Cu1 126.5(3) . . ? C32 O37 Ag2 124.1(2) . . ? Cu1 O37 Ag2 108.47(12) . . ? C39A C38A C35 114.7(9) . . ? C39A C38A C40A 108.3(10) . . ? C35 C38A C40A 105.1(8) . . ? C39A C38A C41A 105.7(9) . . ? C35 C38A C41A 111.8(9) . . ? C40A C38A C41A 111.2(10) . . ? C39B C38B C41B 108.8(10) . . ? C39B C38B C35 113.0(9) . . ? C41B C38B C35 114.1(9) . . ? C39B C38B C40B 109.6(10) . . ? C41B C38B C40B 107.4(10) . . ? C35 C38B C40B 103.7(9) . . ? C41C C38C C40C 109.4(14) . . ? C41C C38C C39C 110.3(14) . . ? C40C C38C C39C 108.8(14) . . ? C41C C38C C35 113.6(14) . . ? C40C C38C C35 107.0(12) . . ? C39C C38C C35 107.7(13) . . ? C33 S42 C43 103.74(18) . . ? C33 S42 Ag2 103.70(13) . . ? C43 S42 Ag2 102.99(12) . . ? C44 C43 C48 120.6(4) . . ? C44 C43 S42 117.4(3) . . ? C48 C43 S42 121.9(3) . . ? C45 C44 C43 119.8(4) . . ? C44 C45 C46 120.1(4) . . ? C45 C46 C47 120.2(4) . . ? C46 C47 C48 120.0(4) . . ? C47 C48 C43 119.2(4) . . ? F53A B49A F50A 115.6(9) . . ? F53A B49A F52A 106.0(8) . . ? F50A B49A F52A 116.0(9) . . ? F53A B49A F51A 107.9(7) . . ? F50A B49A F51A 108.9(9) . . ? F52A B49A F51A 101.2(7) . . ? F52B B49A F51B 122.1(10) . . ? F52B B49A F53B 109.9(11) . . ? F51B B49A F53B 108.5(11) . . ? F52B B49A F50B 110.1(9) . . ? F51B B49A F50B 104.3(9) . . ? F53B B49A F50B 99.5(10) . . ? F50C B49C F52C 109.8(13) . . ? F50C B49C F53C 103.9(12) . . ? F52C B49C F53C 114.9(14) . . ? F50C B49C F51C 120.8(15) . . ? F52C B49C F51C 106.3(13) . . ? F53C B49C F51C 101.3(12) . . ? B49A F50A Cu1 143.2(9) . . ? B49A F50B Cu1 135.2(7) . . ? B49C F50C Cu1 143.1(12) . . ? N56A C55A C54A 154.3(13) . . ? N56B C55B C54B 162(3) . . ? N56C C55C C54C 157(3) . . ? N56D C55D C54D 166(3) . . ? N56E C55E C54E 162(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.598 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.147