Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_lfl21_lfl45_lfl46 _journal_coden_Cambridge 186 #======================================================================= _publ_contact_author_name 'Leonard F. Lindoy' _publ_contact_author_address ; The Centre for Heavy Metal Research, School of Chemistry F11, University of Sydney, Sydney 2006, NSW, Australia. ; _publ_contact_author_email Lindoy@chem.usyd.edu.au _publ_contact_author_fax '+61 2 9351 3329' _publ_contact_author_phone '+61 2 9351 4400' _publ_requested_journal 'RSC Dalton Transactions' _publ_section_title ; A Comparative Investigation Of Supramolecular Structures Involving Copper(II) Complexes Of Imidazolinylalkanimidamides. ; loop_ _publ_author_name _publ_author_address 'Michael M. Bishop' ; Sydney Grammar School, College Street, Sydney 2010, Australia. ; 'Leonard F. Lindoy' ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'Daniel J. Miller' ; Sydney Grammar School, College Street, Sydney 2010, Australia. ; 'Peter Turner' ; School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_lfl21 _database_code_CSD 190103 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cu N8 O3 S' _chemical_formula_weight 724.33 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 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 11.3898(15) _cell_length_b 14.843(2) _cell_length_c 40.196(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.298(2) _cell_angle_gamma 90.00 _cell_volume 6766.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 988 _cell_measurement_theta_min 2.280 _cell_measurement_theta_max 23.436 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.213 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.022 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type 'numerical and empirical' _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details ; Gaussian (XPREP, Bruker 1995) and SADABS (Sheldrick, 1996) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 110 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0008 _diffrn_reflns_number 35758 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8107 _reflns_number_gt 5341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _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^)+(0.04P)^2^+2.0P] 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 8107 _refine_ls_number_parameters 470 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_restrained_S_all 1.262 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.36996(3) 0.23644(2) 0.125547(7) 0.02910(10) Uani 1 1 d . . . O1 O 0.06993(16) 0.19274(15) 0.11628(4) 0.0466(5) Uani 1 1 d . . . O2 O 0.67445(16) 0.23736(14) 0.13412(4) 0.0428(5) Uani 1 1 d . . . N1 N 0.23694(18) 0.21560(15) 0.08845(5) 0.0308(5) Uani 1 1 d . . . N2 N 0.14823(19) 0.23386(16) 0.03609(5) 0.0350(5) Uani 1 1 d D A . H2N H 0.143(3) 0.2435(18) 0.0156(4) 0.044(9) Uiso 1 1 d D . . N3 N 0.35115(18) 0.23240(15) 0.04025(5) 0.0313(5) Uani 1 1 d . . . N4 N 0.4745(2) 0.22475(18) 0.09099(5) 0.0400(6) Uani 1 1 d . . . H4N H 0.557(3) 0.224(2) 0.0978(7) 0.050(9) Uiso 1 1 d . . . N5 N 0.50460(18) 0.24551(13) 0.16233(5) 0.0290(5) Uani 1 1 d . . . N6 N 0.59256(19) 0.27373(16) 0.21409(5) 0.0342(5) Uani 1 1 d D A . H6N H 0.599(3) 0.2772(19) 0.2346(4) 0.041(8) Uiso 1 1 d D . . N7 N 0.38981(18) 0.26899(15) 0.21004(5) 0.0310(5) Uani 1 1 d . . . N8 N 0.2666(2) 0.23332(16) 0.16092(5) 0.0331(5) Uani 1 1 d . . . H8N H 0.193(3) 0.2303(18) 0.1547(6) 0.032(8) Uiso 1 1 d . . . C1 C 0.1184(2) 0.20884(18) 0.09097(6) 0.0323(6) Uani 1 1 d . . . C2 C 0.0491(2) 0.22434(19) 0.05637(6) 0.0321(6) Uani 1 1 d . A . C3 C 0.2518(2) 0.22817(17) 0.05517(6) 0.0289(5) Uani 1 1 d . . . C4 C 0.4572(2) 0.22764(18) 0.05902(6) 0.0312(6) Uani 1 1 d . . . C5 C 0.5616(2) 0.2266(2) 0.03869(7) 0.0460(7) Uani 1 1 d . . . H5A H 0.6329 0.2219 0.0533 0.069 Uiso 1 1 calc R . . H5B H 0.5630 0.2813 0.0260 0.069 Uiso 1 1 calc R . . H5C H 0.5556 0.1759 0.0238 0.069 Uiso 1 1 calc R . . C6 C -0.0209(2) 0.31196(19) 0.05923(7) 0.0356(6) Uani 1 1 d . . . C7 C 0.0118(3) 0.3907(2) 0.04371(7) 0.0453(7) Uani 1 1 d . . . H7 H 0.0729 0.3898 0.0299 0.054 Uiso 1 1 calc R . . C8 C -0.0475(3) 0.4709(2) 0.04893(9) 0.0621(10) Uani 1 1 d . . . H8 H -0.0254 0.5235 0.0386 0.074 Uiso 1 1 calc R A . C9 C -0.1380(3) 0.4732(3) 0.06923(10) 0.0659(10) Uani 1 1 d . . . H9 H -0.1770 0.5271 0.0726 0.079 Uiso 1 1 calc R . . C10 C -0.1708(3) 0.3958(3) 0.08448(9) 0.0622(10) Uani 1 1 d . . . H10 H -0.2320 0.3971 0.0983 0.075 Uiso 1 1 calc R A . C11 C -0.1129(3) 0.3155(2) 0.07938(7) 0.0461(7) Uani 1 1 d . . . H11 H -0.1362 0.2632 0.0897 0.055 Uiso 1 1 calc R . . C12 C -0.0260(2) 0.14180(19) 0.04551(7) 0.0357(6) Uani 1 1 d . . . C13 C -0.1348(2) 0.1489(2) 0.02787(7) 0.0403(7) Uani 1 1 d . . . H13 H -0.1676 0.2054 0.0233 0.048 Uiso 1 1 calc R . . C14 C -0.1961(3) 0.0717(3) 0.01685(8) 0.0597(10) Uani 1 1 d . . . H14 H -0.2691 0.0772 0.0046 0.072 Uiso 1 1 calc R A . C15 C -0.1513(4) -0.0110(3) 0.02366(10) 0.0737(12) Uani 1 1 d . . . H15 H -0.1931 -0.0621 0.0162 0.088 Uiso 1 1 calc R . . C16 C -0.0433(4) -0.0193(2) 0.04170(11) 0.0765(12) Uani 1 1 d . . . H16 H -0.0124 -0.0762 0.0467 0.092 Uiso 1 1 calc R A . C17 C 0.0195(3) 0.0568(2) 0.05242(9) 0.0586(9) Uani 1 1 d . . . H17 H 0.0930 0.0507 0.0644 0.070 Uiso 1 1 calc R . . C18 C 0.6240(2) 0.24645(17) 0.15954(6) 0.0302(6) Uani 1 1 d . . . C19 C 0.6917(2) 0.26338(18) 0.19408(6) 0.0308(6) Uani 1 1 d . A . C20 C 0.4901(2) 0.26233(17) 0.19543(6) 0.0285(5) Uani 1 1 d . . . C21 C 0.2838(2) 0.25478(17) 0.19191(6) 0.0310(6) Uani 1 1 d . . . C22 C 0.1801(2) 0.2677(2) 0.21199(7) 0.0517(8) Uani 1 1 d . . . H22A H 0.1086 0.2676 0.1973 0.078 Uiso 1 1 calc R . . H22B H 0.1877 0.3242 0.2236 0.078 Uiso 1 1 calc R . . H22C H 0.1777 0.2196 0.2279 0.078 Uiso 1 1 calc R . . C23 C 0.7606(2) 0.35198(18) 0.19242(6) 0.0344(6) Uani 1 1 d . . . C24 C 0.7059(3) 0.4237(2) 0.17507(8) 0.0509(8) Uani 1 1 d . . . H24 H 0.6297 0.4168 0.1650 0.061 Uiso 1 1 calc R . . C25 C 0.7631(3) 0.5048(2) 0.17261(10) 0.0673(10) Uani 1 1 d . . . H25 H 0.7254 0.5521 0.1608 0.081 Uiso 1 1 calc R A . C26 C 0.8768(3) 0.5163(2) 0.18776(10) 0.0650(10) Uani 1 1 d . . . H26 H 0.9160 0.5708 0.1859 0.078 Uiso 1 1 calc R . . C27 C 0.9302(3) 0.4470(2) 0.20543(8) 0.0549(9) Uani 1 1 d . . . H27 H 1.0058 0.4547 0.2159 0.066 Uiso 1 1 calc R A . C28 C 0.8731(2) 0.3650(2) 0.20798(7) 0.0402(7) Uani 1 1 d . . . H28 H 0.9106 0.3184 0.2202 0.048 Uiso 1 1 calc R . . C29 C 0.7653(2) 0.17912(18) 0.20283(7) 0.0354(6) Uani 1 1 d . . . C30 C 0.8659(3) 0.1622(2) 0.18647(8) 0.0484(8) Uani 1 1 d . . . H30 H 0.8909 0.2043 0.1715 0.058 Uiso 1 1 calc R . . C31 C 0.9287(3) 0.0827(3) 0.19249(10) 0.0705(11) Uani 1 1 d . . . H31 H 0.9961 0.0719 0.1817 0.085 Uiso 1 1 calc R A . C32 C 0.8914(4) 0.0199(3) 0.21443(12) 0.0789(12) Uani 1 1 d . . . H32 H 0.9338 -0.0331 0.2185 0.095 Uiso 1 1 calc R . . C33 C 0.7927(4) 0.0352(2) 0.23017(9) 0.0687(11) Uani 1 1 d . . . H33 H 0.7675 -0.0076 0.2448 0.082 Uiso 1 1 calc R A . C34 C 0.7294(3) 0.1145(2) 0.22442(7) 0.0505(8) Uani 1 1 d . . . H34 H 0.6619 0.1243 0.2353 0.061 Uiso 1 1 calc R . . S1A S 0.24454(11) 0.43893(7) 0.10793(3) 0.0553(3) Uani 0.80 1 d P A 1 O3A O 0.3543(3) 0.3983(2) 0.12598(9) 0.0626(9) Uani 0.80 1 d P A 1 C35A C 0.2855(5) 0.5565(4) 0.10740(14) 0.0753(17) Uiso 0.80 1 d P A 1 H35A H 0.3675 0.5616 0.1039 0.113 Uiso 0.80 1 calc PR A 1 H35B H 0.2718 0.5837 0.1284 0.113 Uiso 0.80 1 calc PR A 1 H35C H 0.2389 0.5866 0.0896 0.113 Uiso 0.80 1 calc PR A 1 C36A C 0.1359(5) 0.4418(4) 0.13504(14) 0.0820(18) Uiso 0.80 1 d P A 1 H36A H 0.0962 0.3847 0.1347 0.123 Uiso 0.80 1 calc PR A 1 H36B H 0.0802 0.4883 0.1283 0.123 Uiso 0.80 1 calc PR A 1 H36C H 0.1707 0.4539 0.1573 0.123 Uiso 0.80 1 calc PR A 1 S1B S 0.2972(5) 0.4541(4) 0.13268(13) 0.0646(12) Uiso 0.20 1 d P A 2 O3B O 0.3241(16) 0.3842(12) 0.1085(4) 0.078(5) Uiso 0.20 1 d P A 2 C35B C 0.2343(16) 0.5493(11) 0.1022(4) 0.044(3) Uiso 0.20 1 d P A 2 H35D H 0.2971 0.5745 0.0908 0.066 Uiso 0.20 1 calc PR A 2 H35E H 0.1993 0.5956 0.1147 0.066 Uiso 0.20 1 calc PR A 2 H35F H 0.1756 0.5242 0.0861 0.066 Uiso 0.20 1 calc PR A 2 C36B C 0.1541(15) 0.4708(12) 0.1446(4) 0.044(3) Uiso 0.20 1 d P A 2 H36D H 0.1067 0.5002 0.1268 0.066 Uiso 0.20 1 calc PR A 2 H36E H 0.1579 0.5077 0.1643 0.066 Uiso 0.20 1 calc PR A 2 H36F H 0.1197 0.4136 0.1492 0.066 Uiso 0.20 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02349(17) 0.0401(2) 0.02375(15) 0.00091(13) 0.00255(11) 0.00185(14) O1 0.0271(10) 0.0844(16) 0.0286(10) 0.0063(10) 0.0047(8) -0.0107(10) O2 0.0270(10) 0.0704(14) 0.0316(10) -0.0072(9) 0.0062(8) 0.0038(9) N1 0.0238(11) 0.0441(14) 0.0242(11) 0.0021(9) 0.0014(8) -0.0020(9) N2 0.0228(12) 0.0566(15) 0.0255(12) 0.0047(11) 0.0017(9) 0.0026(10) N3 0.0232(11) 0.0462(13) 0.0246(11) 0.0018(9) 0.0028(9) 0.0022(10) N4 0.0220(12) 0.0698(17) 0.0279(12) -0.0027(11) 0.0007(9) 0.0051(11) N5 0.0239(11) 0.0372(13) 0.0263(11) -0.0023(9) 0.0043(8) 0.0018(9) N6 0.0248(12) 0.0534(15) 0.0245(12) -0.0055(10) 0.0029(9) -0.0001(10) N7 0.0248(11) 0.0439(13) 0.0244(11) 0.0005(9) 0.0034(9) 0.0036(10) N8 0.0228(12) 0.0471(14) 0.0293(12) 0.0010(10) 0.0016(9) -0.0017(11) C1 0.0259(14) 0.0406(16) 0.0300(14) 0.0010(11) 0.0012(11) -0.0038(11) C2 0.0231(13) 0.0460(16) 0.0271(13) -0.0010(11) 0.0020(10) 0.0001(12) C3 0.0262(13) 0.0325(14) 0.0278(13) 0.0012(11) 0.0004(10) 0.0032(11) C4 0.0264(14) 0.0394(15) 0.0285(13) -0.0011(11) 0.0059(11) 0.0033(11) C5 0.0302(16) 0.078(2) 0.0299(15) -0.0010(14) 0.0067(12) 0.0019(15) C6 0.0267(15) 0.0428(17) 0.0360(15) -0.0027(12) -0.0040(11) -0.0011(12) C7 0.0383(18) 0.052(2) 0.0447(17) 0.0013(14) -0.0014(13) -0.0037(14) C8 0.062(2) 0.040(2) 0.080(3) 0.0036(17) -0.012(2) 0.0013(17) C9 0.059(2) 0.051(2) 0.085(3) -0.014(2) -0.006(2) 0.0158(18) C10 0.045(2) 0.072(3) 0.071(2) -0.0163(19) 0.0126(17) 0.0121(18) C11 0.0374(17) 0.052(2) 0.0501(18) -0.0055(14) 0.0106(14) 0.0014(14) C12 0.0300(15) 0.0417(17) 0.0363(15) -0.0061(12) 0.0075(12) -0.0014(12) C13 0.0312(16) 0.0555(19) 0.0343(15) -0.0036(13) 0.0033(12) -0.0065(13) C14 0.040(2) 0.084(3) 0.055(2) -0.0259(19) 0.0076(16) -0.0184(18) C15 0.062(3) 0.068(3) 0.095(3) -0.044(2) 0.029(2) -0.025(2) C16 0.070(3) 0.043(2) 0.120(4) -0.020(2) 0.024(3) 0.0014(19) C17 0.045(2) 0.050(2) 0.080(2) -0.0108(18) 0.0049(18) 0.0039(16) C18 0.0238(13) 0.0362(16) 0.0306(13) -0.0030(11) 0.0025(10) 0.0045(11) C19 0.0228(13) 0.0416(15) 0.0283(13) -0.0036(11) 0.0036(10) 0.0001(11) C20 0.0284(14) 0.0294(13) 0.0276(13) 0.0018(10) 0.0025(10) 0.0017(11) C21 0.0246(13) 0.0371(16) 0.0318(14) 0.0053(11) 0.0053(11) 0.0023(11) C22 0.0271(15) 0.094(3) 0.0343(16) 0.0014(15) 0.0047(12) 0.0073(16) C23 0.0319(15) 0.0383(16) 0.0341(15) -0.0033(11) 0.0081(12) 0.0013(12) C24 0.0458(19) 0.0443(19) 0.062(2) 0.0003(15) 0.0028(16) 0.0034(15) C25 0.071(3) 0.040(2) 0.091(3) 0.0088(18) 0.008(2) 0.0008(18) C26 0.067(3) 0.040(2) 0.091(3) -0.0044(19) 0.022(2) -0.0137(18) C27 0.0413(19) 0.057(2) 0.066(2) -0.0081(17) 0.0072(16) -0.0144(16) C28 0.0318(16) 0.0487(18) 0.0407(16) -0.0002(13) 0.0063(12) -0.0060(13) C29 0.0305(15) 0.0379(16) 0.0364(15) -0.0017(12) -0.0045(11) 0.0003(12) C30 0.0361(18) 0.0472(19) 0.062(2) -0.0040(15) 0.0048(15) 0.0065(14) C31 0.048(2) 0.062(3) 0.099(3) -0.015(2) -0.003(2) 0.0199(18) C32 0.080(3) 0.049(2) 0.102(3) 0.003(2) -0.022(3) 0.022(2) C33 0.088(3) 0.044(2) 0.071(2) 0.0095(17) -0.012(2) -0.001(2) C34 0.055(2) 0.049(2) 0.0471(19) 0.0042(14) -0.0014(15) -0.0032(16) S1A 0.0680(8) 0.0476(6) 0.0486(6) -0.0047(5) -0.0041(5) 0.0071(5) O3A 0.055(2) 0.0507(19) 0.080(3) 0.0110(18) -0.0035(18) 0.0069(15) _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 N4 1.919(2) . ? Cu1 N8 1.928(2) . ? Cu1 N5 2.034(2) . ? Cu1 N1 2.049(2) . ? Cu1 O3B 2.342(18) . ? Cu1 O3A 2.409(3) . ? O1 C1 1.225(3) . ? O2 C18 1.225(3) . ? N1 C1 1.367(3) . ? N1 C3 1.376(3) . ? N2 C3 1.349(3) . ? N2 C2 1.459(3) . ? N2 H2N 0.834(17) . ? N3 C3 1.330(3) . ? N3 C4 1.366(3) . ? N4 C4 1.283(3) . ? N4 H4N 0.96(3) . ? N5 C18 1.375(3) . ? N5 C20 1.379(3) . ? N6 C20 1.339(3) . ? N6 C19 1.454(3) . ? N6 H6N 0.822(17) . ? N7 C20 1.335(3) . ? N7 C21 1.368(3) . ? N8 C21 1.283(3) . ? N8 H8N 0.85(3) . ? C1 C2 1.552(3) . ? C2 C12 1.534(4) . ? C2 C6 1.535(4) . ? C4 C5 1.504(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C11 1.383(4) . ? C6 C7 1.391(4) . ? C7 C8 1.394(4) . ? C7 H7 0.9300 . ? C8 C9 1.373(5) . ? C8 H8 0.9300 . ? C9 C10 1.371(5) . ? C9 H9 0.9300 . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.374(4) . ? C12 C17 1.382(4) . ? C13 C14 1.394(4) . ? C13 H13 0.9300 . ? C14 C15 1.347(5) . ? C14 H14 0.9300 . ? C15 C16 1.374(5) . ? C15 H15 0.9300 . ? C16 C17 1.385(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.545(3) . ? C19 C29 1.528(4) . ? C19 C23 1.536(4) . ? C21 C22 1.503(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.386(4) . ? C23 C24 1.388(4) . ? C24 C25 1.377(4) . ? C24 H24 0.9300 . ? C25 C26 1.390(5) . ? C25 H25 0.9300 . ? C26 C27 1.361(5) . ? C26 H26 0.9300 . ? C27 C28 1.388(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.380(4) . ? C29 C30 1.395(4) . ? C30 C31 1.390(4) . ? C30 H30 0.9300 . ? C31 C32 1.378(6) . ? C31 H31 0.9300 . ? C32 C33 1.358(5) . ? C32 H32 0.9300 . ? C33 C34 1.389(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? S1A O3A 1.512(3) . ? S1A C36A 1.723(6) . ? S1A C35A 1.807(6) . ? C35A H35A 0.9600 . ? C35A H35B 0.9600 . ? C35A H35C 0.9600 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? S1B O3B 1.475(17) . ? S1B C36B 1.757(17) . ? S1B C35B 1.962(17) . ? C35B H35D 0.9600 . ? C35B H35E 0.9600 . ? C35B H35F 0.9600 . ? C36B H36D 0.9600 . ? C36B H36E 0.9600 . ? C36B H36F 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 N4 Cu1 N8 173.37(10) . . ? N4 Cu1 N5 93.18(9) . . ? N8 Cu1 N5 86.35(9) . . ? N4 Cu1 N1 85.76(9) . . ? N8 Cu1 N1 94.14(9) . . ? N5 Cu1 N1 175.07(8) . . ? N4 Cu1 O3B 90.5(4) . . ? N8 Cu1 O3B 96.0(4) . . ? N5 Cu1 O3B 106.5(4) . . ? N1 Cu1 O3B 78.3(4) . . ? N4 Cu1 O3A 98.44(12) . . ? N8 Cu1 O3A 88.16(11) . . ? N5 Cu1 O3A 88.87(10) . . ? N1 Cu1 O3A 96.06(11) . . ? O3B Cu1 O3A 18.9(4) . . ? C1 N1 C3 107.0(2) . . ? C1 N1 Cu1 128.76(16) . . ? C3 N1 Cu1 122.54(16) . . ? C3 N2 C2 111.0(2) . . ? C3 N2 H2N 123(2) . . ? C2 N2 H2N 126(2) . . ? C3 N3 C4 119.6(2) . . ? C4 N4 Cu1 132.4(2) . . ? C4 N4 H4N 110.0(17) . . ? Cu1 N4 H4N 117.0(17) . . ? C18 N5 C20 106.5(2) . . ? C18 N5 Cu1 128.79(16) . . ? C20 N5 Cu1 124.32(16) . . ? C20 N6 C19 111.0(2) . . ? C20 N6 H6N 124(2) . . ? C19 N6 H6N 124(2) . . ? C20 N7 C21 120.2(2) . . ? C21 N8 Cu1 131.4(2) . . ? C21 N8 H8N 110.8(18) . . ? Cu1 N8 H8N 115.8(18) . . ? O1 C1 N1 126.9(2) . . ? O1 C1 C2 122.8(2) . . ? N1 C1 C2 110.3(2) . . ? N2 C2 C12 111.0(2) . . ? N2 C2 C6 113.2(2) . . ? C12 C2 C6 114.7(2) . . ? N2 C2 C1 99.16(19) . . ? C12 C2 C1 111.2(2) . . ? C6 C2 C1 106.5(2) . . ? N3 C3 N2 118.5(2) . . ? N3 C3 N1 129.1(2) . . ? N2 C3 N1 112.4(2) . . ? N4 C4 N3 127.0(2) . . ? N4 C4 C5 119.2(2) . . ? N3 C4 C5 113.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 118.6(3) . . ? C11 C6 C2 120.2(2) . . ? C7 C6 C2 121.1(3) . . ? C6 C7 C8 119.8(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 121.1(3) . . ? C6 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C17 118.5(3) . . ? C13 C12 C2 122.5(3) . . ? C17 C12 C2 118.9(3) . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 121.0(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.1(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 120.6(3) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? O2 C18 N5 127.6(2) . . ? O2 C18 C19 122.2(2) . . ? N5 C18 C19 110.1(2) . . ? N6 C19 C29 113.4(2) . . ? N6 C19 C23 111.1(2) . . ? C29 C19 C23 116.0(2) . . ? N6 C19 C18 99.52(19) . . ? C29 C19 C18 106.9(2) . . ? C23 C19 C18 108.4(2) . . ? N7 C20 N6 118.8(2) . . ? N7 C20 N5 128.4(2) . . ? N6 C20 N5 112.8(2) . . ? N8 C21 N7 127.1(2) . . ? N8 C21 C22 119.7(2) . . ? N7 C21 C22 113.1(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 118.2(3) . . ? C28 C23 C19 123.7(2) . . ? C24 C23 C19 118.1(3) . . ? C25 C24 C23 120.9(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 120.6(3) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C34 C29 C30 118.4(3) . . ? C34 C29 C19 121.7(3) . . ? C30 C29 C19 119.7(2) . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.1(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.2(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 121.0(3) . . ? C29 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? O3A S1A C36A 108.4(2) . . ? O3A S1A C35A 100.8(2) . . ? C36A S1A C35A 100.6(3) . . ? S1A O3A Cu1 116.9(2) . . ? O3B S1B C36B 122.2(10) . . ? O3B S1B C35B 100.4(9) . . ? C36B S1B C35B 77.0(8) . . ? S1B O3B Cu1 121.3(9) . . ? S1B C35B H35D 109.5 . . ? S1B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? S1B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? S1B C36B H36D 109.5 . . ? S1B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? S1B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C1 177.0(2) . . . . ? N8 Cu1 N1 C1 3.6(2) . . . . ? N5 Cu1 N1 C1 99.2(9) . . . . ? O3B Cu1 N1 C1 -91.6(5) . . . . ? O3A Cu1 N1 C1 -85.0(2) . . . . ? N4 Cu1 N1 C3 -19.7(2) . . . . ? N8 Cu1 N1 C3 167.0(2) . . . . ? N5 Cu1 N1 C3 -97.5(9) . . . . ? O3B Cu1 N1 C3 71.7(5) . . . . ? O3A Cu1 N1 C3 78.4(2) . . . . ? N8 Cu1 N4 C4 105.1(9) . . . . ? N5 Cu1 N4 C4 -169.1(3) . . . . ? N1 Cu1 N4 C4 15.7(3) . . . . ? O3B Cu1 N4 C4 -62.6(5) . . . . ? O3A Cu1 N4 C4 -79.8(3) . . . . ? N4 Cu1 N5 C18 2.7(2) . . . . ? N8 Cu1 N5 C18 176.1(2) . . . . ? N1 Cu1 N5 C18 80.2(9) . . . . ? O3B Cu1 N5 C18 -88.8(5) . . . . ? O3A Cu1 N5 C18 -95.7(2) . . . . ? N4 Cu1 N5 C20 174.9(2) . . . . ? N8 Cu1 N5 C20 -11.7(2) . . . . ? N1 Cu1 N5 C20 -107.6(9) . . . . ? O3B Cu1 N5 C20 83.5(5) . . . . ? O3A Cu1 N5 C20 76.6(2) . . . . ? N4 Cu1 N8 C21 102.9(9) . . . . ? N5 Cu1 N8 C21 16.7(3) . . . . ? N1 Cu1 N8 C21 -168.2(2) . . . . ? O3B Cu1 N8 C21 -89.5(5) . . . . ? O3A Cu1 N8 C21 -72.3(3) . . . . ? C3 N1 C1 O1 176.0(3) . . . . ? Cu1 N1 C1 O1 -18.7(4) . . . . ? C3 N1 C1 C2 -3.8(3) . . . . ? Cu1 N1 C1 C2 161.54(17) . . . . ? C3 N2 C2 C12 -118.7(2) . . . . ? C3 N2 C2 C6 110.6(2) . . . . ? C3 N2 C2 C1 -1.8(3) . . . . ? O1 C1 C2 N2 -176.4(3) . . . . ? N1 C1 C2 N2 3.4(3) . . . . ? O1 C1 C2 C12 -59.5(3) . . . . ? N1 C1 C2 C12 120.3(2) . . . . ? O1 C1 C2 C6 66.0(3) . . . . ? N1 C1 C2 C6 -114.2(2) . . . . ? C4 N3 C3 N2 179.4(2) . . . . ? C4 N3 C3 N1 -2.9(4) . . . . ? C2 N2 C3 N3 177.7(2) . . . . ? C2 N2 C3 N1 -0.4(3) . . . . ? C1 N1 C3 N3 -175.1(3) . . . . ? Cu1 N1 C3 N3 18.4(4) . . . . ? C1 N1 C3 N2 2.7(3) . . . . ? Cu1 N1 C3 N2 -163.77(18) . . . . ? Cu1 N4 C4 N3 -6.5(5) . . . . ? Cu1 N4 C4 C5 173.0(2) . . . . ? C3 N3 C4 N4 -4.6(4) . . . . ? C3 N3 C4 C5 175.9(2) . . . . ? N2 C2 C6 C11 -175.8(2) . . . . ? C12 C2 C6 C11 55.4(3) . . . . ? C1 C2 C6 C11 -67.9(3) . . . . ? N2 C2 C6 C7 -0.5(4) . . . . ? C12 C2 C6 C7 -129.3(3) . . . . ? C1 C2 C6 C7 107.4(3) . . . . ? C11 C6 C7 C8 0.5(4) . . . . ? C2 C6 C7 C8 -174.8(3) . . . . ? C6 C7 C8 C9 -0.1(5) . . . . ? C7 C8 C9 C10 -0.1(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C7 C6 C11 C10 -0.8(4) . . . . ? C2 C6 C11 C10 174.6(3) . . . . ? C9 C10 C11 C6 0.6(5) . . . . ? N2 C2 C12 C13 -106.2(3) . . . . ? C6 C2 C12 C13 23.7(4) . . . . ? C1 C2 C12 C13 144.5(3) . . . . ? N2 C2 C12 C17 70.9(3) . . . . ? C6 C2 C12 C17 -159.2(3) . . . . ? C1 C2 C12 C17 -38.4(3) . . . . ? C17 C12 C13 C14 -1.1(4) . . . . ? C2 C12 C13 C14 176.1(2) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C17 -0.8(6) . . . . ? C13 C12 C17 C16 0.1(5) . . . . ? C2 C12 C17 C16 -177.1(3) . . . . ? C15 C16 C17 C12 0.8(6) . . . . ? C20 N5 C18 O2 -177.4(3) . . . . ? Cu1 N5 C18 O2 -4.0(4) . . . . ? C20 N5 C18 C19 1.3(3) . . . . ? Cu1 N5 C18 C19 174.64(16) . . . . ? C20 N6 C19 C29 -111.5(3) . . . . ? C20 N6 C19 C23 115.7(2) . . . . ? C20 N6 C19 C18 1.7(3) . . . . ? O2 C18 C19 N6 177.0(2) . . . . ? N5 C18 C19 N6 -1.8(3) . . . . ? O2 C18 C19 C29 -64.9(3) . . . . ? N5 C18 C19 C29 116.3(2) . . . . ? O2 C18 C19 C23 60.9(3) . . . . ? N5 C18 C19 C23 -117.9(2) . . . . ? C21 N7 C20 N6 -177.8(2) . . . . ? C21 N7 C20 N5 2.9(4) . . . . ? C19 N6 C20 N7 179.5(2) . . . . ? C19 N6 C20 N5 -1.1(3) . . . . ? C18 N5 C20 N7 179.1(3) . . . . ? Cu1 N5 C20 N7 5.4(4) . . . . ? C18 N5 C20 N6 -0.2(3) . . . . ? Cu1 N5 C20 N6 -173.90(17) . . . . ? Cu1 N8 C21 N7 -14.7(4) . . . . ? Cu1 N8 C21 C22 164.7(2) . . . . ? C20 N7 C21 N8 1.1(4) . . . . ? C20 N7 C21 C22 -178.3(2) . . . . ? N6 C19 C23 C28 110.3(3) . . . . ? C29 C19 C23 C28 -21.2(4) . . . . ? C18 C19 C23 C28 -141.4(3) . . . . ? N6 C19 C23 C24 -68.0(3) . . . . ? C29 C19 C23 C24 160.5(2) . . . . ? C18 C19 C23 C24 40.3(3) . . . . ? C28 C23 C24 C25 1.7(4) . . . . ? C19 C23 C24 C25 -179.9(3) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C24 C25 C26 C27 -1.0(6) . . . . ? C25 C26 C27 C28 1.0(5) . . . . ? C24 C23 C28 C27 -1.7(4) . . . . ? C19 C23 C28 C27 -180.0(2) . . . . ? C26 C27 C28 C23 0.3(5) . . . . ? N6 C19 C29 C34 8.3(4) . . . . ? C23 C19 C29 C34 138.6(3) . . . . ? C18 C19 C29 C34 -100.4(3) . . . . ? N6 C19 C29 C30 -177.7(2) . . . . ? C23 C19 C29 C30 -47.3(3) . . . . ? C18 C19 C29 C30 73.7(3) . . . . ? C34 C29 C30 C31 -1.2(4) . . . . ? C19 C29 C30 C31 -175.4(3) . . . . ? C29 C30 C31 C32 0.6(5) . . . . ? C30 C31 C32 C33 0.3(6) . . . . ? C31 C32 C33 C34 -0.5(6) . . . . ? C30 C29 C34 C33 1.0(5) . . . . ? C19 C29 C34 C33 175.1(3) . . . . ? C32 C33 C34 C29 -0.2(5) . . . . ? C36A S1A O3A Cu1 86.2(3) . . . . ? C35A S1A O3A Cu1 -168.6(2) . . . . ? N4 Cu1 O3A S1A 100.6(2) . . . . ? N8 Cu1 O3A S1A -79.9(2) . . . . ? N5 Cu1 O3A S1A -166.3(2) . . . . ? N1 Cu1 O3A S1A 14.1(2) . . . . ? O3B Cu1 O3A S1A 34.5(13) . . . . ? C36B S1B O3B Cu1 -87.0(13) . . . . ? C35B S1B O3B Cu1 -168.1(10) . . . . ? N4 Cu1 O3B S1B -147.1(11) . . . . ? N8 Cu1 O3B S1B 34.3(11) . . . . ? N5 Cu1 O3B S1B -53.7(12) . . . . ? N1 Cu1 O3B S1B 127.3(11) . . . . ? O3A Cu1 O3B S1B -31.9(7) . . . . ? 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 N4 H4N O2 0.96(3) 1.89(3) 2.738(3) 146(3) . N2 H2N N3 0.834(17) 2.279(18) 3.110(3) 175(3) 7 N8 H8N O1 0.85(3) 2.07(3) 2.803(3) 145(2) . N6 H6N N7 0.822(17) 2.221(18) 3.039(3) 173(3) 2_655 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.537 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.069 #===END data_lfl45 _database_code_CSD 190104 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cu N8 O2' _chemical_formula_weight 674.25 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.184(3) _cell_length_b 27.498(7) _cell_length_c 19.121(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.662(4) _cell_angle_gamma 90.00 _cell_volume 6567(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.705 _cell_measurement_theta_max 26.592 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.366 _exptl_crystal_size_mid 0.333 _exptl_crystal_size_min 0.149 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 393 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 57558 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 28.30 _reflns_number_total 15233 _reflns_number_gt 10799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _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^)+(0.03P)^2^] 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 15233 _refine_ls_number_parameters 878 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _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 0.322530(18) 0.269440(9) 0.141115(12) 0.02354(7) Uani 1 1 d . . . O1 O 0.07497(11) 0.26908(6) 0.15836(8) 0.0355(4) Uani 1 1 d . . . O2 O 0.56655(10) 0.31871(5) 0.15958(7) 0.0285(3) Uani 1 1 d . . . N1 N 0.17277(12) 0.28067(6) 0.07815(8) 0.0233(4) Uani 1 1 d . . . N2 N 0.03568(13) 0.28466(6) -0.02876(9) 0.0237(4) Uani 1 1 d . . . N3 N 0.20371(12) 0.29439(6) -0.03901(8) 0.0235(4) Uani 1 1 d . . . H3N H 0.0079(16) 0.2847(7) -0.0744(11) 0.029(6) Uiso 1 1 d . . . N4 N 0.36559(14) 0.29424(7) 0.06072(9) 0.0293(4) Uani 1 1 d . . . H4N H 0.4276(17) 0.3001(8) 0.0712(12) 0.041(7) Uiso 1 1 d . . . N5 N 0.46905(12) 0.26947(6) 0.21345(8) 0.0213(3) Uani 1 1 d . . . N6 N 0.60230(13) 0.24887(7) 0.31667(9) 0.0256(4) Uani 1 1 d . . . H6N H 0.6318(15) 0.2336(7) 0.3550(11) 0.025(6) Uiso 1 1 d . . . N7 N 0.43833(12) 0.21695(6) 0.30803(8) 0.0249(4) Uani 1 1 d . . . N8 N 0.28225(14) 0.22436(7) 0.20515(10) 0.0308(4) Uani 1 1 d D . . H8N H 0.2201(12) 0.2173(7) 0.1938(11) 0.033(6) Uiso 1 1 d D . . C1 C 0.08053(15) 0.27488(7) 0.09645(11) 0.0260(5) Uani 1 1 d . . . C2 C -0.01811(15) 0.27522(7) 0.02578(10) 0.0228(4) Uani 1 1 d . . . C3 C 0.14258(15) 0.28677(7) 0.00304(10) 0.0217(4) Uani 1 1 d . . . C4 C 0.31167(15) 0.30087(7) -0.00793(10) 0.0252(4) Uani 1 1 d . . . C5 C 0.36532(16) 0.31751(9) -0.06273(11) 0.0385(6) Uani 1 1 d . . . H5A H 0.3390 0.2968 -0.1072 0.046 Uiso 1 1 calc R . . H5B H 0.3414 0.3512 -0.0778 0.046 Uiso 1 1 calc R . . C6 C 0.48512(18) 0.31688(12) -0.03805(14) 0.0676(9) Uani 1 1 d . . . H6A H 0.5131 0.3382 0.0049 0.101 Uiso 1 1 calc R . . H6B H 0.5100 0.3283 -0.0783 0.101 Uiso 1 1 calc R . . H6C H 0.5107 0.2836 -0.0246 0.101 Uiso 1 1 calc R . . C7 C -0.09311(14) 0.31583(7) 0.03129(10) 0.0215(4) Uani 1 1 d . . . C8 C -0.09310(17) 0.35983(7) -0.00313(11) 0.0312(5) Uani 1 1 d . . . H8 H -0.0439 0.3653 -0.0293 0.037 Uiso 1 1 calc R . . C9 C -0.1643(2) 0.39608(8) 0.00014(13) 0.0434(6) Uani 1 1 d . . . H9 H -0.1642 0.4261 -0.0244 0.052 Uiso 1 1 calc R . . C10 C -0.23510(19) 0.38898(8) 0.03855(12) 0.0427(6) Uani 1 1 d . . . H10 H -0.2854 0.4136 0.0392 0.051 Uiso 1 1 calc R . . C11 C -0.23279(16) 0.34575(8) 0.07638(11) 0.0337(5) Uani 1 1 d . . . H11 H -0.2802 0.3410 0.1042 0.040 Uiso 1 1 calc R . . C12 C -0.16126(15) 0.30963(7) 0.07352(10) 0.0260(5) Uani 1 1 d . . . H12 H -0.1584 0.2804 0.1005 0.031 Uiso 1 1 calc R . . C13 C -0.06929(17) 0.22455(7) 0.01371(11) 0.0279(5) Uani 1 1 d . . . C14 C -0.17778(18) 0.21740(8) -0.01652(13) 0.0403(6) Uani 1 1 d . . . H14 H -0.2247 0.2444 -0.0315 0.048 Uiso 1 1 calc R . . C15 C -0.2192(2) 0.16940(10) -0.02519(14) 0.0531(7) Uani 1 1 d . . . H15 H -0.2940 0.1640 -0.0460 0.064 Uiso 1 1 calc R . . C16 C -0.1501(2) 0.13072(9) -0.00329(14) 0.0520(7) Uani 1 1 d . . . H16 H -0.1780 0.0986 -0.0076 0.062 Uiso 1 1 calc R . . C17 C -0.0426(2) 0.13772(9) 0.02440(14) 0.0530(7) Uani 1 1 d . . . H17 H 0.0042 0.1106 0.0378 0.064 Uiso 1 1 calc R . . C18 C -0.0019(2) 0.18404(8) 0.03297(13) 0.0421(6) Uani 1 1 d . . . H18 H 0.0733 0.1887 0.0523 0.051 Uiso 1 1 calc R . . C19 C 0.55944(15) 0.29311(7) 0.20983(10) 0.0223(4) Uani 1 1 d . . . C20 C 0.65476(14) 0.28188(7) 0.28010(10) 0.0226(4) Uani 1 1 d . . . C21 C 0.49822(15) 0.24402(7) 0.27895(10) 0.0219(4) Uani 1 1 d . . . C22 C 0.33313(15) 0.20855(7) 0.27057(11) 0.0263(5) Uani 1 1 d . . . C23 C 0.27991(17) 0.17779(9) 0.31378(13) 0.0440(6) Uani 1 1 d . . . H23A H 0.3252 0.1487 0.3313 0.053 Uiso 1 1 calc R . . H23B H 0.2802 0.1965 0.3581 0.053 Uiso 1 1 calc R . . C24 C 0.16913(18) 0.16085(10) 0.27706(14) 0.0556(7) Uani 1 1 d . . . H24A H 0.1228 0.1889 0.2575 0.083 Uiso 1 1 calc R . . H24B H 0.1432 0.1436 0.3128 0.083 Uiso 1 1 calc R . . H24C H 0.1680 0.1389 0.2364 0.083 Uiso 1 1 calc R . . C25 C 0.69195(15) 0.32858(8) 0.32426(11) 0.0276(5) Uani 1 1 d . . . C26 C 0.72336(19) 0.36835(8) 0.29221(13) 0.0443(6) Uani 1 1 d . . . H26 H 0.7225 0.3665 0.2424 0.053 Uiso 1 1 calc R . . C27 C 0.7560(2) 0.41079(9) 0.33145(15) 0.0560(7) Uani 1 1 d . . . H27 H 0.7774 0.4378 0.3084 0.067 Uiso 1 1 calc R . . C28 C 0.7580(2) 0.41433(10) 0.40354(15) 0.0536(7) Uani 1 1 d . . . H28 H 0.7810 0.4435 0.4307 0.064 Uiso 1 1 calc R . . C29 C 0.7262(2) 0.37523(10) 0.43563(14) 0.0538(7) Uani 1 1 d . . . H29 H 0.7269 0.3775 0.4854 0.065 Uiso 1 1 calc R . . C30 C 0.69312(18) 0.33238(9) 0.39680(12) 0.0405(6) Uani 1 1 d . . . H30 H 0.6712 0.3056 0.4199 0.049 Uiso 1 1 calc R . . C31 C 0.74156(15) 0.25546(7) 0.25741(10) 0.0231(4) Uani 1 1 d . . . C32 C 0.84684(16) 0.27032(8) 0.27783(11) 0.0316(5) Uani 1 1 d . . . H32 H 0.8689 0.2981 0.3084 0.038 Uiso 1 1 calc R . . C33 C 0.92093(17) 0.24492(9) 0.25408(13) 0.0394(6) Uani 1 1 d . . . H33 H 0.9931 0.2557 0.2681 0.047 Uiso 1 1 calc R . . C34 C 0.89048(18) 0.20444(8) 0.21048(13) 0.0395(6) Uani 1 1 d . . . H34 H 0.9413 0.1871 0.1945 0.047 Uiso 1 1 calc R . . C35 C 0.78599(19) 0.18920(8) 0.19021(14) 0.0449(6) Uani 1 1 d . . . H35 H 0.7645 0.1612 0.1601 0.054 Uiso 1 1 calc R . . C36 C 0.71185(17) 0.21435(8) 0.21330(13) 0.0367(5) Uani 1 1 d . . . H36 H 0.6397 0.2034 0.1989 0.044 Uiso 1 1 calc R . . Cu2 Cu 0.0000 0.5000 0.0000 0.02359(9) Uani 1 2 d S . . O3 O 0.22757(12) 0.42717(6) 0.03197(8) 0.0426(4) Uani 1 1 d . . . N9 N 0.14290(12) 0.48770(6) 0.07866(8) 0.0244(4) Uani 1 1 d . . . N10 N 0.28232(14) 0.50723(6) 0.17869(9) 0.0262(4) Uani 1 1 d . . . H10N H 0.3130(14) 0.5192(7) 0.2172(10) 0.015(5) Uiso 1 1 d . . . N11 N 0.12698(12) 0.54843(6) 0.16825(8) 0.0220(4) Uani 1 1 d . . . N12 N -0.03406(12) 0.54250(6) 0.06873(8) 0.0272(4) Uani 1 1 d . . . H12N H -0.1010 0.5525 0.0542 0.033 Uiso 1 1 calc R . . C37 C 0.22623(16) 0.45682(8) 0.07880(11) 0.0302(5) Uani 1 1 d . . . C38 C 0.32250(15) 0.46521(7) 0.14954(10) 0.0262(5) Uani 1 1 d . . . C39 C 0.17883(15) 0.51580(7) 0.14143(10) 0.0223(4) Uani 1 1 d . . . C40 C 0.02247(15) 0.55933(7) 0.13236(10) 0.0224(4) Uani 1 1 d . . . C41 C -0.02331(15) 0.59621(7) 0.17269(11) 0.0284(5) Uani 1 1 d . . . H41A H -0.0045 0.6291 0.1597 0.034 Uiso 1 1 calc R . . H41B H 0.0123 0.5918 0.2264 0.034 Uiso 1 1 calc R . . C42 C -0.14321(17) 0.59443(9) 0.15767(13) 0.0441(6) Uani 1 1 d . . . H42A H -0.1800 0.6012 0.1053 0.066 Uiso 1 1 calc R . . H42B H -0.1636 0.6189 0.1880 0.066 Uiso 1 1 calc R . . H42C H -0.1636 0.5621 0.1700 0.066 Uiso 1 1 calc R . . C43 C 0.42316(16) 0.47740(8) 0.12983(11) 0.0297(5) Uani 1 1 d . . . C44 C 0.43932(19) 0.52346(9) 0.10726(12) 0.0404(6) Uani 1 1 d . . . H44 H 0.3868 0.5479 0.1033 0.048 Uiso 1 1 calc R . . C45 C 0.5314(2) 0.53478(10) 0.09018(13) 0.0513(7) Uani 1 1 d . . . H45 H 0.5410 0.5667 0.0742 0.062 Uiso 1 1 calc R . . C46 C 0.6085(2) 0.49990(12) 0.09636(14) 0.0586(8) Uani 1 1 d . . . H46 H 0.6718 0.5074 0.0850 0.070 Uiso 1 1 calc R . . C47 C 0.5926(2) 0.45414(12) 0.11922(15) 0.0664(9) Uani 1 1 d . . . H47 H 0.6462 0.4301 0.1246 0.080 Uiso 1 1 calc R . . C48 C 0.50019(19) 0.44236(9) 0.13459(13) 0.0462(6) Uani 1 1 d . . . H48 H 0.4895 0.4101 0.1485 0.055 Uiso 1 1 calc R . . C49 C 0.33770(15) 0.42289(7) 0.20437(10) 0.0264(5) Uani 1 1 d . . . C50 C 0.42159(17) 0.42572(8) 0.27048(11) 0.0324(5) Uani 1 1 d . . . H50 H 0.4702 0.4522 0.2790 0.039 Uiso 1 1 calc R . . C51 C 0.43474(18) 0.39015(8) 0.32396(12) 0.0392(6) Uani 1 1 d . . . H51 H 0.4920 0.3925 0.3691 0.047 Uiso 1 1 calc R . . C52 C 0.3654(2) 0.35149(9) 0.31200(13) 0.0433(6) Uani 1 1 d . . . H52 H 0.3748 0.3270 0.3486 0.052 Uiso 1 1 calc R . . C53 C 0.2823(2) 0.34848(8) 0.24674(13) 0.0436(6) Uani 1 1 d . . . H53 H 0.2339 0.3219 0.2384 0.052 Uiso 1 1 calc R . . C54 C 0.26860(17) 0.38415(8) 0.19280(12) 0.0357(5) Uani 1 1 d . . . H54 H 0.2111 0.3817 0.1478 0.043 Uiso 1 1 calc R . . Cu3 Cu 0.5000 0.5000 0.5000 0.01925(8) Uani 1 2 d S . . O4 O 0.23320(10) 0.48370(5) 0.49220(7) 0.0249(3) Uani 1 1 d . . . N13 N 0.34802(12) 0.51264(5) 0.43115(8) 0.0202(4) Uani 1 1 d . . . N14 N 0.22232(13) 0.53986(7) 0.32794(9) 0.0274(4) Uani 1 1 d . . . H14N H 0.1984(15) 0.5451(7) 0.2846(11) 0.020(6) Uiso 1 1 d . . . N15 N 0.39444(12) 0.54524(6) 0.32624(8) 0.0229(4) Uani 1 1 d . . . N16 N 0.55058(12) 0.51991(6) 0.42049(8) 0.0230(4) Uani 1 1 d . . . H16N H 0.6196 0.5154 0.4294 0.028 Uiso 1 1 calc R . . C55 C 0.24988(15) 0.50294(7) 0.43932(10) 0.0214(4) Uani 1 1 d . . . C56 C 0.15810(15) 0.52013(8) 0.37027(10) 0.0261(5) Uani 1 1 d . . . C57 C 0.32720(15) 0.53267(7) 0.36189(10) 0.0222(4) Uani 1 1 d . . . C58 C 0.50205(15) 0.53867(7) 0.35647(10) 0.0221(4) Uani 1 1 d . . . C59 C 0.56213(16) 0.55694(8) 0.30634(11) 0.0322(5) Uani 1 1 d . . . H59A H 0.5295 0.5418 0.2573 0.039 Uiso 1 1 calc R . . H59B H 0.5497 0.5924 0.3000 0.039 Uiso 1 1 calc R . . C60 C 0.68070(18) 0.54850(10) 0.32895(14) 0.0521(7) Uani 1 1 d . . . H60A H 0.7154 0.5643 0.3766 0.078 Uiso 1 1 calc R . . H60B H 0.7089 0.5622 0.2916 0.078 Uiso 1 1 calc R . . H60C H 0.6952 0.5135 0.3334 0.078 Uiso 1 1 calc R . . C61 C 0.09228(15) 0.55910(8) 0.39266(10) 0.0290(5) Uani 1 1 d . . . C62 C 0.10390(16) 0.60801(8) 0.37975(11) 0.0337(5) Uani 1 1 d . . . H62 H 0.1526 0.6178 0.3551 0.040 Uiso 1 1 calc R . . C63 C 0.04491(19) 0.64278(9) 0.40260(13) 0.0450(6) Uani 1 1 d . . . H63 H 0.0530 0.6762 0.3930 0.054 Uiso 1 1 calc R . . C64 C -0.0255(2) 0.62907(10) 0.43918(14) 0.0517(7) Uani 1 1 d . . . H64 H -0.0654 0.6530 0.4551 0.062 Uiso 1 1 calc R . . C65 C -0.03766(19) 0.58030(10) 0.45250(14) 0.0498(7) Uani 1 1 d . . . H65 H -0.0859 0.5707 0.4777 0.060 Uiso 1 1 calc R . . C66 C 0.02017(17) 0.54558(9) 0.42925(12) 0.0381(6) Uani 1 1 d . . . H66 H 0.0109 0.5122 0.4382 0.046 Uiso 1 1 calc R . . C67 C 0.09072(16) 0.47742(8) 0.32808(11) 0.0316(5) Uani 1 1 d . . . C68 C -0.0086(2) 0.48673(10) 0.27748(14) 0.0566(8) Uani 1 1 d . . . H68 H -0.0380 0.5185 0.2734 0.068 Uiso 1 1 calc R . . C69 C -0.0659(2) 0.44956(12) 0.23224(15) 0.0737(10) Uani 1 1 d . . . H69 H -0.1335 0.4563 0.1968 0.088 Uiso 1 1 calc R . . C70 C -0.0249(2) 0.40307(12) 0.23880(15) 0.0646(9) Uani 1 1 d . . . H70 H -0.0636 0.3776 0.2081 0.078 Uiso 1 1 calc R . . C71 C 0.0709(2) 0.39439(11) 0.28931(18) 0.0767(10) Uani 1 1 d . . . H71 H 0.0990 0.3623 0.2952 0.092 Uiso 1 1 calc R . . C72 C 0.1299(2) 0.43161(10) 0.33332(16) 0.0622(8) Uani 1 1 d . . . H72 H 0.1986 0.4247 0.3674 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01744(12) 0.03296(15) 0.01716(12) 0.00314(11) 0.00125(9) 0.00020(10) O1 0.0262(8) 0.0591(10) 0.0223(8) 0.0090(7) 0.0092(6) 0.0064(7) O2 0.0224(7) 0.0374(9) 0.0236(8) 0.0071(6) 0.0043(6) -0.0036(6) N1 0.0194(9) 0.0339(10) 0.0155(8) 0.0023(7) 0.0043(7) 0.0017(7) N2 0.0175(9) 0.0370(11) 0.0147(9) 0.0016(7) 0.0023(7) -0.0003(7) N3 0.0181(8) 0.0346(10) 0.0164(8) -0.0004(7) 0.0033(7) -0.0003(7) N4 0.0177(10) 0.0459(12) 0.0208(9) 0.0040(8) 0.0012(8) -0.0028(8) N5 0.0163(8) 0.0288(9) 0.0168(8) 0.0028(7) 0.0026(6) 0.0010(7) N6 0.0175(9) 0.0399(11) 0.0165(9) 0.0072(8) 0.0015(7) -0.0008(8) N7 0.0184(9) 0.0338(10) 0.0204(9) 0.0052(7) 0.0034(7) -0.0011(7) N8 0.0167(9) 0.0396(11) 0.0296(10) 0.0080(8) -0.0015(8) -0.0061(8) C1 0.0231(11) 0.0313(12) 0.0210(11) 0.0037(9) 0.0033(8) 0.0040(9) C2 0.0187(10) 0.0293(12) 0.0199(10) 0.0026(9) 0.0058(8) 0.0003(8) C3 0.0188(10) 0.0234(11) 0.0193(10) -0.0009(8) 0.0011(8) 0.0009(8) C4 0.0214(11) 0.0329(12) 0.0194(10) -0.0001(9) 0.0037(8) -0.0014(9) C5 0.0242(12) 0.0671(17) 0.0228(11) 0.0038(11) 0.0054(9) -0.0063(11) C6 0.0283(14) 0.136(3) 0.0411(16) 0.0227(17) 0.0144(12) -0.0057(16) C7 0.0189(10) 0.0254(11) 0.0173(10) -0.0013(8) 0.0015(8) -0.0014(8) C8 0.0366(13) 0.0303(12) 0.0299(12) 0.0032(9) 0.0152(10) 0.0004(10) C9 0.0643(17) 0.0289(13) 0.0432(14) 0.0086(11) 0.0257(13) 0.0092(12) C10 0.0540(16) 0.0375(14) 0.0395(14) 0.0038(11) 0.0192(12) 0.0197(12) C11 0.0301(12) 0.0453(14) 0.0277(12) -0.0028(10) 0.0120(10) 0.0035(10) C12 0.0242(11) 0.0294(12) 0.0226(11) 0.0010(9) 0.0048(9) 0.0000(9) C13 0.0337(12) 0.0272(12) 0.0253(11) -0.0002(9) 0.0128(9) -0.0015(10) C14 0.0404(14) 0.0377(14) 0.0444(14) -0.0104(11) 0.0159(12) -0.0093(11) C15 0.0477(16) 0.0634(19) 0.0526(17) -0.0164(14) 0.0220(13) -0.0228(14) C16 0.082(2) 0.0296(14) 0.0481(16) -0.0035(12) 0.0265(15) -0.0117(14) C17 0.075(2) 0.0354(15) 0.0457(16) 0.0037(12) 0.0148(15) 0.0035(14) C18 0.0526(16) 0.0329(14) 0.0391(14) 0.0034(11) 0.0122(12) 0.0024(12) C19 0.0200(10) 0.0264(11) 0.0192(10) -0.0030(8) 0.0044(8) 0.0020(8) C20 0.0171(10) 0.0303(12) 0.0185(10) 0.0023(8) 0.0029(8) -0.0007(8) C21 0.0201(10) 0.0274(11) 0.0170(10) -0.0024(8) 0.0042(8) 0.0019(8) C22 0.0203(10) 0.0310(12) 0.0246(11) 0.0039(9) 0.0032(9) 0.0006(9) C23 0.0291(13) 0.0607(17) 0.0386(14) 0.0178(12) 0.0057(11) -0.0064(11) C24 0.0378(15) 0.0674(19) 0.0580(17) 0.0185(14) 0.0101(13) -0.0189(13) C25 0.0180(10) 0.0348(12) 0.0258(11) -0.0060(9) 0.0012(9) 0.0030(9) C26 0.0576(16) 0.0402(14) 0.0380(14) -0.0125(11) 0.0192(12) -0.0137(12) C27 0.0703(19) 0.0399(15) 0.0609(19) -0.0159(13) 0.0252(15) -0.0154(14) C28 0.0516(17) 0.0442(16) 0.0528(17) -0.0252(14) -0.0004(13) 0.0024(13) C29 0.0616(18) 0.0582(18) 0.0302(14) -0.0161(13) -0.0013(13) 0.0110(14) C30 0.0442(14) 0.0443(15) 0.0258(12) -0.0044(11) 0.0012(10) 0.0038(11) C31 0.0217(10) 0.0280(12) 0.0193(10) 0.0048(8) 0.0059(8) 0.0024(8) C32 0.0246(11) 0.0386(13) 0.0310(12) -0.0050(10) 0.0078(9) -0.0029(10) C33 0.0223(12) 0.0544(16) 0.0427(14) 0.0014(12) 0.0122(10) 0.0006(11) C34 0.0353(13) 0.0424(15) 0.0452(15) 0.0028(12) 0.0189(11) 0.0132(11) C35 0.0464(15) 0.0340(14) 0.0541(16) -0.0140(12) 0.0161(13) 0.0042(11) C36 0.0268(12) 0.0353(13) 0.0456(14) -0.0073(11) 0.0084(11) -0.0008(10) Cu2 0.02218(18) 0.02585(19) 0.01639(17) -0.00325(14) -0.00273(14) 0.00271(15) O3 0.0397(9) 0.0453(10) 0.0281(8) -0.0156(7) -0.0097(7) 0.0199(7) N9 0.0244(9) 0.0239(9) 0.0181(9) -0.0029(7) -0.0028(7) 0.0052(7) N10 0.0238(9) 0.0306(10) 0.0168(9) -0.0078(8) -0.0038(7) 0.0051(8) N11 0.0218(9) 0.0246(9) 0.0153(8) -0.0010(7) 0.0001(7) 0.0017(7) N12 0.0196(9) 0.0354(10) 0.0209(9) -0.0046(8) -0.0014(7) 0.0059(7) C37 0.0315(12) 0.0297(12) 0.0210(11) -0.0013(9) -0.0035(9) 0.0056(9) C38 0.0255(11) 0.0284(11) 0.0185(10) -0.0044(9) -0.0015(8) 0.0064(9) C39 0.0253(11) 0.0230(11) 0.0146(10) 0.0027(8) 0.0008(8) 0.0011(8) C40 0.0245(11) 0.0235(11) 0.0173(10) 0.0024(8) 0.0039(8) 0.0002(8) C41 0.0283(11) 0.0328(12) 0.0207(11) -0.0026(9) 0.0029(9) 0.0040(9) C42 0.0334(13) 0.0607(17) 0.0345(13) -0.0083(12) 0.0056(11) 0.0132(12) C43 0.0301(12) 0.0379(13) 0.0170(11) -0.0024(9) 0.0020(9) 0.0043(10) C44 0.0427(15) 0.0412(15) 0.0350(14) 0.0003(11) 0.0092(11) 0.0038(11) C45 0.0612(18) 0.0509(17) 0.0424(15) -0.0035(13) 0.0174(14) -0.0127(14) C46 0.0448(16) 0.091(2) 0.0448(16) -0.0005(16) 0.0215(13) -0.0011(16) C47 0.0600(19) 0.086(2) 0.066(2) 0.0161(17) 0.0369(16) 0.0307(17) C48 0.0512(16) 0.0492(16) 0.0461(15) 0.0080(12) 0.0265(13) 0.0180(13) C49 0.0251(11) 0.0293(12) 0.0217(11) -0.0028(9) 0.0033(9) 0.0071(9) C50 0.0319(12) 0.0334(13) 0.0268(12) 0.0000(10) 0.0022(9) 0.0053(10) C51 0.0448(15) 0.0432(15) 0.0250(12) 0.0041(10) 0.0047(11) 0.0122(12) C52 0.0627(17) 0.0367(14) 0.0365(14) 0.0077(11) 0.0242(13) 0.0140(13) C53 0.0514(16) 0.0322(14) 0.0529(16) -0.0056(12) 0.0248(13) -0.0033(11) C54 0.0324(13) 0.0350(13) 0.0356(13) -0.0041(10) 0.0052(10) 0.0028(10) Cu3 0.01751(17) 0.02311(18) 0.01398(16) 0.00056(14) 0.00060(13) -0.00138(14) O4 0.0206(7) 0.0306(8) 0.0216(7) 0.0041(6) 0.0042(6) -0.0004(6) N13 0.0185(8) 0.0251(9) 0.0148(8) 0.0007(6) 0.0020(7) -0.0017(7) N14 0.0184(9) 0.0474(12) 0.0131(9) 0.0054(8) 0.0005(7) -0.0001(8) N15 0.0199(9) 0.0306(10) 0.0158(8) 0.0010(7) 0.0022(7) -0.0022(7) N16 0.0162(8) 0.0308(10) 0.0194(9) 0.0017(7) 0.0019(7) 0.0000(7) C55 0.0209(10) 0.0225(10) 0.0175(10) -0.0026(8) 0.0016(8) 0.0005(8) C56 0.0192(11) 0.0392(13) 0.0167(10) 0.0023(9) 0.0014(8) -0.0011(9) C57 0.0230(10) 0.0233(11) 0.0160(10) -0.0027(8) 0.0001(8) -0.0009(8) C58 0.0231(10) 0.0232(11) 0.0178(10) -0.0029(8) 0.0034(8) -0.0044(8) C59 0.0264(12) 0.0463(14) 0.0218(11) 0.0050(10) 0.0045(9) -0.0053(10) C60 0.0388(15) 0.0707(19) 0.0555(16) 0.0323(14) 0.0272(13) 0.0132(13) C61 0.0195(10) 0.0439(14) 0.0191(11) 0.0061(9) -0.0002(8) 0.0052(9) C62 0.0255(12) 0.0447(14) 0.0278(12) 0.0054(10) 0.0043(9) 0.0007(10) C63 0.0414(15) 0.0446(15) 0.0454(15) 0.0071(12) 0.0089(12) 0.0114(12) C64 0.0442(16) 0.0591(18) 0.0537(17) 0.0077(14) 0.0186(13) 0.0238(13) C65 0.0349(14) 0.0678(19) 0.0519(16) 0.0167(14) 0.0211(12) 0.0174(13) C66 0.0301(12) 0.0485(15) 0.0372(13) 0.0157(11) 0.0131(10) 0.0100(11) C67 0.0219(11) 0.0511(15) 0.0205(11) -0.0051(10) 0.0049(9) -0.0092(10) C68 0.0433(16) 0.0580(18) 0.0480(16) 0.0156(13) -0.0140(13) -0.0172(13) C69 0.0553(19) 0.087(2) 0.0504(18) 0.0105(17) -0.0225(14) -0.0366(18) C70 0.0462(17) 0.088(2) 0.0568(19) -0.0386(17) 0.0122(15) -0.0282(16) C71 0.0434(17) 0.071(2) 0.103(3) -0.0529(19) 0.0057(17) 0.0001(15) C72 0.0335(14) 0.0618(19) 0.075(2) -0.0388(16) -0.0052(14) 0.0033(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 Cu1 N4 1.9257(18) . ? Cu1 N8 1.9323(18) . ? Cu1 N1 1.9804(16) . ? Cu1 N5 1.9835(15) . ? O1 C1 1.220(2) . ? O2 C19 1.219(2) . ? N1 C3 1.372(2) . ? N1 C1 1.378(2) . ? N2 C3 1.346(2) . ? N2 C2 1.460(2) . ? N2 H3N 0.83(2) . ? N3 C3 1.325(2) . ? N3 C4 1.367(2) . ? N4 C4 1.290(2) . ? N4 H4N 0.79(2) . ? N5 C21 1.378(2) . ? N5 C19 1.378(2) . ? N6 C21 1.337(2) . ? N6 C20 1.449(2) . ? N6 H6N 0.83(2) . ? N7 C21 1.330(2) . ? N7 C22 1.362(2) . ? N8 C22 1.291(2) . ? N8 H8N 0.801(14) . ? C1 C2 1.547(3) . ? C2 C7 1.517(3) . ? C2 C13 1.533(3) . ? C4 C5 1.510(3) . ? C5 C6 1.497(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.377(3) . ? C7 C12 1.397(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.375(3) . ? C13 C18 1.399(3) . ? C14 C15 1.418(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(4) . ? C15 H15 0.9500 . ? C16 C17 1.359(3) . ? C16 H16 0.9500 . ? C17 C18 1.371(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.549(2) . ? C20 C25 1.529(3) . ? C20 C31 1.531(3) . ? C22 C23 1.504(3) . ? C23 C24 1.479(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.380(3) . ? C25 C30 1.386(3) . ? C26 C27 1.380(3) . ? C26 H26 0.9500 . ? C27 C28 1.374(4) . ? C27 H27 0.9500 . ? C28 C29 1.368(4) . ? C28 H28 0.9500 . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.378(3) . ? C31 C36 1.390(3) . ? C32 C33 1.390(3) . ? C32 H32 0.9500 . ? C33 C34 1.371(3) . ? C33 H33 0.9500 . ? C34 C35 1.372(3) . ? C34 H34 0.9500 . ? C35 C36 1.380(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? Cu2 N12 1.9163(16) . ? Cu2 N12 1.9163(16) 3_565 ? Cu2 N9 2.0279(15) 3_565 ? Cu2 N9 2.0279(15) . ? O3 C37 1.215(2) . ? N9 C39 1.378(2) . ? N9 C37 1.388(2) . ? N10 C39 1.343(2) . ? N10 C38 1.454(2) . ? N10 H10N 0.789(18) . ? N11 C39 1.327(2) . ? N11 C40 1.362(2) . ? N12 C40 1.292(2) . ? N12 H12N 0.8800 . ? C37 C38 1.548(3) . ? C38 C43 1.528(3) . ? C38 C49 1.536(3) . ? C40 C41 1.512(3) . ? C41 C42 1.514(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.376(3) . ? C43 C48 1.382(3) . ? C44 C45 1.389(3) . ? C44 H44 0.9500 . ? C45 C46 1.375(4) . ? C45 H45 0.9500 . ? C46 C47 1.370(4) . ? C46 H46 0.9500 . ? C47 C48 1.380(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.373(3) . ? C49 C50 1.390(3) . ? C50 C51 1.385(3) . ? C50 H50 0.9500 . ? C51 C52 1.373(3) . ? C51 H51 0.9500 . ? C52 C53 1.375(3) . ? C52 H52 0.9500 . ? C53 C54 1.393(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? Cu3 N16 1.9247(16) . ? Cu3 N16 1.9247(16) 3_666 ? Cu3 N13 2.0447(15) . ? Cu3 N13 2.0447(15) 3_666 ? O4 C55 1.222(2) . ? N13 C55 1.378(2) . ? N13 C57 1.378(2) . ? N14 C57 1.341(2) . ? N14 C56 1.451(2) . ? N14 H14N 0.800(18) . ? N15 C57 1.325(2) . ? N15 C58 1.362(2) . ? N16 C58 1.293(2) . ? N16 H16N 0.8800 . ? C55 C56 1.552(2) . ? C56 C61 1.524(3) . ? C56 C67 1.536(3) . ? C58 C59 1.511(3) . ? C59 C60 1.501(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.385(3) . ? C61 C66 1.399(3) . ? C62 C63 1.388(3) . ? C62 H62 0.9500 . ? C63 C64 1.382(3) . ? C63 H63 0.9500 . ? C64 C65 1.384(3) . ? C64 H64 0.9500 . ? C65 C66 1.381(3) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.353(3) . ? C67 C68 1.380(3) . ? C68 C69 1.395(4) . ? C68 H68 0.9500 . ? C69 C70 1.378(4) . ? C69 H69 0.9500 . ? C70 C71 1.343(4) . ? C70 H70 0.9500 . ? C71 C72 1.394(3) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? 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 N4 Cu1 N8 160.72(8) . . ? N4 Cu1 N1 87.18(7) . . ? N8 Cu1 N1 93.59(7) . . ? N4 Cu1 N5 94.95(7) . . ? N8 Cu1 N5 87.84(7) . . ? N1 Cu1 N5 169.37(6) . . ? C3 N1 C1 107.21(15) . . ? C3 N1 Cu1 123.65(12) . . ? C1 N1 Cu1 128.08(13) . . ? C3 N2 C2 111.27(16) . . ? C3 N2 H3N 121.3(14) . . ? C2 N2 H3N 126.8(14) . . ? C3 N3 C4 120.52(16) . . ? C4 N4 Cu1 130.93(15) . . ? C4 N4 H4N 114.6(17) . . ? Cu1 N4 H4N 114.4(16) . . ? C21 N5 C19 106.91(15) . . ? C21 N5 Cu1 124.05(12) . . ? C19 N5 Cu1 129.04(13) . . ? C21 N6 C20 111.59(16) . . ? C21 N6 H6N 122.6(14) . . ? C20 N6 H6N 125.8(14) . . ? C21 N7 C22 121.08(16) . . ? C22 N8 Cu1 131.84(15) . . ? C22 N8 H8N 110.5(15) . . ? Cu1 N8 H8N 116.6(15) . . ? O1 C1 N1 126.41(18) . . ? O1 C1 C2 123.63(18) . . ? N1 C1 C2 109.94(16) . . ? N2 C2 C7 113.27(16) . . ? N2 C2 C13 110.19(16) . . ? C7 C2 C13 114.46(16) . . ? N2 C2 C1 99.23(15) . . ? C7 C2 C1 109.15(16) . . ? C13 C2 C1 109.42(16) . . ? N3 C3 N2 119.02(17) . . ? N3 C3 N1 128.72(17) . . ? N2 C3 N1 112.25(17) . . ? N4 C4 N3 125.57(18) . . ? N4 C4 C5 121.39(18) . . ? N3 C4 C5 113.04(16) . . ? C6 C5 C4 117.31(18) . . ? C6 C5 H5A 108.0 . . ? C4 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? C4 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.79(18) . . ? C8 C7 C2 120.90(17) . . ? C12 C7 C2 120.28(17) . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.6(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.7(2) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 120.53(19) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C14 C13 C18 119.0(2) . . ? C14 C13 C2 122.82(19) . . ? C18 C13 C2 118.19(19) . . ? C13 C14 C15 119.5(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.5(2) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 121.0(2) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 121.1(2) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? O2 C19 N5 126.71(17) . . ? O2 C19 C20 123.59(17) . . ? N5 C19 C20 109.69(16) . . ? N6 C20 C25 112.19(16) . . ? N6 C20 C31 110.80(16) . . ? C25 C20 C31 114.73(16) . . ? N6 C20 C19 99.41(15) . . ? C25 C20 C19 109.84(16) . . ? C31 C20 C19 108.74(15) . . ? N7 C21 N6 118.34(17) . . ? N7 C21 N5 129.36(17) . . ? N6 C21 N5 112.30(17) . . ? N8 C22 N7 125.35(19) . . ? N8 C22 C23 122.18(18) . . ? N7 C22 C23 112.47(17) . . ? C24 C23 C22 118.68(19) . . ? C24 C23 H23A 107.6 . . ? C22 C23 H23A 107.6 . . ? C24 C23 H23B 107.6 . . ? C22 C23 H23B 107.6 . . ? H23A C23 H23B 107.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.4(2) . . ? C26 C25 C20 120.60(18) . . ? C30 C25 C20 121.0(2) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.5(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 119.0(2) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 121.1(2) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C25 C30 C29 120.0(2) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C36 118.41(19) . . ? C32 C31 C20 123.75(18) . . ? C36 C31 C20 117.84(17) . . ? C31 C32 C33 120.5(2) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.5(2) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.7(2) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? N12 Cu2 N12 180.00(10) . 3_565 ? N12 Cu2 N9 92.34(6) . 3_565 ? N12 Cu2 N9 87.66(6) 3_565 3_565 ? N12 Cu2 N9 87.66(6) . . ? N12 Cu2 N9 92.34(6) 3_565 . ? N9 Cu2 N9 180.00(9) 3_565 . ? C39 N9 C37 106.87(16) . . ? C39 N9 Cu2 122.10(13) . . ? C37 N9 Cu2 130.58(13) . . ? C39 N10 C38 111.66(16) . . ? C39 N10 H10N 123.5(14) . . ? C38 N10 H10N 123.2(14) . . ? C39 N11 C40 121.17(16) . . ? C40 N12 Cu2 132.30(14) . . ? C40 N12 H12N 113.9 . . ? Cu2 N12 H12N 113.8 . . ? O3 C37 N9 127.38(18) . . ? O3 C37 C38 122.87(18) . . ? N9 C37 C38 109.75(16) . . ? N10 C38 C43 111.83(17) . . ? N10 C38 C49 108.92(16) . . ? C43 C38 C49 113.61(16) . . ? N10 C38 C37 98.97(15) . . ? C43 C38 C37 110.56(16) . . ? C49 C38 C37 112.02(16) . . ? N11 C39 N10 118.39(17) . . ? N11 C39 N9 129.80(17) . . ? N10 C39 N9 111.81(17) . . ? N12 C40 N11 125.55(18) . . ? N12 C40 C41 121.10(17) . . ? N11 C40 C41 113.29(16) . . ? C40 C41 C42 116.39(17) . . ? C40 C41 H41A 108.2 . . ? C42 C41 H41A 108.2 . . ? C40 C41 H41B 108.2 . . ? C42 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 118.6(2) . . ? C44 C43 C38 120.86(19) . . ? C48 C43 C38 120.6(2) . . ? C43 C44 C45 121.0(2) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 120.1(3) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C45 118.9(3) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 121.3(3) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 120.2(2) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C54 C49 C50 118.9(2) . . ? C54 C49 C38 122.89(18) . . ? C50 C49 C38 118.06(18) . . ? C51 C50 C49 120.5(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 120.3(2) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 119.5(2) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C54 120.4(2) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C49 C54 C53 120.3(2) . . ? C49 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? N16 Cu3 N16 180.00(9) . 3_666 ? N16 Cu3 N13 87.64(6) . . ? N16 Cu3 N13 92.36(6) 3_666 . ? N16 Cu3 N13 92.36(6) . 3_666 ? N16 Cu3 N13 87.64(6) 3_666 3_666 ? N13 Cu3 N13 180.000(1) . 3_666 ? C55 N13 C57 106.31(15) . . ? C55 N13 Cu3 131.02(12) . . ? C57 N13 Cu3 122.64(12) . . ? C57 N14 C56 111.74(16) . . ? C57 N14 H14N 122.1(14) . . ? C56 N14 H14N 122.5(14) . . ? C57 N15 C58 121.63(16) . . ? C58 N16 Cu3 132.04(14) . . ? C58 N16 H16N 114.0 . . ? Cu3 N16 H16N 114.0 . . ? O4 C55 N13 127.00(17) . . ? O4 C55 C56 122.56(17) . . ? N13 C55 C56 110.44(16) . . ? N14 C56 C61 112.36(17) . . ? N14 C56 C67 109.60(16) . . ? C61 C56 C67 113.55(17) . . ? N14 C56 C55 98.81(15) . . ? C61 C56 C55 109.52(15) . . ? C67 C56 C55 112.09(17) . . ? N15 C57 N14 117.93(17) . . ? N15 C57 N13 129.65(17) . . ? N14 C57 N13 112.42(17) . . ? N16 C58 N15 125.96(18) . . ? N16 C58 C59 122.14(17) . . ? N15 C58 C59 111.89(16) . . ? C60 C59 C58 118.34(17) . . ? C60 C59 H59A 107.7 . . ? C58 C59 H59A 107.7 . . ? C60 C59 H59B 107.7 . . ? C58 C59 H59B 107.7 . . ? H59A C59 H59B 107.1 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C66 118.6(2) . . ? C62 C61 C56 121.83(19) . . ? C66 C61 C56 119.5(2) . . ? C61 C62 C63 120.5(2) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 120.4(2) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 119.6(2) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C66 C65 C64 120.2(2) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C61 120.7(2) . . ? C65 C66 H66 119.6 . . ? C61 C66 H66 119.6 . . ? C72 C67 C68 118.6(2) . . ? C72 C67 C56 122.0(2) . . ? C68 C67 C56 119.0(2) . . ? C67 C68 C69 120.2(3) . . ? C67 C68 H68 119.9 . . ? C69 C68 H68 119.9 . . ? C70 C69 C68 120.3(3) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C71 C70 C69 118.8(3) . . ? C71 C70 H70 120.6 . . ? C69 C70 H70 120.6 . . ? C70 C71 C72 121.2(3) . . ? C70 C71 H71 119.4 . . ? C72 C71 H71 119.4 . . ? C67 C72 C71 120.9(2) . . ? C67 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C3 18.05(16) . . . . ? N8 Cu1 N1 C3 -142.65(16) . . . . ? N5 Cu1 N1 C3 119.9(3) . . . . ? N4 Cu1 N1 C1 -175.24(17) . . . . ? N8 Cu1 N1 C1 24.05(17) . . . . ? N5 Cu1 N1 C1 -73.4(4) . . . . ? N8 Cu1 N4 C4 76.9(3) . . . . ? N1 Cu1 N4 C4 -15.9(2) . . . . ? N5 Cu1 N4 C4 174.6(2) . . . . ? N4 Cu1 N5 C21 -162.98(15) . . . . ? N8 Cu1 N5 C21 -2.10(15) . . . . ? N1 Cu1 N5 C21 95.8(4) . . . . ? N4 Cu1 N5 C19 16.52(17) . . . . ? N8 Cu1 N5 C19 177.41(17) . . . . ? N1 Cu1 N5 C19 -84.7(4) . . . . ? N4 Cu1 N8 C22 106.2(3) . . . . ? N1 Cu1 N8 C22 -162.1(2) . . . . ? N5 Cu1 N8 C22 7.3(2) . . . . ? C3 N1 C1 O1 -179.1(2) . . . . ? Cu1 N1 C1 O1 12.4(3) . . . . ? C3 N1 C1 C2 2.5(2) . . . . ? Cu1 N1 C1 C2 -165.90(12) . . . . ? C3 N2 C2 C7 118.23(18) . . . . ? C3 N2 C2 C13 -112.10(18) . . . . ? C3 N2 C2 C1 2.7(2) . . . . ? O1 C1 C2 N2 178.49(19) . . . . ? N1 C1 C2 N2 -3.1(2) . . . . ? O1 C1 C2 C7 59.8(3) . . . . ? N1 C1 C2 C7 -121.83(17) . . . . ? O1 C1 C2 C13 -66.2(2) . . . . ? N1 C1 C2 C13 112.21(18) . . . . ? C4 N3 C3 N2 174.40(18) . . . . ? C4 N3 C3 N1 -5.1(3) . . . . ? C2 N2 C3 N3 179.00(17) . . . . ? C2 N2 C3 N1 -1.4(2) . . . . ? C1 N1 C3 N3 178.8(2) . . . . ? Cu1 N1 C3 N3 -12.2(3) . . . . ? C1 N1 C3 N2 -0.8(2) . . . . ? Cu1 N1 C3 N2 168.28(13) . . . . ? Cu1 N4 C4 N3 5.1(3) . . . . ? Cu1 N4 C4 C5 -175.29(16) . . . . ? C3 N3 C4 N4 9.5(3) . . . . ? C3 N3 C4 C5 -170.15(18) . . . . ? N4 C4 C5 C6 11.4(3) . . . . ? N3 C4 C5 C6 -169.0(2) . . . . ? N2 C2 C7 C8 -10.6(3) . . . . ? C13 C2 C7 C8 -138.08(18) . . . . ? C1 C2 C7 C8 98.9(2) . . . . ? N2 C2 C7 C12 171.41(16) . . . . ? C13 C2 C7 C12 43.9(2) . . . . ? C1 C2 C7 C12 -79.1(2) . . . . ? C12 C7 C8 C9 -4.2(3) . . . . ? C2 C7 C8 C9 177.81(19) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C8 C9 C10 C11 2.1(4) . . . . ? C9 C10 C11 C12 -1.7(3) . . . . ? C10 C11 C12 C7 -1.6(3) . . . . ? C8 C7 C12 C11 4.6(3) . . . . ? C2 C7 C12 C11 -177.40(18) . . . . ? N2 C2 C13 C14 -105.9(2) . . . . ? C7 C2 C13 C14 23.2(3) . . . . ? C1 C2 C13 C14 146.0(2) . . . . ? N2 C2 C13 C18 72.7(2) . . . . ? C7 C2 C13 C18 -158.28(18) . . . . ? C1 C2 C13 C18 -35.4(2) . . . . ? C18 C13 C14 C15 2.1(3) . . . . ? C2 C13 C14 C15 -179.3(2) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 -2.1(4) . . . . ? C15 C16 C17 C18 2.1(4) . . . . ? C16 C17 C18 C13 0.1(4) . . . . ? C14 C13 C18 C17 -2.1(3) . . . . ? C2 C13 C18 C17 179.2(2) . . . . ? C21 N5 C19 O2 178.66(19) . . . . ? Cu1 N5 C19 O2 -0.9(3) . . . . ? C21 N5 C19 C20 -0.5(2) . . . . ? Cu1 N5 C19 C20 179.91(12) . . . . ? C21 N6 C20 C25 112.91(18) . . . . ? C21 N6 C20 C31 -117.43(18) . . . . ? C21 N6 C20 C19 -3.1(2) . . . . ? O2 C19 C20 N6 -177.05(18) . . . . ? N5 C19 C20 N6 2.17(19) . . . . ? O2 C19 C20 C25 65.1(2) . . . . ? N5 C19 C20 C25 -115.66(18) . . . . ? O2 C19 C20 C31 -61.2(2) . . . . ? N5 C19 C20 C31 118.03(17) . . . . ? C22 N7 C21 N6 -176.53(18) . . . . ? C22 N7 C21 N5 4.1(3) . . . . ? C20 N6 C21 N7 -176.24(17) . . . . ? C20 N6 C21 N5 3.2(2) . . . . ? C19 N5 C21 N7 177.79(19) . . . . ? Cu1 N5 C21 N7 -2.6(3) . . . . ? C19 N5 C21 N6 -1.6(2) . . . . ? Cu1 N5 C21 N6 178.01(12) . . . . ? Cu1 N8 C22 N7 -8.1(3) . . . . ? Cu1 N8 C22 C23 172.27(17) . . . . ? C21 N7 C22 N8 1.3(3) . . . . ? C21 N7 C22 C23 -179.09(19) . . . . ? N8 C22 C23 C24 6.6(4) . . . . ? N7 C22 C23 C24 -173.0(2) . . . . ? N6 C20 C25 C26 -166.61(19) . . . . ? C31 C20 C25 C26 65.8(2) . . . . ? C19 C20 C25 C26 -57.0(2) . . . . ? N6 C20 C25 C30 12.2(3) . . . . ? C31 C20 C25 C30 -115.4(2) . . . . ? C19 C20 C25 C30 121.8(2) . . . . ? C30 C25 C26 C27 0.5(3) . . . . ? C20 C25 C26 C27 179.4(2) . . . . ? C25 C26 C27 C28 0.0(4) . . . . ? C26 C27 C28 C29 -0.5(4) . . . . ? C27 C28 C29 C30 0.4(4) . . . . ? C26 C25 C30 C29 -0.6(3) . . . . ? C20 C25 C30 C29 -179.4(2) . . . . ? C28 C29 C30 C25 0.1(4) . . . . ? N6 C20 C31 C32 -124.9(2) . . . . ? C25 C20 C31 C32 3.4(3) . . . . ? C19 C20 C31 C32 126.8(2) . . . . ? N6 C20 C31 C36 55.5(2) . . . . ? C25 C20 C31 C36 -176.16(18) . . . . ? C19 C20 C31 C36 -52.7(2) . . . . ? C36 C31 C32 C33 0.6(3) . . . . ? C20 C31 C32 C33 -178.93(19) . . . . ? C31 C32 C33 C34 -0.6(3) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C31 0.0(4) . . . . ? C32 C31 C36 C35 -0.4(3) . . . . ? C20 C31 C36 C35 179.2(2) . . . . ? N12 Cu2 N9 C39 -12.28(15) . . . . ? N12 Cu2 N9 C39 167.72(15) 3_565 . . . ? N9 Cu2 N9 C39 -154(100) 3_565 . . . ? N12 Cu2 N9 C37 176.52(18) . . . . ? N12 Cu2 N9 C37 -3.48(18) 3_565 . . . ? N9 Cu2 N9 C37 34(100) 3_565 . . . ? N12 Cu2 N12 C40 114(91) 3_565 . . . ? N9 Cu2 N12 C40 -171.11(19) 3_565 . . . ? N9 Cu2 N12 C40 8.89(19) . . . . ? C39 N9 C37 O3 -178.0(2) . . . . ? Cu2 N9 C37 O3 -5.8(3) . . . . ? C39 N9 C37 C38 1.9(2) . . . . ? Cu2 N9 C37 C38 174.08(13) . . . . ? C39 N10 C38 C43 126.13(18) . . . . ? C39 N10 C38 C49 -107.47(18) . . . . ? C39 N10 C38 C37 9.6(2) . . . . ? O3 C37 C38 N10 173.1(2) . . . . ? N9 C37 C38 N10 -6.8(2) . . . . ? O3 C37 C38 C43 55.6(3) . . . . ? N9 C37 C38 C43 -124.25(19) . . . . ? O3 C37 C38 C49 -72.2(3) . . . . ? N9 C37 C38 C49 107.93(19) . . . . ? C40 N11 C39 N10 178.87(17) . . . . ? C40 N11 C39 N9 -1.2(3) . . . . ? C38 N10 C39 N11 170.31(17) . . . . ? C38 N10 C39 N9 -9.7(2) . . . . ? C37 N9 C39 N11 -175.4(2) . . . . ? Cu2 N9 C39 N11 11.6(3) . . . . ? C37 N9 C39 N10 4.6(2) . . . . ? Cu2 N9 C39 N10 -168.45(13) . . . . ? Cu2 N12 C40 N11 -2.0(3) . . . . ? Cu2 N12 C40 C41 174.86(14) . . . . ? C39 N11 C40 N12 -4.6(3) . . . . ? C39 N11 C40 C41 178.30(17) . . . . ? N12 C40 C41 C42 28.8(3) . . . . ? N11 C40 C41 C42 -153.95(18) . . . . ? N10 C38 C43 C44 -30.1(3) . . . . ? C49 C38 C43 C44 -153.89(19) . . . . ? C37 C38 C43 C44 79.2(2) . . . . ? N10 C38 C43 C48 149.68(19) . . . . ? C49 C38 C43 C48 25.9(3) . . . . ? C37 C38 C43 C48 -101.1(2) . . . . ? C48 C43 C44 C45 -0.6(3) . . . . ? C38 C43 C44 C45 179.2(2) . . . . ? C43 C44 C45 C46 -0.6(4) . . . . ? C44 C45 C46 C47 0.3(4) . . . . ? C45 C46 C47 C48 1.3(4) . . . . ? C46 C47 C48 C43 -2.5(4) . . . . ? C44 C43 C48 C47 2.1(4) . . . . ? C38 C43 C48 C47 -177.7(2) . . . . ? N10 C38 C49 C54 104.4(2) . . . . ? C43 C38 C49 C54 -130.2(2) . . . . ? C37 C38 C49 C54 -4.0(3) . . . . ? N10 C38 C49 C50 -71.6(2) . . . . ? C43 C38 C49 C50 53.8(2) . . . . ? C37 C38 C49 C50 180.00(18) . . . . ? C54 C49 C50 C51 -0.4(3) . . . . ? C38 C49 C50 C51 175.73(18) . . . . ? C49 C50 C51 C52 0.5(3) . . . . ? C50 C51 C52 C53 -0.5(3) . . . . ? C51 C52 C53 C54 0.4(3) . . . . ? C50 C49 C54 C53 0.3(3) . . . . ? C38 C49 C54 C53 -175.61(19) . . . . ? C52 C53 C54 C49 -0.3(3) . . . . ? N16 Cu3 N13 C55 172.13(17) . . . . ? N16 Cu3 N13 C55 -7.87(17) 3_666 . . . ? N13 Cu3 N13 C55 75(100) 3_666 . . . ? N16 Cu3 N13 C57 -5.41(14) . . . . ? N16 Cu3 N13 C57 174.59(14) 3_666 . . . ? N13 Cu3 N13 C57 -103(100) 3_666 . . . ? N16 Cu3 N16 C58 85(100) 3_666 . . . ? N13 Cu3 N16 C58 7.52(18) . . . . ? N13 Cu3 N16 C58 -172.48(18) 3_666 . . . ? C57 N13 C55 O4 177.69(19) . . . . ? Cu3 N13 C55 O4 -0.2(3) . . . . ? C57 N13 C55 C56 -2.4(2) . . . . ? Cu3 N13 C55 C56 179.77(12) . . . . ? C57 N14 C56 C61 119.15(18) . . . . ? C57 N14 C56 C67 -113.62(19) . . . . ? C57 N14 C56 C55 3.7(2) . . . . ? O4 C55 C56 N14 179.23(18) . . . . ? N13 C55 C56 N14 -0.7(2) . . . . ? O4 C55 C56 C61 61.6(2) . . . . ? N13 C55 C56 C61 -118.30(18) . . . . ? O4 C55 C56 C67 -65.3(2) . . . . ? N13 C55 C56 C67 114.73(18) . . . . ? C58 N15 C57 N14 -179.29(17) . . . . ? C58 N15 C57 N13 0.8(3) . . . . ? C56 N14 C57 N15 174.37(17) . . . . ? C56 N14 C57 N13 -5.7(2) . . . . ? C55 N13 C57 N15 -175.16(19) . . . . ? Cu3 N13 C57 N15 2.9(3) . . . . ? C55 N13 C57 N14 5.0(2) . . . . ? Cu3 N13 C57 N14 -176.96(13) . . . . ? Cu3 N16 C58 N15 -6.4(3) . . . . ? Cu3 N16 C58 C59 172.55(14) . . . . ? C57 N15 C58 N16 0.6(3) . . . . ? C57 N15 C58 C59 -178.51(17) . . . . ? N16 C58 C59 C60 6.0(3) . . . . ? N15 C58 C59 C60 -174.9(2) . . . . ? N14 C56 C61 C62 -6.4(3) . . . . ? C67 C56 C61 C62 -131.5(2) . . . . ? C55 C56 C61 C62 102.3(2) . . . . ? N14 C56 C61 C66 175.47(17) . . . . ? C67 C56 C61 C66 50.4(2) . . . . ? C55 C56 C61 C66 -75.8(2) . . . . ? C66 C61 C62 C63 -0.1(3) . . . . ? C56 C61 C62 C63 -178.22(19) . . . . ? C61 C62 C63 C64 0.6(3) . . . . ? C62 C63 C64 C65 -0.5(4) . . . . ? C63 C64 C65 C66 -0.1(4) . . . . ? C64 C65 C66 C61 0.6(4) . . . . ? C62 C61 C66 C65 -0.5(3) . . . . ? C56 C61 C66 C65 177.7(2) . . . . ? N14 C56 C67 C72 85.3(3) . . . . ? C61 C56 C67 C72 -148.2(2) . . . . ? C55 C56 C67 C72 -23.4(3) . . . . ? N14 C56 C67 C68 -87.8(2) . . . . ? C61 C56 C67 C68 38.7(3) . . . . ? C55 C56 C67 C68 163.5(2) . . . . ? C72 C67 C68 C69 -0.9(4) . . . . ? C56 C67 C68 C69 172.4(2) . . . . ? C67 C68 C69 C70 1.4(4) . . . . ? C68 C69 C70 C71 0.0(5) . . . . ? C69 C70 C71 C72 -1.7(5) . . . . ? C68 C67 C72 C71 -0.8(4) . . . . ? C56 C67 C72 C71 -174.0(2) . . . . ? C70 C71 C72 C67 2.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4N O2 0.79(2) 2.12(2) 2.800(2) 144(2) . N2 H3N N7 0.83(2) 2.14(2) 2.971(2) 178(2) 4_565 N8 H8N O1 0.801(14) 2.306(19) 2.866(2) 127.6(19) . N6 H6N N3 0.83(2) 2.09(2) 2.908(2) 170.6(19) 4_666 N10 H10N N15 0.789(18) 2.141(19) 2.927(2) 174.5(18) . N12 H12N O3 0.88 2.01 2.787(2) 146.1 3_565 N14 H14N N11 0.800(18) 2.122(19) 2.916(2) 171.7(19) . N16 H16N O4 0.88 2.04 2.807(2) 145.4 3_666 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.665 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.058 #===END data_lfl46 _database_code_CSD 190105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Cu N8 O4 S2' _chemical_formula_weight 830.51 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.592(5) _cell_length_b 16.662(5) _cell_length_c 10.435(5) _cell_angle_alpha 93.233(5) _cell_angle_beta 94.704(5) _cell_angle_gamma 99.777(5) _cell_volume 1974.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 825 _cell_measurement_theta_min 2.487 _cell_measurement_theta_max 24.874 _exptl_crystal_description columnar _exptl_crystal_colour red _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 93 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.014 _diffrn_reflns_number 19578 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9136 _reflns_number_gt 5806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976) WinGX (Farrugia, 1999) ; _computing_publication_material ? _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^)] 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 9136 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.002 _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 0.99668(3) 0.257072(19) 0.24745(3) 0.02210(9) Uani 1 1 d . . . O1 O 1.18340(14) 0.23328(10) 0.51624(15) 0.0258(4) Uani 1 1 d . . . O2 O 0.83666(15) 0.29865(10) -0.03032(15) 0.0286(4) Uani 1 1 d . . . N1 N 1.12302(17) 0.19166(11) 0.30102(18) 0.0214(5) Uani 1 1 d . . . N2 N 1.23021(17) 0.08798(12) 0.27367(19) 0.0269(5) Uani 1 1 d . . . H2N H 1.2570 0.0474 0.2353 0.032 Uiso 0.25 1 calc PR . . N3 N 1.11684(19) 0.11358(14) 0.0957(2) 0.0284(6) Uani 1 1 d . . . H3N H 1.145(3) 0.0723(17) 0.061(3) 0.024(10) Uiso 0.75 1 d P . . N4 N 0.9984(2) 0.21110(14) 0.0740(2) 0.0266(6) Uani 1 1 d . . . H4N H 0.961(2) 0.2329(14) 0.022(2) 0.021(8) Uiso 1 1 d . . . N5 N 0.86829(17) 0.32035(11) 0.19309(18) 0.0198(5) Uani 1 1 d . . . N6 N 0.71993(18) 0.38921(13) 0.2242(2) 0.0232(5) Uani 1 1 d . . . H6N H 0.6788(17) 0.4197(12) 0.2670(18) 0.010(6) Uiso 1 1 d . . . N7 N 0.84146(17) 0.38201(12) 0.40565(18) 0.0236(5) Uani 1 1 d . . . N8 N 0.9929(2) 0.30307(13) 0.4197(2) 0.0260(6) Uani 1 1 d . . . H8N H 1.0422(19) 0.2894(13) 0.471(2) 0.023(8) Uiso 1 1 d . . . C1 C 1.1854(2) 0.18994(15) 0.4172(2) 0.0219(6) Uani 1 1 d . . . C2 C 1.2606(2) 0.12173(15) 0.4071(2) 0.0242(6) Uani 1 1 d . . . C3 C 1.1559(2) 0.13006(15) 0.2235(3) 0.0278(7) Uani 1 1 d . . . C4 C 1.0463(2) 0.15391(16) 0.0242(2) 0.0241(6) Uani 1 1 d . . . C5 C 1.0274(2) 0.12610(16) -0.1160(2) 0.0359(7) Uani 1 1 d . . . H5A H 0.9500 0.0898 -0.1330 0.043 Uiso 1 1 calc R . . H5B H 1.0884 0.0937 -0.1368 0.043 Uiso 1 1 calc R . . C6 C 1.0314(3) 0.19520(17) -0.2043(2) 0.0519(9) Uani 1 1 d . . . H6A H 0.9651 0.2235 -0.1921 0.078 Uiso 1 1 calc R . . H6B H 1.0262 0.1732 -0.2941 0.078 Uiso 1 1 calc R . . H6C H 1.1054 0.2337 -0.1839 0.078 Uiso 1 1 calc R . . C7 C 1.2225(2) 0.05839(15) 0.5032(3) 0.0251(6) Uani 1 1 d . . . C8 C 1.1450(2) -0.01370(16) 0.4658(3) 0.0314(7) Uani 1 1 d . . . H18 H 1.1155 -0.0254 0.3779 0.038 Uiso 1 1 calc R . . C9 C 1.1100(2) -0.06900(16) 0.5565(3) 0.0367(7) Uani 1 1 d . . . H17 H 1.0579 -0.1186 0.5297 0.044 Uiso 1 1 calc R . . C10 C 1.1500(2) -0.05227(16) 0.6836(3) 0.0375(7) Uani 1 1 d . . . H16 H 1.1252 -0.0898 0.7453 0.045 Uiso 1 1 calc R . . C11 C 1.2265(2) 0.01932(16) 0.7219(3) 0.0373(7) Uani 1 1 d . . . H15 H 1.2550 0.0311 0.8101 0.045 Uiso 1 1 calc R . . C12 C 1.2619(2) 0.07424(16) 0.6315(3) 0.0325(7) Uani 1 1 d . . . H14 H 1.3143 0.1236 0.6589 0.039 Uiso 1 1 calc R . . C13 C 1.3930(2) 0.15362(15) 0.4284(2) 0.0238(6) Uani 1 1 d . . . C14 C 1.4687(2) 0.09740(16) 0.4212(3) 0.0361(7) Uani 1 1 d . . . H12 H 1.4369 0.0409 0.4061 0.043 Uiso 1 1 calc R . . C15 C 1.5887(2) 0.12196(17) 0.4356(3) 0.0417(8) Uani 1 1 d . . . H11 H 1.6388 0.0826 0.4297 0.050 Uiso 1 1 calc R . . C16 C 1.6366(2) 0.20380(17) 0.4586(2) 0.0357(7) Uani 1 1 d . . . H10 H 1.7195 0.2208 0.4689 0.043 Uiso 1 1 calc R . . C17 C 1.5635(2) 0.26021(17) 0.4664(2) 0.0350(7) Uani 1 1 d . . . H9 H 1.5957 0.3166 0.4821 0.042 Uiso 1 1 calc R . . C18 C 1.4420(2) 0.23467(16) 0.4512(2) 0.0300(7) Uani 1 1 d . . . H8 H 1.3920 0.2742 0.4568 0.036 Uiso 1 1 calc R . . C19 C 0.8121(2) 0.32575(14) 0.0744(2) 0.0218(6) Uani 1 1 d . . . C20 C 0.7096(2) 0.37315(14) 0.0856(2) 0.0210(6) Uani 1 1 d . . . C21 C 0.8134(2) 0.36295(14) 0.2811(2) 0.0216(6) Uani 1 1 d . . . C22 C 0.9321(2) 0.35362(15) 0.4679(2) 0.0240(6) Uani 1 1 d . . . C23 C 0.9593(2) 0.38765(18) 0.6069(2) 0.0403(8) Uani 1 1 d . . . H23A H 1.0170 0.3580 0.6498 0.048 Uiso 1 1 calc R . . H23B H 0.9969 0.4457 0.6080 0.048 Uiso 1 1 calc R . . C24 C 0.8560(3) 0.3823(2) 0.6832(3) 0.0650(11) Uani 1 1 d . . . H24A H 0.7963 0.4090 0.6396 0.098 Uiso 1 1 calc R . . H24B H 0.8805 0.4096 0.7692 0.098 Uiso 1 1 calc R . . H24C H 0.8231 0.3248 0.6913 0.098 Uiso 1 1 calc R . . C25 C 0.5944(2) 0.31844(14) 0.0330(2) 0.0241(6) Uani 1 1 d . . . C26 C 0.5134(2) 0.28524(15) 0.1137(3) 0.0288(7) Uani 1 1 d . . . H36 H 0.5284 0.2976 0.2042 0.035 Uiso 1 1 calc R . . C27 C 0.4104(2) 0.23399(16) 0.0641(3) 0.0369(7) Uani 1 1 d . . . H35 H 0.3548 0.2121 0.1206 0.044 Uiso 1 1 calc R . . C28 C 0.3882(2) 0.21475(16) -0.0671(3) 0.0406(8) Uani 1 1 d . . . H34 H 0.3176 0.1798 -0.1010 0.049 Uiso 1 1 calc R . . C29 C 0.4693(2) 0.24670(16) -0.1487(3) 0.0379(7) Uani 1 1 d . . . H33 H 0.4540 0.2342 -0.2390 0.046 Uiso 1 1 calc R . . C30 C 0.5733(2) 0.29707(15) -0.0991(2) 0.0314(7) Uani 1 1 d . . . H32 H 0.6302 0.3170 -0.1554 0.038 Uiso 1 1 calc R . . C31 C 0.7343(2) 0.45442(15) 0.0210(2) 0.0220(6) Uani 1 1 d . . . C32 C 0.6474(2) 0.48508(15) -0.0504(2) 0.0273(6) Uani 1 1 d . . . H30 H 0.5703 0.4539 -0.0651 0.033 Uiso 1 1 calc R . . C33 C 0.6717(2) 0.56066(16) -0.1006(2) 0.0324(7) Uani 1 1 d . . . H29 H 0.6116 0.5806 -0.1504 0.039 Uiso 1 1 calc R . . C34 C 0.7826(2) 0.60712(16) -0.0787(3) 0.0350(7) Uani 1 1 d . . . H28 H 0.7989 0.6592 -0.1126 0.042 Uiso 1 1 calc R . . C35 C 0.8702(2) 0.57785(15) -0.0074(2) 0.0322(7) Uani 1 1 d . . . H27 H 0.9469 0.6096 0.0081 0.039 Uiso 1 1 calc R . . C36 C 0.8455(2) 0.50194(15) 0.0414(2) 0.0281(7) Uani 1 1 d . . . H26 H 0.9062 0.4819 0.0899 0.034 Uiso 1 1 calc R . . S1 S 0.60022(6) 0.56282(4) 0.38736(7) 0.03360(19) Uani 1 1 d . . . O3 O 0.56004(14) 0.47499(10) 0.33492(16) 0.0347(5) Uani 1 1 d . . . C37 C 0.7012(2) 0.60846(15) 0.2813(2) 0.0412(8) Uani 1 1 d . . . H37A H 0.6600 0.6093 0.1956 0.062 Uiso 1 1 calc R . . H37B H 0.7646 0.5767 0.2751 0.062 Uiso 1 1 calc R . . H37C H 0.7344 0.6645 0.3148 0.062 Uiso 1 1 calc R . . C38 C 0.7037(2) 0.55941(15) 0.5222(2) 0.0378(7) Uani 1 1 d . . . H38A H 0.7605 0.5252 0.4980 0.057 Uiso 1 1 calc R . . H38B H 0.6623 0.5363 0.5936 0.057 Uiso 1 1 calc R . . H38C H 0.7452 0.6148 0.5493 0.057 Uiso 1 1 calc R . . S2 S 1.32743(10) -0.03380(7) 0.05954(11) 0.0316(3) Uani 0.75 1 d P A 1 S3A S 1.4149(5) -0.0659(3) 0.1186(5) 0.0487(15) Uiso 0.15 1 d P B 2 S3B S 1.2943(9) -0.0706(6) 0.0731(10) 0.042(3) Uiso 0.10 1 d P C 3 O4 O 1.20627(19) -0.02364(13) 0.0084(2) 0.0295(6) Uani 0.75 1 d P A 1 O5 O 1.3728(8) 0.0138(5) 0.1178(8) 0.057(3) Uiso 0.25 1 d P B 2 C39 C 1.3619(7) -0.1064(6) -0.0528(10) 0.059(3) Uani 0.75 1 d P A 1 H39A H 1.3623 -0.0846 -0.1381 0.089 Uiso 0.75 1 calc PR A 1 H39B H 1.3030 -0.1564 -0.0565 0.089 Uiso 0.75 1 calc PR A 1 H39C H 1.4397 -0.1188 -0.0267 0.089 Uiso 0.75 1 calc PR A 1 C40 C 1.3086(4) -0.0995(3) 0.1886(4) 0.0402(12) Uani 0.75 1 d P A 1 H40A H 1.2610 -0.1521 0.1558 0.060 Uiso 0.75 1 calc PR A 1 H40B H 1.2688 -0.0743 0.2554 0.060 Uiso 0.75 1 calc PR A 1 H40C H 1.3857 -0.1081 0.2254 0.060 Uiso 0.75 1 calc PR A 1 C41 C 1.380(2) -0.1107(15) -0.046(2) 0.017(4) Uiso 0.25 1 d P B 2 H41A H 1.4243 -0.0757 -0.1044 0.026 Uiso 0.25 1 calc PR B 2 H41B H 1.2959 -0.1155 -0.0703 0.026 Uiso 0.25 1 calc PR B 2 H41C H 1.4023 -0.1650 -0.0519 0.026 Uiso 0.25 1 calc PR B 2 C42 C 1.3321(16) -0.1249(11) 0.2117(18) 0.065(7) Uiso 0.25 1 d P B 2 H42A H 1.2526 -0.1414 0.1683 0.098 Uiso 0.25 1 calc PR B 2 H42B H 1.3283 -0.0945 0.2940 0.098 Uiso 0.25 1 calc PR B 2 H42C H 1.3666 -0.1736 0.2275 0.098 Uiso 0.25 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02072(18) 0.02258(19) 0.02334(18) -0.00012(14) 0.00232(14) 0.00524(14) O1 0.0252(10) 0.0248(11) 0.0284(11) -0.0032(8) -0.0004(9) 0.0101(8) O2 0.0322(11) 0.0341(12) 0.0208(10) 0.0002(8) 0.0020(9) 0.0104(9) N1 0.0177(12) 0.0217(13) 0.0251(13) -0.0018(10) 0.0014(10) 0.0053(10) N2 0.0220(13) 0.0263(14) 0.0326(13) -0.0054(11) -0.0009(11) 0.0087(10) N3 0.0256(14) 0.0314(15) 0.0299(14) -0.0106(11) -0.0003(12) 0.0154(11) N4 0.0322(15) 0.0277(15) 0.0226(14) 0.0021(11) 0.0012(12) 0.0135(12) N5 0.0203(12) 0.0206(12) 0.0195(12) -0.0013(9) 0.0021(10) 0.0069(10) N6 0.0199(13) 0.0290(14) 0.0232(13) 0.0000(10) 0.0035(11) 0.0110(11) N7 0.0214(13) 0.0311(14) 0.0196(12) -0.0013(10) -0.0019(10) 0.0110(10) N8 0.0253(14) 0.0311(14) 0.0240(14) 0.0010(11) -0.0017(12) 0.0142(11) C1 0.0146(14) 0.0205(15) 0.0301(16) 0.0013(12) 0.0028(13) 0.0015(11) C2 0.0201(15) 0.0228(15) 0.0291(16) -0.0050(12) -0.0004(13) 0.0058(12) C3 0.0188(15) 0.0257(17) 0.0377(18) -0.0055(13) 0.0076(14) 0.0007(12) C4 0.0203(15) 0.0263(16) 0.0256(15) -0.0015(12) 0.0065(13) 0.0024(12) C5 0.0301(17) 0.049(2) 0.0290(17) -0.0100(15) 0.0015(15) 0.0127(15) C6 0.072(2) 0.058(2) 0.0234(17) 0.0013(15) 0.0120(17) 0.0034(18) C7 0.0189(15) 0.0210(15) 0.0381(17) 0.0011(13) 0.0021(13) 0.0116(12) C8 0.0183(15) 0.0304(17) 0.0449(19) -0.0028(14) -0.0017(14) 0.0068(13) C9 0.0199(16) 0.0290(18) 0.059(2) -0.0001(15) 0.0025(16) 0.0001(13) C10 0.0287(18) 0.0310(18) 0.058(2) 0.0132(16) 0.0136(17) 0.0126(14) C11 0.0394(19) 0.0336(18) 0.0415(18) 0.0024(15) 0.0048(16) 0.0133(15) C12 0.0304(17) 0.0239(16) 0.0427(18) -0.0002(14) 0.0001(15) 0.0061(13) C13 0.0197(15) 0.0260(16) 0.0269(15) 0.0015(12) 0.0027(13) 0.0079(12) C14 0.0247(17) 0.0267(17) 0.057(2) 0.0018(14) 0.0021(15) 0.0065(13) C15 0.0238(17) 0.038(2) 0.067(2) 0.0061(16) 0.0035(16) 0.0150(14) C16 0.0201(16) 0.043(2) 0.0436(18) 0.0065(15) 0.0009(14) 0.0046(14) C17 0.0289(17) 0.0313(18) 0.0416(18) 0.0015(14) 0.0023(15) -0.0029(14) C18 0.0231(16) 0.0280(17) 0.0403(18) -0.0003(13) 0.0033(14) 0.0093(13) C19 0.0184(15) 0.0214(15) 0.0238(15) 0.0026(12) 0.0014(13) -0.0012(12) C20 0.0196(15) 0.0241(15) 0.0194(14) 0.0010(12) 0.0007(12) 0.0048(12) C21 0.0195(15) 0.0205(15) 0.0246(15) 0.0034(12) 0.0032(13) 0.0011(12) C22 0.0241(16) 0.0260(16) 0.0227(15) 0.0015(12) 0.0040(13) 0.0052(13) C23 0.0370(19) 0.065(2) 0.0235(16) -0.0038(15) -0.0030(15) 0.0259(16) C24 0.057(2) 0.122(3) 0.0269(18) 0.0058(19) 0.0070(18) 0.047(2) C25 0.0202(15) 0.0217(15) 0.0309(16) 0.0058(12) 0.0004(13) 0.0045(12) C26 0.0266(16) 0.0277(16) 0.0338(16) 0.0022(13) 0.0035(14) 0.0088(13) C27 0.0243(17) 0.0343(18) 0.053(2) 0.0061(15) 0.0124(16) 0.0030(14) C28 0.0238(17) 0.0367(19) 0.056(2) -0.0001(16) -0.0079(16) -0.0015(14) C29 0.0355(18) 0.0374(19) 0.0364(18) 0.0001(14) -0.0083(16) 0.0002(15) C30 0.0279(17) 0.0336(17) 0.0309(17) 0.0070(13) 0.0002(14) 0.0002(13) C31 0.0214(15) 0.0245(16) 0.0204(14) 0.0012(11) 0.0008(12) 0.0054(12) C32 0.0204(15) 0.0306(17) 0.0298(16) -0.0007(13) -0.0004(13) 0.0037(13) C33 0.0287(17) 0.0316(18) 0.0374(17) 0.0070(14) -0.0047(14) 0.0091(14) C34 0.0380(19) 0.0243(17) 0.0447(19) 0.0087(14) 0.0094(16) 0.0067(14) C35 0.0225(16) 0.0289(17) 0.0449(18) 0.0055(14) 0.0063(14) 0.0015(13) C36 0.0188(15) 0.0343(18) 0.0313(16) 0.0023(13) -0.0015(13) 0.0066(13) S1 0.0275(4) 0.0334(5) 0.0399(5) -0.0057(3) 0.0020(4) 0.0089(3) O3 0.0234(11) 0.0317(12) 0.0466(12) -0.0114(9) 0.0043(9) 0.0024(9) C37 0.049(2) 0.0373(19) 0.0342(17) -0.0016(14) 0.0043(16) -0.0005(15) C38 0.0384(18) 0.0378(18) 0.0342(17) -0.0012(14) -0.0008(15) 0.0012(14) S2 0.0286(6) 0.0248(7) 0.0423(7) 0.0020(6) 0.0053(5) 0.0067(5) O4 0.0334(15) 0.0282(15) 0.0305(14) -0.0010(11) 0.0038(12) 0.0162(12) C39 0.054(5) 0.067(4) 0.071(4) 0.007(3) 0.010(3) 0.045(3) C40 0.042(3) 0.046(3) 0.037(3) 0.002(2) 0.005(2) 0.021(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 N8 1.921(2) . ? Cu1 N4 1.928(2) . ? Cu1 N5 2.0275(19) . ? Cu1 N1 2.0303(19) . ? O1 C1 1.231(3) . ? O2 C19 1.232(3) . ? N1 C1 1.364(3) . ? N1 C3 1.393(3) . ? N2 C3 1.296(3) . ? N2 C2 1.464(3) . ? N2 H2N 0.8800 . ? N3 C4 1.349(3) . ? N3 C3 1.370(3) . ? N3 H3N 0.88(3) . ? N4 C4 1.287(3) . ? N4 H4N 0.81(2) . ? N5 C19 1.367(3) . ? N5 C21 1.388(3) . ? N6 C21 1.342(3) . ? N6 C20 1.447(3) . ? N6 H6N 0.881(18) . ? N7 C21 1.321(3) . ? N7 C22 1.357(3) . ? N8 C22 1.293(3) . ? N8 H8N 0.82(2) . ? C1 C2 1.549(3) . ? C2 C13 1.530(3) . ? C2 C7 1.532(3) . ? C4 C5 1.497(3) . ? C5 C6 1.511(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.375(3) . ? C7 C8 1.387(3) . ? C8 C9 1.394(3) . ? C8 H18 0.9500 . ? C9 C10 1.366(3) . ? C9 H17 0.9500 . ? C10 C11 1.378(3) . ? C10 H16 0.9500 . ? C11 C12 1.388(3) . ? C11 H15 0.9500 . ? C12 H14 0.9500 . ? C13 C18 1.373(3) . ? C13 C14 1.391(3) . ? C14 C15 1.375(3) . ? C14 H12 0.9500 . ? C15 C16 1.382(3) . ? C15 H11 0.9500 . ? C16 C17 1.371(3) . ? C16 H10 0.9500 . ? C17 C18 1.394(3) . ? C17 H9 0.9500 . ? C18 H8 0.9500 . ? C19 C20 1.543(3) . ? C20 C25 1.525(3) . ? C20 C31 1.540(3) . ? C22 C23 1.516(3) . ? C23 C24 1.484(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.379(3) . ? C25 C30 1.395(3) . ? C26 C27 1.388(3) . ? C26 H36 0.9500 . ? C27 C28 1.381(3) . ? C27 H35 0.9500 . ? C28 C29 1.380(3) . ? C28 H34 0.9500 . ? C29 C30 1.389(3) . ? C29 H33 0.9500 . ? C30 H32 0.9500 . ? C31 C36 1.387(3) . ? C31 C32 1.388(3) . ? C32 C33 1.385(3) . ? C32 H30 0.9500 . ? C33 C34 1.378(3) . ? C33 H29 0.9500 . ? C34 C35 1.381(3) . ? C34 H28 0.9500 . ? C35 C36 1.384(3) . ? C35 H27 0.9500 . ? C36 H26 0.9500 . ? S1 O3 1.5147(17) . ? S1 C37 1.783(3) . ? S1 C38 1.783(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? S2 O4 1.501(2) . ? S2 C39 1.755(10) . ? S2 C40 1.787(5) . ? S3A O5 1.491(9) . ? S3A C42 1.665(19) . ? S3A C41 1.82(2) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Cu1 N4 179.27(10) . . ? N8 Cu1 N5 87.21(9) . . ? N4 Cu1 N5 92.12(9) . . ? N8 Cu1 N1 93.23(9) . . ? N4 Cu1 N1 87.43(9) . . ? N5 Cu1 N1 178.89(9) . . ? C1 N1 C3 104.3(2) . . ? C1 N1 Cu1 130.70(16) . . ? C3 N1 Cu1 124.74(17) . . ? C3 N2 C2 106.0(2) . . ? C3 N2 H2N 127.0 . . ? C2 N2 H2N 127.0 . . ? C4 N3 C3 127.1(2) . . ? C4 N3 H3N 121.0(19) . . ? C3 N3 H3N 111.8(19) . . ? C4 N4 Cu1 133.9(2) . . ? C4 N4 H4N 113.8(17) . . ? Cu1 N4 H4N 112.4(16) . . ? C19 N5 C21 106.6(2) . . ? C19 N5 Cu1 130.55(16) . . ? C21 N5 Cu1 122.67(16) . . ? C21 N6 C20 111.9(2) . . ? C21 N6 H6N 121.9(13) . . ? C20 N6 H6N 125.4(13) . . ? C21 N7 C22 120.1(2) . . ? C22 N8 Cu1 132.46(19) . . ? C22 N8 H8N 114.7(16) . . ? Cu1 N8 H8N 112.8(16) . . ? O1 C1 N1 127.4(2) . . ? O1 C1 C2 123.9(2) . . ? N1 C1 C2 108.7(2) . . ? N2 C2 C13 109.3(2) . . ? N2 C2 C7 111.6(2) . . ? C13 C2 C7 110.9(2) . . ? N2 C2 C1 102.68(19) . . ? C13 C2 C1 113.4(2) . . ? C7 C2 C1 108.7(2) . . ? N2 C3 N3 118.2(2) . . ? N2 C3 N1 118.4(2) . . ? N3 C3 N1 123.3(2) . . ? N4 C4 N3 122.1(2) . . ? N4 C4 C5 123.1(2) . . ? N3 C4 C5 114.7(2) . . ? C4 C5 C6 113.7(2) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 118.4(3) . . ? C12 C7 C2 119.6(2) . . ? C8 C7 C2 122.0(2) . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H18 119.8 . . ? C9 C8 H18 119.8 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H17 119.8 . . ? C8 C9 H17 119.8 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H16 120.2 . . ? C11 C10 H16 120.2 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H15 120.0 . . ? C12 C11 H15 120.0 . . ? C7 C12 C11 121.2(3) . . ? C7 C12 H14 119.4 . . ? C11 C12 H14 119.4 . . ? C18 C13 C14 117.8(2) . . ? C18 C13 C2 124.0(2) . . ? C14 C13 C2 118.2(2) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H12 119.3 . . ? C13 C14 H12 119.3 . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H11 119.9 . . ? C16 C15 H11 119.9 . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H10 120.3 . . ? C15 C16 H10 120.3 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H9 120.0 . . ? C18 C17 H9 120.0 . . ? C13 C18 C17 121.4(2) . . ? C13 C18 H8 119.3 . . ? C17 C18 H8 119.3 . . ? O2 C19 N5 127.2(2) . . ? O2 C19 C20 122.1(2) . . ? N5 C19 C20 110.7(2) . . ? N6 C20 C25 113.3(2) . . ? N6 C20 C31 109.6(2) . . ? C25 C20 C31 113.8(2) . . ? N6 C20 C19 99.02(19) . . ? C25 C20 C19 109.5(2) . . ? C31 C20 C19 110.6(2) . . ? N7 C21 N6 118.3(2) . . ? N7 C21 N5 130.1(2) . . ? N6 C21 N5 111.6(2) . . ? N8 C22 N7 126.5(2) . . ? N8 C22 C23 120.5(2) . . ? N7 C22 C23 113.0(2) . . ? C24 C23 C22 115.0(2) . . ? C24 C23 H23A 108.5 . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23B 108.5 . . ? C22 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.9(2) . . ? C26 C25 C20 121.5(2) . . ? C30 C25 C20 119.4(2) . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H36 119.7 . . ? C27 C26 H36 119.7 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H35 119.9 . . ? C26 C27 H35 119.9 . . ? C29 C28 C27 119.6(3) . . ? C29 C28 H34 120.2 . . ? C27 C28 H34 120.2 . . ? C28 C29 C30 120.3(3) . . ? C28 C29 H33 119.9 . . ? C30 C29 H33 119.9 . . ? C29 C30 C25 120.2(3) . . ? C29 C30 H32 119.9 . . ? C25 C30 H32 119.9 . . ? C36 C31 C32 118.1(2) . . ? C36 C31 C20 119.2(2) . . ? C32 C31 C20 122.6(2) . . ? C33 C32 C31 120.8(2) . . ? C33 C32 H30 119.6 . . ? C31 C32 H30 119.6 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H29 119.9 . . ? C32 C33 H29 119.9 . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H28 120.1 . . ? C35 C34 H28 120.1 . . ? C34 C35 C36 119.5(2) . . ? C34 C35 H27 120.2 . . ? C36 C35 H27 120.2 . . ? C35 C36 C31 121.5(2) . . ? C35 C36 H26 119.2 . . ? C31 C36 H26 119.2 . . ? O3 S1 C37 106.32(11) . . ? O3 S1 C38 105.68(11) . . ? C37 S1 C38 97.79(13) . . ? S1 C37 H37A 109.5 . . ? S1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? S1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? S1 C38 H38A 109.5 . . ? S1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? S1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 S2 C39 102.8(3) . . ? O4 S2 C40 106.29(19) . . ? C39 S2 C40 96.6(4) . . ? O5 S3A C42 107.5(8) . . ? O5 S3A C41 104.8(9) . . ? C42 S3A C41 107.2(10) . . ? S3A C41 H41A 109.5 . . ? S3A C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S3A C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S3A C42 H42A 109.5 . . ? S3A C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S3A C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Cu1 N1 C1 -4.8(2) . . . . ? N4 Cu1 N1 C1 175.5(2) . . . . ? N5 Cu1 N1 C1 -118(4) . . . . ? N8 Cu1 N1 C3 168.0(2) . . . . ? N4 Cu1 N1 C3 -11.7(2) . . . . ? N5 Cu1 N1 C3 54(4) . . . . ? N8 Cu1 N4 C4 -145(8) . . . . ? N5 Cu1 N4 C4 -169.2(3) . . . . ? N1 Cu1 N4 C4 9.8(3) . . . . ? N8 Cu1 N5 C19 178.9(2) . . . . ? N4 Cu1 N5 C19 -1.4(2) . . . . ? N1 Cu1 N5 C19 -67(4) . . . . ? N8 Cu1 N5 C21 -7.08(19) . . . . ? N4 Cu1 N5 C21 172.62(19) . . . . ? N1 Cu1 N5 C21 107(4) . . . . ? N4 Cu1 N8 C22 -25(8) . . . . ? N5 Cu1 N8 C22 -1.2(3) . . . . ? N1 Cu1 N8 C22 179.8(3) . . . . ? C3 N1 C1 O1 -179.1(2) . . . . ? Cu1 N1 C1 O1 -5.1(4) . . . . ? C3 N1 C1 C2 -0.2(3) . . . . ? Cu1 N1 C1 C2 173.75(16) . . . . ? C3 N2 C2 C13 -120.1(2) . . . . ? C3 N2 C2 C7 116.9(2) . . . . ? C3 N2 C2 C1 0.6(3) . . . . ? O1 C1 C2 N2 178.7(2) . . . . ? N1 C1 C2 N2 -0.3(3) . . . . ? O1 C1 C2 C13 -63.5(3) . . . . ? N1 C1 C2 C13 117.5(2) . . . . ? O1 C1 C2 C7 60.4(3) . . . . ? N1 C1 C2 C7 -118.6(2) . . . . ? C2 N2 C3 N3 176.9(2) . . . . ? C2 N2 C3 N1 -0.8(3) . . . . ? C4 N3 C3 N2 -175.2(2) . . . . ? C4 N3 C3 N1 2.4(4) . . . . ? C1 N1 C3 N2 0.6(3) . . . . ? Cu1 N1 C3 N2 -173.75(17) . . . . ? C1 N1 C3 N3 -176.9(2) . . . . ? Cu1 N1 C3 N3 8.7(3) . . . . ? Cu1 N4 C4 N3 -3.1(4) . . . . ? Cu1 N4 C4 C5 176.07(19) . . . . ? C3 N3 C4 N4 -5.9(4) . . . . ? C3 N3 C4 C5 174.9(2) . . . . ? N4 C4 C5 C6 42.8(4) . . . . ? N3 C4 C5 C6 -137.9(2) . . . . ? N2 C2 C7 C12 168.5(2) . . . . ? C13 C2 C7 C12 46.4(3) . . . . ? C1 C2 C7 C12 -79.0(3) . . . . ? N2 C2 C7 C8 -14.2(3) . . . . ? C13 C2 C7 C8 -136.3(2) . . . . ? C1 C2 C7 C8 98.3(3) . . . . ? C12 C7 C8 C9 -1.1(4) . . . . ? C2 C7 C8 C9 -178.4(2) . . . . ? C7 C8 C9 C10 1.1(4) . . . . ? C8 C9 C10 C11 -0.7(4) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C8 C7 C12 C11 0.7(4) . . . . ? C2 C7 C12 C11 178.1(2) . . . . ? C10 C11 C12 C7 -0.4(4) . . . . ? N2 C2 C13 C18 112.4(3) . . . . ? C7 C2 C13 C18 -124.2(3) . . . . ? C1 C2 C13 C18 -1.5(4) . . . . ? N2 C2 C13 C14 -66.0(3) . . . . ? C7 C2 C13 C14 57.4(3) . . . . ? C1 C2 C13 C14 -179.9(2) . . . . ? C18 C13 C14 C15 -0.5(4) . . . . ? C2 C13 C14 C15 178.1(3) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C14 C13 C18 C17 0.2(4) . . . . ? C2 C13 C18 C17 -178.2(2) . . . . ? C16 C17 C18 C13 0.0(4) . . . . ? C21 N5 C19 O2 177.2(2) . . . . ? Cu1 N5 C19 O2 -8.1(4) . . . . ? C21 N5 C19 C20 -2.0(3) . . . . ? Cu1 N5 C19 C20 172.74(15) . . . . ? C21 N6 C20 C25 120.0(2) . . . . ? C21 N6 C20 C31 -111.7(2) . . . . ? C21 N6 C20 C19 4.1(3) . . . . ? O2 C19 C20 N6 179.6(2) . . . . ? N5 C19 C20 N6 -1.1(2) . . . . ? O2 C19 C20 C25 60.9(3) . . . . ? N5 C19 C20 C25 -119.9(2) . . . . ? O2 C19 C20 C31 -65.4(3) . . . . ? N5 C19 C20 C31 113.8(2) . . . . ? C22 N7 C21 N6 177.1(2) . . . . ? C22 N7 C21 N5 -5.1(4) . . . . ? C20 N6 C21 N7 172.3(2) . . . . ? C20 N6 C21 N5 -5.9(3) . . . . ? C19 N5 C21 N7 -173.1(3) . . . . ? Cu1 N5 C21 N7 11.7(4) . . . . ? C19 N5 C21 N6 4.8(3) . . . . ? Cu1 N5 C21 N6 -170.47(15) . . . . ? Cu1 N8 C22 N7 7.6(4) . . . . ? Cu1 N8 C22 C23 -172.23(19) . . . . ? C21 N7 C22 N8 -5.2(4) . . . . ? C21 N7 C22 C23 174.7(2) . . . . ? N8 C22 C23 C24 -130.7(3) . . . . ? N7 C22 C23 C24 49.4(3) . . . . ? N6 C20 C25 C26 -3.3(3) . . . . ? C31 C20 C25 C26 -129.4(2) . . . . ? C19 C20 C25 C26 106.2(3) . . . . ? N6 C20 C25 C30 -179.2(2) . . . . ? C31 C20 C25 C30 54.8(3) . . . . ? C19 C20 C25 C30 -69.7(3) . . . . ? C30 C25 C26 C27 -2.6(4) . . . . ? C20 C25 C26 C27 -178.4(2) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C29 0.1(4) . . . . ? C27 C28 C29 C30 0.8(4) . . . . ? C28 C29 C30 C25 -2.6(4) . . . . ? C26 C25 C30 C29 3.5(4) . . . . ? C20 C25 C30 C29 179.4(2) . . . . ? N6 C20 C31 C36 64.7(3) . . . . ? C25 C20 C31 C36 -167.2(2) . . . . ? C19 C20 C31 C36 -43.4(3) . . . . ? N6 C20 C31 C32 -110.9(3) . . . . ? C25 C20 C31 C32 17.1(3) . . . . ? C19 C20 C31 C32 140.9(2) . . . . ? C36 C31 C32 C33 0.5(4) . . . . ? C20 C31 C32 C33 176.2(2) . . . . ? C31 C32 C33 C34 -0.9(4) . . . . ? C32 C33 C34 C35 0.6(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C31 -0.4(4) . . . . ? C32 C31 C36 C35 0.1(4) . . . . ? C20 C31 C36 C35 -175.7(2) . . . . ? 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 N2 H2N O5 0.88 2.02 2.794(9) 146.8 . N3 H3N O4 0.88(3) 1.93(3) 2.803(3) 172(3) . N4 H4N O2 0.81(2) 2.01(2) 2.757(3) 153(2) . N6 H6N O3 0.881(18) 1.940(19) 2.807(3) 167.6(19) . N8 H8N O1 0.82(2) 2.05(2) 2.807(3) 152(2) . _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.943 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.067