#Electronic Supplementary Material for Dalton Transactions #This Journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name R.Kohn G.Kociok-Kohn L.T.Laudo Z.Pan F.Speiser _publ_contact_author_name 'Randolf Kohn' _publ_contact_author_email R.D.KOHN@BATH.AC.UK # Attachment '1a.cif' data_k08rdk5 _database_code_depnum_ccdc_archive 'CCDC 707388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 N6' _chemical_formula_sum 'C21 H24 N6' _chemical_formula_weight 360.46 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0590(3) _cell_length_b 10.0802(3) _cell_length_c 10.5680(4) _cell_angle_alpha 88.1730(10) _cell_angle_beta 82.2380(10) _cell_angle_gamma 61.5410(10) _cell_volume 932.79(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9804 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '162 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12625 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4238 _reflns_number_gt 3344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0464P)^2^+0.2226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4238 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.76890(14) 0.00797(13) 0.13187(12) 0.0258(3) Uani 1 1 d . . . H1A H 0.8094 0.0311 0.0483 0.031 Uiso 1 1 calc R . . H1B H 0.6783 -0.0023 0.1198 0.031 Uiso 1 1 calc R . . N1 N 0.72287(11) 0.13241(11) 0.22242(10) 0.0236(2) Uani 1 1 d . . . C11 C 0.84376(14) 0.17500(14) 0.22580(13) 0.0285(3) Uani 1 1 d . . . H11A H 0.8775 0.1943 0.1380 0.034 Uiso 1 1 calc R . . H11B H 0.9326 0.0901 0.2578 0.034 Uiso 1 1 calc R . . C12 C 0.78913(14) 0.31397(13) 0.31039(12) 0.0257(3) Uani 1 1 d . . . N11 N 0.88075(12) 0.30722(12) 0.39382(12) 0.0324(3) Uani 1 1 d . . . C13 C 0.83280(16) 0.42904(15) 0.47139(15) 0.0357(3) Uani 1 1 d . . . H13 H 0.8974 0.4254 0.5308 0.043 Uiso 1 1 calc R . . C14 C 0.69590(16) 0.55887(15) 0.47014(14) 0.0343(3) Uani 1 1 d . . . H14 H 0.6659 0.6414 0.5281 0.041 Uiso 1 1 calc R . . C15 C 0.60370(16) 0.56543(15) 0.38219(15) 0.0372(3) Uani 1 1 d . . . H15 H 0.5090 0.6536 0.3776 0.045 Uiso 1 1 calc R . . C16 C 0.65087(15) 0.44223(14) 0.30089(14) 0.0332(3) Uani 1 1 d . . . H16 H 0.5894 0.4450 0.2390 0.040 Uiso 1 1 calc R . . C2 C 0.67109(13) 0.09497(12) 0.34654(11) 0.0222(2) Uani 1 1 d . . . H2A H 0.5794 0.0839 0.3409 0.027 Uiso 1 1 calc R . . H2B H 0.6420 0.1785 0.4091 0.027 Uiso 1 1 calc R . . N2 N 0.79022(11) -0.04600(10) 0.39156(9) 0.0205(2) Uani 1 1 d . . . C21 C 0.73653(14) -0.08363(13) 0.51571(11) 0.0231(2) Uani 1 1 d . . . H21A H 0.8112 -0.1876 0.5347 0.028 Uiso 1 1 calc R . . H21B H 0.6385 -0.0826 0.5105 0.028 Uiso 1 1 calc R . . C22 C 0.71372(13) 0.02127(12) 0.62463(11) 0.0215(2) Uani 1 1 d . . . N21 N 0.61018(12) 0.03137(12) 0.72336(10) 0.0279(2) Uani 1 1 d . . . C23 C 0.59205(16) 0.11696(15) 0.82550(13) 0.0318(3) Uani 1 1 d . . . H23 H 0.5191 0.1249 0.8961 0.038 Uiso 1 1 calc R . . C24 C 0.67284(15) 0.19412(14) 0.83428(12) 0.0293(3) Uani 1 1 d . . . H24 H 0.6563 0.2529 0.9090 0.035 Uiso 1 1 calc R . . C25 C 0.77844(14) 0.18364(14) 0.73145(13) 0.0294(3) Uani 1 1 d . . . H25 H 0.8359 0.2356 0.7340 0.035 Uiso 1 1 calc R . . C26 C 0.79927(14) 0.09634(14) 0.62481(12) 0.0264(3) Uani 1 1 d . . . H26 H 0.8709 0.0878 0.5528 0.032 Uiso 1 1 calc R . . C3 C 0.82826(13) -0.16738(12) 0.29928(11) 0.0214(2) Uani 1 1 d . . . H3A H 0.7362 -0.1776 0.2929 0.026 Uiso 1 1 calc R . . H3B H 0.9065 -0.2639 0.3287 0.026 Uiso 1 1 calc R . . N3 N 0.88599(11) -0.13646(10) 0.17406(9) 0.0215(2) Uani 1 1 d . . . C31 C 0.91967(14) -0.25755(13) 0.08128(11) 0.0239(3) Uani 1 1 d . . . H31A H 0.9401 -0.2265 -0.0059 0.029 Uiso 1 1 calc R . . H31B H 0.8293 -0.2732 0.0847 0.029 Uiso 1 1 calc R . . C32 C 1.05540(13) -0.40423(13) 0.10704(11) 0.0226(2) Uani 1 1 d . . . N31 N 1.19336(12) -0.41984(12) 0.06208(11) 0.0315(3) Uani 1 1 d . . . C33 C 1.31514(16) -0.54817(17) 0.08792(16) 0.0393(3) Uani 1 1 d . . . H33 H 1.4137 -0.5606 0.0567 0.047 Uiso 1 1 calc R . . C34 C 1.30650(16) -0.66321(16) 0.15684(14) 0.0376(3) Uani 1 1 d . . . H34 H 1.3964 -0.7513 0.1731 0.045 Uiso 1 1 calc R . . C35 C 1.16409(16) -0.64683(14) 0.20135(13) 0.0331(3) Uani 1 1 d . . . H35 H 1.1534 -0.7237 0.2487 0.040 Uiso 1 1 calc R . . C36 C 1.03683(15) -0.51575(14) 0.17555(12) 0.0270(3) Uani 1 1 d . . . H36 H 0.9373 -0.5021 0.2045 0.032 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 C1 0.0297(6) 0.0226(6) 0.0226(6) 0.0035(5) -0.0063(5) -0.0099(5) N1 0.0257(5) 0.0196(5) 0.0245(5) 0.0027(4) -0.0033(4) -0.0102(4) C11 0.0267(6) 0.0224(6) 0.0347(7) 0.0018(5) 0.0024(5) -0.0121(5) C12 0.0253(6) 0.0212(6) 0.0312(7) 0.0057(5) -0.0018(5) -0.0125(5) N11 0.0285(6) 0.0273(6) 0.0420(7) 0.0044(5) -0.0088(5) -0.0129(5) C13 0.0372(7) 0.0341(7) 0.0408(8) 0.0038(6) -0.0126(6) -0.0194(6) C14 0.0405(8) 0.0244(6) 0.0392(8) -0.0003(5) -0.0048(6) -0.0166(6) C15 0.0346(7) 0.0216(6) 0.0484(9) 0.0017(6) -0.0105(6) -0.0065(5) C16 0.0334(7) 0.0239(6) 0.0409(8) 0.0029(5) -0.0128(6) -0.0107(5) C2 0.0205(5) 0.0185(5) 0.0251(6) 0.0021(4) -0.0022(4) -0.0076(4) N2 0.0229(5) 0.0170(5) 0.0191(5) 0.0000(4) -0.0016(4) -0.0077(4) C21 0.0274(6) 0.0196(5) 0.0224(6) 0.0006(4) -0.0016(5) -0.0117(5) C22 0.0213(5) 0.0174(5) 0.0219(6) 0.0014(4) -0.0041(4) -0.0059(4) N21 0.0327(6) 0.0278(5) 0.0239(5) -0.0015(4) 0.0009(4) -0.0159(5) C23 0.0377(7) 0.0340(7) 0.0222(6) -0.0030(5) 0.0032(5) -0.0174(6) C24 0.0335(7) 0.0261(6) 0.0247(6) -0.0032(5) -0.0074(5) -0.0102(5) C25 0.0240(6) 0.0294(6) 0.0354(7) -0.0037(5) -0.0068(5) -0.0122(5) C26 0.0207(6) 0.0275(6) 0.0286(6) -0.0029(5) -0.0007(5) -0.0101(5) C3 0.0233(5) 0.0182(5) 0.0209(6) -0.0002(4) -0.0027(4) -0.0085(4) N3 0.0249(5) 0.0186(5) 0.0188(5) 0.0005(4) -0.0031(4) -0.0086(4) C31 0.0286(6) 0.0236(6) 0.0197(6) -0.0008(4) -0.0036(5) -0.0123(5) C32 0.0262(6) 0.0228(6) 0.0192(6) -0.0052(4) -0.0020(4) -0.0119(5) N31 0.0282(5) 0.0288(6) 0.0362(6) -0.0062(5) 0.0021(5) -0.0136(5) C33 0.0258(7) 0.0376(8) 0.0488(9) -0.0116(6) 0.0002(6) -0.0111(6) C34 0.0339(7) 0.0289(7) 0.0374(8) -0.0067(6) -0.0112(6) -0.0028(6) C35 0.0439(8) 0.0242(6) 0.0253(7) -0.0004(5) -0.0069(6) -0.0108(6) C36 0.0306(6) 0.0263(6) 0.0236(6) -0.0018(5) -0.0022(5) -0.0133(5) _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 C1 N1 1.4515(15) . ? C1 N3 1.4738(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.4510(15) . ? N1 C11 1.4747(16) . ? C11 C12 1.5089(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.3368(17) . ? C12 C16 1.3898(17) . ? N11 C13 1.3437(18) . ? C13 C14 1.377(2) . ? C13 H13 0.9500 . ? C14 C15 1.378(2) . ? C14 H14 0.9500 . ? C15 C16 1.3791(19) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C2 N2 1.4730(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.4573(14) . ? N2 C21 1.4591(15) . ? C21 C22 1.5070(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.3401(15) . ? C22 C26 1.3908(17) . ? N21 C23 1.3412(17) . ? C23 C24 1.3788(19) . ? C23 H23 0.9500 . ? C24 C25 1.3816(19) . ? C24 H24 0.9500 . ? C25 C26 1.3828(18) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C3 N3 1.4574(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.4692(14) . ? C31 C32 1.5083(16) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.3398(16) . ? C32 C36 1.3909(17) . ? N31 C33 1.3439(18) . ? C33 C34 1.381(2) . ? C33 H33 0.9500 . ? C34 C35 1.378(2) . ? C34 H34 0.9500 . ? C35 C36 1.3850(18) . ? C35 H35 0.9500 . ? C36 H36 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 N1 C1 N3 112.59(10) . . ? N1 C1 H1A 109.1 . . ? N3 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? N3 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C2 N1 C1 109.03(9) . . ? C2 N1 C11 113.21(10) . . ? C1 N1 C11 112.27(10) . . ? N1 C11 C12 111.69(10) . . ? N1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N11 C12 C16 122.08(12) . . ? N11 C12 C11 116.58(11) . . ? C16 C12 C11 121.33(12) . . ? C12 N11 C13 117.41(11) . . ? N11 C13 C14 124.06(13) . . ? N11 C13 H13 118.0 . . ? C14 C13 H13 118.0 . . ? C13 C14 C15 117.97(13) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C14 C15 C16 119.07(12) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C12 119.38(13) . . ? C15 C16 H16 120.3 . . ? C12 C16 H16 120.3 . . ? N1 C2 N2 111.61(9) . . ? N1 C2 H2A 109.3 . . ? N2 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? N2 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C3 N2 C21 108.56(9) . . ? C3 N2 C2 108.13(9) . . ? C21 N2 C2 111.21(9) . . ? N2 C21 C22 114.39(9) . . ? N2 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N2 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? N21 C22 C26 122.63(11) . . ? N21 C22 C21 115.09(10) . . ? C26 C22 C21 122.22(11) . . ? C22 N21 C23 117.20(11) . . ? N21 C23 C24 124.03(12) . . ? N21 C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? C23 C24 C25 118.19(12) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C24 C25 C26 118.99(12) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C22 118.96(12) . . ? C25 C26 H26 120.5 . . ? C22 C26 H26 120.5 . . ? N2 C3 N3 110.58(9) . . ? N2 C3 H3A 109.5 . . ? N3 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 N3 C31 109.95(9) . . ? C3 N3 C1 108.95(9) . . ? C31 N3 C1 109.18(9) . . ? N3 C31 C32 112.13(9) . . ? N3 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? N3 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N31 C32 C36 122.26(11) . . ? N31 C32 C31 116.52(11) . . ? C36 C32 C31 121.21(11) . . ? C32 N31 C33 116.99(12) . . ? N31 C33 C34 124.31(13) . . ? N31 C33 H33 117.8 . . ? C34 C33 H33 117.8 . . ? C35 C34 C33 118.24(12) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 118.51(13) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C32 119.67(12) . . ? C35 C36 H36 120.2 . . ? C32 C36 H36 120.2 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.180 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.040 # Attachment '2a.cif' data_pan29 _database_code_depnum_ccdc_archive 'CCDC 707389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 Cl3 Cu3 N6, C2 H3 N' _chemical_formula_sum 'C23 H27 Cl3 Cu3 N7' _chemical_formula_weight 698.49 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3310(8) _cell_length_b 16.0940(9) _cell_length_c 16.8830(13) _cell_angle_alpha 62.264(3) _cell_angle_beta 84.221(2) _cell_angle_gamma 79.050(3) _cell_volume 2675.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18337 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 24.108 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '79 1.9 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10962 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 24.07 _reflns_number_total 6886 _reflns_number_gt 4771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0021P)^2^+5.8789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6886 _refine_ls_number_parameters 675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 -0.08330(8) 0.45103(6) 0.19021(6) 0.0336(3) Uani 1 1 d . . . Cu2 Cu -0.28028(8) 0.35468(6) 0.28449(6) 0.0349(3) Uani 1 1 d . . . Cu3 Cu -0.26172(8) 0.52312(6) 0.28633(6) 0.0364(3) Uani 1 1 d . . . Cl1 Cl -0.16993(17) 0.35019(13) 0.16483(12) 0.0353(5) Uani 1 1 d . . . Cl2 Cl -0.42702(17) 0.49184(12) 0.24027(13) 0.0388(5) Uani 1 1 d . . . Cl3 Cl -0.14155(17) 0.60756(12) 0.17273(13) 0.0365(5) Uani 1 1 d . . . C1 C -0.0037(6) 0.4167(5) 0.3746(5) 0.0303(18) Uani 1 1 d . . . H1A H 0.0231 0.4791 0.3388 0.036 Uiso 1 1 calc R . . H1B H 0.0470 0.3802 0.4284 0.036 Uiso 1 1 calc R . . N1 N 0.0100(5) 0.3650(4) 0.3219(4) 0.0268(15) Uani 1 1 d . . . C11 C 0.1394(6) 0.3491(5) 0.2970(5) 0.0317(19) Uani 1 1 d . . . H11A H 0.1558 0.2943 0.2835 0.038 Uiso 1 1 calc R . . H11B H 0.1903 0.3343 0.3477 0.038 Uiso 1 1 calc R . . C12 C 0.1698(6) 0.4375(5) 0.2157(5) 0.0289(18) Uani 1 1 d . . . C13 C 0.2724(7) 0.4755(5) 0.2131(5) 0.0342(19) Uani 1 1 d . . . H13 H 0.3240 0.4484 0.2630 0.041 Uiso 1 1 calc R . . C14 C 0.2957(7) 0.5551(5) 0.1339(6) 0.040(2) Uani 1 1 d . . . H14 H 0.3633 0.5840 0.1299 0.048 Uiso 1 1 calc R . . C15 C 0.2206(7) 0.5915(5) 0.0617(5) 0.0335(19) Uani 1 1 d . . . H15 H 0.2362 0.6444 0.0069 0.040 Uiso 1 1 calc R . . C16 C 0.1235(7) 0.5488(5) 0.0722(5) 0.038(2) Uani 1 1 d . . . H16 H 0.0715 0.5745 0.0227 0.046 Uiso 1 1 calc R . . N11 N 0.0952(6) 0.4738(4) 0.1462(4) 0.0341(17) Uani 1 1 d . . . C2 C -0.0271(7) 0.2706(5) 0.3783(5) 0.0329(19) Uani 1 1 d . . . H2A H -0.0155 0.2330 0.3447 0.039 Uiso 1 1 calc R . . H2B H 0.0223 0.2351 0.4328 0.039 Uiso 1 1 calc R . . C21 C -0.1910(6) 0.1910(4) 0.4573(5) 0.0262(17) Uani 1 1 d . . . H21A H -0.1668 0.1659 0.5201 0.031 Uiso 1 1 calc R . . H21B H -0.1482 0.1466 0.4345 0.031 Uiso 1 1 calc R . . C22 C -0.3247(6) 0.1947(5) 0.4548(5) 0.0264(17) Uani 1 1 d . . . C23 C -0.3864(7) 0.1343(5) 0.5272(5) 0.0335(19) Uani 1 1 d . . . H23 H -0.3463 0.0936 0.5822 0.040 Uiso 1 1 calc R . . C24 C -0.5051(7) 0.1330(5) 0.5199(5) 0.037(2) Uani 1 1 d . . . H24 H -0.5479 0.0913 0.5694 0.045 Uiso 1 1 calc R . . C25 C -0.5625(7) 0.1939(5) 0.4385(6) 0.043(2) Uani 1 1 d . . . H25 H -0.6440 0.1929 0.4305 0.051 Uiso 1 1 calc R . . C26 C -0.4959(7) 0.2565(5) 0.3689(5) 0.036(2) Uani 1 1 d . . . H26 H -0.5348 0.3009 0.3144 0.043 Uiso 1 1 calc R . . N2 N -0.1546(5) 0.2859(4) 0.4030(4) 0.0278(15) Uani 1 1 d . . . N21 N -0.3788(5) 0.2553(4) 0.3770(4) 0.0286(15) Uani 1 1 d . . . C3 C -0.1672(7) 0.3360(5) 0.4573(5) 0.0291(17) Uani 1 1 d . . . H3A H -0.1154 0.2992 0.5105 0.035 Uiso 1 1 calc R . . H3B H -0.2516 0.3433 0.4781 0.035 Uiso 1 1 calc R . . N3 N -0.1312(5) 0.4309(4) 0.4017(4) 0.0289(15) Uani 1 1 d . . . C31 C -0.1443(7) 0.4832(5) 0.4541(5) 0.036(2) Uani 1 1 d . . . H31A H -0.0921 0.5328 0.4277 0.043 Uiso 1 1 calc R . . H31B H -0.1174 0.4390 0.5159 0.043 Uiso 1 1 calc R . . C32 C -0.2734(7) 0.5297(5) 0.4566(6) 0.034(2) Uani 1 1 d . . . C33 C -0.3186(9) 0.5416(6) 0.5330(6) 0.056(3) Uani 1 1 d . . . H33 H -0.2729 0.5160 0.5858 0.067 Uiso 1 1 calc R . . C34 C -0.4359(10) 0.5937(6) 0.5256(8) 0.061(3) Uani 1 1 d . . . H34 H -0.4711 0.6039 0.5745 0.073 Uiso 1 1 calc R . . C35 C -0.4979(9) 0.6290(6) 0.4499(8) 0.060(3) Uani 1 1 d . . . H35 H -0.5741 0.6679 0.4438 0.072 Uiso 1 1 calc R . . C36 C -0.4503(8) 0.6084(5) 0.3799(6) 0.049(3) Uani 1 1 d . . . H36 H -0.4983 0.6278 0.3294 0.059 Uiso 1 1 calc R . . N31 N -0.3353(6) 0.5607(4) 0.3833(5) 0.0354(17) Uani 1 1 d . . . Cu4 Cu 0.28104(9) 0.12489(6) 0.23246(6) 0.0366(3) Uani 1 1 d . . . Cu5 Cu 0.33895(9) -0.03561(6) 0.19660(6) 0.0365(3) Uani 1 1 d . . . Cu6 Cu 0.12570(8) -0.02186(6) 0.29205(6) 0.0363(3) Uani 1 1 d . . . Cl4 Cl 0.46594(16) 0.02559(12) 0.24035(13) 0.0354(5) Uani 1 1 d . . . Cl5 Cl 0.24005(18) -0.15981(12) 0.30916(13) 0.0380(5) Uani 1 1 d . . . Cl6 Cl 0.16006(17) 0.07682(12) 0.35421(12) 0.0356(5) Uani 1 1 d . . . C4 C 0.0410(6) 0.1633(5) 0.1245(5) 0.0307(18) Uani 1 1 d . . . H4A H -0.0034 0.1796 0.1703 0.037 Uiso 1 1 calc R . . H4B H -0.0038 0.1998 0.0678 0.037 Uiso 1 1 calc R . . N4 N 0.1625(5) 0.1880(4) 0.1113(4) 0.0268(15) Uani 1 1 d . . . C41 C 0.1529(6) 0.2910(5) 0.0828(5) 0.0304(18) Uani 1 1 d . . . H41A H 0.0981 0.3085 0.1241 0.037 Uiso 1 1 calc R . . H41B H 0.1192 0.3281 0.0220 0.037 Uiso 1 1 calc R . . C42 C 0.2749(7) 0.3143(5) 0.0831(5) 0.0304(19) Uani 1 1 d . . . C43 C 0.3200(7) 0.3897(5) 0.0118(5) 0.0310(19) Uani 1 1 d . . . H43 H 0.2740 0.4291 -0.0406 0.037 Uiso 1 1 calc R . . C44 C 0.4323(7) 0.4065(5) 0.0183(6) 0.036(2) Uani 1 1 d . . . H44 H 0.4646 0.4576 -0.0297 0.043 Uiso 1 1 calc R . . C45 C 0.4979(7) 0.3487(5) 0.0950(6) 0.036(2) Uani 1 1 d . . . H45 H 0.5749 0.3601 0.1012 0.044 Uiso 1 1 calc R . . C46 C 0.4487(7) 0.2734(5) 0.1628(5) 0.0314(18) Uani 1 1 d . . . H46 H 0.4945 0.2327 0.2151 0.038 Uiso 1 1 calc R . . N41 N 0.3395(5) 0.2552(4) 0.1581(4) 0.0321(15) Uani 1 1 d . . . C5 C 0.2237(7) 0.1669(4) 0.0403(5) 0.0296(18) Uani 1 1 d . . . H5A H 0.1764 0.2025 -0.0152 0.035 Uiso 1 1 calc R . . H5B H 0.3040 0.1865 0.0276 0.035 Uiso 1 1 calc R . . C51 C 0.3005(7) 0.0441(5) -0.0008(5) 0.0293(18) Uani 1 1 d . . . H51A H 0.3623 0.0859 -0.0283 0.035 Uiso 1 1 calc R . . H51B H 0.2429 0.0595 -0.0479 0.035 Uiso 1 1 calc R . . C52 C 0.3612(7) -0.0596(5) 0.0336(5) 0.0292(18) Uani 1 1 d . . . C53 C 0.3873(7) -0.0993(6) -0.0231(6) 0.043(2) Uani 1 1 d . . . H53 H 0.3645 -0.0639 -0.0841 0.051 Uiso 1 1 calc R . . C54 C 0.4478(8) -0.1928(6) 0.0096(6) 0.049(3) Uani 1 1 d . . . H54 H 0.4661 -0.2227 -0.0282 0.058 Uiso 1 1 calc R . . C55 C 0.4801(7) -0.2401(5) 0.0976(6) 0.041(2) Uani 1 1 d . . . H55 H 0.5218 -0.3036 0.1225 0.050 Uiso 1 1 calc R . . C56 C 0.4507(7) -0.1935(5) 0.1493(6) 0.042(2) Uani 1 1 d . . . H56 H 0.4721 -0.2273 0.2107 0.050 Uiso 1 1 calc R . . N5 N 0.2362(5) 0.0645(4) 0.0700(4) 0.0278(15) Uani 1 1 d . . . N51 N 0.3937(6) -0.1032(4) 0.1186(4) 0.0366(17) Uani 1 1 d . . . C6 C 0.1138(6) 0.0377(5) 0.0828(5) 0.0308(18) Uani 1 1 d . . . H6A H 0.0686 0.0738 0.0262 0.037 Uiso 1 1 calc R . . H6B H 0.1201 -0.0311 0.1015 0.037 Uiso 1 1 calc R . . N6 N 0.0513(5) 0.0613(4) 0.1536(4) 0.0305(16) Uani 1 1 d . . . C61 C -0.0715(7) 0.0359(6) 0.1654(5) 0.037(2) Uani 1 1 d . . . H61A H -0.0664 -0.0262 0.1654 0.044 Uiso 1 1 calc R . . H61B H -0.1225 0.0845 0.1150 0.044 Uiso 1 1 calc R . . C62 C -0.1280(7) 0.0301(5) 0.2535(6) 0.034(2) Uani 1 1 d . . . C63 C -0.2492(7) 0.0642(5) 0.2582(5) 0.035(2) Uani 1 1 d . . . H63 H -0.2969 0.0967 0.2060 0.042 Uiso 1 1 calc R . . C64 C -0.2988(7) 0.0494(5) 0.3416(6) 0.039(2) Uani 1 1 d . . . H64 H -0.3812 0.0723 0.3474 0.047 Uiso 1 1 calc R . . C65 C -0.2267(7) 0.0013(5) 0.4153(5) 0.033(2) Uani 1 1 d . . . H65 H -0.2592 -0.0122 0.4734 0.040 Uiso 1 1 calc R . . C66 C -0.1062(7) -0.0272(5) 0.4035(5) 0.0325(19) Uani 1 1 d . . . H66 H -0.0557 -0.0571 0.4543 0.039 Uiso 1 1 calc R . . N61 N -0.0570(6) -0.0148(4) 0.3240(5) 0.0395(19) Uani 1 1 d . . . N7 N 0.8755(13) 0.7219(8) 0.3995(8) 0.108(4) Uani 1 1 d . . . C71 C 0.8032(12) 0.7650(7) 0.3497(9) 0.071(3) Uani 1 1 d . . . C72 C 0.7109(11) 0.8159(8) 0.2848(10) 0.097(4) Uani 1 1 d . . . H72A H 0.7078 0.7826 0.2492 0.145 Uiso 1 1 calc R . . H72B H 0.7281 0.8802 0.2453 0.145 Uiso 1 1 calc R . . H72C H 0.6332 0.8201 0.3152 0.145 Uiso 1 1 calc R . . N8 N 0.1146(18) -0.1790(13) 0.0783(17) 0.071(7) Uani 0.49(2) 1 d P A 1 C81 C 0.115(2) -0.234(2) 0.146(3) 0.057(7) Uani 0.49(2) 1 d P A 1 C82 C 0.114(6) -0.312(4) 0.239(3) 0.068(15) Uani 0.49(2) 1 d P A 1 H82A H 0.1031 -0.2847 0.2808 0.103 Uiso 0.49(2) 1 calc PR A 1 H82B H 0.1911 -0.3550 0.2500 0.103 Uiso 0.49(2) 1 calc PR A 1 H82C H 0.0486 -0.3465 0.2461 0.103 Uiso 0.49(2) 1 calc PR A 1 N8A N -0.026(3) -0.1645(16) 0.1417(15) 0.102(9) Uani 0.51(2) 1 d P A 2 C81A C 0.037(5) -0.234(2) 0.1900(18) 0.082(11) Uani 0.51(2) 1 d P A 2 C82A C 0.110(5) -0.311(5) 0.253(4) 0.065(14) Uiso 0.51(2) 1 d P A 2 H82D H 0.0746 -0.3273 0.3131 0.097 Uiso 0.51(2) 1 calc PR A 2 H82E H 0.1900 -0.2940 0.2511 0.097 Uiso 0.51(2) 1 calc PR A 2 H82F H 0.1184 -0.3651 0.2409 0.097 Uiso 0.51(2) 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 0.0287(5) 0.0345(5) 0.0318(5) -0.0109(4) -0.0004(5) -0.0034(4) Cu2 0.0343(5) 0.0332(5) 0.0263(5) -0.0067(4) 0.0032(5) -0.0018(4) Cu3 0.0326(6) 0.0375(5) 0.0313(5) -0.0112(4) 0.0045(5) -0.0030(4) Cl1 0.0342(11) 0.0427(10) 0.0291(10) -0.0165(9) 0.0029(9) -0.0078(8) Cl2 0.0319(11) 0.0329(9) 0.0398(11) -0.0077(9) -0.0025(10) -0.0015(8) Cl3 0.0363(11) 0.0297(9) 0.0326(11) -0.0067(8) 0.0053(9) -0.0042(8) C1 0.025(4) 0.025(4) 0.034(4) -0.007(3) 0.000(4) -0.003(3) N1 0.025(3) 0.024(3) 0.028(3) -0.011(3) 0.008(3) -0.005(2) C11 0.021(4) 0.031(4) 0.032(4) -0.009(3) 0.002(4) 0.003(3) C12 0.024(4) 0.034(4) 0.026(4) -0.014(3) 0.005(4) -0.002(3) C13 0.026(4) 0.042(4) 0.035(5) -0.020(4) 0.002(4) -0.002(3) C14 0.035(5) 0.036(4) 0.046(5) -0.016(4) 0.011(5) -0.011(4) C15 0.030(4) 0.035(4) 0.028(4) -0.009(4) -0.001(4) -0.003(3) C16 0.027(4) 0.047(5) 0.029(5) -0.012(4) 0.001(4) 0.004(4) N11 0.030(4) 0.031(3) 0.029(4) -0.007(3) 0.005(3) 0.002(3) C2 0.034(4) 0.028(4) 0.032(4) -0.010(3) 0.006(4) -0.005(3) C21 0.027(4) 0.019(3) 0.024(4) -0.004(3) -0.009(3) 0.006(3) C22 0.025(4) 0.027(4) 0.019(4) -0.004(3) 0.000(3) -0.001(3) C23 0.031(4) 0.032(4) 0.029(4) -0.009(4) -0.005(4) 0.002(3) C24 0.032(5) 0.039(4) 0.028(4) -0.005(4) -0.001(4) -0.005(3) C25 0.026(4) 0.043(5) 0.054(6) -0.018(4) 0.004(4) -0.008(4) C26 0.038(5) 0.030(4) 0.034(5) -0.012(4) -0.006(4) 0.005(3) N2 0.023(3) 0.029(3) 0.028(3) -0.011(3) 0.006(3) -0.004(3) N21 0.030(4) 0.030(3) 0.027(3) -0.015(3) 0.003(3) -0.004(3) C3 0.026(4) 0.036(4) 0.024(4) -0.013(3) 0.002(3) -0.004(3) N3 0.025(3) 0.022(3) 0.032(4) -0.008(3) 0.004(3) 0.000(2) C31 0.039(5) 0.039(4) 0.035(5) -0.022(4) 0.008(4) -0.008(4) C32 0.039(5) 0.027(4) 0.040(5) -0.018(4) 0.012(5) -0.009(3) C33 0.078(7) 0.040(5) 0.050(6) -0.023(4) 0.025(6) -0.018(5) C34 0.065(7) 0.048(6) 0.067(8) -0.031(6) 0.036(7) -0.013(5) C35 0.056(7) 0.032(5) 0.082(8) -0.025(5) 0.039(7) -0.011(4) C36 0.045(5) 0.027(4) 0.053(6) -0.005(4) 0.012(5) 0.003(4) N31 0.031(4) 0.026(3) 0.034(4) -0.005(3) 0.004(4) 0.003(3) Cu4 0.0352(6) 0.0342(5) 0.0296(5) -0.0073(4) 0.0027(5) -0.0031(4) Cu5 0.0405(6) 0.0361(5) 0.0301(5) -0.0141(4) 0.0009(5) -0.0037(4) Cu6 0.0313(5) 0.0370(5) 0.0335(6) -0.0123(4) 0.0015(5) -0.0003(4) Cl4 0.0290(10) 0.0345(9) 0.0357(11) -0.0114(8) 0.0016(9) -0.0030(8) Cl5 0.0446(12) 0.0301(9) 0.0322(11) -0.0102(8) 0.0061(10) -0.0041(8) Cl6 0.0389(11) 0.0327(9) 0.0288(10) -0.0115(8) 0.0051(9) -0.0016(8) C4 0.028(4) 0.031(4) 0.023(4) -0.007(3) 0.004(4) -0.003(3) N4 0.025(3) 0.024(3) 0.025(3) -0.007(3) 0.003(3) -0.002(2) C41 0.032(4) 0.028(4) 0.028(4) -0.012(3) 0.002(4) -0.003(3) C42 0.033(4) 0.024(4) 0.033(4) -0.015(3) 0.002(4) 0.003(3) C43 0.039(5) 0.028(4) 0.025(4) -0.013(3) 0.003(4) -0.005(3) C44 0.045(5) 0.029(4) 0.035(5) -0.015(4) 0.008(4) -0.008(4) C45 0.033(5) 0.033(4) 0.052(5) -0.027(4) 0.008(4) -0.009(4) C46 0.032(4) 0.034(4) 0.030(4) -0.018(4) -0.007(4) 0.004(3) N41 0.026(4) 0.038(3) 0.032(4) -0.017(3) 0.001(3) -0.003(3) C5 0.029(4) 0.024(4) 0.028(4) -0.007(3) 0.002(4) -0.002(3) C51 0.028(4) 0.029(4) 0.025(4) -0.010(3) 0.002(4) 0.002(3) C52 0.028(4) 0.030(4) 0.027(4) -0.013(3) 0.010(4) -0.007(3) C53 0.041(5) 0.049(5) 0.044(5) -0.029(4) 0.012(5) -0.007(4) C54 0.059(6) 0.043(5) 0.052(6) -0.031(5) 0.016(5) -0.012(4) C55 0.042(5) 0.027(4) 0.049(6) -0.016(4) 0.013(5) -0.006(4) C56 0.052(6) 0.035(4) 0.034(5) -0.015(4) 0.012(5) -0.005(4) N5 0.026(3) 0.026(3) 0.027(3) -0.010(3) 0.006(3) -0.006(3) N51 0.044(4) 0.023(3) 0.030(4) -0.005(3) 0.006(3) -0.001(3) C6 0.028(4) 0.040(4) 0.027(4) -0.016(4) 0.000(4) -0.008(3) N6 0.024(3) 0.035(3) 0.032(4) -0.016(3) 0.009(3) -0.007(3) C61 0.029(4) 0.053(5) 0.035(5) -0.024(4) 0.002(4) -0.011(4) C62 0.030(5) 0.032(4) 0.040(5) -0.015(4) 0.009(5) -0.012(3) C63 0.030(4) 0.042(4) 0.036(5) -0.017(4) -0.001(4) -0.011(4) C64 0.029(5) 0.039(4) 0.047(5) -0.019(4) 0.002(5) -0.003(4) C65 0.032(5) 0.031(4) 0.036(5) -0.014(4) 0.005(4) -0.009(3) C66 0.036(5) 0.027(4) 0.030(4) -0.008(3) -0.003(4) -0.009(3) N61 0.040(4) 0.033(3) 0.038(4) -0.013(3) 0.013(4) -0.003(3) N7 0.147(12) 0.089(8) 0.075(8) -0.006(6) -0.035(9) -0.053(8) C71 0.086(9) 0.046(6) 0.063(8) -0.003(6) -0.004(8) -0.028(6) C72 0.073(8) 0.066(7) 0.117(11) -0.006(7) -0.040(9) -0.011(6) N8 0.074(14) 0.050(11) 0.093(18) -0.029(12) -0.025(14) -0.016(10) C81 0.058(16) 0.053(15) 0.078(18) -0.042(14) 0.005(16) -0.021(12) C82 0.12(3) 0.046(16) 0.04(2) -0.014(17) -0.028(19) -0.009(14) N8A 0.16(3) 0.074(15) 0.067(14) -0.020(12) -0.047(17) -0.017(15) C81A 0.15(3) 0.055(16) 0.055(16) -0.018(15) -0.02(2) -0.063(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.121(6) . ? Cu1 N1 2.243(7) . ? Cu1 Cl1 2.262(2) . ? Cu1 Cl3 2.3632(19) . ? Cu1 Cu2 2.8674(12) . ? Cu1 Cu3 2.8753(12) . ? Cu2 N21 2.060(5) . ? Cu2 N2 2.274(7) . ? Cu2 Cl1 2.2897(18) . ? Cu2 Cl2 2.349(2) . ? Cu2 Cu3 2.7730(13) . ? Cu3 N31 2.049(6) . ? Cu3 Cl3 2.2650(17) . ? Cu3 N3 2.289(7) . ? Cu3 Cl2 2.320(2) . ? C1 N1 1.455(9) . ? C1 N3 1.480(8) . ? N1 C2 1.486(8) . ? N1 C11 1.492(8) . ? C11 C12 1.516(9) . ? C12 N11 1.344(10) . ? C12 C13 1.402(10) . ? C13 C14 1.400(10) . ? C14 C15 1.381(12) . ? C15 C16 1.360(11) . ? C16 N11 1.337(9) . ? C2 N2 1.470(8) . ? C21 N2 1.485(8) . ? C21 C22 1.509(10) . ? C22 N21 1.340(10) . ? C22 C23 1.381(9) . ? C23 C24 1.368(11) . ? C24 C25 1.399(12) . ? C25 C26 1.405(9) . ? C26 N21 1.344(10) . ? N2 C3 1.459(9) . ? C3 N3 1.486(8) . ? N3 C31 1.459(9) . ? C31 C32 1.517(11) . ? C32 N31 1.319(11) . ? C32 C33 1.421(11) . ? C33 C34 1.414(14) . ? C34 C35 1.342(16) . ? C35 C36 1.402(13) . ? C36 N31 1.373(10) . ? Cu4 N41 2.079(6) . ? Cu4 Cl6 2.2491(17) . ? Cu4 N4 2.263(7) . ? Cu4 Cl4 2.355(2) . ? Cu4 Cu5 2.8637(13) . ? Cu4 Cu6 2.9495(13) . ? Cu5 N51 2.053(6) . ? Cu5 Cl4 2.240(2) . ? Cu5 N5 2.259(7) . ? Cu5 Cl5 2.3977(18) . ? Cu5 Cu6 2.7980(12) . ? Cu6 N61 2.081(6) . ? Cu6 N6 2.241(7) . ? Cu6 Cl5 2.253(2) . ? Cu6 Cl6 2.376(2) . ? C4 N6 1.463(8) . ? C4 N4 1.472(9) . ? N4 C5 1.469(8) . ? N4 C41 1.480(8) . ? C41 C42 1.500(10) . ? C42 N41 1.358(10) . ? C42 C43 1.392(9) . ? C43 C44 1.375(11) . ? C44 C45 1.380(12) . ? C45 C46 1.389(9) . ? C46 N41 1.342(10) . ? C5 N5 1.464(8) . ? C51 N5 1.470(8) . ? C51 C52 1.530(9) . ? C52 N51 1.326(10) . ? C52 C53 1.361(10) . ? C53 C54 1.396(11) . ? C54 C55 1.368(13) . ? C55 C56 1.374(11) . ? C56 N51 1.345(9) . ? N5 C6 1.496(9) . ? C6 N6 1.491(8) . ? N6 C61 1.492(9) . ? C61 C62 1.527(10) . ? C62 N61 1.326(11) . ? C62 C63 1.387(11) . ? C63 C64 1.390(10) . ? C64 C65 1.372(12) . ? C65 C66 1.381(10) . ? C66 N61 1.340(9) . ? N7 C71 1.113(17) . ? C71 C72 1.427(18) . ? N8 C81 1.08(3) . ? C81 C82 1.47(6) . ? N8A C81A 1.17(4) . ? C81A C82A 1.39(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cu1 N1 80.9(2) . . ? N11 Cu1 Cl1 121.10(18) . . ? N1 Cu1 Cl1 106.95(15) . . ? N11 Cu1 Cl3 92.32(16) . . ? N1 Cu1 Cl3 106.94(15) . . ? Cl1 Cu1 Cl3 135.33(8) . . ? N11 Cu1 Cu2 160.00(16) . . ? N1 Cu1 Cu2 84.27(13) . . ? Cl1 Cu1 Cu2 51.38(5) . . ? Cl3 Cu1 Cu2 104.85(5) . . ? N11 Cu1 Cu3 133.60(18) . . ? N1 Cu1 Cu3 85.51(13) . . ? Cl1 Cu1 Cu3 105.30(5) . . ? Cl3 Cu1 Cu3 50.07(4) . . ? Cu2 Cu1 Cu3 57.75(3) . . ? N21 Cu2 N2 80.0(2) . . ? N21 Cu2 Cl1 128.34(16) . . ? N2 Cu2 Cl1 107.07(14) . . ? N21 Cu2 Cl2 99.76(17) . . ? N2 Cu2 Cl2 128.99(15) . . ? Cl1 Cu2 Cl2 111.71(8) . . ? N21 Cu2 Cu3 123.84(16) . . ? N2 Cu2 Cu3 84.49(14) . . ? Cl1 Cu2 Cu3 107.82(6) . . ? Cl2 Cu2 Cu3 53.08(6) . . ? N21 Cu2 Cu1 162.10(19) . . ? N2 Cu2 Cu1 83.72(13) . . ? Cl1 Cu2 Cu1 50.53(5) . . ? Cl2 Cu2 Cu1 96.22(5) . . ? Cu3 Cu2 Cu1 61.27(3) . . ? N31 Cu3 Cl3 124.54(17) . . ? N31 Cu3 N3 78.1(2) . . ? Cl3 Cu3 N3 103.42(14) . . ? N31 Cu3 Cl2 102.1(2) . . ? Cl3 Cu3 Cl2 114.08(8) . . ? N3 Cu3 Cl2 132.01(14) . . ? N31 Cu3 Cu2 124.49(16) . . ? Cl3 Cu3 Cu2 110.79(6) . . ? N3 Cu3 Cu2 85.80(14) . . ? Cl2 Cu3 Cu2 54.04(5) . . ? N31 Cu3 Cu1 159.0(2) . . ? Cl3 Cu3 Cu1 53.14(5) . . ? N3 Cu3 Cu1 82.35(13) . . ? Cl2 Cu3 Cu1 96.66(6) . . ? Cu2 Cu3 Cu1 60.98(3) . . ? Cu1 Cl1 Cu2 78.09(7) . . ? Cu3 Cl2 Cu2 72.88(7) . . ? Cu3 Cl3 Cu1 76.79(6) . . ? N1 C1 N3 109.6(6) . . ? C1 N1 C2 108.5(5) . . ? C1 N1 C11 109.0(6) . . ? C2 N1 C11 108.1(5) . . ? C1 N1 Cu1 111.9(4) . . ? C2 N1 Cu1 114.9(5) . . ? C11 N1 Cu1 104.2(4) . . ? N1 C11 C12 109.8(6) . . ? N11 C12 C13 122.9(7) . . ? N11 C12 C11 115.8(6) . . ? C13 C12 C11 121.3(8) . . ? C14 C13 C12 117.3(8) . . ? C15 C14 C13 120.1(7) . . ? C16 C15 C14 117.4(7) . . ? N11 C16 C15 125.5(9) . . ? C16 N11 C12 116.9(7) . . ? C16 N11 Cu1 124.3(5) . . ? C12 N11 Cu1 111.3(4) . . ? N2 C2 N1 108.3(5) . . ? N2 C21 C22 112.2(5) . . ? N21 C22 C23 121.9(7) . . ? N21 C22 C21 116.5(5) . . ? C23 C22 C21 121.5(7) . . ? C24 C23 C22 120.1(8) . . ? C23 C24 C25 119.0(7) . . ? C24 C25 C26 117.9(8) . . ? N21 C26 C25 122.0(8) . . ? C3 N2 C2 108.6(6) . . ? C3 N2 C21 109.2(5) . . ? C2 N2 C21 107.6(5) . . ? C3 N2 Cu2 114.4(4) . . ? C2 N2 Cu2 113.7(5) . . ? C21 N2 Cu2 103.1(4) . . ? C22 N21 C26 119.0(6) . . ? C22 N21 Cu2 116.1(5) . . ? C26 N21 Cu2 124.3(5) . . ? N2 C3 N3 108.4(5) . . ? C31 N3 C1 109.3(6) . . ? C31 N3 C3 109.7(5) . . ? C1 N3 C3 108.3(5) . . ? C31 N3 Cu3 103.6(4) . . ? C1 N3 Cu3 115.1(5) . . ? C3 N3 Cu3 110.8(5) . . ? N3 C31 C32 111.9(7) . . ? N31 C32 C33 124.2(8) . . ? N31 C32 C31 115.6(7) . . ? C33 C32 C31 120.1(9) . . ? C34 C33 C32 115.8(11) . . ? C35 C34 C33 120.5(9) . . ? C34 C35 C36 120.1(9) . . ? N31 C36 C35 121.0(11) . . ? C32 N31 C36 118.1(7) . . ? C32 N31 Cu3 118.3(5) . . ? C36 N31 Cu3 123.3(7) . . ? N41 Cu4 Cl6 129.66(16) . . ? N41 Cu4 N4 79.7(2) . . ? Cl6 Cu4 N4 107.18(14) . . ? N41 Cu4 Cl4 98.11(17) . . ? Cl6 Cu4 Cl4 117.13(7) . . ? N4 Cu4 Cl4 121.24(14) . . ? N41 Cu4 Cu5 125.92(15) . . ? Cl6 Cu4 Cu5 104.42(6) . . ? N4 Cu4 Cu5 84.36(14) . . ? Cl4 Cu4 Cu5 49.66(6) . . ? N41 Cu4 Cu6 159.1(2) . . ? Cl6 Cu4 Cu6 52.30(6) . . ? N4 Cu4 Cu6 80.34(13) . . ? Cl4 Cu4 Cu6 97.37(5) . . ? Cu5 Cu4 Cu6 57.52(3) . . ? N51 Cu5 Cl4 122.3(2) . . ? N51 Cu5 N5 79.0(2) . . ? Cl4 Cu5 N5 116.61(15) . . ? N51 Cu5 Cl5 95.78(16) . . ? Cl4 Cu5 Cl5 118.45(8) . . ? N5 Cu5 Cl5 116.87(15) . . ? N51 Cu5 Cu6 132.30(19) . . ? Cl4 Cu5 Cu6 104.72(6) . . ? N5 Cu5 Cu6 87.69(13) . . ? Cl5 Cu5 Cu6 50.69(5) . . ? N51 Cu5 Cu4 155.25(15) . . ? Cl4 Cu5 Cu4 53.28(5) . . ? N5 Cu5 Cu4 82.77(14) . . ? Cl5 Cu5 Cu4 107.38(5) . . ? Cu6 Cu5 Cu4 62.78(3) . . ? N61 Cu6 N6 80.8(2) . . ? N61 Cu6 Cl5 120.93(17) . . ? N6 Cu6 Cl5 110.73(15) . . ? N61 Cu6 Cl6 94.8(2) . . ? N6 Cu6 Cl6 112.85(15) . . ? Cl5 Cu6 Cl6 126.90(9) . . ? N61 Cu6 Cu5 158.8(2) . . ? N6 Cu6 Cu5 81.85(13) . . ? Cl5 Cu6 Cu5 55.42(5) . . ? Cl6 Cu6 Cu5 103.01(6) . . ? N61 Cu6 Cu4 130.20(17) . . ? N6 Cu6 Cu4 85.04(14) . . ? Cl5 Cu6 Cu4 108.76(6) . . ? Cl6 Cu6 Cu4 48.51(5) . . ? Cu5 Cu6 Cu4 59.70(3) . . ? Cu5 Cl4 Cu4 77.06(7) . . ? Cu6 Cl5 Cu5 73.90(6) . . ? Cu4 Cl6 Cu6 79.19(6) . . ? N6 C4 N4 108.9(5) . . ? C5 N4 C4 108.4(6) . . ? C5 N4 C41 109.0(5) . . ? C4 N4 C41 109.2(5) . . ? C5 N4 Cu4 110.6(4) . . ? C4 N4 Cu4 118.0(4) . . ? C41 N4 Cu4 101.2(5) . . ? N4 C41 C42 109.7(6) . . ? N41 C42 C43 122.0(7) . . ? N41 C42 C41 114.9(6) . . ? C43 C42 C41 123.0(8) . . ? C44 C43 C42 119.0(8) . . ? C43 C44 C45 119.7(7) . . ? C44 C45 C46 118.3(8) . . ? N41 C46 C45 123.2(8) . . ? C46 N41 C42 117.7(6) . . ? C46 N41 Cu4 125.4(5) . . ? C42 N41 Cu4 113.9(5) . . ? N5 C5 N4 108.7(5) . . ? N5 C51 C52 113.0(5) . . ? N51 C52 C53 124.0(7) . . ? N51 C52 C51 115.3(6) . . ? C53 C52 C51 120.6(7) . . ? C52 C53 C54 119.1(9) . . ? C55 C54 C53 118.1(8) . . ? C54 C55 C56 118.5(7) . . ? N51 C56 C55 124.1(8) . . ? C5 N5 C51 108.1(5) . . ? C5 N5 C6 108.9(5) . . ? C51 N5 C6 108.9(6) . . ? C5 N5 Cu5 118.1(5) . . ? C51 N5 Cu5 105.5(4) . . ? C6 N5 Cu5 107.1(4) . . ? C52 N51 C56 116.2(7) . . ? C52 N51 Cu5 118.8(5) . . ? C56 N51 Cu5 124.6(6) . . ? N6 C6 N5 107.0(6) . . ? C4 N6 C6 109.7(5) . . ? C4 N6 C61 109.2(6) . . ? C6 N6 C61 107.0(6) . . ? C4 N6 Cu6 110.1(5) . . ? C6 N6 Cu6 117.3(4) . . ? C61 N6 Cu6 103.0(4) . . ? N6 C61 C62 110.3(7) . . ? N61 C62 C63 123.5(7) . . ? N61 C62 C61 116.0(7) . . ? C63 C62 C61 120.3(9) . . ? C62 C63 C64 118.1(9) . . ? C65 C64 C63 118.9(7) . . ? C64 C65 C66 118.7(7) . . ? N61 C66 C65 123.2(9) . . ? C62 N61 C66 117.5(7) . . ? C62 N61 Cu6 114.1(4) . . ? C66 N61 Cu6 125.9(7) . . ? N7 C71 C72 176.8(15) . . ? N8 C81 C82 178(3) . . ? N8A C81A C82A 174(4) . . ? _diffrn_measured_fraction_theta_max 0.813 _diffrn_reflns_theta_full 24.07 _diffrn_measured_fraction_theta_full 0.813 _refine_diff_density_max 0.518 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.095 # Attachment '2e.cif' data_k04rdk2 _database_code_depnum_ccdc_archive 'CCDC 707390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H63 Cl3 Cu3 N3 S3' _chemical_formula_sum 'C30 H63 Cl3 Cu3 N3 S3' _chemical_formula_weight 858.98 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 22.3040(3) _cell_length_b 7.12300(10) _cell_length_c 25.6510(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.4270(10) _cell_angle_gamma 90.00 _cell_volume 3979.73(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42631 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7180 _exptl_absorpt_correction_T_max 0.8582 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '241 1.3 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38731 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6925 _reflns_number_gt 5227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0473P)^2^+9.6714P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6925 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.30791(3) 0.04333(8) 0.14579(3) 0.05061(18) Uani 1 1 d . . . Cu2 Cu 0.16635(3) 0.03864(8) 0.11886(2) 0.04654(17) Uani 1 1 d . . . Cu3 Cu 0.23712(3) 0.09857(9) 0.03649(2) 0.05191(18) Uani 1 1 d . . . Cl1 Cl 0.23986(5) -0.10440(15) 0.18607(4) 0.0414(3) Uani 1 1 d . . . Cl2 Cl 0.14661(5) -0.06131(16) 0.03341(4) 0.0451(3) Uani 1 1 d . . . Cl3 Cl 0.33116(6) -0.04082(19) 0.06624(6) 0.0584(3) Uani 1 1 d . . . S1 S 0.40483(6) 0.0881(2) 0.20528(6) 0.0617(4) Uani 1 1 d . . . S2 S 0.08395(6) 0.0564(2) 0.16385(5) 0.0536(3) Uani 1 1 d . . . S3 S 0.22650(7) 0.1983(3) -0.05411(6) 0.0733(5) Uani 1 1 d . . . C1 C 0.2928(2) 0.4447(6) 0.10324(19) 0.0486(12) Uani 1 1 d . . . H1A H 0.2923 0.5817 0.1097 0.058 Uiso 1 1 calc R . . H1B H 0.3311 0.4138 0.0916 0.058 Uiso 1 1 calc R . . N1 N 0.29138(18) 0.3441(5) 0.15276(15) 0.0447(9) Uani 1 1 d . . . C11 C 0.3420(2) 0.4150(8) 0.1964(2) 0.0586(14) Uani 1 1 d . . . H11A H 0.3427 0.5539 0.1949 0.070 Uiso 1 1 calc R . . H11B H 0.3334 0.3784 0.2312 0.070 Uiso 1 1 calc R . . C12 C 0.4024(3) 0.3431(8) 0.1927(2) 0.0638(15) Uani 1 1 d . . . H12A H 0.4347 0.4065 0.2194 0.077 Uiso 1 1 calc R . . H12B H 0.4101 0.3687 0.1568 0.077 Uiso 1 1 calc R . . C13 C 0.4647(3) 0.0144(8) 0.1711(3) 0.0682(16) Uani 1 1 d . . . H13 H 0.4515 0.0496 0.1326 0.082 Uiso 1 1 calc R . . C14 C 0.5256(3) 0.1070(10) 0.1932(3) 0.0808(19) Uani 1 1 d . . . H14A H 0.5556 0.0606 0.1728 0.097 Uiso 1 1 calc R . . H14B H 0.5209 0.2437 0.1866 0.097 Uiso 1 1 calc R . . C15 C 0.5522(3) 0.0774(12) 0.2515(3) 0.101(3) Uani 1 1 d . . . H15A H 0.5571 -0.0588 0.2589 0.121 Uiso 1 1 calc R . . H15B H 0.5236 0.1279 0.2726 0.121 Uiso 1 1 calc R . . C16 C 0.6149(4) 0.1747(14) 0.2690(4) 0.130(3) Uani 1 1 d . . . H16A H 0.6311 0.1524 0.3071 0.194 Uiso 1 1 calc R . . H16B H 0.6101 0.3100 0.2624 0.194 Uiso 1 1 calc R . . H16C H 0.6436 0.1237 0.2485 0.194 Uiso 1 1 calc R . . C17 C 0.4657(3) -0.2034(9) 0.1751(3) 0.086(2) Uani 1 1 d . . . H17A H 0.4786 -0.2382 0.2132 0.104 Uiso 1 1 calc R . . H17B H 0.4232 -0.2496 0.1623 0.104 Uiso 1 1 calc R . . C18 C 0.5062(4) -0.3046(12) 0.1449(4) 0.107(3) Uani 1 1 d . . . H18A H 0.5471 -0.2439 0.1525 0.129 Uiso 1 1 calc R . . H18B H 0.5117 -0.4354 0.1581 0.129 Uiso 1 1 calc R . . C19 C 0.4826(4) -0.3083(17) 0.0868(5) 0.140(4) Uani 1 1 d . . . H19A H 0.5116 -0.3759 0.0698 0.210 Uiso 1 1 calc R . . H19B H 0.4778 -0.1794 0.0732 0.210 Uiso 1 1 calc R . . H19C H 0.4427 -0.3719 0.0787 0.210 Uiso 1 1 calc R . . C2 C 0.2346(2) 0.3871(6) 0.17040(19) 0.0475(11) Uani 1 1 d . . . H2A H 0.2339 0.5221 0.1794 0.057 Uiso 1 1 calc R . . H2B H 0.2334 0.3140 0.2030 0.057 Uiso 1 1 calc R . . N2 N 0.18053(18) 0.3414(5) 0.12856(15) 0.0441(9) Uani 1 1 d . . . C21 C 0.1245(3) 0.4115(8) 0.1462(2) 0.0629(15) Uani 1 1 d . . . H21A H 0.0899 0.4190 0.1148 0.076 Uiso 1 1 calc R . . H21B H 0.1326 0.5399 0.1608 0.076 Uiso 1 1 calc R . . C22 C 0.1059(3) 0.2888(8) 0.1878(2) 0.0626(14) Uani 1 1 d . . . H22A H 0.0711 0.3483 0.1998 0.075 Uiso 1 1 calc R . . H22B H 0.1407 0.2798 0.2191 0.075 Uiso 1 1 calc R . . C23 C 0.0072(3) 0.1099(9) 0.1225(2) 0.0656(15) Uani 1 1 d . . . H23 H 0.0093 0.2378 0.1069 0.079 Uiso 1 1 calc R . . C24 C -0.0052(3) -0.0248(9) 0.0778(3) 0.0703(16) Uani 1 1 d . . . H24A H 0.0296 -0.0199 0.0596 0.084 Uiso 1 1 calc R . . H24B H -0.0422 0.0181 0.0520 0.084 Uiso 1 1 calc R . . C25 C -0.0149(4) -0.2258(9) 0.0915(3) 0.086(2) Uani 1 1 d . . . H25A H -0.0513 -0.2349 0.1076 0.103 Uiso 1 1 calc R . . H25B H 0.0213 -0.2706 0.1181 0.103 Uiso 1 1 calc R . . C26 C -0.0241(4) -0.3481(13) 0.0428(3) 0.109(3) Uani 1 1 d . . . H26A H -0.0297 -0.4786 0.0529 0.164 Uiso 1 1 calc R . . H26B H 0.0120 -0.3394 0.0268 0.164 Uiso 1 1 calc R . . H26C H -0.0605 -0.3062 0.0169 0.164 Uiso 1 1 calc R . . C27 C -0.0428(3) 0.1157(10) 0.1560(3) 0.0769(18) Uani 1 1 d . . . H27A H -0.0497 -0.0138 0.1675 0.092 Uiso 1 1 calc R . . H27B H -0.0271 0.1906 0.1886 0.092 Uiso 1 1 calc R . . C28 C -0.1038(3) 0.1968(12) 0.1278(3) 0.092(2) Uani 1 1 d . . . H28A H -0.0977 0.3289 0.1181 0.111 Uiso 1 1 calc R . . H28B H -0.1189 0.1262 0.0943 0.111 Uiso 1 1 calc R . . C29 C -0.1518(3) 0.1904(12) 0.1610(4) 0.109(3) Uani 1 1 d . . . H29A H -0.1903 0.2436 0.1406 0.163 Uiso 1 1 calc R . . H29B H -0.1378 0.2635 0.1937 0.163 Uiso 1 1 calc R . . H29C H -0.1586 0.0598 0.1703 0.163 Uiso 1 1 calc R . . C3 C 0.1842(3) 0.4452(7) 0.0798(2) 0.0523(12) Uani 1 1 d . . . H3A H 0.1476 0.4173 0.0515 0.063 Uiso 1 1 calc R . . H3B H 0.1848 0.5818 0.0871 0.063 Uiso 1 1 calc R . . N3 N 0.23986(19) 0.3929(5) 0.06131(16) 0.0472(9) Uani 1 1 d . . . C31 C 0.2441(3) 0.5067(8) 0.0133(2) 0.0655(16) Uani 1 1 d . . . H31A H 0.2293 0.6354 0.0180 0.079 Uiso 1 1 calc R . . H31B H 0.2877 0.5158 0.0110 0.079 Uiso 1 1 calc R . . C32 C 0.2080(3) 0.4287(10) -0.0379(3) 0.082(2) Uani 1 1 d . . . H32A H 0.2135 0.5130 -0.0672 0.098 Uiso 1 1 calc R . . H32B H 0.1640 0.4317 -0.0366 0.098 Uiso 1 1 calc R . . C33 C 0.3050(3) 0.1963(10) -0.0633(3) 0.0796(19) Uani 1 1 d . . . H33 H 0.3312 0.2391 -0.0286 0.096 Uiso 1 1 calc R . . C34 C 0.3242(4) -0.0050(11) -0.0712(3) 0.100(3) Uani 1 1 d . . . H34A H 0.3056 -0.0451 -0.1081 0.120 Uiso 1 1 calc R . . H34B H 0.3083 -0.0883 -0.0464 0.120 Uiso 1 1 calc R . . C35 C 0.3949(5) -0.0275(15) -0.0615(5) 0.132(4) Uani 1 1 d . . . H35A H 0.4108 0.0474 -0.0881 0.159 Uiso 1 1 calc R . . H35B H 0.4141 0.0205 -0.0255 0.159 Uiso 1 1 calc R . . C36 C 0.4111(7) -0.2209(14) -0.0655(5) 0.176(5) Uani 1 1 d . . . H36A H 0.4559 -0.2326 -0.0591 0.264 Uiso 1 1 calc R . . H36B H 0.3928 -0.2676 -0.1013 0.264 Uiso 1 1 calc R . . H36C H 0.3957 -0.2946 -0.0389 0.264 Uiso 1 1 calc R . . C37 C 0.3171(4) 0.3314(13) -0.1053(3) 0.104(3) Uani 1 1 d . . . H37A H 0.3058 0.4591 -0.0956 0.124 Uiso 1 1 calc R . . H37B H 0.3617 0.3317 -0.1040 0.124 Uiso 1 1 calc R . . C38 C 0.2848(5) 0.2940(15) -0.1605(3) 0.119(3) Uani 1 1 d . . . H38A H 0.2401 0.2902 -0.1620 0.143 Uiso 1 1 calc R . . H38B H 0.2972 0.1687 -0.1712 0.143 Uiso 1 1 calc R . . C39 C 0.2975(6) 0.4404(19) -0.2010(5) 0.179(6) Uani 1 1 d . . . H39A H 0.2748 0.4065 -0.2368 0.268 Uiso 1 1 calc R . . H39B H 0.3415 0.4433 -0.2004 0.268 Uiso 1 1 calc R . . H39C H 0.2842 0.5645 -0.1914 0.268 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 0.0502(4) 0.0398(3) 0.0642(4) 0.0044(3) 0.0177(3) -0.0040(3) Cu2 0.0582(4) 0.0377(3) 0.0425(3) -0.0019(2) 0.0081(3) -0.0031(3) Cu3 0.0577(4) 0.0487(4) 0.0518(4) -0.0056(3) 0.0172(3) -0.0100(3) Cl1 0.0488(6) 0.0332(5) 0.0425(6) 0.0039(4) 0.0105(5) -0.0024(5) Cl2 0.0471(6) 0.0468(7) 0.0405(6) -0.0028(5) 0.0073(5) -0.0050(5) Cl3 0.0580(8) 0.0552(8) 0.0664(8) -0.0026(6) 0.0229(6) 0.0035(6) S1 0.0477(8) 0.0760(10) 0.0606(9) 0.0146(7) 0.0103(6) -0.0050(7) S2 0.0475(7) 0.0686(9) 0.0441(7) 0.0053(6) 0.0086(5) 0.0001(6) S3 0.0697(10) 0.1081(13) 0.0446(8) -0.0020(8) 0.0178(7) -0.0136(9) C1 0.066(3) 0.032(2) 0.049(3) 0.000(2) 0.013(2) -0.012(2) N1 0.057(2) 0.032(2) 0.043(2) -0.0015(16) 0.0074(18) -0.0116(17) C11 0.061(3) 0.060(3) 0.052(3) -0.005(3) 0.005(3) -0.021(3) C12 0.066(4) 0.063(4) 0.062(3) -0.007(3) 0.012(3) -0.021(3) C13 0.050(3) 0.069(4) 0.090(4) 0.010(3) 0.023(3) -0.006(3) C14 0.063(4) 0.074(4) 0.108(5) 0.007(4) 0.025(4) -0.012(3) C15 0.072(5) 0.109(6) 0.111(6) 0.030(5) -0.002(4) -0.015(4) C16 0.087(6) 0.131(8) 0.164(9) -0.001(7) 0.012(6) -0.039(5) C17 0.065(4) 0.060(4) 0.137(6) 0.000(4) 0.029(4) -0.002(3) C18 0.086(5) 0.076(5) 0.168(9) 0.005(5) 0.046(6) 0.000(4) C19 0.100(7) 0.184(11) 0.144(9) -0.040(8) 0.046(7) 0.008(7) C2 0.066(3) 0.028(2) 0.048(3) -0.009(2) 0.013(2) -0.005(2) N2 0.052(2) 0.034(2) 0.047(2) 0.0019(17) 0.0116(18) 0.0029(17) C21 0.068(4) 0.049(3) 0.074(4) 0.000(3) 0.022(3) 0.016(3) C22 0.059(3) 0.067(4) 0.066(4) -0.012(3) 0.022(3) 0.005(3) C23 0.070(4) 0.064(4) 0.062(4) 0.002(3) 0.011(3) -0.002(3) C24 0.070(4) 0.078(4) 0.068(4) 0.002(3) 0.027(3) 0.010(3) C25 0.103(5) 0.071(4) 0.082(5) -0.008(4) 0.018(4) 0.022(4) C26 0.096(6) 0.110(6) 0.113(6) -0.028(5) 0.002(5) 0.003(5) C27 0.074(4) 0.083(4) 0.079(4) -0.011(3) 0.028(3) 0.016(3) C28 0.065(4) 0.111(6) 0.098(5) -0.001(5) 0.012(4) -0.002(4) C29 0.073(5) 0.104(6) 0.143(7) -0.030(5) 0.007(5) 0.008(4) C3 0.065(3) 0.031(2) 0.060(3) 0.009(2) 0.011(3) 0.005(2) N3 0.061(3) 0.035(2) 0.046(2) 0.0085(17) 0.0132(19) -0.0032(18) C31 0.093(4) 0.050(3) 0.053(3) 0.019(3) 0.013(3) -0.006(3) C32 0.083(4) 0.097(5) 0.066(4) 0.034(4) 0.017(3) 0.008(4) C33 0.088(5) 0.086(5) 0.076(4) 0.000(4) 0.040(4) -0.023(4) C34 0.140(7) 0.090(5) 0.088(5) 0.002(4) 0.064(5) -0.007(5) C35 0.149(9) 0.119(8) 0.156(9) -0.003(7) 0.092(8) 0.003(7) C36 0.276(16) 0.085(7) 0.199(12) -0.006(7) 0.122(12) -0.007(8) C37 0.098(6) 0.114(6) 0.103(6) 0.025(5) 0.031(5) -0.014(5) C38 0.130(7) 0.156(9) 0.073(5) 0.022(5) 0.025(5) -0.029(6) C39 0.169(11) 0.231(14) 0.156(10) 0.097(10) 0.078(9) 0.014(10) _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 N1 2.188(4) . ? Cu1 Cl1 2.2702(12) . ? Cu1 Cl3 2.2907(15) . ? Cu1 S1 2.3839(15) . ? Cu1 Cu3 2.9331(9) . ? Cu2 N2 2.186(4) . ? Cu2 Cl2 2.2561(13) . ? Cu2 Cl1 2.3413(13) . ? Cu2 S2 2.3745(14) . ? Cu2 Cu3 2.9279(8) . ? Cu3 N3 2.188(4) . ? Cu3 Cl3 2.2976(15) . ? Cu3 Cl2 2.3043(13) . ? Cu3 S3 2.3925(16) . ? S1 C13 1.826(6) . ? S1 C12 1.843(6) . ? S2 C22 1.798(6) . ? S2 C23 1.850(6) . ? S3 C32 1.764(7) . ? S3 C33 1.816(7) . ? C1 N3 1.463(6) . ? C1 N1 1.464(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.466(6) . ? N1 C11 1.495(6) . ? C11 C12 1.463(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.505(8) . ? C13 C17 1.555(9) . ? C13 H13 1.0000 . ? C14 C15 1.502(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.539(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.494(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.470(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C2 N2 1.468(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.470(6) . ? N2 C21 1.504(6) . ? C21 C22 1.505(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.473(8) . ? C23 C27 1.548(8) . ? C23 H23 1.0000 . ? C24 C25 1.500(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.512(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.505(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C3 N3 1.469(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.494(6) . ? C31 C32 1.492(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C37 1.512(9) . ? C33 C34 1.523(10) . ? C33 H33 1.0000 . ? C34 C35 1.551(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.433(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.469(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.539(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 N1 Cu1 Cl1 106.01(11) . . ? N1 Cu1 Cl3 113.80(11) . . ? Cl1 Cu1 Cl3 125.86(5) . . ? N1 Cu1 S1 87.84(11) . . ? Cl1 Cu1 S1 111.94(5) . . ? Cl3 Cu1 S1 104.91(6) . . ? N1 Cu1 Cu3 83.18(10) . . ? Cl1 Cu1 Cu3 102.83(4) . . ? Cl3 Cu1 Cu3 50.37(4) . . ? S1 Cu1 Cu3 145.23(4) . . ? N2 Cu2 Cl2 114.52(11) . . ? N2 Cu2 Cl1 106.52(11) . . ? Cl2 Cu2 Cl1 122.51(5) . . ? N2 Cu2 S2 90.02(11) . . ? Cl2 Cu2 S2 118.64(5) . . ? Cl1 Cu2 S2 99.09(5) . . ? N2 Cu2 Cu3 81.43(10) . . ? Cl2 Cu2 Cu3 50.78(3) . . ? Cl1 Cu2 Cu3 101.19(4) . . ? S2 Cu2 Cu3 159.51(4) . . ? N3 Cu3 Cl3 110.55(12) . . ? N3 Cu3 Cl2 116.94(12) . . ? Cl3 Cu3 Cl2 121.89(5) . . ? N3 Cu3 S3 89.37(11) . . ? Cl3 Cu3 S3 110.08(6) . . ? Cl2 Cu3 S3 102.15(5) . . ? N3 Cu3 Cu2 85.15(10) . . ? Cl3 Cu3 Cu2 107.02(4) . . ? Cl2 Cu3 Cu2 49.34(3) . . ? S3 Cu3 Cu2 142.02(5) . . ? N3 Cu3 Cu1 82.81(11) . . ? Cl3 Cu3 Cu1 50.16(4) . . ? Cl2 Cu3 Cu1 104.71(4) . . ? S3 Cu3 Cu1 152.71(5) . . ? Cu2 Cu3 Cu1 63.49(2) . . ? Cu1 Cl1 Cu2 83.92(4) . . ? Cu2 Cl2 Cu3 79.88(4) . . ? Cu1 Cl3 Cu3 79.48(5) . . ? C13 S1 C12 101.3(3) . . ? C13 S1 Cu1 108.1(2) . . ? C12 S1 Cu1 91.81(19) . . ? C22 S2 C23 99.0(3) . . ? C22 S2 Cu2 91.87(18) . . ? C23 S2 Cu2 116.74(19) . . ? C32 S3 C33 108.6(3) . . ? C32 S3 Cu3 91.5(2) . . ? C33 S3 Cu3 103.1(2) . . ? N3 C1 N1 110.5(4) . . ? N3 C1 H1A 109.6 . . ? N1 C1 H1A 109.6 . . ? N3 C1 H1B 109.6 . . ? N1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 N1 C2 110.3(4) . . ? C1 N1 C11 109.3(4) . . ? C2 N1 C11 105.2(4) . . ? C1 N1 Cu1 111.9(3) . . ? C2 N1 Cu1 113.7(3) . . ? C11 N1 Cu1 106.2(3) . . ? C12 C11 N1 113.1(5) . . ? C12 C11 H11A 109.0 . . ? N1 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? N1 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 S1 109.1(4) . . ? C11 C12 H12A 109.9 . . ? S1 C12 H12A 109.9 . . ? C11 C12 H12B 109.9 . . ? S1 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C14 C13 C17 114.5(5) . . ? C14 C13 S1 112.8(5) . . ? C17 C13 S1 104.9(4) . . ? C14 C13 H13 108.1 . . ? C17 C13 H13 108.1 . . ? S1 C13 H13 108.1 . . ? C15 C14 C13 116.3(6) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 111.5(7) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C13 116.7(6) . . ? C18 C17 H17A 108.1 . . ? C13 C17 H17A 108.1 . . ? C18 C17 H17B 108.1 . . ? C13 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C19 C18 C17 114.2(8) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C2 N2 110.9(4) . . ? N1 C2 H2A 109.5 . . ? N2 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C2 N2 C3 108.8(4) . . ? C2 N2 C21 108.1(4) . . ? C3 N2 C21 107.0(4) . . ? C2 N2 Cu2 112.2(3) . . ? C3 N2 Cu2 115.6(3) . . ? C21 N2 Cu2 104.6(3) . . ? N2 C21 C22 113.2(4) . . ? N2 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N2 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 S2 112.9(4) . . ? C21 C22 H22A 109.0 . . ? S2 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? S2 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C27 114.3(5) . . ? C24 C23 S2 107.9(4) . . ? C27 C23 S2 112.0(4) . . ? C24 C23 H23 107.4 . . ? C27 C23 H23 107.4 . . ? S2 C23 H23 107.4 . . ? C23 C24 C25 116.9(5) . . ? C23 C24 H24A 108.1 . . ? C25 C24 H24A 108.1 . . ? C23 C24 H24B 108.1 . . ? C25 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C24 C25 C26 111.2(6) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 115.2(6) . . ? C28 C27 H27A 108.5 . . ? C23 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C23 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C27 113.2(6) . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C3 N2 110.7(4) . . ? N3 C3 H3A 109.5 . . ? N2 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C1 N3 C3 107.6(4) . . ? C1 N3 C31 106.6(4) . . ? C3 N3 C31 109.6(4) . . ? C1 N3 Cu3 115.0(3) . . ? C3 N3 Cu3 111.4(3) . . ? C31 N3 Cu3 106.5(3) . . ? C32 C31 N3 114.0(5) . . ? C32 C31 H31A 108.8 . . ? N3 C31 H31A 108.8 . . ? C32 C31 H31B 108.8 . . ? N3 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 S3 116.5(5) . . ? C31 C32 H32A 108.2 . . ? S3 C32 H32A 108.2 . . ? C31 C32 H32B 108.2 . . ? S3 C32 H32B 108.2 . . ? H32A C32 H32B 107.3 . . ? C37 C33 C34 113.9(6) . . ? C37 C33 S3 114.3(6) . . ? C34 C33 S3 109.4(5) . . ? C37 C33 H33 106.2 . . ? C34 C33 H33 106.2 . . ? S3 C33 H33 106.2 . . ? C33 C34 C35 112.4(7) . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 110.5(10) . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C33 116.6(7) . . ? C38 C37 H37A 108.1 . . ? C33 C37 H37A 108.1 . . ? C38 C37 H37B 108.1 . . ? C33 C37 H37B 108.1 . . ? H37A C37 H37B 107.3 . . ? C37 C38 C39 113.9(9) . . ? C37 C38 H38A 108.8 . . ? C39 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? C39 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.858 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.080 # Attachment '3a-A.cif' data_k08rdk13 _database_code_depnum_ccdc_archive 'CCDC 707391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 Br3 Cu3 N6' _chemical_formula_sum 'C21 H24 Br3 Cu3 N6' _chemical_formula_weight 790.81 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3337(3) _cell_length_b 10.5558(5) _cell_length_c 18.1198(8) _cell_angle_alpha 74.658(2) _cell_angle_beta 81.920(2) _cell_angle_gamma 86.404(2) _cell_volume 1338.81(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10626 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 6.859 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '166 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18540 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6127 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR2004- Burla M.C., Caliandro R., Camalli M., Carrozzini B, Cascarano G.L., De Caro L., Giacovazzo C., Polidori G.,Spagna R. (2005) J. Appl. Cryst. 38, 381-388. ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6127 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _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 0.73797(10) 0.40751(8) 0.15062(4) 0.0308(2) Uani 1 1 d . . . Cu2 Cu 0.75095(10) 0.27068(8) 0.31461(4) 0.0307(2) Uani 1 1 d . . . Cu3 Cu 0.81499(10) 0.12913(7) 0.20495(4) 0.0292(2) Uani 1 1 d . . . Br1 Br 0.58389(9) 0.47319(6) 0.26556(4) 0.03452(18) Uani 1 1 d . . . Br2 Br 0.59154(8) 0.06960(6) 0.32271(4) 0.03088(17) Uani 1 1 d . . . Br3 Br 0.67974(8) 0.24104(6) 0.08908(3) 0.02880(17) Uani 1 1 d . . . C1 C 1.1466(8) 0.3157(6) 0.1252(3) 0.0257(14) Uani 1 1 d . . . H1A H 1.2797 0.3335 0.1187 0.031 Uiso 1 1 calc R . . H1B H 1.1156 0.3047 0.0759 0.031 Uiso 1 1 calc R . . N1 N 1.0381(6) 0.4257(5) 0.1457(3) 0.0227(11) Uani 1 1 d . . . C11 C 1.0859(8) 0.5467(5) 0.0853(3) 0.0239(14) Uani 1 1 d . . . H11A H 1.1107 0.5256 0.0346 0.029 Uiso 1 1 calc R . . H11B H 1.2001 0.5813 0.0950 0.029 Uiso 1 1 calc R . . C12 C 0.9351(8) 0.6516(6) 0.0819(3) 0.0278(15) Uani 1 1 d . . . C13 C 0.9707(10) 0.7824(6) 0.0757(4) 0.0346(16) Uani 1 1 d . . . H13 H 1.0920 0.8087 0.0761 0.041 Uiso 1 1 calc R . . C14 C 0.8246(11) 0.8735(7) 0.0690(4) 0.0425(19) Uani 1 1 d . . . H14 H 0.8439 0.9633 0.0652 0.051 Uiso 1 1 calc R . . C15 C 0.6508(11) 0.8307(7) 0.0681(4) 0.046(2) Uani 1 1 d . . . H15 H 0.5495 0.8915 0.0613 0.055 Uiso 1 1 calc R . . C16 C 0.6263(10) 0.6993(7) 0.0771(4) 0.0429(19) Uani 1 1 d . . . H16 H 0.5054 0.6708 0.0782 0.051 Uiso 1 1 calc R . . N11 N 0.7658(7) 0.6084(5) 0.0843(3) 0.0299(13) Uani 1 1 d . . . C2 C 1.0836(9) 0.4421(6) 0.2197(3) 0.0288(15) Uani 1 1 d . . . H2A H 1.2150 0.4639 0.2141 0.035 Uiso 1 1 calc R . . H2B H 1.0080 0.5152 0.2338 0.035 Uiso 1 1 calc R . . N2 N 1.0475(7) 0.3200(5) 0.2807(3) 0.0235(11) Uani 1 1 d . . . C21 C 1.1054(9) 0.3392(6) 0.3522(3) 0.0286(15) Uani 1 1 d . . . H21A H 1.0752 0.4308 0.3548 0.034 Uiso 1 1 calc R . . H21B H 1.2407 0.3257 0.3502 0.034 Uiso 1 1 calc R . . C22 C 1.0128(8) 0.2460(6) 0.4241(3) 0.0267(14) Uani 1 1 d . . . C23 C 1.1041(9) 0.1964(6) 0.4881(3) 0.0303(15) Uani 1 1 d . . . H23 H 1.2310 0.2128 0.4857 0.036 Uiso 1 1 calc R . . C24 C 1.0088(10) 0.1227(6) 0.5554(3) 0.0347(17) Uani 1 1 d . . . H24 H 1.0671 0.0905 0.6007 0.042 Uiso 1 1 calc R . . C25 C 0.8254(10) 0.0968(6) 0.5552(4) 0.0348(16) Uani 1 1 d . . . H25 H 0.7553 0.0473 0.6006 0.042 Uiso 1 1 calc R . . C26 C 0.7470(9) 0.1439(6) 0.4883(3) 0.0329(16) Uani 1 1 d . . . H26 H 0.6234 0.1224 0.4878 0.039 Uiso 1 1 calc R . . N21 N 0.8379(7) 0.2189(5) 0.4235(3) 0.0296(13) Uani 1 1 d . . . C3 C 1.1594(8) 0.2117(6) 0.2587(3) 0.0245(14) Uani 1 1 d . . . H3A H 1.2917 0.2323 0.2507 0.029 Uiso 1 1 calc R . . H3B H 1.1399 0.1296 0.3003 0.029 Uiso 1 1 calc R . . N3 N 1.1045(6) 0.1950(4) 0.1875(3) 0.0222(11) Uani 1 1 d . . . C31 C 1.2145(9) 0.0836(6) 0.1656(4) 0.0308(16) Uani 1 1 d . . . H31A H 1.3444 0.0891 0.1734 0.037 Uiso 1 1 calc R . . H31B H 1.2114 0.0906 0.1102 0.037 Uiso 1 1 calc R . . C32 C 1.1403(9) -0.0477(6) 0.2131(3) 0.0286(15) Uani 1 1 d . . . C33 C 1.2556(9) -0.1519(7) 0.2414(4) 0.0361(17) Uani 1 1 d . . . H33 H 1.3856 -0.1435 0.2328 0.043 Uiso 1 1 calc R . . C34 C 1.1753(11) -0.2705(7) 0.2833(4) 0.0432(19) Uani 1 1 d . . . H34 H 1.2501 -0.3450 0.3034 0.052 Uiso 1 1 calc R . . C35 C 0.9884(10) -0.2778(6) 0.2949(4) 0.0347(17) Uani 1 1 d . . . H35 H 0.9314 -0.3574 0.3235 0.042 Uiso 1 1 calc R . . C36 C 0.8819(10) -0.1681(6) 0.2647(4) 0.0355(17) Uani 1 1 d . . . H36 H 0.7516 -0.1745 0.2730 0.043 Uiso 1 1 calc R . . N31 N 0.9558(7) -0.0534(5) 0.2242(3) 0.0273(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0237(4) 0.0310(4) 0.0358(4) -0.0055(4) -0.0024(3) -0.0033(3) Cu2 0.0296(4) 0.0302(4) 0.0290(4) -0.0004(3) -0.0069(3) -0.0011(3) Cu3 0.0249(4) 0.0281(4) 0.0307(4) -0.0008(3) -0.0047(3) 0.0005(3) Br1 0.0286(4) 0.0315(4) 0.0368(4) -0.0019(3) 0.0018(3) 0.0049(3) Br2 0.0252(3) 0.0301(4) 0.0323(3) 0.0008(3) -0.0025(3) -0.0027(3) Br3 0.0261(3) 0.0304(3) 0.0272(3) -0.0005(3) -0.0062(3) -0.0044(3) C1 0.023(3) 0.025(3) 0.025(3) -0.001(3) 0.002(3) -0.005(3) N1 0.022(3) 0.022(3) 0.022(3) -0.002(2) -0.003(2) -0.002(2) C11 0.026(3) 0.023(3) 0.020(3) 0.000(2) -0.003(3) -0.004(3) C12 0.032(4) 0.022(3) 0.025(3) 0.000(3) -0.003(3) 0.002(3) C13 0.046(4) 0.027(4) 0.032(4) -0.005(3) -0.013(3) -0.001(3) C14 0.068(5) 0.026(4) 0.031(4) -0.006(3) -0.002(4) 0.003(4) C15 0.047(5) 0.041(5) 0.035(4) 0.005(3) 0.007(3) 0.013(4) C16 0.031(4) 0.042(5) 0.044(4) 0.002(4) 0.006(3) 0.000(3) N11 0.023(3) 0.034(3) 0.029(3) -0.002(2) -0.007(2) 0.006(2) C2 0.028(3) 0.024(3) 0.031(3) -0.001(3) -0.001(3) -0.005(3) N2 0.030(3) 0.020(3) 0.020(2) -0.004(2) -0.004(2) -0.004(2) C21 0.034(4) 0.031(4) 0.023(3) -0.005(3) -0.010(3) -0.006(3) C22 0.032(4) 0.026(3) 0.021(3) -0.005(3) -0.004(3) -0.001(3) C23 0.032(4) 0.037(4) 0.025(3) -0.011(3) -0.009(3) -0.006(3) C24 0.053(5) 0.032(4) 0.020(3) -0.004(3) -0.009(3) 0.000(3) C25 0.048(4) 0.028(4) 0.029(4) -0.008(3) -0.003(3) -0.005(3) C26 0.034(4) 0.030(4) 0.030(4) -0.003(3) 0.001(3) -0.004(3) N21 0.031(3) 0.027(3) 0.027(3) -0.001(2) 0.000(2) 0.002(2) C3 0.022(3) 0.022(3) 0.029(3) -0.004(3) -0.006(3) 0.002(3) N3 0.025(3) 0.018(3) 0.023(3) -0.005(2) -0.001(2) -0.001(2) C31 0.032(4) 0.026(3) 0.029(3) -0.002(3) 0.002(3) 0.007(3) C32 0.033(4) 0.023(3) 0.029(3) -0.005(3) -0.005(3) 0.000(3) C33 0.025(4) 0.043(4) 0.040(4) -0.009(3) -0.007(3) 0.012(3) C34 0.053(5) 0.029(4) 0.045(4) -0.009(3) -0.008(4) 0.013(3) C35 0.055(5) 0.013(3) 0.033(4) -0.003(3) 0.001(3) -0.005(3) C36 0.041(4) 0.024(4) 0.040(4) -0.008(3) 0.002(3) -0.006(3) N31 0.029(3) 0.025(3) 0.029(3) -0.009(2) -0.003(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.150(5) . ? Cu1 N1 2.209(5) . ? Cu1 Br3 2.4038(11) . ? Cu1 Br1 2.4697(11) . ? Cu1 Cu3 2.8880(11) . ? Cu1 Cu2 2.9523(10) . ? Cu2 N21 2.083(5) . ? Cu2 N2 2.231(5) . ? Cu2 Br1 2.4151(9) . ? Cu2 Br2 2.4478(11) . ? Cu2 Cu3 2.7609(12) . ? Cu3 N31 2.096(5) . ? Cu3 N3 2.229(5) . ? Cu3 Br3 2.4317(9) . ? Cu3 Br2 2.4638(9) . ? C1 N1 1.466(7) . ? C1 N3 1.478(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.470(6) . ? N1 C2 1.481(8) . ? C11 C12 1.511(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.340(8) . ? C12 C13 1.394(9) . ? C13 C14 1.390(9) . ? C13 H13 0.9500 . ? C14 C15 1.383(10) . ? C14 H14 0.9500 . ? C15 C16 1.373(10) . ? C15 H15 0.9500 . ? C16 N11 1.354(8) . ? C16 H16 0.9500 . ? C2 N2 1.469(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.473(7) . ? N2 C21 1.486(7) . ? C21 C22 1.511(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.333(8) . ? C22 C23 1.385(8) . ? C23 C24 1.381(8) . ? C23 H23 0.9500 . ? C24 C25 1.390(9) . ? C24 H24 0.9500 . ? C25 C26 1.374(8) . ? C25 H25 0.9500 . ? C26 N21 1.343(7) . ? C26 H26 0.9500 . ? C3 N3 1.462(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.493(7) . ? C31 C32 1.513(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.342(8) . ? C32 C33 1.377(8) . ? C33 C34 1.398(9) . ? C33 H33 0.9500 . ? C34 C35 1.361(10) . ? C34 H34 0.9500 . ? C35 C36 1.386(8) . ? C35 H35 0.9500 . ? C36 N31 1.342(7) . ? C36 H36 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 N11 Cu1 N1 80.62(17) . . ? N11 Cu1 Br3 119.95(15) . . ? N1 Cu1 Br3 109.60(14) . . ? N11 Cu1 Br1 92.23(15) . . ? N1 Cu1 Br1 108.26(14) . . ? Br3 Cu1 Br1 133.32(4) . . ? N11 Cu1 Cu3 160.24(14) . . ? N1 Cu1 Cu3 84.52(12) . . ? Br3 Cu1 Cu3 53.77(3) . . ? Br1 Cu1 Cu3 104.80(3) . . ? N11 Cu1 Cu2 134.21(15) . . ? N1 Cu1 Cu2 84.96(12) . . ? Br3 Cu1 Cu2 105.84(3) . . ? Br1 Cu1 Cu2 51.98(3) . . ? Cu3 Cu1 Cu2 56.41(3) . . ? N21 Cu2 N2 80.79(18) . . ? N21 Cu2 Br1 123.15(15) . . ? N2 Cu2 Br1 104.95(12) . . ? N21 Cu2 Br2 98.82(15) . . ? N2 Cu2 Br2 130.60(13) . . ? Br1 Cu2 Br2 115.30(4) . . ? N21 Cu2 Cu3 126.51(15) . . ? N2 Cu2 Cu3 84.41(13) . . ? Br1 Cu2 Cu3 110.31(4) . . ? Br2 Cu2 Cu3 56.07(3) . . ? N21 Cu2 Cu1 159.54(15) . . ? N2 Cu2 Cu1 81.07(11) . . ? Br1 Cu2 Cu1 53.66(3) . . ? Br2 Cu2 Cu1 100.14(3) . . ? Cu3 Cu2 Cu1 60.62(3) . . ? N31 Cu3 N3 79.95(18) . . ? N31 Cu3 Br3 126.19(14) . . ? N3 Cu3 Br3 106.87(12) . . ? N31 Cu3 Br2 95.52(13) . . ? N3 Cu3 Br2 130.84(13) . . ? Br3 Cu3 Br2 114.42(3) . . ? N31 Cu3 Cu2 122.69(14) . . ? N3 Cu3 Cu2 85.86(13) . . ? Br3 Cu3 Cu2 111.09(3) . . ? Br2 Cu3 Cu2 55.52(3) . . ? N31 Cu3 Cu1 161.05(14) . . ? N3 Cu3 Cu1 82.63(12) . . ? Br3 Cu3 Cu1 52.88(3) . . ? Br2 Cu3 Cu1 101.52(3) . . ? Cu2 Cu3 Cu1 62.97(3) . . ? Cu2 Br1 Cu1 74.36(3) . . ? Cu2 Br2 Cu3 68.40(3) . . ? Cu1 Br3 Cu3 73.34(3) . . ? N1 C1 N3 108.7(4) . . ? N1 C1 H1A 110.0 . . ? N3 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? N3 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? C1 N1 C11 108.6(4) . . ? C1 N1 C2 110.1(4) . . ? C11 N1 C2 108.3(5) . . ? C1 N1 Cu1 113.6(4) . . ? C11 N1 Cu1 105.5(3) . . ? C2 N1 Cu1 110.6(3) . . ? N1 C11 C12 112.6(5) . . ? N1 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N1 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N11 C12 C13 123.2(6) . . ? N11 C12 C11 114.3(5) . . ? C13 C12 C11 122.5(6) . . ? C14 C13 C12 118.5(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N11 C16 C15 123.3(7) . . ? N11 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C12 N11 C16 117.0(6) . . ? C12 N11 Cu1 111.7(4) . . ? C16 N11 Cu1 124.5(4) . . ? N2 C2 N1 109.8(5) . . ? N2 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 N2 C3 109.2(5) . . ? C2 N2 C21 107.5(5) . . ? C3 N2 C21 108.8(4) . . ? C2 N2 Cu2 115.1(4) . . ? C3 N2 Cu2 112.3(4) . . ? C21 N2 Cu2 103.6(3) . . ? N2 C21 C22 112.3(5) . . ? N2 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? N2 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? N21 C22 C23 122.3(5) . . ? N21 C22 C21 116.5(5) . . ? C23 C22 C21 121.1(6) . . ? C24 C23 C22 119.3(6) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 118.2(6) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C26 C25 C24 119.1(6) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N21 C26 C25 122.7(6) . . ? N21 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C22 N21 C26 118.3(5) . . ? C22 N21 Cu2 114.6(4) . . ? C26 N21 Cu2 126.2(4) . . ? N3 C3 N2 108.6(4) . . ? N3 C3 H3A 110.0 . . ? N2 C3 H3A 110.0 . . ? N3 C3 H3B 110.0 . . ? N2 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? C3 N3 C1 108.8(5) . . ? C3 N3 C31 109.0(4) . . ? C1 N3 C31 108.2(4) . . ? C3 N3 Cu3 111.6(3) . . ? C1 N3 Cu3 115.5(3) . . ? C31 N3 Cu3 103.4(4) . . ? N3 C31 C32 111.4(5) . . ? N3 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? N3 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? N31 C32 C33 123.7(6) . . ? N31 C32 C31 114.6(5) . . ? C33 C32 C31 121.7(6) . . ? C32 C33 C34 117.9(6) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C35 C34 C33 119.1(6) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C36 119.5(6) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? N31 C36 C35 122.5(6) . . ? N31 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 N31 C32 117.4(5) . . ? C36 N31 Cu3 124.9(4) . . ? C32 N31 Cu3 115.2(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.717 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.160 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.064 0.500 0.500 151.2 6.0 2 0.500 0.500 0.000 8.6 -0.6 _platon_squeeze_details ; The asymmetrical unit contains one disordered solvent molecule of acetonitrile. ; # Attachment '3a-B.cif' data_k08rdk11 _database_code_depnum_ccdc_archive 'CCDC 707392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H24 Br3 Cu3 N6), 0.5(C4 H6 N2), C2 H3 N' _chemical_formula_sum 'C46 H54 Br6 Cu6 N14' _chemical_formula_weight 1663.73 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.50940(10) _cell_length_b 16.16180(10) _cell_length_c 17.23840(10) _cell_angle_alpha 62.5160(10) _cell_angle_beta 83.9880(10) _cell_angle_gamma 79.1640(10) _cell_volume 2793.35(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40592 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 6.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.232 _exptl_absorpt_correction_T_max 0.307 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '281 2.0 degree images with \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 70160 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 30.06 _reflns_number_total 16330 _reflns_number_gt 13505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0432P)^2^+1.1353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16330 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _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 0.26281(3) -1.01807(2) -0.79418(2) 0.02631(7) Uani 1 1 d . . . Cu2 Cu 0.28164(3) -0.85462(2) -0.790083(19) 0.02492(7) Uani 1 1 d . . . Cu3 Cu 0.09158(3) -0.94959(2) -0.69691(2) 0.02501(7) Uani 1 1 d . . . Cu4 Cu -0.13096(3) -0.47778(2) -0.78755(2) 0.02843(7) Uani 1 1 d . . . Cu5 Cu -0.28520(3) -0.62227(2) -0.72773(2) 0.02777(7) Uani 1 1 d . . . Cu6 Cu -0.34005(3) -0.46354(2) -0.69309(2) 0.02819(7) Uani 1 1 d . . . Br1 Br 0.14790(2) -1.116223(17) -0.673045(16) 0.02853(6) Uani 1 1 d . . . Br2 Br 0.43654(2) -0.994180(18) -0.741394(18) 0.03019(6) Uani 1 1 d . . . Br3 Br 0.17436(2) -0.842884(19) -0.665395(16) 0.02745(6) Uani 1 1 d . . . Br4 Br -0.24626(2) -0.329934(17) -0.810973(16) 0.02891(6) Uani 1 1 d . . . Br5 Br -0.16249(2) -0.578092(18) -0.856437(16) 0.02718(6) Uani 1 1 d . . . Br6 Br -0.47829(2) -0.520794(18) -0.741256(17) 0.02873(6) Uani 1 1 d . . . C1 C 0.0114(2) -0.91568(17) -0.87540(16) 0.0225(4) Uani 1 1 d . . . H1A H -0.0392 -0.8804 -0.9274 0.027 Uiso 1 1 calc R . . H1B H -0.0143 -0.9779 -0.8397 0.027 Uiso 1 1 calc R . . N1 N 0.13545(17) -0.92893(14) -0.90313(13) 0.0206(4) Uani 1 1 d . . . C11 C 0.1465(2) -0.98084(19) -0.95550(17) 0.0285(5) Uani 1 1 d . . . H11A H 0.1197 -0.9364 -1.0156 0.034 Uiso 1 1 calc R . . H11B H 0.0940 -1.0295 -0.9297 0.034 Uiso 1 1 calc R . . C12 C 0.2716(2) -1.02794(18) -0.95994(17) 0.0285(5) Uani 1 1 d . . . C13 C 0.3159(3) -1.0411(2) -1.0322(2) 0.0401(7) Uani 1 1 d . . . H13 H 0.2709 -1.0147 -1.0837 0.048 Uiso 1 1 calc R . . C14 C 0.4283(3) -1.0940(2) -1.0273(2) 0.0483(9) Uani 1 1 d . . . H14 H 0.4604 -1.1049 -1.0755 0.058 Uiso 1 1 calc R . . C15 C 0.4915(3) -1.1300(2) -0.9529(2) 0.0470(9) Uani 1 1 d . . . H15 H 0.5668 -1.1682 -0.9476 0.056 Uiso 1 1 calc R . . C16 C 0.4441(3) -1.1098(2) -0.8850(2) 0.0380(7) Uani 1 1 d . . . H16 H 0.4901 -1.1316 -0.8346 0.046 Uiso 1 1 calc R . . N11 N 0.3350(2) -1.06037(15) -0.88815(15) 0.0297(5) Uani 1 1 d . . . C2 C 0.1724(2) -0.83590(16) -0.95668(15) 0.0205(4) Uani 1 1 d . . . H2A H 0.2553 -0.8441 -0.9774 0.025 Uiso 1 1 calc R . . H2B H 0.1216 -0.7991 -1.0084 0.025 Uiso 1 1 calc R . . N2 N 0.16192(17) -0.78544(14) -0.90367(13) 0.0203(4) Uani 1 1 d . . . C21 C 0.1986(2) -0.69145(16) -0.95675(16) 0.0221(4) Uani 1 1 d . . . H21A H 0.1551 -0.6468 -0.9352 0.027 Uiso 1 1 calc R . . H21B H 0.1766 -0.6676 -1.0183 0.027 Uiso 1 1 calc R . . C22 C 0.3297(2) -0.69388(16) -0.95346(16) 0.0216(4) Uani 1 1 d . . . C23 C 0.3908(2) -0.63249(19) -1.02432(17) 0.0290(5) Uani 1 1 d . . . H23 H 0.3533 -0.5930 -1.0788 0.035 Uiso 1 1 calc R . . C24 C 0.5080(3) -0.6302(2) -1.01362(19) 0.0362(6) Uani 1 1 d . . . H24 H 0.5515 -0.5880 -1.0604 0.043 Uiso 1 1 calc R . . C25 C 0.5606(2) -0.6901(2) -0.9342(2) 0.0354(6) Uani 1 1 d . . . H25 H 0.6400 -0.6887 -0.9249 0.042 Uiso 1 1 calc R . . C26 C 0.4951(2) -0.75203(19) -0.86838(17) 0.0282(5) Uani 1 1 d . . . H26 H 0.5323 -0.7954 -0.8147 0.034 Uiso 1 1 calc R . . N21 N 0.38120(18) -0.75328(14) -0.87737(13) 0.0231(4) Uani 1 1 d . . . C3 C 0.0369(2) -0.77106(16) -0.87711(15) 0.0216(4) Uani 1 1 d . . . H3A H 0.0273 -0.7351 -0.8427 0.026 Uiso 1 1 calc R . . H3B H -0.0125 -0.7342 -0.9296 0.026 Uiso 1 1 calc R . . N3 N -0.00147(17) -0.86328(14) -0.82407(13) 0.0203(4) Uani 1 1 d . . . C31 C -0.1275(2) -0.84723(18) -0.79803(16) 0.0247(5) Uani 1 1 d . . . H31A H -0.1784 -0.8325 -0.8471 0.030 Uiso 1 1 calc R . . H31B H -0.1419 -0.7922 -0.7854 0.030 Uiso 1 1 calc R . . C32 C -0.1605(2) -0.93283(17) -0.71823(16) 0.0228(5) Uani 1 1 d . . . C33 C -0.2632(2) -0.96875(19) -0.71307(17) 0.0270(5) Uani 1 1 d . . . H33 H -0.3145 -0.9414 -0.7614 0.032 Uiso 1 1 calc R . . C34 C -0.2895(2) -1.0451(2) -0.63627(18) 0.0311(5) Uani 1 1 d . . . H34 H -0.3588 -1.0714 -0.6315 0.037 Uiso 1 1 calc R . . C35 C -0.2144(2) -1.0826(2) -0.56688(17) 0.0312(5) Uani 1 1 d . . . H35 H -0.2313 -1.1345 -0.5133 0.037 Uiso 1 1 calc R . . C36 C -0.1136(2) -1.0430(2) -0.57712(17) 0.0294(5) Uani 1 1 d . . . H36 H -0.0619 -1.0687 -0.5292 0.035 Uiso 1 1 calc R . . N31 N -0.08563(18) -0.97001(15) -0.65146(14) 0.0252(4) Uani 1 1 d . . . C4 C -0.1220(2) -0.53515(18) -0.58505(16) 0.0244(5) Uani 1 1 d . . . H4A H -0.0780 -0.5700 -0.5298 0.029 Uiso 1 1 calc R . . H4B H -0.1286 -0.4667 -0.6036 0.029 Uiso 1 1 calc R . . N4 N -0.05843(18) -0.55852(15) -0.65327(13) 0.0228(4) Uani 1 1 d . . . C41 C 0.0619(2) -0.5333(2) -0.66528(18) 0.0312(6) Uani 1 1 d . . . H41A H 0.1112 -0.5808 -0.6154 0.037 Uiso 1 1 calc R . . H41B H 0.0566 -0.4712 -0.6659 0.037 Uiso 1 1 calc R . . C42 C 0.1199(2) -0.52897(18) -0.74948(17) 0.0263(5) Uani 1 1 d . . . C43 C 0.2369(2) -0.5664(2) -0.75399(19) 0.0316(6) Uani 1 1 d . . . H43 H 0.2825 -0.6008 -0.7026 0.038 Uiso 1 1 calc R . . C44 C 0.2872(2) -0.5526(2) -0.83560(19) 0.0322(6) Uani 1 1 d . . . H44 H 0.3678 -0.5771 -0.8407 0.039 Uiso 1 1 calc R . . C45 C 0.2179(2) -0.50284(19) -0.90859(18) 0.0303(5) Uani 1 1 d . . . H45 H 0.2504 -0.4908 -0.9651 0.036 Uiso 1 1 calc R . . C46 C 0.1000(2) -0.4708(2) -0.89775(18) 0.0322(6) Uani 1 1 d . . . H46 H 0.0515 -0.4387 -0.9478 0.039 Uiso 1 1 calc R . . N41 N 0.0510(2) -0.48312(16) -0.81975(15) 0.0299(5) Uani 1 1 d . . . C5 C -0.0485(2) -0.65994(17) -0.62602(16) 0.0238(5) Uani 1 1 d . . . H5A H -0.0053 -0.6753 -0.6717 0.029 Uiso 1 1 calc R . . H5B H -0.0037 -0.6965 -0.5712 0.029 Uiso 1 1 calc R . . N5 N -0.16720(17) -0.68523(14) -0.61227(13) 0.0205(4) Uani 1 1 d . . . C51 C -0.1574(2) -0.78746(16) -0.58420(16) 0.0237(5) Uani 1 1 d . . . H51A H -0.1246 -0.8235 -0.5247 0.028 Uiso 1 1 calc R . . H51B H -0.1027 -0.8050 -0.6244 0.028 Uiso 1 1 calc R . . C52 C -0.2771(2) -0.81226(16) -0.58413(16) 0.0227(5) Uani 1 1 d . . . C53 C -0.3191(2) -0.88773(17) -0.51414(17) 0.0268(5) Uani 1 1 d . . . H53 H -0.2729 -0.9258 -0.4635 0.032 Uiso 1 1 calc R . . C54 C -0.4303(3) -0.90684(19) -0.51934(18) 0.0310(6) Uani 1 1 d . . . H54 H -0.4611 -0.9582 -0.4722 0.037 Uiso 1 1 calc R . . C55 C -0.4953(2) -0.84984(19) -0.59423(19) 0.0307(5) Uani 1 1 d . . . H55 H -0.5702 -0.8625 -0.6003 0.037 Uiso 1 1 calc R . . C56 C -0.4484(2) -0.77412(19) -0.65981(18) 0.0279(5) Uani 1 1 d . . . H56 H -0.4943 -0.7338 -0.7102 0.034 Uiso 1 1 calc R . . N51 N -0.34150(19) -0.75457(15) -0.65602(14) 0.0248(4) Uani 1 1 d . . . C6 C -0.2287(2) -0.66355(16) -0.54312(15) 0.0213(4) Uani 1 1 d . . . H6A H -0.3080 -0.6828 -0.5313 0.026 Uiso 1 1 calc R . . H6B H -0.1832 -0.6989 -0.4885 0.026 Uiso 1 1 calc R . . N6 N -0.24045(18) -0.56164(14) -0.57164(13) 0.0208(4) Uani 1 1 d . . . C61 C -0.3051(2) -0.54217(18) -0.50143(16) 0.0263(5) Uani 1 1 d . . . H61A H -0.2494 -0.5588 -0.4545 0.032 Uiso 1 1 calc R . . H61B H -0.3672 -0.5829 -0.4759 0.032 Uiso 1 1 calc R . . C62 C -0.3619(2) -0.44034(18) -0.53348(16) 0.0265(5) Uani 1 1 d . . . C63 C -0.3816(3) -0.3986(2) -0.4780(2) 0.0378(6) Uani 1 1 d . . . H63 H -0.3537 -0.4320 -0.4199 0.045 Uiso 1 1 calc R . . C64 C -0.4424(3) -0.3077(2) -0.5087(2) 0.0471(8) Uani 1 1 d . . . H64 H -0.4583 -0.2781 -0.4714 0.056 Uiso 1 1 calc R . . C65 C -0.4800(3) -0.2598(2) -0.5943(2) 0.0481(9) Uani 1 1 d . . . H65 H -0.5215 -0.1969 -0.6170 0.058 Uiso 1 1 calc R . . C66 C -0.4554(3) -0.3062(2) -0.6455(2) 0.0438(8) Uani 1 1 d . . . H66 H -0.4800 -0.2736 -0.7045 0.053 Uiso 1 1 calc R . . N61 N -0.3982(2) -0.39510(16) -0.61593(15) 0.0318(5) Uani 1 1 d . . . N7 N 0.1032(5) -1.2107(3) -0.8991(3) 0.0898(14) Uani 1 1 d . . . C71 C 0.1761(4) -1.2552(3) -0.8512(3) 0.0638(11) Uani 1 1 d . . . C72 C 0.2669(5) -1.3087(3) -0.7856(4) 0.0955(19) Uani 1 1 d . . . H72A H 0.2853 -1.2690 -0.7609 0.143 Uiso 1 1 calc R . . H72B H 0.3385 -1.3284 -0.8129 0.143 Uiso 1 1 calc R . . H72C H 0.2380 -1.3646 -0.7390 0.143 Uiso 1 1 calc R . . N8 N -0.1039(8) -1.3239(5) -0.5755(5) 0.071(2) Uani 0.50 1 d P A 1 C81 C -0.1107(8) -1.2644(6) -0.6433(7) 0.0518(19) Uani 0.50 1 d P A 1 C82 C -0.117(2) -1.1858(15) -0.7348(10) 0.068(8) Uani 0.50 1 d P A 1 H82A H -0.1995 -1.1546 -0.7476 0.101 Uiso 0.50 1 calc PR A 1 H82B H -0.0884 -1.2115 -0.7760 0.101 Uiso 0.50 1 calc PR A 1 H82C H -0.0681 -1.1398 -0.7404 0.101 Uiso 0.50 1 calc PR A 1 N8A N 0.0148(11) -1.3389(6) -0.6323(6) 0.102(4) Uani 0.50 1 d P B 2 C81A C -0.0433(12) -1.2711(6) -0.6779(6) 0.065(3) Uani 0.50 1 d P B 2 C82A C -0.1150(16) -1.1882(14) -0.7364(14) 0.069(8) Uani 0.50 1 d P B 2 H82D H -0.1404 -1.1461 -0.7092 0.104 Uiso 0.50 1 calc PR B 2 H82E H -0.1847 -1.2052 -0.7504 0.104 Uiso 0.50 1 calc PR B 2 H82F H -0.0696 -1.1560 -0.7903 0.104 Uiso 0.50 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 0.02247(15) 0.02960(16) 0.02295(14) -0.00950(12) 0.00238(11) -0.00321(12) Cu2 0.02313(15) 0.02664(15) 0.01968(14) -0.00666(12) 0.00168(11) -0.00335(12) Cu3 0.01966(14) 0.02862(15) 0.02473(15) -0.01016(12) 0.00001(11) -0.00465(11) Cu4 0.02351(16) 0.03064(16) 0.02746(16) -0.01135(13) 0.00164(12) -0.00195(12) Cu5 0.02560(16) 0.02855(16) 0.02295(15) -0.00695(12) 0.00186(12) -0.00415(12) Cu6 0.03093(17) 0.03060(16) 0.02278(15) -0.01241(13) 0.00125(12) -0.00439(13) Br1 0.03062(13) 0.02438(12) 0.02402(12) -0.00569(10) 0.00480(9) -0.00657(10) Br2 0.02002(12) 0.02751(12) 0.03402(13) -0.00635(10) -0.00475(9) -0.00140(9) Br3 0.02496(12) 0.03852(14) 0.02450(12) -0.01882(11) 0.00381(9) -0.00787(10) Br4 0.03614(14) 0.02296(12) 0.02494(12) -0.00925(10) 0.00556(10) -0.00625(10) Br5 0.02970(13) 0.02722(12) 0.02238(11) -0.01138(10) 0.00508(9) -0.00204(10) Br6 0.01950(12) 0.03129(13) 0.03133(13) -0.01061(10) -0.00066(9) -0.00430(9) C1 0.0193(11) 0.0236(11) 0.0231(11) -0.0092(9) -0.0007(8) -0.0037(9) N1 0.0187(9) 0.0222(9) 0.0206(9) -0.0097(8) 0.0028(7) -0.0041(7) C11 0.0316(14) 0.0308(13) 0.0275(12) -0.0171(11) -0.0007(10) -0.0043(10) C12 0.0349(14) 0.0235(12) 0.0301(13) -0.0152(10) 0.0106(10) -0.0095(10) C13 0.0512(19) 0.0399(16) 0.0395(16) -0.0272(14) 0.0168(14) -0.0153(14) C14 0.058(2) 0.0407(17) 0.056(2) -0.0337(16) 0.0306(17) -0.0156(15) C15 0.0427(18) 0.0307(15) 0.063(2) -0.0224(15) 0.0258(16) -0.0056(13) C16 0.0305(15) 0.0282(13) 0.0431(16) -0.0092(12) 0.0115(12) -0.0019(11) N11 0.0276(11) 0.0259(11) 0.0308(11) -0.0111(9) 0.0077(9) -0.0026(9) C2 0.0217(11) 0.0211(10) 0.0176(10) -0.0083(9) 0.0017(8) -0.0032(8) N2 0.0172(9) 0.0200(9) 0.0220(9) -0.0083(8) 0.0030(7) -0.0041(7) C21 0.0200(11) 0.0182(10) 0.0230(11) -0.0051(9) 0.0002(9) -0.0032(8) C22 0.0208(11) 0.0206(10) 0.0239(11) -0.0109(9) 0.0010(9) -0.0027(8) C23 0.0282(13) 0.0274(12) 0.0254(12) -0.0062(10) -0.0002(10) -0.0067(10) C24 0.0254(13) 0.0362(15) 0.0352(14) -0.0042(12) 0.0035(11) -0.0126(11) C25 0.0208(13) 0.0369(15) 0.0432(16) -0.0119(13) -0.0035(11) -0.0080(11) C26 0.0239(12) 0.0314(13) 0.0286(12) -0.0125(11) -0.0042(10) -0.0035(10) N21 0.0226(10) 0.0228(10) 0.0232(10) -0.0100(8) 0.0006(8) -0.0039(8) C3 0.0192(11) 0.0202(11) 0.0214(11) -0.0069(9) 0.0024(8) -0.0024(8) N3 0.0148(9) 0.0212(9) 0.0216(9) -0.0080(8) 0.0025(7) -0.0018(7) C31 0.0154(11) 0.0269(12) 0.0250(11) -0.0076(10) 0.0025(9) -0.0009(9) C32 0.0178(11) 0.0234(11) 0.0238(11) -0.0094(9) 0.0025(9) -0.0004(9) C33 0.0176(11) 0.0341(13) 0.0263(12) -0.0112(10) -0.0003(9) -0.0040(9) C34 0.0233(13) 0.0372(14) 0.0301(13) -0.0111(11) 0.0042(10) -0.0129(11) C35 0.0255(13) 0.0346(14) 0.0263(12) -0.0081(11) 0.0064(10) -0.0077(11) C36 0.0218(12) 0.0380(14) 0.0222(12) -0.0092(11) 0.0006(9) -0.0035(10) N31 0.0187(10) 0.0300(11) 0.0237(10) -0.0102(9) 0.0025(8) -0.0038(8) C4 0.0235(12) 0.0305(12) 0.0227(11) -0.0137(10) 0.0028(9) -0.0097(9) N4 0.0195(10) 0.0284(10) 0.0224(9) -0.0120(8) 0.0024(7) -0.0081(8) C41 0.0258(13) 0.0455(15) 0.0290(13) -0.0190(12) 0.0056(10) -0.0186(11) C42 0.0230(12) 0.0298(12) 0.0282(12) -0.0123(10) 0.0042(9) -0.0134(10) C43 0.0226(13) 0.0425(15) 0.0324(13) -0.0177(12) 0.0004(10) -0.0097(11) C44 0.0229(13) 0.0417(15) 0.0381(14) -0.0231(13) 0.0049(10) -0.0087(11) C45 0.0291(13) 0.0329(13) 0.0322(13) -0.0172(11) 0.0085(10) -0.0108(11) C46 0.0282(14) 0.0341(14) 0.0275(13) -0.0082(11) 0.0032(10) -0.0068(11) N41 0.0239(11) 0.0323(11) 0.0282(11) -0.0099(9) 0.0046(8) -0.0055(9) C5 0.0173(11) 0.0281(12) 0.0256(11) -0.0128(10) 0.0012(9) -0.0021(9) N5 0.0192(9) 0.0218(9) 0.0210(9) -0.0103(8) 0.0029(7) -0.0043(7) C51 0.0217(11) 0.0202(11) 0.0271(12) -0.0101(9) 0.0008(9) -0.0009(9) C52 0.0240(12) 0.0199(10) 0.0257(11) -0.0126(9) 0.0024(9) -0.0024(9) C53 0.0325(14) 0.0215(11) 0.0273(12) -0.0113(10) 0.0000(10) -0.0057(10) C54 0.0370(15) 0.0270(12) 0.0339(14) -0.0164(11) 0.0096(11) -0.0149(11) C55 0.0281(13) 0.0331(13) 0.0393(14) -0.0222(12) 0.0016(11) -0.0098(11) C56 0.0261(13) 0.0304(13) 0.0314(13) -0.0173(11) -0.0025(10) -0.0039(10) N51 0.0255(11) 0.0258(10) 0.0247(10) -0.0125(8) 0.0005(8) -0.0051(8) C6 0.0209(11) 0.0194(10) 0.0209(10) -0.0077(9) 0.0032(8) -0.0033(8) N6 0.0223(10) 0.0209(9) 0.0193(9) -0.0094(8) 0.0030(7) -0.0045(7) C61 0.0328(13) 0.0265(12) 0.0190(11) -0.0110(9) 0.0054(9) -0.0051(10) C62 0.0275(13) 0.0270(12) 0.0261(12) -0.0133(10) 0.0111(10) -0.0095(10) C63 0.0405(16) 0.0410(16) 0.0418(16) -0.0280(14) 0.0098(13) -0.0096(13) C64 0.054(2) 0.0405(17) 0.059(2) -0.0361(16) 0.0204(16) -0.0115(15) C65 0.053(2) 0.0233(13) 0.059(2) -0.0167(14) 0.0244(16) -0.0048(13) C66 0.055(2) 0.0280(14) 0.0333(15) -0.0064(12) 0.0125(14) 0.0008(13) N61 0.0401(13) 0.0241(10) 0.0256(11) -0.0098(9) 0.0082(9) -0.0011(9) N7 0.113(4) 0.072(3) 0.072(3) -0.011(2) -0.031(3) -0.031(3) C71 0.075(3) 0.043(2) 0.067(3) -0.0137(19) -0.006(2) -0.021(2) C72 0.069(3) 0.052(3) 0.131(5) -0.008(3) -0.028(3) -0.007(2) N8 0.092(6) 0.048(4) 0.071(5) -0.016(4) -0.031(4) -0.019(4) C81 0.059(5) 0.039(4) 0.066(6) -0.030(4) -0.015(4) -0.006(4) C82 0.117(16) 0.058(13) 0.045(8) -0.030(9) -0.023(8) -0.024(10) N8A 0.181(11) 0.048(4) 0.077(6) -0.007(4) -0.073(7) -0.034(5) C81A 0.114(9) 0.043(4) 0.048(5) -0.018(4) -0.019(5) -0.032(5) C82A 0.050(9) 0.041(11) 0.111(16) -0.030(10) 0.004(8) -0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.076(2) . ? Cu1 N1 2.244(2) . ? Cu1 Br1 2.4039(4) . ? Cu1 Br2 2.4436(4) . ? Cu1 Cu2 2.7242(5) . ? Cu1 Cu3 2.8497(4) . ? Cu2 N21 2.081(2) . ? Cu2 N2 2.224(2) . ? Cu2 Br3 2.4316(4) . ? Cu2 Br2 2.4545(4) . ? Cu2 Cu3 2.8234(4) . ? Cu3 N31 2.136(2) . ? Cu3 N3 2.237(2) . ? Cu3 Br3 2.4016(4) . ? Cu3 Br1 2.4938(4) . ? Cu4 N41 2.106(2) . ? Cu4 N4 2.228(2) . ? Cu4 Br4 2.3798(4) . ? Cu4 Br5 2.5017(4) . ? Cu4 Cu6 2.7951(5) . ? Cu4 Cu5 2.9361(5) . ? Cu5 N51 2.105(2) . ? Cu5 N5 2.240(2) . ? Cu5 Br5 2.3849(4) . ? Cu5 Br6 2.4634(4) . ? Cu5 Cu6 2.8395(5) . ? Cu6 N61 2.082(2) . ? Cu6 N6 2.229(2) . ? Cu6 Br6 2.3700(4) . ? Cu6 Br4 2.5148(4) . ? C1 N3 1.463(3) . ? C1 N1 1.466(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.473(3) . ? N1 C11 1.473(3) . ? C11 C12 1.509(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.337(4) . ? C12 C13 1.388(4) . ? C13 C14 1.398(5) . ? C13 H13 0.9500 . ? C14 C15 1.365(6) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 N11 1.347(4) . ? C16 H16 0.9500 . ? C2 N2 1.464(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.473(3) . ? N2 C21 1.483(3) . ? C21 C22 1.508(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.334(3) . ? C22 C23 1.391(4) . ? C23 C24 1.390(4) . ? C23 H23 0.9500 . ? C24 C25 1.381(4) . ? C24 H24 0.9500 . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C26 N21 1.341(3) . ? C26 H26 0.9500 . ? C3 N3 1.469(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.484(3) . ? C31 C32 1.511(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.343(3) . ? C32 C33 1.389(3) . ? C33 C34 1.384(4) . ? C33 H33 0.9500 . ? C34 C35 1.377(4) . ? C34 H34 0.9500 . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 N31 1.341(3) . ? C36 H36 0.9500 . ? C4 N6 1.469(3) . ? C4 N4 1.479(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C5 1.466(3) . ? N4 C41 1.483(3) . ? C41 C42 1.510(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N41 1.340(3) . ? C42 C43 1.378(4) . ? C43 C44 1.397(4) . ? C43 H43 0.9500 . ? C44 C45 1.379(4) . ? C44 H44 0.9500 . ? C45 C46 1.385(4) . ? C45 H45 0.9500 . ? C46 N41 1.342(3) . ? C46 H46 0.9500 . ? C5 N5 1.464(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N5 C6 1.470(3) . ? N5 C51 1.476(3) . ? C51 C52 1.505(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 N51 1.349(3) . ? C52 C53 1.385(4) . ? C53 C54 1.392(4) . ? C53 H53 0.9500 . ? C54 C55 1.386(4) . ? C54 H54 0.9500 . ? C55 C56 1.382(4) . ? C55 H55 0.9500 . ? C56 N51 1.342(3) . ? C56 H56 0.9500 . ? C6 N6 1.468(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N6 C61 1.481(3) . ? C61 C62 1.508(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 N61 1.334(3) . ? C62 C63 1.383(4) . ? C63 C64 1.379(5) . ? C63 H63 0.9500 . ? C64 C65 1.385(5) . ? C64 H64 0.9500 . ? C65 C66 1.379(5) . ? C65 H65 0.9500 . ? C66 N61 1.340(4) . ? C66 H66 0.9500 . ? N7 C71 1.128(6) . ? C71 C72 1.457(7) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N8 C81 1.118(11) . ? C81 C82 1.50(2) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N8A C81A 1.142(13) . ? C81A C82A 1.42(2) . ? C82A H82D 0.9800 . ? C82A H82E 0.9800 . ? C82A H82F 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 N11 Cu1 N1 79.45(8) . . ? N11 Cu1 Br1 120.63(6) . . ? N1 Cu1 Br1 106.00(5) . . ? N11 Cu1 Br2 102.61(7) . . ? N1 Cu1 Br2 135.49(5) . . ? Br1 Cu1 Br2 110.238(15) . . ? N11 Cu1 Cu2 126.74(6) . . ? N1 Cu1 Cu2 86.34(5) . . ? Br1 Cu1 Cu2 112.627(15) . . ? Br2 Cu1 Cu2 56.399(11) . . ? N11 Cu1 Cu3 160.07(7) . . ? N1 Cu1 Cu3 82.99(5) . . ? Br1 Cu1 Cu3 55.904(11) . . ? Br2 Cu1 Cu3 96.493(14) . . ? Cu2 Cu1 Cu3 60.818(11) . . ? N21 Cu2 N2 80.79(8) . . ? N21 Cu2 Br3 122.68(6) . . ? N2 Cu2 Br3 108.58(5) . . ? N21 Cu2 Br2 99.36(6) . . ? N2 Cu2 Br2 132.35(5) . . ? Br3 Cu2 Br2 110.693(15) . . ? N21 Cu2 Cu1 125.58(6) . . ? N2 Cu2 Cu1 85.00(5) . . ? Br3 Cu2 Cu1 111.668(14) . . ? Br2 Cu2 Cu1 56.018(11) . . ? N21 Cu2 Cu3 163.20(6) . . ? N2 Cu2 Cu3 85.22(5) . . ? Br3 Cu2 Cu3 53.764(11) . . ? Br2 Cu2 Cu3 96.924(13) . . ? Cu1 Cu2 Cu3 61.788(11) . . ? N31 Cu3 N3 80.89(8) . . ? N31 Cu3 Br3 116.69(6) . . ? N3 Cu3 Br3 107.07(5) . . ? N31 Cu3 Br1 92.04(6) . . ? N3 Cu3 Br1 109.32(5) . . ? Br3 Cu3 Br1 136.513(16) . . ? N31 Cu3 Cu2 158.96(6) . . ? N3 Cu3 Cu2 83.87(5) . . ? Br3 Cu3 Cu2 54.752(11) . . ? Br1 Cu3 Cu2 106.707(14) . . ? N31 Cu3 Cu1 134.82(6) . . ? N3 Cu3 Cu1 85.17(5) . . ? Br3 Cu3 Cu1 108.474(14) . . ? Br1 Cu3 Cu1 52.962(11) . . ? Cu2 Cu3 Cu1 57.394(11) . . ? N41 Cu4 N4 80.80(8) . . ? N41 Cu4 Br4 118.70(7) . . ? N4 Cu4 Br4 112.41(6) . . ? N41 Cu4 Br5 94.03(7) . . ? N4 Cu4 Br5 114.49(5) . . ? Br4 Cu4 Br5 125.987(16) . . ? N41 Cu4 Cu6 158.09(7) . . ? N4 Cu4 Cu6 81.59(5) . . ? Br4 Cu4 Cu6 57.480(11) . . ? Br5 Cu4 Cu6 105.111(15) . . ? N41 Cu4 Cu5 131.45(7) . . ? N4 Cu4 Cu5 85.04(5) . . ? Br4 Cu4 Cu5 109.665(15) . . ? Br5 Cu4 Cu5 51.270(11) . . ? Cu6 Cu4 Cu5 59.336(11) . . ? N51 Cu5 N5 79.86(8) . . ? N51 Cu5 Br5 125.41(6) . . ? N5 Cu5 Br5 107.83(5) . . ? N51 Cu5 Br6 98.51(6) . . ? N5 Cu5 Br6 125.29(5) . . ? Br5 Cu5 Br6 116.131(15) . . ? N51 Cu5 Cu6 127.56(6) . . ? N5 Cu5 Cu6 85.26(5) . . ? Br5 Cu5 Cu6 107.030(14) . . ? Br6 Cu5 Cu6 52.510(11) . . ? N51 Cu5 Cu4 158.87(6) . . ? N5 Cu5 Cu4 80.45(5) . . ? Br5 Cu5 Cu4 54.913(11) . . ? Br6 Cu5 Cu4 99.055(14) . . ? Cu6 Cu5 Cu4 57.860(11) . . ? N61 Cu6 N6 79.94(8) . . ? N61 Cu6 Br6 119.56(7) . . ? N6 Cu6 Br6 118.93(5) . . ? N61 Cu6 Br4 95.51(7) . . ? N6 Cu6 Br4 119.16(5) . . ? Br6 Cu6 Br4 115.617(15) . . ? N61 Cu6 Cu4 133.76(7) . . ? N6 Cu6 Cu4 87.71(5) . . ? Br6 Cu6 Cu4 105.480(15) . . ? Br4 Cu6 Cu4 52.933(11) . . ? N61 Cu6 Cu5 154.84(6) . . ? N6 Cu6 Cu5 82.51(5) . . ? Br6 Cu6 Cu5 55.563(11) . . ? Br4 Cu6 Cu5 108.789(14) . . ? Cu4 Cu6 Cu5 62.804(12) . . ? Cu1 Br1 Cu3 71.134(12) . . ? Cu1 Br2 Cu2 67.583(12) . . ? Cu3 Br3 Cu2 71.484(12) . . ? Cu4 Br4 Cu6 69.587(13) . . ? Cu5 Br5 Cu4 73.817(13) . . ? Cu6 Br6 Cu5 71.927(13) . . ? N3 C1 N1 109.52(19) . . ? N3 C1 H1A 109.8 . . ? N1 C1 H1A 109.8 . . ? N3 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C1 N1 C2 109.26(18) . . ? C1 N1 C11 108.78(19) . . ? C2 N1 C11 109.56(19) . . ? C1 N1 Cu1 115.14(14) . . ? C2 N1 Cu1 109.79(14) . . ? C11 N1 Cu1 104.12(14) . . ? N1 C11 C12 112.6(2) . . ? N1 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N1 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N11 C12 C13 122.1(3) . . ? N11 C12 C11 115.7(2) . . ? C13 C12 C11 122.2(3) . . ? C12 C13 C14 118.5(3) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 118.9(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? N11 C16 C15 122.2(3) . . ? N11 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C12 N11 C16 118.8(2) . . ? C12 N11 Cu1 116.30(17) . . ? C16 N11 Cu1 124.6(2) . . ? N2 C2 N1 108.99(18) . . ? N2 C2 H2A 109.9 . . ? N1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? N1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 N2 C3 108.44(18) . . ? C2 N2 C21 109.67(18) . . ? C3 N2 C21 108.27(18) . . ? C2 N2 Cu2 113.94(14) . . ? C3 N2 Cu2 112.22(14) . . ? C21 N2 Cu2 104.10(14) . . ? N2 C21 C22 112.82(19) . . ? N2 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N2 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N21 C22 C23 122.3(2) . . ? N21 C22 C21 116.3(2) . . ? C23 C22 C21 121.3(2) . . ? C24 C23 C22 118.5(2) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 118.6(3) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? N21 C26 C25 122.6(2) . . ? N21 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C22 N21 C26 118.7(2) . . ? C22 N21 Cu2 114.89(16) . . ? C26 N21 Cu2 125.63(17) . . ? N3 C3 N2 109.32(18) . . ? N3 C3 H3A 109.8 . . ? N2 C3 H3A 109.8 . . ? N3 C3 H3B 109.8 . . ? N2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C1 N3 C3 109.67(18) . . ? C1 N3 C31 109.74(19) . . ? C3 N3 C31 108.46(18) . . ? C1 N3 Cu3 110.79(14) . . ? C3 N3 Cu3 113.89(15) . . ? C31 N3 Cu3 104.08(14) . . ? N3 C31 C32 111.44(19) . . ? N3 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? N3 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? N31 C32 C33 122.2(2) . . ? N31 C32 C31 115.3(2) . . ? C33 C32 C31 122.4(2) . . ? C34 C33 C32 118.8(2) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C35 C34 C33 119.3(2) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 118.4(2) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? N31 C36 C35 123.1(2) . . ? N31 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? C36 N31 C32 118.0(2) . . ? C36 N31 Cu3 123.98(17) . . ? C32 N31 Cu3 111.44(16) . . ? N6 C4 N4 108.58(19) . . ? N6 C4 H4A 110.0 . . ? N4 C4 H4A 110.0 . . ? N6 C4 H4B 110.0 . . ? N4 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C5 N4 C4 110.14(19) . . ? C5 N4 C41 109.2(2) . . ? C4 N4 C41 108.29(19) . . ? C5 N4 Cu4 109.14(14) . . ? C4 N4 Cu4 116.65(15) . . ? C41 N4 Cu4 103.06(15) . . ? N4 C41 C42 111.4(2) . . ? N4 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? N4 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? N41 C42 C43 122.7(2) . . ? N41 C42 C41 115.2(2) . . ? C43 C42 C41 122.0(2) . . ? C42 C43 C44 118.7(3) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C45 C44 C43 118.9(3) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 118.6(3) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? N41 C46 C45 122.9(3) . . ? N41 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? C42 N41 C46 118.1(2) . . ? C42 N41 Cu4 113.13(17) . . ? C46 N41 Cu4 125.79(19) . . ? N5 C5 N4 109.17(19) . . ? N5 C5 H5A 109.8 . . ? N4 C5 H5A 109.8 . . ? N5 C5 H5B 109.8 . . ? N4 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 N5 C6 108.87(18) . . ? C5 N5 C51 109.28(18) . . ? C6 N5 C51 109.02(18) . . ? C5 N5 Cu5 118.18(14) . . ? C6 N5 Cu5 108.85(14) . . ? C51 N5 Cu5 102.24(14) . . ? N5 C51 C52 110.18(19) . . ? N5 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? N5 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? N51 C52 C53 122.5(2) . . ? N51 C52 C51 115.3(2) . . ? C53 C52 C51 122.2(2) . . ? C52 C53 C54 118.8(2) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? C55 C54 C53 119.0(2) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C56 C55 C54 118.4(2) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? N51 C56 C55 123.4(3) . . ? N51 C56 H56 118.3 . . ? C55 C56 H56 118.3 . . ? C56 N51 C52 117.8(2) . . ? C56 N51 Cu5 125.85(18) . . ? C52 N51 Cu5 113.19(16) . . ? N6 C6 N5 109.07(18) . . ? N6 C6 H6A 109.9 . . ? N5 C6 H6A 109.9 . . ? N6 C6 H6B 109.9 . . ? N5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 N6 C4 109.10(19) . . ? C6 N6 C61 107.54(18) . . ? C4 N6 C61 109.97(19) . . ? C6 N6 Cu6 118.04(15) . . ? C4 N6 Cu6 106.68(14) . . ? C61 N6 Cu6 105.32(15) . . ? N6 C61 C62 112.8(2) . . ? N6 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? N6 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? N61 C62 C63 122.2(3) . . ? N61 C62 C61 116.5(2) . . ? C63 C62 C61 121.1(2) . . ? C64 C63 C62 118.8(3) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C63 C64 C65 119.5(3) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C66 C65 C64 117.9(3) . . ? C66 C65 H65 121.1 . . ? C64 C65 H65 121.1 . . ? N61 C66 C65 123.1(3) . . ? N61 C66 H66 118.5 . . ? C65 C66 H66 118.5 . . ? C62 N61 C66 118.5(2) . . ? C62 N61 Cu6 115.99(17) . . ? C66 N61 Cu6 125.0(2) . . ? N7 C71 C72 175.7(6) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N8 C81 C82 178.7(14) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N8A C81A C82A 178.2(13) . . ? C81A C82A H82D 109.5 . . ? C81A C82A H82E 109.5 . . ? H82D C82A H82E 109.5 . . ? C81A C82A H82F 109.5 . . ? H82D C82A H82F 109.5 . . ? H82E C82A H82F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.758 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.124 # Attachment '707393.cif' data_k07rdk8 _database_code_depnum_ccdc_archive 'CCDC 707393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H48 Br3 Cu3 N6' _chemical_formula_sum 'C33 H48 Br3 Cu3 N6' _chemical_formula_weight 959.12 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.42200(10) _cell_length_b 12.21700(10) _cell_length_c 20.9620(2) _cell_angle_alpha 82.5910(10) _cell_angle_beta 84.0060(10) _cell_angle_gamma 79.9630(10) _cell_volume 1849.46(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33488 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 4.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1612 _exptl_absorpt_correction_T_max 0.3703 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '429 1.4 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35778 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 30.08 _reflns_number_total 10804 _reflns_number_gt 9101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0587P)^2^+1.5027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10804 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.77650(5) 0.42425(3) 0.242485(16) 0.02275(8) Uani 1 1 d . . . Cu2 Cu 0.75946(5) 0.45389(3) 0.380817(17) 0.02546(8) Uani 1 1 d . . . Cu3 Cu 0.61991(4) 0.63121(3) 0.280827(16) 0.02243(8) Uani 1 1 d . . . Br1 Br 0.85665(4) 0.60108(2) 0.189474(12) 0.02200(7) Uani 1 1 d . . . Br2 Br 0.96274(3) 0.30978(2) 0.320895(13) 0.02412(7) Uani 1 1 d . . . Br3 Br 0.75426(4) 0.64995(2) 0.379040(12) 0.02244(7) Uani 1 1 d . . . C1 C 0.3523(3) 0.4752(2) 0.26087(12) 0.0187(5) Uani 1 1 d . . . H1A H 0.3681 0.5082 0.2154 0.022 Uiso 1 1 calc R . . H1B H 0.2305 0.4511 0.2684 0.022 Uiso 1 1 calc R . . N1 N 0.4979(3) 0.37813(18) 0.27348(10) 0.0181(4) Uani 1 1 d . . . C11 C 0.4852(4) 0.2912(2) 0.23177(13) 0.0225(5) Uani 1 1 d . . . H11A H 0.3548 0.2837 0.2311 0.027 Uiso 1 1 calc R . . H11B H 0.5516 0.2184 0.2501 0.027 Uiso 1 1 calc R . . C12 C 0.5652(4) 0.3191(2) 0.16364(12) 0.0203(5) Uani 1 1 d . . . C13 C 0.4870(4) 0.2970(2) 0.11043(13) 0.0221(5) Uani 1 1 d . . . H13 H 0.3747 0.2682 0.1163 0.027 Uiso 1 1 calc R . . C14 C 0.5714(4) 0.3166(2) 0.04818(13) 0.0216(5) Uani 1 1 d . . . C15 C 0.4867(4) 0.2895(3) -0.01010(13) 0.0258(6) Uani 1 1 d . . . C16 C 0.2790(4) 0.3304(3) -0.00531(15) 0.0313(6) Uani 1 1 d . . . H16A H 0.2210 0.2892 0.0322 0.047 Uiso 1 1 calc R . . H16B H 0.2284 0.3178 -0.0446 0.047 Uiso 1 1 calc R . . H16C H 0.2546 0.4105 -0.0005 0.047 Uiso 1 1 calc R . . C17 C 0.5233(5) 0.1618(3) -0.01017(16) 0.0338(7) Uani 1 1 d . . . H17A H 0.6559 0.1359 -0.0163 0.051 Uiso 1 1 calc R . . H17B H 0.4630 0.1416 -0.0454 0.051 Uiso 1 1 calc R . . H17C H 0.4744 0.1265 0.0311 0.051 Uiso 1 1 calc R . . C18 C 0.5717(5) 0.3445(3) -0.07378(14) 0.0334(7) Uani 1 1 d . . . H18A H 0.5608 0.4251 -0.0718 0.050 Uiso 1 1 calc R . . H18B H 0.5068 0.3316 -0.1098 0.050 Uiso 1 1 calc R . . H18C H 0.7017 0.3118 -0.0802 0.050 Uiso 1 1 calc R . . C19 C 0.7365(4) 0.3579(2) 0.04365(13) 0.0238(5) Uani 1 1 d . . . H19 H 0.8028 0.3703 0.0028 0.029 Uiso 1 1 calc R . . C20 C 0.8042(4) 0.3811(2) 0.09915(13) 0.0243(5) Uani 1 1 d . . . H20 H 0.9142 0.4122 0.0946 0.029 Uiso 1 1 calc R . . N11 N 0.7221(3) 0.36172(19) 0.15865(11) 0.0217(4) Uani 1 1 d . . . C2 C 0.4713(3) 0.3285(2) 0.34086(12) 0.0183(5) Uani 1 1 d . . . H2A H 0.3511 0.3024 0.3483 0.022 Uiso 1 1 calc R . . H2B H 0.5686 0.2631 0.3495 0.022 Uiso 1 1 calc R . . N2 N 0.4782(3) 0.41198(18) 0.38476(10) 0.0178(4) Uani 1 1 d . . . C21 C 0.4393(3) 0.3636(2) 0.45227(12) 0.0214(5) Uani 1 1 d . . . H21A H 0.3501 0.3118 0.4532 0.026 Uiso 1 1 calc R . . H21B H 0.3820 0.4245 0.4784 0.026 Uiso 1 1 calc R . . C22 C 0.6094(4) 0.3012(2) 0.48247(12) 0.0218(5) Uani 1 1 d . . . C23 C 0.6061(4) 0.2022(2) 0.52232(13) 0.0265(6) Uani 1 1 d . . . H23 H 0.5003 0.1670 0.5270 0.032 Uiso 1 1 calc R . . C24 C 0.7608(5) 0.1537(2) 0.55605(14) 0.0302(6) Uani 1 1 d . . . C25 C 0.7586(6) 0.0423(3) 0.59921(17) 0.0450(10) Uani 1 1 d . . . C26 C 0.7667(6) -0.0508(3) 0.55618(19) 0.0449(9) Uani 1 1 d . . . H26A H 0.8747 -0.0512 0.5250 0.067 Uiso 1 1 calc R . . H26B H 0.6554 -0.0378 0.5330 0.067 Uiso 1 1 calc R . . H26C H 0.7750 -0.1232 0.5830 0.067 Uiso 1 1 calc R . . C27 C 0.5821(10) 0.0477(4) 0.6440(2) 0.086(2) Uani 1 1 d . . . H27A H 0.4762 0.0604 0.6181 0.129 Uiso 1 1 calc R . . H27B H 0.5731 0.1092 0.6705 0.129 Uiso 1 1 calc R . . H27C H 0.5836 -0.0231 0.6720 0.129 Uiso 1 1 calc R . . C28 C 0.9250(10) 0.0146(4) 0.6394(3) 0.098(3) Uani 1 1 d . . . H28A H 0.9104 -0.0497 0.6716 0.147 Uiso 1 1 calc R . . H28B H 0.9341 0.0793 0.6614 0.147 Uiso 1 1 calc R . . H28C H 1.0370 -0.0036 0.6110 0.147 Uiso 1 1 calc R . . C29 C 0.9080(5) 0.2113(3) 0.54683(15) 0.0333(7) Uani 1 1 d . . . H29 H 1.0137 0.1841 0.5697 0.040 Uiso 1 1 calc R . . C30 C 0.9020(4) 0.3083(3) 0.50456(14) 0.0290(6) Uani 1 1 d . . . H30 H 1.0067 0.3446 0.4984 0.035 Uiso 1 1 calc R . . N21 N 0.7568(3) 0.3537(2) 0.47196(11) 0.0237(5) Uani 1 1 d . . . C3 C 0.3361(3) 0.5091(2) 0.37144(12) 0.0190(5) Uani 1 1 d . . . H3A H 0.3411 0.5654 0.4010 0.023 Uiso 1 1 calc R . . H3B H 0.2136 0.4860 0.3792 0.023 Uiso 1 1 calc R . . N3 N 0.3634(3) 0.55871(18) 0.30424(10) 0.0177(4) Uani 1 1 d . . . C31 C 0.2105(3) 0.6533(2) 0.29459(13) 0.0196(5) Uani 1 1 d . . . H31A H 0.1721 0.6842 0.3362 0.023 Uiso 1 1 calc R . . H31B H 0.1046 0.6248 0.2814 0.023 Uiso 1 1 calc R . . C32 C 0.2586(3) 0.7458(2) 0.24473(12) 0.0176(5) Uani 1 1 d . . . C33 C 0.1208(3) 0.8180(2) 0.21389(13) 0.0199(5) Uani 1 1 d . . . H33 H -0.0014 0.8026 0.2201 0.024 Uiso 1 1 calc R . . C34 C 0.1592(4) 0.9131(2) 0.17383(13) 0.0209(5) Uani 1 1 d . . . C35 C 0.0039(4) 0.9920(2) 0.14098(15) 0.0267(6) Uani 1 1 d . . . C36 C -0.0801(4) 0.9268(3) 0.09716(15) 0.0324(7) Uani 1 1 d . . . H36A H 0.0119 0.9030 0.0625 0.049 Uiso 1 1 calc R . . H36B H -0.1859 0.9749 0.0784 0.049 Uiso 1 1 calc R . . H36C H -0.1201 0.8609 0.1226 0.049 Uiso 1 1 calc R . . C37 C -0.1425(4) 1.0362(3) 0.19258(18) 0.0365(7) Uani 1 1 d . . . H37A H -0.1848 0.9731 0.2202 0.055 Uiso 1 1 calc R . . H37B H -0.2464 1.0824 0.1717 0.055 Uiso 1 1 calc R . . H37C H -0.0899 1.0815 0.2189 0.055 Uiso 1 1 calc R . . C38 C 0.0731(5) 1.0910(3) 0.0993(2) 0.0433(9) Uani 1 1 d . . . H38A H 0.1274 1.1340 0.1264 0.065 Uiso 1 1 calc R . . H38B H -0.0299 1.1393 0.0789 0.065 Uiso 1 1 calc R . . H38C H 0.1660 1.0633 0.0658 0.065 Uiso 1 1 calc R . . C39 C 0.3428(4) 0.9281(2) 0.16635(14) 0.0246(5) Uani 1 1 d . . . H39 H 0.3779 0.9918 0.1402 0.030 Uiso 1 1 calc R . . C40 C 0.4730(4) 0.8504(2) 0.19697(14) 0.0263(6) Uani 1 1 d . . . H40 H 0.5976 0.8610 0.1895 0.032 Uiso 1 1 calc R . . N31 N 0.4346(3) 0.76090(19) 0.23651(11) 0.0212(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02145(16) 0.02654(18) 0.02086(16) 0.00009(13) -0.00434(12) -0.00607(13) Cu2 0.01973(16) 0.02853(18) 0.02798(18) 0.00004(14) -0.00227(13) -0.00577(13) Cu3 0.01568(14) 0.02839(18) 0.02303(16) -0.00045(13) -0.00480(12) -0.00300(12) Br1 0.02213(12) 0.02541(14) 0.01903(12) -0.00059(10) -0.00117(9) -0.00721(10) Br2 0.01616(12) 0.02776(14) 0.02594(14) 0.00244(11) -0.00314(9) 0.00007(10) Br3 0.02073(12) 0.02871(14) 0.01956(12) -0.00491(10) -0.00262(9) -0.00644(10) C1 0.0174(11) 0.0216(12) 0.0165(11) 0.0010(9) -0.0049(9) -0.0020(9) N1 0.0196(10) 0.0187(10) 0.0156(9) -0.0003(8) -0.0038(8) -0.0023(8) C11 0.0280(13) 0.0227(13) 0.0180(12) -0.0029(10) 0.0008(10) -0.0083(10) C12 0.0232(12) 0.0201(12) 0.0171(11) -0.0020(9) -0.0002(9) -0.0029(10) C13 0.0234(12) 0.0237(13) 0.0203(12) -0.0029(10) -0.0017(10) -0.0063(10) C14 0.0263(13) 0.0180(12) 0.0197(12) -0.0009(10) -0.0030(10) -0.0018(10) C15 0.0309(14) 0.0301(14) 0.0180(12) -0.0039(11) -0.0032(10) -0.0076(11) C16 0.0309(15) 0.0366(17) 0.0262(14) 0.0013(12) -0.0085(12) -0.0049(13) C17 0.0419(17) 0.0337(16) 0.0283(15) -0.0099(13) -0.0042(13) -0.0075(14) C18 0.0436(18) 0.0399(18) 0.0191(13) -0.0016(12) -0.0042(12) -0.0138(14) C19 0.0257(13) 0.0257(13) 0.0200(12) -0.0043(10) 0.0022(10) -0.0050(11) C20 0.0219(12) 0.0294(14) 0.0227(13) -0.0049(11) 0.0015(10) -0.0075(11) N11 0.0233(11) 0.0220(11) 0.0203(10) -0.0029(9) -0.0014(8) -0.0052(9) C2 0.0176(11) 0.0204(12) 0.0162(11) 0.0027(9) -0.0037(9) -0.0035(9) N2 0.0166(9) 0.0217(10) 0.0145(9) 0.0003(8) -0.0043(7) -0.0017(8) C21 0.0161(11) 0.0313(14) 0.0151(11) 0.0022(10) -0.0018(9) -0.0027(10) C22 0.0222(12) 0.0273(13) 0.0146(11) -0.0005(10) -0.0038(9) -0.0005(10) C23 0.0354(15) 0.0248(14) 0.0187(12) -0.0034(10) -0.0043(11) -0.0010(11) C24 0.0460(18) 0.0210(13) 0.0219(13) -0.0055(11) -0.0143(12) 0.0075(12) C25 0.082(3) 0.0211(15) 0.0294(16) -0.0030(12) -0.0227(17) 0.0083(16) C26 0.069(3) 0.0278(17) 0.0389(19) -0.0099(14) -0.0098(17) -0.0023(16) C27 0.161(6) 0.038(2) 0.038(2) 0.0116(19) 0.028(3) 0.011(3) C28 0.179(7) 0.028(2) 0.099(4) 0.011(2) -0.108(5) -0.004(3) C29 0.0349(16) 0.0362(16) 0.0272(14) -0.0099(13) -0.0154(12) 0.0113(13) C30 0.0208(12) 0.0428(17) 0.0237(13) -0.0075(12) -0.0084(10) 0.0008(12) N21 0.0182(10) 0.0337(13) 0.0174(10) -0.0014(9) -0.0033(8) 0.0009(9) C3 0.0170(11) 0.0241(12) 0.0142(11) 0.0008(9) -0.0016(8) -0.0003(9) N3 0.0146(9) 0.0202(10) 0.0170(10) 0.0006(8) -0.0026(7) -0.0003(8) C31 0.0147(10) 0.0202(12) 0.0214(12) 0.0024(10) 0.0000(9) -0.0008(9) C32 0.0166(11) 0.0196(12) 0.0166(11) -0.0030(9) -0.0004(8) -0.0025(9) C33 0.0149(10) 0.0207(12) 0.0240(12) -0.0008(10) -0.0039(9) -0.0029(9) C34 0.0200(12) 0.0200(12) 0.0224(12) -0.0002(10) -0.0045(9) -0.0019(9) C35 0.0234(13) 0.0230(13) 0.0319(15) 0.0065(11) -0.0076(11) -0.0030(10) C36 0.0264(14) 0.0392(17) 0.0313(15) 0.0037(13) -0.0117(12) -0.0042(13) C37 0.0280(15) 0.0291(15) 0.050(2) -0.0057(14) -0.0104(14) 0.0077(12) C38 0.0362(17) 0.0296(17) 0.061(2) 0.0197(16) -0.0162(16) -0.0066(14) C39 0.0222(12) 0.0240(13) 0.0276(14) 0.0038(11) -0.0022(10) -0.0085(10) C40 0.0195(12) 0.0288(14) 0.0309(14) 0.0021(12) -0.0024(10) -0.0085(11) N31 0.0168(10) 0.0241(11) 0.0221(11) 0.0007(9) -0.0035(8) -0.0032(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 2.106(2) . ? Cu1 N1 2.246(2) . ? Cu1 Br2 2.4033(4) . ? Cu1 Br1 2.4386(4) . ? Cu1 Cu3 2.7739(5) . ? Cu1 Cu2 2.9553(5) . ? Cu2 N21 2.132(2) . ? Cu2 N2 2.225(2) . ? Cu2 Br3 2.3843(5) . ? Cu2 Br2 2.4905(5) . ? Cu2 Cu3 2.9426(5) . ? Cu3 N31 2.096(2) . ? Cu3 N3 2.221(2) . ? Cu3 Br3 2.4320(4) . ? Cu3 Br1 2.4786(4) . ? C1 N3 1.469(3) . ? C1 N1 1.475(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.471(3) . ? N1 C11 1.481(3) . ? C11 C12 1.509(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.346(3) . ? C12 C13 1.386(4) . ? C13 C14 1.398(4) . ? C13 H13 0.9500 . ? C14 C19 1.395(4) . ? C14 C15 1.528(4) . ? C15 C16 1.532(4) . ? C15 C17 1.536(4) . ? C15 C18 1.541(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 N11 1.341(4) . ? C20 H20 0.9500 . ? C2 N2 1.470(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.462(3) . ? N2 C21 1.481(3) . ? C21 C22 1.511(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.347(4) . ? C22 C23 1.380(4) . ? C23 C24 1.412(4) . ? C23 H23 0.9500 . ? C24 C29 1.384(5) . ? C24 C25 1.535(5) . ? C25 C27 1.527(7) . ? C25 C26 1.530(5) . ? C25 C28 1.532(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.382(5) . ? C29 H29 0.9500 . ? C30 N21 1.335(3) . ? C30 H30 0.9500 . ? C3 N3 1.468(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.481(3) . ? C31 C32 1.502(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.341(3) . ? C32 C33 1.385(3) . ? C33 C34 1.397(4) . ? C33 H33 0.9500 . ? C34 C39 1.397(4) . ? C34 C35 1.529(4) . ? C35 C38 1.530(4) . ? C35 C37 1.531(5) . ? C35 C36 1.532(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.379(4) . ? C39 H39 0.9500 . ? C40 N31 1.338(4) . ? C40 H40 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 N11 Cu1 N1 79.61(8) . . ? N11 Cu1 Br2 121.32(7) . . ? N1 Cu1 Br2 102.10(5) . . ? N11 Cu1 Br1 96.84(6) . . ? N1 Cu1 Br1 129.23(6) . . ? Br2 Cu1 Br1 121.362(16) . . ? N11 Cu1 Cu3 125.24(7) . . ? N1 Cu1 Cu3 84.43(6) . . ? Br2 Cu1 Cu3 113.158(16) . . ? Br1 Cu1 Cu3 56.343(12) . . ? N11 Cu1 Cu2 158.63(6) . . ? N1 Cu1 Cu2 81.26(5) . . ? Br2 Cu1 Cu2 54.212(12) . . ? Br1 Cu1 Cu2 102.619(15) . . ? Cu3 Cu1 Cu2 61.714(12) . . ? N21 Cu2 N2 81.30(8) . . ? N21 Cu2 Br3 118.36(7) . . ? N2 Cu2 Br3 111.93(6) . . ? N21 Cu2 Br2 95.63(7) . . ? N2 Cu2 Br2 105.65(6) . . ? Br3 Cu2 Br2 131.921(17) . . ? N21 Cu2 Cu3 156.65(6) . . ? N2 Cu2 Cu3 83.05(6) . . ? Br3 Cu2 Cu3 53.080(11) . . ? Br2 Cu2 Cu3 105.237(15) . . ? N21 Cu2 Cu1 138.57(7) . . ? N2 Cu2 Cu1 84.57(6) . . ? Br3 Cu2 Cu1 103.056(15) . . ? Br2 Cu2 Cu1 51.515(11) . . ? Cu3 Cu2 Cu1 56.110(12) . . ? N31 Cu3 N3 80.52(8) . . ? N31 Cu3 Br3 121.99(7) . . ? N3 Cu3 Br3 110.59(6) . . ? N31 Cu3 Br1 99.87(6) . . ? N3 Cu3 Br1 128.71(6) . . ? Br3 Cu3 Br1 111.859(15) . . ? N31 Cu3 Cu1 130.67(7) . . ? N3 Cu3 Cu1 85.87(6) . . ? Br3 Cu3 Cu1 107.212(15) . . ? Br1 Cu3 Cu1 54.979(12) . . ? N31 Cu3 Cu2 157.85(6) . . ? N3 Cu3 Cu2 83.02(5) . . ? Br3 Cu3 Cu2 51.608(11) . . ? Br1 Cu3 Cu2 101.976(14) . . ? Cu1 Cu3 Cu2 62.176(12) . . ? Cu1 Br1 Cu3 68.679(13) . . ? Cu1 Br2 Cu2 74.273(14) . . ? Cu2 Br3 Cu3 75.312(14) . . ? N3 C1 N1 108.98(19) . . ? N3 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? N3 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C2 N1 C1 109.5(2) . . ? C2 N1 C11 107.3(2) . . ? C1 N1 C11 109.9(2) . . ? C2 N1 Cu1 115.71(15) . . ? C1 N1 Cu1 110.79(15) . . ? C11 N1 Cu1 103.46(16) . . ? N1 C11 C12 111.9(2) . . ? N1 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N11 C12 C13 122.7(2) . . ? N11 C12 C11 115.1(2) . . ? C13 C12 C11 122.1(2) . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C19 C14 C13 116.1(2) . . ? C19 C14 C15 123.4(2) . . ? C13 C14 C15 120.4(2) . . ? C14 C15 C16 110.6(2) . . ? C14 C15 C17 107.7(2) . . ? C16 C15 C17 109.2(3) . . ? C14 C15 C18 111.4(2) . . ? C16 C15 C18 108.6(2) . . ? C17 C15 C18 109.4(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C14 119.9(3) . . ? C20 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? N11 C20 C19 123.4(3) . . ? N11 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? C20 N11 C12 117.1(2) . . ? C20 N11 Cu1 126.45(19) . . ? C12 N11 Cu1 114.89(17) . . ? N2 C2 N1 109.8(2) . . ? N2 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 N2 C2 109.69(19) . . ? C3 N2 C21 107.5(2) . . ? C2 N2 C21 109.4(2) . . ? C3 N2 Cu2 113.86(16) . . ? C2 N2 Cu2 111.12(15) . . ? C21 N2 Cu2 104.99(14) . . ? N2 C21 C22 112.9(2) . . ? N2 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N2 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N21 C22 C23 123.3(2) . . ? N21 C22 C21 115.2(2) . . ? C23 C22 C21 121.3(3) . . ? C22 C23 C24 119.7(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C29 C24 C23 116.2(3) . . ? C29 C24 C25 124.1(3) . . ? C23 C24 C25 119.7(3) . . ? C27 C25 C26 108.8(4) . . ? C27 C25 C28 109.6(5) . . ? C26 C25 C28 108.5(3) . . ? C27 C25 C24 110.2(3) . . ? C26 C25 C24 108.7(3) . . ? C28 C25 C24 110.9(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C24 120.4(3) . . ? C30 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? N21 C30 C29 123.5(3) . . ? N21 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C30 N21 C22 116.9(3) . . ? C30 N21 Cu2 126.8(2) . . ? C22 N21 Cu2 111.49(17) . . ? N2 C3 N3 110.2(2) . . ? N2 C3 H3A 109.6 . . ? N3 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? N3 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C3 N3 C1 109.2(2) . . ? C3 N3 C31 106.38(19) . . ? C1 N3 C31 109.21(19) . . ? C3 N3 Cu3 114.58(15) . . ? C1 N3 Cu3 111.23(15) . . ? C31 N3 Cu3 106.02(15) . . ? N3 C31 C32 113.6(2) . . ? N3 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? N3 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? N31 C32 C33 122.5(2) . . ? N31 C32 C31 117.3(2) . . ? C33 C32 C31 119.9(2) . . ? C32 C33 C34 120.8(2) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C34 C39 115.9(2) . . ? C33 C34 C35 119.7(2) . . ? C39 C34 C35 124.5(2) . . ? C34 C35 C38 111.9(2) . . ? C34 C35 C37 109.2(2) . . ? C38 C35 C37 109.1(3) . . ? C34 C35 C36 108.7(2) . . ? C38 C35 C36 108.1(3) . . ? C37 C35 C36 109.8(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C34 119.8(3) . . ? C40 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? N31 C40 C39 124.0(3) . . ? N31 C40 H40 118.0 . . ? C39 C40 H40 118.0 . . ? C40 N31 C32 117.0(2) . . ? C40 N31 Cu3 127.77(18) . . ? C32 N31 Cu3 114.98(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.904 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.139 data_k07rdk3 _database_code_depnum_ccdc_archive 'CCDC 707394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Br3 Cu3 N3 S3' _chemical_formula_sum 'C33 H45 Br3 Cu3 N3 S3' _chemical_formula_weight 1010.25 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 19.5700(8) _cell_length_b 8.1390(3) _cell_length_c 23.9110(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.246(2) _cell_angle_gamma 90.00 _cell_volume 3707.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 73328 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 5.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2331 _exptl_absorpt_correction_T_max 0.8612 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '287 1.3 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27748 _diffrn_reflns_av_R_equivalents 0.2015 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 24.08 _reflns_number_total 5791 _reflns_number_gt 4015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0009P)^2^+822.3577P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5791 _refine_ls_number_parameters 338 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2383 _refine_ls_R_factor_gt 0.1991 _refine_ls_wR_factor_ref 0.4677 _refine_ls_wR_factor_gt 0.4477 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _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 0.2145(2) 0.3341(5) 0.1385(2) 0.0367(11) Uani 1 1 d . . . Cu2 Cu 0.3259(2) 0.4716(5) 0.2300(2) 0.0388(11) Uani 1 1 d . . . Cu3 Cu 0.2279(2) 0.2580(6) 0.2599(2) 0.0412(12) Uani 1 1 d . . . Br1 Br 0.2796(2) 0.5862(4) 0.13408(16) 0.0377(9) Uani 1 1 d . . . Br2 Br 0.2962(2) 0.4599(5) 0.32182(18) 0.0462(11) Uani 1 1 d . . . Br3 Br 0.1225(2) 0.2839(6) 0.18559(19) 0.0548(12) Uani 1 1 d . . . S1 S 0.1784(5) 0.3063(11) 0.0348(4) 0.039(2) Uani 1 1 d . . . S2 S 0.4358(5) 0.6201(13) 0.2451(4) 0.043(2) Uani 1 1 d . . . S3 S 0.1783(6) 0.0666(13) 0.3175(4) 0.047(2) Uani 1 1 d . . . C1 C 0.280(2) -0.004(4) 0.1810(11) 0.042(10) Uani 1 1 d D . . H1A H 0.2323 -0.0535 0.1699 0.051 Uiso 1 1 calc R . . H1B H 0.3149 -0.0883 0.1777 0.051 Uiso 1 1 calc R . . N1 N 0.2852(12) 0.146(3) 0.1414(9) 0.014(5) Uiso 1 1 d . . . C11 C 0.2731(18) 0.063(4) 0.0809(14) 0.030(7) Uiso 1 1 d . . . H11A H 0.3165 0.0066 0.0768 0.037 Uiso 1 1 calc R . . H11B H 0.2351 -0.0197 0.0766 0.037 Uiso 1 1 calc R . . C12 C 0.2538(19) 0.189(4) 0.0368(13) 0.030(8) Uani 1 1 d . . . H12A H 0.2481 0.1341 -0.0010 0.037 Uiso 1 1 calc R . . H12B H 0.2940 0.2652 0.0408 0.037 Uiso 1 1 calc R . . C13 C 0.116(2) 0.164(7) 0.012(3) 0.09(2) Uani 1 1 d . . . H13A H 0.1367 0.0756 -0.0072 0.103 Uiso 1 1 calc R . . H13B H 0.1038 0.1148 0.0464 0.103 Uiso 1 1 calc R . . C14 C 0.0456(11) 0.221(3) -0.0301(10) 0.036(9) Uani 1 1 d G . . C15 C 0.0460(11) 0.241(4) -0.0877(10) 0.054(12) Uani 1 1 d G . . H15 H 0.0877 0.2193 -0.1006 0.065 Uiso 1 1 calc R . . C16 C -0.0144(14) 0.292(4) -0.1266(8) 0.052(11) Uani 1 1 d G . . H16 H -0.0141 0.3055 -0.1660 0.062 Uiso 1 1 calc R . . C17 C -0.0753(11) 0.323(4) -0.1078(11) 0.13(3) Uani 1 1 d G . . H17 H -0.1166 0.3580 -0.1344 0.161 Uiso 1 1 calc R . . C18 C -0.0758(11) 0.303(4) -0.0502(12) 0.070(15) Uani 1 1 d G . . H18 H -0.1174 0.3244 -0.0374 0.084 Uiso 1 1 calc R . . C19 C -0.0153(14) 0.252(3) -0.0113(9) 0.056(12) Uani 1 1 d G . . C20 C -0.018(3) 0.235(6) 0.050(2) 0.063(12) Uiso 1 1 d . . . H20A H -0.0635 0.2720 0.0556 0.095 Uiso 1 1 calc R . . H20B H 0.0194 0.3018 0.0742 0.095 Uiso 1 1 calc R . . H20C H -0.0108 0.1193 0.0619 0.095 Uiso 1 1 calc R . . C2 C 0.359(4) 0.192(6) 0.158(2) 0.09(2) Uani 1 1 d . . . H2A H 0.3885 0.0970 0.1516 0.113 Uiso 1 1 calc R . . H2B H 0.3682 0.2827 0.1327 0.113 Uiso 1 1 calc R . . N2 N 0.3805(16) 0.244(3) 0.2176(15) 0.042(8) Uani 1 1 d . . . C21 C 0.458(2) 0.287(3) 0.2327(18) 0.040(9) Uani 1 1 d D . . H21A H 0.4839 0.2086 0.2138 0.048 Uiso 1 1 calc R . . H21B H 0.4760 0.2780 0.2748 0.048 Uiso 1 1 calc R . . C22 C 0.4679(19) 0.465(4) 0.2125(17) 0.046(11) Uani 1 1 d D . . H22A H 0.4463 0.4719 0.1709 0.055 Uiso 1 1 calc R . . H22B H 0.5189 0.4840 0.2173 0.055 Uiso 1 1 calc R . . C23 C 0.4845(17) 0.606(5) 0.3170(14) 0.034(8) Uani 1 1 d . . . H23A H 0.4651 0.5156 0.3362 0.041 Uiso 1 1 calc R . . H23B H 0.5336 0.5777 0.3169 0.041 Uiso 1 1 calc R . . C24 C 0.4846(16) 0.763(3) 0.3522(11) 0.065(14) Uani 1 1 d G . . C25 C 0.4407(15) 0.774(4) 0.3903(13) 0.078(19) Uani 1 1 d G . . H25 H 0.4125 0.6827 0.3954 0.094 Uiso 1 1 calc R . . C26 C 0.4382(13) 0.918(5) 0.4209(12) 0.09(2) Uani 1 1 d G . . H26 H 0.4083 0.9254 0.4470 0.109 Uiso 1 1 calc R . . C27 C 0.4795(14) 1.052(3) 0.4134(13) 0.053(12) Uani 1 1 d G . . H27 H 0.4777 1.1502 0.4343 0.063 Uiso 1 1 calc R . . C28 C 0.5233(13) 1.041(3) 0.3753(14) 0.060(13) Uani 1 1 d G . . H28 H 0.5515 1.1323 0.3702 0.072 Uiso 1 1 calc R . . C29 C 0.5258(14) 0.897(4) 0.3447(11) 0.083(19) Uani 1 1 d G . . C30 C 0.576(3) 0.891(6) 0.3055(18) 0.071(15) Uani 1 1 d . . . H30A H 0.6024 0.7880 0.3119 0.107 Uiso 1 1 calc R . . H30B H 0.6079 0.9841 0.3136 0.107 Uiso 1 1 calc R . . H30C H 0.5490 0.8957 0.2655 0.107 Uiso 1 1 calc R . . C3 C 0.3684(16) 0.081(7) 0.247(2) 0.08(2) Uani 1 1 d D . . H3A H 0.3893 -0.0115 0.2304 0.101 Uiso 1 1 calc R . . H3B H 0.3907 0.0870 0.2889 0.101 Uiso 1 1 calc R . . N3 N 0.2926(14) 0.058(4) 0.2390(11) 0.043(8) Uiso 1 1 d D . . C31 C 0.2893(19) -0.080(5) 0.2772(16) 0.040(9) Uiso 1 1 d . . . H31A H 0.3200 -0.0583 0.3155 0.049 Uiso 1 1 calc R . . H31B H 0.3065 -0.1810 0.2616 0.049 Uiso 1 1 calc R . . C32 C 0.212(3) -0.108(4) 0.2831(16) 0.053(12) Uani 1 1 d . . . H32A H 0.2097 -0.2082 0.3061 0.064 Uiso 1 1 calc R . . H32B H 0.1809 -0.1255 0.2445 0.064 Uiso 1 1 calc R . . C33 C 0.229(2) 0.047(5) 0.3923(17) 0.050(11) Uani 1 1 d . . . H33A H 0.2799 0.0418 0.3923 0.060 Uiso 1 1 calc R . . H33B H 0.2218 0.1467 0.4139 0.060 Uiso 1 1 calc R . . C34 C 0.2109(16) -0.099(2) 0.4225(11) 0.042(9) Uani 1 1 d G . . C35 C 0.2480(14) -0.244(3) 0.4214(12) 0.064(14) Uani 1 1 d G . . H35 H 0.2867 -0.2464 0.4036 0.077 Uiso 1 1 calc R . . C36 C 0.2284(13) -0.385(3) 0.4463(12) 0.046(10) Uiso 1 1 d G . . H36 H 0.2537 -0.4845 0.4456 0.055 Uiso 1 1 calc R . . C37 C 0.1718(14) -0.381(3) 0.4723(12) 0.069(15) Uani 1 1 d G . . H37 H 0.1584 -0.4781 0.4893 0.083 Uiso 1 1 calc R . . C38 C 0.1347(12) -0.236(4) 0.4734(12) 0.058(13) Uani 1 1 d G . . H38 H 0.0960 -0.2336 0.4912 0.070 Uiso 1 1 calc R . . C39 C 0.1543(14) -0.095(3) 0.4485(11) 0.081(19) Uani 1 1 d G . . C40 C 0.107(3) 0.055(8) 0.447(3) 0.088(17) Uiso 1 1 d . . . H40A H 0.1149 0.1041 0.4856 0.132 Uiso 1 1 calc R . . H40B H 0.0573 0.0214 0.4350 0.132 Uiso 1 1 calc R . . H40C H 0.1169 0.1367 0.4200 0.132 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 0.038(2) 0.029(2) 0.047(3) -0.002(2) 0.017(2) -0.0024(19) Cu2 0.040(3) 0.031(2) 0.047(3) 0.001(2) 0.012(2) 0.008(2) Cu3 0.045(3) 0.033(2) 0.045(3) 0.002(2) 0.010(2) -0.002(2) Br1 0.043(2) 0.0237(17) 0.044(2) 0.0027(15) 0.0043(16) -0.0034(15) Br2 0.057(2) 0.037(2) 0.049(2) -0.0058(18) 0.0219(19) -0.0072(18) Br3 0.037(2) 0.075(3) 0.054(3) 0.016(2) 0.0135(18) -0.001(2) S1 0.040(5) 0.032(5) 0.044(5) 0.007(4) 0.011(4) -0.003(4) S2 0.039(5) 0.046(6) 0.045(6) 0.000(5) 0.009(4) 0.003(4) S3 0.052(6) 0.043(6) 0.044(6) 0.003(5) 0.007(5) -0.010(5) C1 0.07(3) 0.04(2) 0.018(17) 0.024(16) 0.002(17) 0.022(19) C12 0.04(2) 0.032(18) 0.016(16) -0.008(14) 0.010(14) 0.016(16) C13 0.02(2) 0.08(4) 0.15(6) 0.05(4) 0.01(3) 0.01(2) C14 0.027(18) 0.023(17) 0.05(2) 0.003(16) -0.004(17) 0.004(14) C15 0.04(2) 0.07(3) 0.04(2) -0.02(2) -0.020(18) 0.01(2) C16 0.06(3) 0.07(3) 0.04(2) -0.01(2) 0.03(2) 0.01(2) C17 0.21(8) 0.14(6) 0.07(4) -0.02(4) 0.06(5) -0.12(6) C18 0.03(2) 0.05(3) 0.12(4) 0.03(3) 0.00(3) 0.00(2) C19 0.07(3) 0.06(3) 0.04(2) 0.00(2) 0.01(2) -0.03(2) C2 0.18(6) 0.04(3) 0.09(4) 0.03(3) 0.09(4) 0.07(4) N2 0.046(18) 0.024(15) 0.07(2) -0.013(15) 0.032(16) -0.018(14) C21 0.05(2) 0.008(15) 0.06(3) 0.005(16) 0.02(2) -0.003(15) C22 0.03(2) 0.04(2) 0.05(2) 0.023(19) -0.011(18) -0.030(17) C23 0.020(16) 0.05(2) 0.030(18) -0.013(16) -0.006(14) -0.014(15) C24 0.05(3) 0.11(4) 0.03(2) 0.00(2) 0.002(19) 0.04(3) C25 0.06(3) 0.14(5) 0.04(2) 0.01(3) 0.00(2) -0.06(3) C26 0.02(2) 0.21(7) 0.05(3) -0.02(4) 0.02(2) 0.03(3) C27 0.007(16) 0.07(3) 0.08(3) -0.04(2) -0.005(18) 0.015(18) C28 0.05(2) 0.03(2) 0.09(4) -0.01(2) 0.00(2) -0.002(19) C29 0.07(3) 0.08(4) 0.08(4) -0.03(3) -0.02(3) 0.06(3) C30 0.12(4) 0.07(3) 0.03(2) 0.00(2) 0.01(3) -0.01(3) C3 0.05(3) 0.12(5) 0.07(3) 0.08(3) -0.02(2) 0.00(3) C32 0.11(4) 0.023(18) 0.020(18) 0.009(15) 0.01(2) 0.01(2) C33 0.06(3) 0.05(2) 0.04(2) 0.03(2) 0.02(2) 0.03(2) C34 0.07(3) 0.03(2) 0.03(2) -0.001(16) 0.03(2) 0.008(19) C35 0.08(3) 0.06(3) 0.07(3) 0.00(2) 0.04(3) -0.05(3) C37 0.07(3) 0.09(4) 0.04(2) 0.05(3) 0.00(2) 0.01(3) C38 0.04(2) 0.08(3) 0.06(3) 0.04(2) -0.005(19) -0.02(2) C39 0.12(5) 0.05(3) 0.04(3) -0.01(2) -0.05(3) 0.00(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 N1 2.05(2) . ? Cu1 Br3 2.367(6) . ? Cu1 S1 2.428(11) . ? Cu1 Br1 2.431(5) . ? Cu1 Cu3 2.919(7) . ? Cu1 Cu2 2.934(7) . ? Cu2 N2 2.19(3) . ? Cu2 Br2 2.398(6) . ? Cu2 S2 2.421(11) . ? Cu2 Br1 2.449(6) . ? Cu2 Cu3 2.800(7) . ? Cu3 N3 2.19(3) . ? Cu3 Br3 2.403(6) . ? Cu3 Br2 2.403(6) . ? Cu3 S3 2.425(11) . ? S1 C13 1.68(5) . ? S1 C12 1.75(3) . ? S2 C22 1.68(4) . ? S2 C23 1.77(3) . ? S3 C32 1.83(4) . ? S3 C33 1.85(4) . ? C1 N3 1.441(19) . ? C1 N1 1.56(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.47(7) . ? N1 C11 1.56(4) . ? C11 C12 1.46(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.58(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.49(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C2 N2 1.46(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C21 1.51(5) . ? N2 C3 1.54(5) . ? C21 C22 1.561(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.53(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.50(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C3 N3 1.463(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.46(5) . ? C31 C32 1.58(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.47(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 C40 1.53(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 N1 Cu1 Br3 115.7(7) . . ? N1 Cu1 S1 90.1(7) . . ? Br3 Cu1 S1 113.3(3) . . ? N1 Cu1 Br1 106.0(7) . . ? Br3 Cu1 Br1 129.1(2) . . ? S1 Cu1 Br1 93.8(3) . . ? N1 Cu1 Cu3 84.4(6) . . ? Br3 Cu1 Cu3 52.83(17) . . ? S1 Cu1 Cu3 159.1(3) . . ? Br1 Cu1 Cu3 107.1(2) . . ? N1 Cu1 Cu2 83.1(6) . . ? Br3 Cu1 Cu2 103.2(2) . . ? S1 Cu1 Cu2 142.1(3) . . ? Br1 Cu1 Cu2 53.33(15) . . ? Cu3 Cu1 Cu2 57.16(16) . . ? N2 Cu2 Br2 108.5(9) . . ? N2 Cu2 S2 90.0(8) . . ? Br2 Cu2 S2 106.1(3) . . ? N2 Cu2 Br1 106.4(9) . . ? Br2 Cu2 Br1 139.2(2) . . ? S2 Cu2 Br1 94.3(3) . . ? N2 Cu2 Cu3 83.8(7) . . ? Br2 Cu2 Cu3 54.41(17) . . ? S2 Cu2 Cu3 155.4(3) . . ? Br1 Cu2 Cu3 110.3(2) . . ? N2 Cu2 Cu1 83.0(9) . . ? Br2 Cu2 Cu1 111.9(2) . . ? S2 Cu2 Cu1 141.7(3) . . ? Br1 Cu2 Cu1 52.75(15) . . ? Cu3 Cu2 Cu1 61.15(16) . . ? N3 Cu3 Br3 109.9(7) . . ? N3 Cu3 Br2 112.3(7) . . ? Br3 Cu3 Br2 131.2(3) . . ? N3 Cu3 S3 88.8(9) . . ? Br3 Cu3 S3 95.1(3) . . ? Br2 Cu3 S3 109.1(3) . . ? N3 Cu3 Cu2 86.5(8) . . ? Br3 Cu3 Cu2 106.2(2) . . ? Br2 Cu3 Cu2 54.24(16) . . ? S3 Cu3 Cu2 158.5(3) . . ? N3 Cu3 Cu1 81.8(8) . . ? Br3 Cu3 Cu1 51.72(16) . . ? Br2 Cu3 Cu1 112.2(2) . . ? S3 Cu3 Cu1 138.1(3) . . ? Cu2 Cu3 Cu1 61.70(16) . . ? Cu1 Br1 Cu2 73.92(19) . . ? Cu2 Br2 Cu3 71.3(2) . . ? Cu1 Br3 Cu3 75.5(2) . . ? C13 S1 C12 100(2) . . ? C13 S1 Cu1 114(2) . . ? C12 S1 Cu1 88.7(11) . . ? C22 S2 C23 103.2(18) . . ? C22 S2 Cu2 88.3(11) . . ? C23 S2 Cu2 112.0(12) . . ? C32 S3 C33 101.4(18) . . ? C32 S3 Cu3 90.8(13) . . ? C33 S3 Cu3 114.1(14) . . ? N3 C1 N1 107(3) . . ? N3 C1 H1A 110.3 . . ? N1 C1 H1A 110.3 . . ? N3 C1 H1B 110.3 . . ? N1 C1 H1B 110.3 . . ? H1A C1 H1B 108.6 . . ? C2 N1 C1 104(3) . . ? C2 N1 C11 107(3) . . ? C1 N1 C11 102(2) . . ? C2 N1 Cu1 116(2) . . ? C1 N1 Cu1 117.6(19) . . ? C11 N1 Cu1 109.4(17) . . ? C12 C11 N1 109(3) . . ? C12 C11 H11A 109.9 . . ? N1 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? N1 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 S1 119(2) . . ? C11 C12 H12A 107.6 . . ? S1 C12 H12A 107.6 . . ? C11 C12 H12B 107.6 . . ? S1 C12 H12B 107.6 . . ? H12A C12 H12B 107.1 . . ? C14 C13 S1 118(3) . . ? C14 C13 H13A 107.8 . . ? S1 C13 H13A 107.8 . . ? C14 C13 H13B 107.8 . . ? S1 C13 H13B 107.8 . . ? H13A C13 H13B 107.2 . . ? C15 C14 C19 120.0 . . ? C15 C14 C13 118(3) . . ? C19 C14 C13 122(3) . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 120.0 . . ? C18 C19 C20 118(3) . . ? C14 C19 C20 122(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C2 N1 112(3) . . ? N2 C2 H2A 109.2 . . ? N1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? N1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 N2 C21 110(4) . . ? C2 N2 C3 100(4) . . ? C21 N2 C3 110(3) . . ? C2 N2 Cu2 110(3) . . ? C21 N2 Cu2 105.2(18) . . ? C3 N2 Cu2 122(3) . . ? N2 C21 C22 110(3) . . ? N2 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N2 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 S2 118(3) . . ? C21 C22 H22A 107.8 . . ? S2 C22 H22A 107.8 . . ? C21 C22 H22B 107.8 . . ? S2 C22 H22B 107.8 . . ? H22A C22 H22B 107.2 . . ? C24 C23 S2 114(2) . . ? C24 C23 H23A 108.6 . . ? S2 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? S2 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 119(2) . . ? C29 C24 C23 121(2) . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 120.0 . . ? C28 C29 C30 118(3) . . ? C24 C29 C30 122(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C3 N2 108(3) . . ? N3 C3 H3A 110.1 . . ? N2 C3 H3A 110.1 . . ? N3 C3 H3B 110.1 . . ? N2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C1 N3 C31 108(3) . . ? C1 N3 C3 97(3) . . ? C31 N3 C3 102(3) . . ? C1 N3 Cu3 120(2) . . ? C31 N3 Cu3 109(2) . . ? C3 N3 Cu3 119(3) . . ? N3 C31 C32 110(3) . . ? N3 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? N3 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C31 C32 S3 112(3) . . ? C31 C32 H32A 109.1 . . ? S3 C32 H32A 109.1 . . ? C31 C32 H32B 109.1 . . ? S3 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C34 C33 S3 114(3) . . ? C34 C33 H33A 108.8 . . ? S3 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? S3 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C39 120.0 . . ? C35 C34 C33 119(2) . . ? C39 C34 C33 121(2) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 C40 116(3) . . ? C34 C39 C40 124(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.929 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.355 # Attachment '4i.cif' data_h08rdk3 _database_code_depnum_ccdc_archive 'CCDC 707395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 Cu3 F3 I3 N3 S3, C H2 Cl2' _chemical_formula_sum 'C31 H38 Cl2 Cu3 F3 I3 N3 S3' _chemical_formula_weight 1248.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 12.78690(10) _cell_length_b 12.88420(10) _cell_length_c 24.9879(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.3490(10) _cell_angle_gamma 90.00 _cell_volume 4073.10(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58852 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 4.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2238 _exptl_absorpt_correction_T_max 0.6611 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '639 1.2 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68317 _diffrn_reflns_av_R_equivalents 0.1269 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 30.07 _reflns_number_total 11880 _reflns_number_gt 7865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11880 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.26655(5) 0.49401(5) 0.13768(3) 0.02979(16) Uani 1 1 d . . . Cu2 Cu 0.06982(5) 0.38555(5) 0.14003(3) 0.02966(16) Uani 1 1 d . . . Cu3 Cu 0.19479(5) 0.45569(5) 0.24156(3) 0.03003(16) Uani 1 1 d . . . I1 I 0.18882(3) 0.35683(3) 0.066074(16) 0.03235(11) Uani 1 1 d . . . I2 I 0.07058(3) 0.29385(3) 0.230908(15) 0.03006(10) Uani 1 1 d . . . I3 I 0.38791(3) 0.45316(3) 0.226199(15) 0.02926(10) Uani 1 1 d . . . C1 C 0.1613(5) 0.6723(4) 0.1936(3) 0.0324(13) Uani 1 1 d . . . H1A H 0.2329 0.6849 0.2135 0.039 Uiso 1 1 calc R . . H1B H 0.1230 0.7393 0.1904 0.039 Uiso 1 1 calc R . . N1 N 0.1702(4) 0.6329(3) 0.1394(2) 0.0309(11) Uani 1 1 d . . . C11 C 0.2242(6) 0.7154(5) 0.1134(3) 0.0453(17) Uani 1 1 d . . . H11A H 0.2781 0.7469 0.1411 0.054 Uiso 1 1 calc R . . H11B H 0.1718 0.7701 0.1010 0.054 Uiso 1 1 calc R . . C12 C 0.2764(5) 0.6840(5) 0.0672(3) 0.0474(17) Uani 1 1 d . . . H12A H 0.3102 0.7460 0.0537 0.057 Uiso 1 1 calc R . . H12B H 0.2214 0.6598 0.0378 0.057 Uiso 1 1 calc R . . S1 S 0.37361(12) 0.58501(13) 0.08048(7) 0.0396(4) Uani 1 1 d . . . C13 C 0.4808(5) 0.6434(5) 0.1270(3) 0.0429(15) Uani 1 1 d . . . H13A H 0.4510 0.6718 0.1584 0.052 Uiso 1 1 calc R . . H13B H 0.5316 0.5882 0.1406 0.052 Uiso 1 1 calc R . . C14 C 0.5395(5) 0.7276(5) 0.1034(3) 0.0390(14) Uani 1 1 d . . . C15 C 0.5158(6) 0.8323(6) 0.1100(3) 0.0541(19) Uani 1 1 d . . . H15 H 0.4595 0.8514 0.1290 0.065 Uiso 1 1 calc R . . C16 C 0.5740(7) 0.9073(6) 0.0890(4) 0.069(3) Uani 1 1 d . . . H16 H 0.5575 0.9782 0.0941 0.083 Uiso 1 1 calc R . . C17 C 0.6558(6) 0.8832(7) 0.0609(3) 0.057(2) Uani 1 1 d . . . H17 H 0.6946 0.9365 0.0464 0.068 Uiso 1 1 calc R . . C18 C 0.6802(5) 0.7801(7) 0.0542(3) 0.052(2) Uani 1 1 d . . . H18 H 0.7368 0.7614 0.0354 0.062 Uiso 1 1 calc R . . C19 C 0.6225(5) 0.7060(5) 0.0747(3) 0.0405(15) Uani 1 1 d . . . F1 F 0.6468(3) 0.6053(4) 0.0681(2) 0.0648(12) Uani 1 1 d . . . C2 C 0.0613(5) 0.6168(5) 0.1104(3) 0.0415(15) Uani 1 1 d . . . H2A H 0.0233 0.6839 0.1067 0.050 Uiso 1 1 calc R . . H2B H 0.0648 0.5894 0.0737 0.050 Uiso 1 1 calc R . . N2 N 0.0035(3) 0.5425(4) 0.1407(2) 0.0342(12) Uani 1 1 d . . . C21 C -0.1102(5) 0.5353(6) 0.1156(4) 0.058(2) Uani 1 1 d . . . H21A H -0.1528 0.5149 0.1439 0.069 Uiso 1 1 calc R . . H21B H -0.1341 0.6051 0.1025 0.069 Uiso 1 1 calc R . . C22 C -0.1319(6) 0.4617(6) 0.0703(3) 0.058(2) Uani 1 1 d . . . H22A H -0.0958 0.4868 0.0403 0.069 Uiso 1 1 calc R . . H22B H -0.2089 0.4623 0.0573 0.069 Uiso 1 1 calc R . . S2 S -0.09175(12) 0.32962(13) 0.08535(7) 0.0370(3) Uani 1 1 d . . . C23 C -0.1774(5) 0.2794(7) 0.1302(3) 0.054(2) Uani 1 1 d . . . H23A H -0.1527 0.2091 0.1421 0.065 Uiso 1 1 calc R . . H23B H -0.1712 0.3241 0.1628 0.065 Uiso 1 1 calc R . . C24 C -0.2911(5) 0.2729(6) 0.1063(3) 0.0399(15) Uani 1 1 d . . . C25 C -0.3283(5) 0.2000(5) 0.0668(3) 0.0459(17) Uani 1 1 d . . . H25 H -0.2794 0.1538 0.0541 0.055 Uiso 1 1 calc R . . C26 C -0.4337(5) 0.1929(6) 0.0456(3) 0.0500(18) Uani 1 1 d . . . H26 H -0.4565 0.1441 0.0178 0.060 Uiso 1 1 calc R . . C27 C -0.5054(5) 0.2572(6) 0.0648(3) 0.0489(17) Uani 1 1 d . . . H27 H -0.5784 0.2510 0.0511 0.059 Uiso 1 1 calc R . . C28 C -0.4735(5) 0.3288(7) 0.1029(4) 0.060(2) Uani 1 1 d . . . H28 H -0.5230 0.3743 0.1156 0.072 Uiso 1 1 calc R . . C29 C -0.3676(6) 0.3347(7) 0.1231(4) 0.063(2) Uani 1 1 d . . . F2 F -0.3358(5) 0.4097(6) 0.1593(3) 0.129(3) Uani 1 1 d . . . C3 C -0.0014(4) 0.5822(5) 0.1947(3) 0.0350(14) Uani 1 1 d . . . H3A H -0.0396 0.5322 0.2149 0.042 Uiso 1 1 calc R . . H3B H -0.0409 0.6486 0.1921 0.042 Uiso 1 1 calc R . . N3 N 0.1053(4) 0.5990(3) 0.2240(2) 0.0302(10) Uani 1 1 d . . . C31 C 0.0992(6) 0.6498(5) 0.2779(3) 0.0424(16) Uani 1 1 d . . . H31A H 0.1659 0.6877 0.2898 0.051 Uiso 1 1 calc R . . H31B H 0.0410 0.7011 0.2736 0.051 Uiso 1 1 calc R . . C32 C 0.0811(5) 0.5729(5) 0.3212(3) 0.0460(16) Uani 1 1 d . . . H32A H 0.0158 0.5330 0.3089 0.055 Uiso 1 1 calc R . . H32B H 0.0709 0.6108 0.3545 0.055 Uiso 1 1 calc R . . S3 S 0.19057(12) 0.48404(13) 0.33631(7) 0.0394(4) Uani 1 1 d . . . C33 C 0.2989(6) 0.5674(5) 0.3687(3) 0.0487(18) Uani 1 1 d . . . H33A H 0.3316 0.6051 0.3409 0.058 Uiso 1 1 calc R . . H33B H 0.2712 0.6191 0.3924 0.058 Uiso 1 1 calc R . . C34 C 0.3790(5) 0.4997(4) 0.4013(2) 0.0327(13) Uani 1 1 d . . . C35 C 0.4733(5) 0.4733(5) 0.3830(3) 0.0450(16) Uani 1 1 d . . . H35 H 0.4886 0.4997 0.3495 0.054 Uiso 1 1 calc R . . C36 C 0.5444(6) 0.4086(7) 0.4137(3) 0.058(2) Uani 1 1 d . . . H36 H 0.6089 0.3916 0.4011 0.069 Uiso 1 1 calc R . . C37 C 0.5239(6) 0.3683(5) 0.4623(4) 0.058(2) Uani 1 1 d . . . H37 H 0.5736 0.3237 0.4828 0.069 Uiso 1 1 calc R . . C38 C 0.4324(6) 0.3928(5) 0.4802(3) 0.0449(17) Uani 1 1 d . . . H38 H 0.4169 0.3648 0.5133 0.054 Uiso 1 1 calc R . . C39 C 0.3622(5) 0.4579(5) 0.4507(3) 0.0369(14) Uani 1 1 d . . . F3 F 0.2713(3) 0.4822(4) 0.46885(18) 0.0604(11) Uani 1 1 d . . . C40 C -0.3275(11) 0.5829(11) 0.2557(6) 0.126(5) Uani 1 1 d . . . H40A H -0.3906 0.6104 0.2697 0.151 Uiso 1 1 calc R . . H40B H -0.3519 0.5333 0.2263 0.151 Uiso 1 1 calc R . . Cl1 Cl -0.2617(4) 0.6838(6) 0.2300(2) 0.208(3) Uani 1 1 d . . . Cl2 Cl -0.2529(4) 0.5221(5) 0.3042(3) 0.222(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0290(3) 0.0262(4) 0.0334(4) 0.0008(3) 0.0018(3) -0.0004(3) Cu2 0.0273(3) 0.0297(4) 0.0323(4) 0.0027(3) 0.0055(3) 0.0030(3) Cu3 0.0273(3) 0.0254(3) 0.0372(4) 0.0006(3) 0.0040(3) 0.0000(3) I1 0.03178(19) 0.0345(2) 0.0321(2) -0.00847(16) 0.00926(15) -0.00500(14) I2 0.02857(18) 0.0285(2) 0.0318(2) 0.00526(15) -0.00019(14) -0.00550(13) I3 0.02492(17) 0.0302(2) 0.0321(2) 0.00247(15) 0.00211(14) 0.00121(13) C1 0.039(3) 0.014(2) 0.045(4) -0.001(2) 0.008(3) -0.001(2) N1 0.035(2) 0.023(2) 0.035(3) 0.005(2) 0.006(2) 0.0001(18) C11 0.054(4) 0.026(3) 0.059(5) 0.016(3) 0.020(3) 0.001(3) C12 0.049(4) 0.044(4) 0.049(4) 0.019(3) 0.008(3) -0.001(3) S1 0.0371(8) 0.0470(9) 0.0357(9) 0.0022(7) 0.0084(7) -0.0085(7) C13 0.037(3) 0.060(4) 0.031(3) 0.002(3) 0.006(3) -0.013(3) C14 0.037(3) 0.045(4) 0.034(3) -0.007(3) 0.005(3) -0.012(3) C15 0.058(4) 0.053(4) 0.057(5) -0.019(4) 0.030(4) -0.016(3) C16 0.089(6) 0.046(4) 0.080(7) -0.021(4) 0.040(5) -0.032(4) C17 0.055(4) 0.066(5) 0.051(5) 0.000(4) 0.012(4) -0.028(4) C18 0.035(3) 0.086(6) 0.037(4) -0.019(4) 0.014(3) -0.022(3) C19 0.029(3) 0.053(4) 0.038(4) -0.007(3) 0.002(3) -0.003(3) F1 0.045(2) 0.068(3) 0.084(4) -0.011(3) 0.019(2) 0.013(2) C2 0.051(4) 0.030(3) 0.040(4) 0.001(3) -0.003(3) 0.013(3) N2 0.026(2) 0.025(2) 0.049(3) 0.003(2) -0.005(2) 0.0042(18) C21 0.031(3) 0.058(5) 0.078(6) -0.005(4) -0.015(4) 0.011(3) C22 0.047(4) 0.061(5) 0.056(5) 0.000(4) -0.022(4) 0.003(3) S2 0.0325(7) 0.0417(8) 0.0353(9) -0.0030(7) 0.0003(6) -0.0075(6) C23 0.034(3) 0.085(6) 0.043(4) 0.017(4) 0.002(3) -0.010(3) C24 0.029(3) 0.061(4) 0.030(3) 0.008(3) 0.006(2) -0.003(3) C25 0.031(3) 0.047(4) 0.063(5) 0.002(3) 0.017(3) -0.002(3) C26 0.046(4) 0.067(5) 0.038(4) -0.010(3) 0.011(3) -0.023(3) C27 0.028(3) 0.078(5) 0.041(4) 0.004(4) 0.004(3) 0.003(3) C28 0.028(3) 0.081(5) 0.074(6) -0.010(5) 0.016(3) 0.003(3) C29 0.045(4) 0.083(6) 0.063(6) -0.028(5) 0.013(4) -0.008(4) F2 0.087(4) 0.165(6) 0.139(6) -0.086(6) 0.028(4) -0.019(4) C3 0.025(3) 0.031(3) 0.050(4) 0.004(3) 0.010(3) 0.008(2) N3 0.034(2) 0.024(2) 0.034(3) 0.004(2) 0.008(2) 0.0026(19) C31 0.061(4) 0.025(3) 0.043(4) -0.008(3) 0.017(3) 0.006(3) C32 0.044(4) 0.045(4) 0.050(4) -0.009(3) 0.012(3) 0.002(3) S3 0.0346(8) 0.0517(10) 0.0312(8) -0.0013(7) 0.0027(6) -0.0030(7) C33 0.071(5) 0.028(3) 0.041(4) -0.004(3) -0.013(3) -0.002(3) C34 0.042(3) 0.026(3) 0.027(3) -0.004(2) -0.007(2) -0.008(2) C35 0.041(3) 0.058(4) 0.036(4) -0.009(3) 0.006(3) -0.014(3) C36 0.041(4) 0.073(5) 0.056(5) -0.021(4) -0.004(3) -0.002(4) C37 0.058(5) 0.041(4) 0.064(6) -0.007(4) -0.025(4) 0.009(3) C38 0.065(5) 0.030(3) 0.035(4) 0.004(3) -0.006(3) -0.013(3) C39 0.048(4) 0.029(3) 0.032(3) -0.008(3) 0.002(3) -0.010(3) F3 0.053(2) 0.083(3) 0.048(3) -0.011(2) 0.017(2) -0.002(2) C40 0.105(10) 0.136(11) 0.130(12) -0.061(10) -0.002(9) 0.016(9) Cl1 0.109(3) 0.388(9) 0.134(4) -0.014(5) 0.039(3) 0.069(4) Cl2 0.175(5) 0.225(6) 0.239(7) -0.058(5) -0.064(5) 0.077(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.177(5) . ? Cu1 S1 2.4206(17) . ? Cu1 I3 2.5654(8) . ? Cu1 I1 2.6070(8) . ? Cu1 Cu2 2.8857(9) . ? Cu1 Cu3 2.9182(11) . ? Cu2 N2 2.194(4) . ? Cu2 S2 2.4155(16) . ? Cu2 I2 2.5585(8) . ? Cu2 I1 2.5854(8) . ? Cu2 Cu3 2.9375(10) . ? Cu3 N3 2.183(4) . ? Cu3 S3 2.4039(18) . ? Cu3 I3 2.5537(8) . ? Cu3 I2 2.6112(7) . ? C1 N3 1.463(7) . ? C1 N1 1.465(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.470(7) . ? N1 C2 1.487(8) . ? C11 C12 1.473(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 S1 1.779(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? S1 C13 1.825(6) . ? C13 C14 1.488(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.394(9) . ? C14 C15 1.397(10) . ? C15 C16 1.370(10) . ? C15 H15 0.9500 . ? C16 C17 1.377(11) . ? C16 H16 0.9500 . ? C17 C18 1.381(11) . ? C17 H17 0.9500 . ? C18 C19 1.351(9) . ? C18 H18 0.9500 . ? C19 F1 1.349(8) . ? C2 N2 1.483(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.453(8) . ? N2 C21 1.500(7) . ? C21 C22 1.471(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 S2 1.802(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? S2 C23 1.799(7) . ? C23 C24 1.492(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.373(10) . ? C24 C25 1.395(10) . ? C25 C26 1.378(9) . ? C25 H25 0.9500 . ? C26 C27 1.373(10) . ? C26 H26 0.9500 . ? C27 C28 1.345(11) . ? C27 H27 0.9500 . ? C28 C29 1.377(10) . ? C28 H28 0.9500 . ? C29 F2 1.346(10) . ? C3 N3 1.467(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.510(8) . ? C31 C32 1.508(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 S3 1.805(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? S3 C33 1.845(6) . ? C33 C34 1.494(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.391(9) . ? C34 C35 1.393(9) . ? C35 C36 1.381(10) . ? C35 H35 0.9500 . ? C36 C37 1.381(12) . ? C36 H36 0.9500 . ? C37 C38 1.350(11) . ? C37 H37 0.9500 . ? C38 C39 1.364(9) . ? C38 H38 0.9500 . ? C39 F3 1.345(7) . ? C40 Cl2 1.630(15) . ? C40 Cl1 1.723(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 N1 Cu1 S1 89.08(13) . . ? N1 Cu1 I3 115.15(13) . . ? S1 Cu1 I3 106.58(5) . . ? N1 Cu1 I1 114.22(13) . . ? S1 Cu1 I1 96.61(5) . . ? I3 Cu1 I1 125.12(3) . . ? N1 Cu1 Cu2 84.25(12) . . ? S1 Cu1 Cu2 144.69(5) . . ? I3 Cu1 Cu2 107.64(3) . . ? I1 Cu1 Cu2 55.88(2) . . ? N1 Cu1 Cu3 82.49(13) . . ? S1 Cu1 Cu3 152.25(5) . . ? I3 Cu1 Cu3 55.06(2) . . ? I1 Cu1 Cu3 110.98(3) . . ? Cu2 Cu1 Cu3 60.81(2) . . ? N2 Cu2 S2 88.83(13) . . ? N2 Cu2 I2 111.72(15) . . ? S2 Cu2 I2 104.89(5) . . ? N2 Cu2 I1 113.96(15) . . ? S2 Cu2 I1 95.55(5) . . ? I2 Cu2 I1 129.91(3) . . ? N2 Cu2 Cu1 83.86(12) . . ? S2 Cu2 Cu1 144.04(5) . . ? I2 Cu2 Cu1 110.53(3) . . ? I1 Cu2 Cu1 56.59(2) . . ? N2 Cu2 Cu3 82.64(13) . . ? S2 Cu2 Cu3 153.33(5) . . ? I2 Cu2 Cu3 56.23(2) . . ? I1 Cu2 Cu3 111.01(3) . . ? Cu1 Cu2 Cu3 60.14(2) . . ? N3 Cu3 S3 89.04(14) . . ? N3 Cu3 I3 118.08(13) . . ? S3 Cu3 I3 108.09(4) . . ? N3 Cu3 I2 111.20(13) . . ? S3 Cu3 I2 96.97(5) . . ? I3 Cu3 I2 124.16(3) . . ? N3 Cu3 Cu1 84.35(13) . . ? S3 Cu3 Cu1 154.87(5) . . ? I3 Cu3 Cu1 55.43(2) . . ? I2 Cu3 Cu1 108.03(3) . . ? N3 Cu3 Cu2 83.29(13) . . ? S3 Cu3 Cu2 144.11(5) . . ? I3 Cu3 Cu2 106.43(3) . . ? I2 Cu3 Cu2 54.53(2) . . ? Cu1 Cu3 Cu2 59.05(2) . . ? Cu2 I1 Cu1 67.52(2) . . ? Cu2 I2 Cu3 69.24(2) . . ? Cu3 I3 Cu1 69.51(2) . . ? N3 C1 N1 111.4(4) . . ? N3 C1 H1A 109.3 . . ? N1 C1 H1A 109.3 . . ? N3 C1 H1B 109.3 . . ? N1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C1 N1 C11 105.2(5) . . ? C1 N1 C2 107.8(5) . . ? C11 N1 C2 110.6(5) . . ? C1 N1 Cu1 115.0(3) . . ? C11 N1 Cu1 106.4(4) . . ? C2 N1 Cu1 111.6(3) . . ? N1 C11 C12 116.3(5) . . ? N1 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N1 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C11 C12 S1 115.7(5) . . ? C11 C12 H12A 108.3 . . ? S1 C12 H12A 108.3 . . ? C11 C12 H12B 108.3 . . ? S1 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C12 S1 C13 105.3(3) . . ? C12 S1 Cu1 91.0(2) . . ? C13 S1 Cu1 105.1(2) . . ? C14 C13 S1 115.1(5) . . ? C14 C13 H13A 108.5 . . ? S1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? S1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C19 C14 C15 116.6(6) . . ? C19 C14 C13 121.6(6) . . ? C15 C14 C13 121.8(6) . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 122.1(8) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C18 118.7(7) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 119.3(7) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? F1 C19 C18 119.0(6) . . ? F1 C19 C14 117.4(6) . . ? C18 C19 C14 123.5(7) . . ? N2 C2 N1 110.0(5) . . ? N2 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 N2 C2 109.8(5) . . ? C3 N2 C21 104.0(5) . . ? C2 N2 C21 110.5(5) . . ? C3 N2 Cu2 113.6(4) . . ? C2 N2 Cu2 111.6(4) . . ? C21 N2 Cu2 107.0(4) . . ? C22 C21 N2 115.2(6) . . ? C22 C21 H21A 108.5 . . ? N2 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? N2 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 S2 115.5(6) . . ? C21 C22 H22A 108.4 . . ? S2 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? S2 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C23 S2 C22 106.8(4) . . ? C23 S2 Cu2 107.6(2) . . ? C22 S2 Cu2 91.8(2) . . ? C24 C23 S2 114.6(5) . . ? C24 C23 H23A 108.6 . . ? S2 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? S2 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C29 C24 C25 115.0(6) . . ? C29 C24 C23 122.7(7) . . ? C25 C24 C23 122.2(6) . . ? C26 C25 C24 122.1(6) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 C25 119.4(7) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 120.8(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 118.5(7) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? F2 C29 C24 117.5(7) . . ? F2 C29 C28 118.1(7) . . ? C24 C29 C28 124.2(7) . . ? N2 C3 N3 110.7(4) . . ? N2 C3 H3A 109.5 . . ? N3 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C1 N3 C3 109.0(5) . . ? C1 N3 C31 106.1(5) . . ? C3 N3 C31 110.1(5) . . ? C1 N3 Cu3 111.6(3) . . ? C3 N3 Cu3 113.5(3) . . ? C31 N3 Cu3 106.3(4) . . ? C32 C31 N3 112.8(5) . . ? C32 C31 H31A 109.0 . . ? N3 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? N3 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 S3 111.8(5) . . ? C31 C32 H32A 109.3 . . ? S3 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? S3 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C32 S3 C33 103.5(3) . . ? C32 S3 Cu3 91.0(2) . . ? C33 S3 Cu3 113.5(3) . . ? C34 C33 S3 108.1(4) . . ? C34 C33 H33A 110.1 . . ? S3 C33 H33A 110.1 . . ? C34 C33 H33B 110.1 . . ? S3 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C39 C34 C35 116.8(6) . . ? C39 C34 C33 121.9(6) . . ? C35 C34 C33 121.4(6) . . ? C36 C35 C34 119.7(7) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 121.4(7) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 119.2(7) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 119.9(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? F3 C39 C38 119.6(6) . . ? F3 C39 C34 117.5(6) . . ? C38 C39 C34 122.9(6) . . ? Cl2 C40 Cl1 112.0(8) . . ? Cl2 C40 H40A 109.2 . . ? Cl1 C40 H40A 109.2 . . ? Cl2 C40 H40B 109.2 . . ? Cl1 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.846 _refine_diff_density_min -2.078 _refine_diff_density_rms 0.209