# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Functionalized 1,2,3-Triazoles as Building Blocks for Photoluminescent POLOs (Polymers of Oligomers) of Copper(I) ; loop_ _publ_author_name S.-Q.Bai 'Jia Yi Kwang.' 'Lip Lin Koh.' T.S.A.Hor # Attachment 'Dalton-CIF.cif' data_9106 _database_code_depnum_ccdc_archive 'CCDC 738739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H67 Cu8 I8 N17' _chemical_formula_weight 2429.73 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' Cu Cu 0.3201 1.2651 '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' _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 14.0574(7) _cell_length_b 16.8368(9) _cell_length_c 17.7546(9) _cell_angle_alpha 77.7820(10) _cell_angle_beta 68.0410(10) _cell_angle_gamma 67.3920(10) _cell_volume 3586.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7372 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 5.812 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2929 _exptl_absorpt_correction_T_max 0.5422 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46584 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16449 _reflns_number_gt 13893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+11.6115P] 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 16449 _refine_ls_number_parameters 727 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.045 _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 0.36355(6) 0.26016(5) 0.82743(5) 0.03589(17) Uani 1 1 d . . . Cu2 Cu 0.11572(5) 0.26552(5) 0.80797(4) 0.03232(15) Uani 1 1 d . . . Cu3 Cu -0.11212(6) 0.25046(5) 0.77788(5) 0.03382(16) Uani 1 1 d . . . Cu4 Cu -0.36637(6) 0.23210(5) 0.81352(5) 0.03696(17) Uani 1 1 d . . . Cu5 Cu -1.04858(7) 0.67911(5) 0.77138(5) 0.04376(19) Uani 1 1 d . . . Cu6 Cu -1.08190(8) 0.83197(5) 0.67532(5) 0.0495(2) Uani 1 1 d . . . Cu7 Cu -1.24687(7) 0.79009(5) 0.77920(5) 0.0470(2) Uani 1 1 d . . . Cu8 Cu -1.11456(7) 0.70172(5) 0.64255(5) 0.0480(2) Uani 1 1 d . . . I1 I 0.55517(3) 0.15854(3) 0.74562(2) 0.03641(9) Uani 1 1 d . . . I2 I 0.22146(3) 0.18090(2) 0.90875(2) 0.03345(9) Uani 1 1 d . . . I3 I -0.09363(3) 0.33789(3) 0.87664(3) 0.04395(11) Uani 1 1 d . . . I4 I -0.26408(3) 0.33692(3) 0.71288(3) 0.04078(10) Uani 1 1 d . . . I5 I -0.91040(4) 0.69881(3) 0.61525(2) 0.04238(10) Uani 1 1 d . . . I6 I -1.20855(3) 0.62165(3) 0.77987(2) 0.03976(10) Uani 1 1 d . . . I7 I -1.26347(4) 0.86599(3) 0.63615(2) 0.05230(13) Uani 1 1 d . . . I8 I -1.10687(4) 0.82616(3) 0.83328(2) 0.04486(11) Uani 1 1 d . . . N1 N 0.2907(4) 0.3519(3) 0.7533(3) 0.0352(11) Uani 1 1 d . A . N2 N 0.2017(3) 0.3527(3) 0.7434(3) 0.0263(9) Uani 1 1 d . . . N3 N 0.1743(4) 0.4210(3) 0.6916(3) 0.0310(10) Uani 1 1 d . . . N4 N 0.0994(5) 0.3540(3) 0.4547(3) 0.0423(13) Uani 1 1 d . . . N5 N 0.1323(4) 0.2042(3) 0.7142(3) 0.0311(10) Uani 1 1 d . A . N6 N 0.0467(4) 0.2132(3) 0.6940(3) 0.0303(10) Uani 1 1 d . . . N7 N 0.0857(4) 0.1830(3) 0.6199(3) 0.0326(10) Uani 1 1 d . . . N8 N -0.0492(5) -0.0569(3) 0.6325(3) 0.0454(13) Uani 1 1 d . . . N9 N -0.1535(3) 0.1473(3) 0.8479(3) 0.0280(9) Uani 1 1 d . . . N10 N -0.2475(3) 0.1381(3) 0.8600(3) 0.0267(9) Uani 1 1 d . . . N11 N -0.2492(3) 0.0652(3) 0.9091(3) 0.0270(9) Uani 1 1 d . . . N12 N -0.5000(4) 0.3125(3) 0.8932(3) 0.0338(11) Uani 1 1 d . A . N13 N -0.6005(3) 0.3206(3) 0.9008(3) 0.0307(10) Uani 1 1 d . . . N14 N -0.6667(3) 0.3747(3) 0.9578(3) 0.0322(10) Uani 1 1 d . . . N15 N -0.9600(4) 0.5883(3) 0.8385(3) 0.0345(11) Uani 1 1 d . . . N16 N -0.6141(4) 0.1549(3) 1.1319(3) 0.0360(11) Uani 1 1 d . . . C1 C 0.3192(5) 0.4208(5) 0.7095(5) 0.062(2) Uani 1 1 d D . . C2 C 0.2457(5) 0.4638(5) 0.6689(5) 0.056(2) Uani 1 1 d . A . H2 H 0.2450 0.5133 0.6324 0.067 Uiso 1 1 calc R . . C7 C 0.0747(5) 0.4442(4) 0.6726(3) 0.0370(14) Uani 1 1 d . . . H7A H 0.0425 0.5072 0.6682 0.044 Uiso 1 1 calc R . . H7B H 0.0231 0.4221 0.7181 0.044 Uiso 1 1 calc R . . C8 C 0.0047(5) 0.3842(4) 0.5129(3) 0.0348(13) Uani 1 1 d . . . H8 H -0.0590 0.3860 0.5055 0.042 Uiso 1 1 calc R . . C9 C -0.0049(5) 0.4131(3) 0.5839(3) 0.0321(12) Uani 1 1 d . . . H9 H -0.0735 0.4338 0.6234 0.038 Uiso 1 1 calc R . . C10 C 0.0884(5) 0.4111(4) 0.5956(3) 0.0334(12) Uani 1 1 d . . . C11 C 0.1864(6) 0.3812(5) 0.5345(4) 0.0529(19) Uani 1 1 d . . . H11 H 0.2513 0.3794 0.5398 0.063 Uiso 1 1 calc R . . C12 C 0.1884(6) 0.3542(5) 0.4657(4) 0.057(2) Uani 1 1 d . . . H12 H 0.2557 0.3350 0.4245 0.069 Uiso 1 1 calc R . . C13 C 0.2242(4) 0.1665(4) 0.6546(4) 0.0376(13) Uani 1 1 d D . . C14 C 0.1947(5) 0.1542(4) 0.5943(4) 0.0425(15) Uani 1 1 d . A . H14 H 0.2415 0.1304 0.5447 0.051 Uiso 1 1 calc R . . C19 C 0.0116(5) 0.1831(4) 0.5799(4) 0.0390(14) Uani 1 1 d . . . H19A H 0.0427 0.1944 0.5210 0.047 Uiso 1 1 calc R . . H19B H -0.0580 0.2296 0.5991 0.047 Uiso 1 1 calc R . . C20 C 0.0489(6) -0.0525(4) 0.5868(4) 0.0476(16) Uani 1 1 d . . . H20 H 0.1048 -0.1036 0.5668 0.057 Uiso 1 1 calc R . . C21 C 0.0721(6) 0.0228(4) 0.5674(4) 0.0451(15) Uani 1 1 d . . . H21 H 0.1421 0.0229 0.5342 0.054 Uiso 1 1 calc R . . C22 C -0.0084(5) 0.0984(4) 0.5972(3) 0.0367(13) Uani 1 1 d . . . C23 C -0.1108(6) 0.0952(4) 0.6423(4) 0.0473(16) Uani 1 1 d . . . H23 H -0.1685 0.1457 0.6617 0.057 Uiso 1 1 calc R . . C24 C -0.1277(7) 0.0157(4) 0.6590(5) 0.0542(18) Uani 1 1 d . . . H24 H -0.1976 0.0138 0.6903 0.065 Uiso 1 1 calc R . . C25 C -0.0957(4) 0.0803(4) 0.8889(3) 0.0306(12) Uani 1 1 d D . . C26 C -0.1570(4) 0.0283(4) 0.9271(3) 0.0311(12) Uani 1 1 d . . . H26 H -0.1380 -0.0233 0.9596 0.037 Uiso 1 1 calc R . . C27 C 0.0166(4) 0.0692(4) 0.8859(4) 0.0417(15) Uani 1 1 d D . . H27A H 0.0146 0.0742 0.9405 0.050 Uiso 1 1 calc R . . H27B H 0.0393 0.1159 0.8496 0.050 Uiso 1 1 calc R . . C28 C 0.0995(7) -0.0158(6) 0.8567(6) 0.081(3) Uani 1 1 d D . . H28A H 0.1706 -0.0181 0.8560 0.098 Uiso 1 1 calc R . . H28B H 0.0801 -0.0621 0.8960 0.098 Uiso 1 1 calc R . . C29 C 0.1100(8) -0.0325(8) 0.7748(6) 0.104(4) Uani 1 1 d D . . H29A H 0.1362 0.0105 0.7345 0.125 Uiso 1 1 calc R . . H29B H 0.0380 -0.0256 0.7739 0.125 Uiso 1 1 calc R . . C30 C 0.1894(11) -0.1244(9) 0.7504(8) 0.153(7) Uani 1 1 d D . . H30A H 0.2637 -0.1275 0.7393 0.229 Uiso 1 1 calc R . . H30B H 0.1824 -0.1363 0.7019 0.229 Uiso 1 1 calc R . . H30C H 0.1716 -0.1668 0.7946 0.229 Uiso 1 1 calc R . . C31 C -0.3396(4) 0.0321(3) 0.9322(3) 0.0300(11) Uani 1 1 d . . . H31A H -0.3133 -0.0302 0.9465 0.036 Uiso 1 1 calc R . . H31B H -0.3643 0.0412 0.8852 0.036 Uiso 1 1 calc R . . C32 C -0.6168(5) 0.1694(4) 1.0561(3) 0.0357(13) Uani 1 1 d . . . H32 H -0.6813 0.2074 1.0464 0.043 Uiso 1 1 calc R . . C33 C -0.5291(4) 0.1311(4) 0.9904(3) 0.0328(12) Uani 1 1 d . . . H33 H -0.5343 0.1437 0.9376 0.039 Uiso 1 1 calc R . . C34 C -0.4349(4) 0.0750(3) 1.0033(3) 0.0278(11) Uani 1 1 d . . . C35 C -0.4313(5) 0.0579(4) 1.0823(4) 0.0446(16) Uani 1 1 d . . . H35 H -0.3679 0.0199 1.0935 0.054 Uiso 1 1 calc R . . C36 C -0.5227(5) 0.0979(4) 1.1441(4) 0.0447(16) Uani 1 1 d . . . H36 H -0.5207 0.0844 1.1978 0.054 Uiso 1 1 calc R . . C37 C -0.5031(5) 0.3633(4) 0.9435(4) 0.0402(14) Uani 1 1 d D . . C38 C -0.6111(5) 0.4036(4) 0.9863(4) 0.0402(14) Uani 1 1 d . A . H38 H -0.6393 0.4425 1.0265 0.048 Uiso 1 1 calc R . . C43 C -0.7858(4) 0.3948(4) 0.9860(3) 0.0325(12) Uani 1 1 d . . . H43A H -0.8163 0.4141 1.0411 0.039 Uiso 1 1 calc R . . H43B H -0.8010 0.3418 0.9892 0.039 Uiso 1 1 calc R . . C44 C -0.8895(6) 0.6041(4) 0.8624(4) 0.0460(16) Uani 1 1 d . . . H44 H -0.8796 0.6581 0.8468 0.055 Uiso 1 1 calc R . . C45 C -0.8305(5) 0.5434(4) 0.9094(4) 0.0434(15) Uani 1 1 d . . . H45 H -0.7824 0.5568 0.9257 0.052 Uiso 1 1 calc R . . C46 C -0.8430(4) 0.4632(4) 0.9322(3) 0.0289(11) Uani 1 1 d . . . C47 C -0.9173(4) 0.4482(4) 0.9086(3) 0.0279(11) Uani 1 1 d . . . H47 H -0.9303 0.3954 0.9246 0.033 Uiso 1 1 calc R . . C48 C -0.9722(4) 0.5110(3) 0.8617(3) 0.0298(11) Uani 1 1 d . . . H48 H -1.0210 0.4989 0.8450 0.036 Uiso 1 1 calc R . . N1S N 0.6354(13) 0.4865(10) 0.5190(10) 0.102(5) Uiso 0.611(5) 1 d PD A 1 C1S C 0.6206(14) 0.4224(10) 0.5281(10) 0.082(5) Uiso 0.611(5) 1 d PD A 1 C2S C 0.6038(15) 0.3374(10) 0.5447(11) 0.090(5) Uiso 0.611(5) 1 d PD A 1 H2S1 H 0.6221 0.3073 0.5930 0.135 Uiso 0.611(5) 1 calc PR A 1 H2S2 H 0.6501 0.3031 0.4985 0.135 Uiso 0.611(5) 1 calc PR A 1 H2S3 H 0.5281 0.3465 0.5533 0.135 Uiso 0.611(5) 1 calc PR A 1 N1SB N 0.4558(19) 0.2990(17) 0.5169(16) 0.107(8) Uiso 0.389(5) 1 d PD A 2 C1SB C 0.5425(17) 0.2666(16) 0.5149(14) 0.075(6) Uiso 0.389(5) 1 d PD A 2 C2SB C 0.6584(19) 0.234(2) 0.5120(19) 0.102(9) Uiso 0.389(5) 1 d PD A 2 H2S4 H 0.6996 0.2631 0.4661 0.153 Uiso 0.389(5) 1 calc PR A 2 H2S5 H 0.6886 0.1722 0.5058 0.153 Uiso 0.389(5) 1 calc PR A 2 H2S6 H 0.6624 0.2444 0.5621 0.153 Uiso 0.389(5) 1 calc PR A 2 C3 C 0.4008(9) 0.4536(7) 0.7298(7) 0.043(2) Uiso 0.611(5) 1 d PD A 1 H3A H 0.3845 0.4478 0.7890 0.052 Uiso 0.611(5) 1 calc PR A 1 H3B H 0.4757 0.4154 0.7061 0.052 Uiso 0.611(5) 1 calc PR A 1 C4 C 0.3948(11) 0.5479(8) 0.6982(9) 0.063(3) Uiso 0.611(5) 1 d PD A 1 H4A H 0.4082 0.5557 0.6393 0.076 Uiso 0.611(5) 1 calc PR A 1 H4B H 0.3221 0.5876 0.7246 0.076 Uiso 0.611(5) 1 calc PR A 1 C5 C 0.4808(14) 0.5679(11) 0.7172(11) 0.089(4) Uiso 0.611(5) 1 d PD A 1 H5A H 0.5534 0.5272 0.6919 0.107 Uiso 0.611(5) 1 calc PR A 1 H5B H 0.4663 0.5617 0.7762 0.107 Uiso 0.611(5) 1 calc PR A 1 C6 C 0.477(3) 0.6610(16) 0.6835(14) 0.195(10) Uiso 0.611(5) 1 d PD A 1 H6A H 0.5441 0.6599 0.6401 0.293 Uiso 0.611(5) 1 calc PR A 1 H6B H 0.4668 0.6931 0.7268 0.293 Uiso 0.611(5) 1 calc PR A 1 H6C H 0.4161 0.6887 0.6623 0.293 Uiso 0.611(5) 1 calc PR A 1 C15 C 0.3330(9) 0.1358(8) 0.6688(7) 0.046(2) Uiso 0.611(5) 1 d PD A 1 H15A H 0.3411 0.1850 0.6839 0.055 Uiso 0.611(5) 1 calc PR A 1 H15B H 0.3304 0.0930 0.7159 0.055 Uiso 0.611(5) 1 calc PR A 1 C16 C 0.4325(13) 0.0971(11) 0.6010(9) 0.087(4) Uiso 0.611(5) 1 d PD A 1 H16A H 0.4197 0.0559 0.5776 0.105 Uiso 0.611(5) 1 calc PR A 1 H16B H 0.4925 0.0650 0.6229 0.105 Uiso 0.611(5) 1 calc PR A 1 C17 C 0.4664(16) 0.1633(12) 0.5337(11) 0.107(5) Uiso 0.611(5) 1 d PD A 1 H17A H 0.4692 0.2089 0.5583 0.128 Uiso 0.611(5) 1 calc PR A 1 H17B H 0.4107 0.1898 0.5068 0.128 Uiso 0.611(5) 1 calc PR A 1 C18 C 0.5778(19) 0.125(2) 0.4690(17) 0.172(10) Uiso 0.611(5) 1 d PD A 1 H18A H 0.6317 0.0922 0.4957 0.259 Uiso 0.611(5) 1 calc PR A 1 H18B H 0.5997 0.1716 0.4330 0.259 Uiso 0.611(5) 1 calc PR A 1 H18C H 0.5720 0.0877 0.4375 0.259 Uiso 0.611(5) 1 calc PR A 1 C39 C -0.4040(9) 0.3633(8) 0.9592(7) 0.039(3) Uiso 0.611(5) 1 d PD A 1 H39A H -0.3454 0.3088 0.9423 0.047 Uiso 0.611(5) 1 calc PR A 1 H39B H -0.3805 0.4098 0.9232 0.047 Uiso 0.611(5) 1 calc PR A 1 C40 C -0.4139(17) 0.3736(11) 1.0438(9) 0.069(5) Uiso 0.611(5) 1 d PD A 1 H40A H -0.3497 0.3839 1.0434 0.082 Uiso 0.611(5) 1 calc PR A 1 H40B H -0.4787 0.4228 1.0662 0.082 Uiso 0.611(5) 1 calc PR A 1 C41 C -0.4231(11) 0.2928(9) 1.0938(9) 0.069(3) Uiso 0.611(5) 1 d PD A 1 H41A H -0.4773 0.2766 1.0844 0.083 Uiso 0.611(5) 1 calc PR A 1 H41B H -0.4476 0.3022 1.1517 0.083 Uiso 0.611(5) 1 calc PR A 1 C42 C -0.3103(16) 0.2177(12) 1.0718(13) 0.130(7) Uiso 0.611(5) 1 d PD A 1 H42A H -0.2924 0.2013 1.0177 0.195 Uiso 0.611(5) 1 calc PR A 1 H42B H -0.3147 0.1684 1.1110 0.195 Uiso 0.611(5) 1 calc PR A 1 H42C H -0.2543 0.2371 1.0730 0.195 Uiso 0.611(5) 1 calc PR A 1 C3B C 0.4323(10) 0.4202(9) 0.6819(9) 0.035(3) Uiso 0.389(5) 1 d PD A 2 H3B1 H 0.4779 0.3840 0.6362 0.041 Uiso 0.389(5) 1 calc PR A 2 H3B2 H 0.4635 0.3986 0.7262 0.041 Uiso 0.389(5) 1 calc PR A 2 C4B C 0.4225(16) 0.5170(11) 0.6547(14) 0.063(3) Uiso 0.389(5) 1 d PD A 2 H4B1 H 0.3983 0.5333 0.6068 0.076 Uiso 0.389(5) 1 calc PR A 2 H4B2 H 0.3641 0.5516 0.6983 0.076 Uiso 0.389(5) 1 calc PR A 2 C5B C 0.5222(18) 0.5445(17) 0.6338(18) 0.089(4) Uiso 0.389(5) 1 d PD A 2 H5B1 H 0.5605 0.5445 0.5750 0.107 Uiso 0.389(5) 1 calc PR A 2 H5B2 H 0.5726 0.5039 0.6617 0.107 Uiso 0.389(5) 1 calc PR A 2 C6B C 0.483(4) 0.6367(19) 0.662(2) 0.195(10) Uiso 0.389(5) 1 d PD A 2 H6B1 H 0.4566 0.6790 0.6211 0.293 Uiso 0.389(5) 1 calc PR A 2 H6B2 H 0.5425 0.6467 0.6681 0.293 Uiso 0.389(5) 1 calc PR A 2 H6B3 H 0.4239 0.6418 0.7133 0.293 Uiso 0.389(5) 1 calc PR A 2 C15B C 0.3373(13) 0.1538(12) 0.6490(13) 0.046(2) Uiso 0.389(5) 1 d PD A 2 H15C H 0.3384 0.1909 0.6842 0.055 Uiso 0.389(5) 1 calc PR A 2 H15D H 0.3818 0.1644 0.5928 0.055 Uiso 0.389(5) 1 calc PR A 2 C16B C 0.377(2) 0.0545(12) 0.6806(16) 0.087(4) Uiso 0.389(5) 1 d PD A 2 H16C H 0.4469 0.0430 0.6875 0.105 Uiso 0.389(5) 1 calc PR A 2 H16D H 0.3254 0.0496 0.7355 0.105 Uiso 0.389(5) 1 calc PR A 2 C17B C 0.391(3) -0.0190(17) 0.6392(18) 0.107(5) Uiso 0.389(5) 1 d PD A 2 H17C H 0.4107 0.0026 0.5817 0.128 Uiso 0.389(5) 1 calc PR A 2 H17D H 0.3165 -0.0182 0.6538 0.128 Uiso 0.389(5) 1 calc PR A 2 C18B C 0.456(3) -0.114(2) 0.635(3) 0.172(10) Uiso 0.389(5) 1 d PD A 2 H18D H 0.5259 -0.1216 0.5931 0.259 Uiso 0.389(5) 1 calc PR A 2 H18E H 0.4164 -0.1428 0.6231 0.259 Uiso 0.389(5) 1 calc PR A 2 H18F H 0.4666 -0.1374 0.6875 0.259 Uiso 0.389(5) 1 calc PR A 2 C39B C -0.4007(11) 0.3790(11) 0.9357(10) 0.027(4) Uiso 0.389(5) 1 d PD A 2 H39C H -0.4036 0.4377 0.9119 0.033 Uiso 0.389(5) 1 calc PR A 2 H39D H -0.3361 0.3377 0.9013 0.033 Uiso 0.389(5) 1 calc PR A 2 C40B C -0.398(2) 0.3666(12) 1.0231(12) 0.047(6) Uiso 0.389(5) 1 d PD A 2 H40C H -0.3431 0.3868 1.0265 0.056 Uiso 0.389(5) 1 calc PR A 2 H40D H -0.4693 0.3964 1.0610 0.056 Uiso 0.389(5) 1 calc PR A 2 C41B C -0.368(2) 0.2698(12) 1.0392(13) 0.069(3) Uiso 0.389(5) 1 d PD A 2 H41C H -0.2916 0.2414 1.0075 0.083 Uiso 0.389(5) 1 calc PR A 2 H41D H -0.4142 0.2495 1.0239 0.083 Uiso 0.389(5) 1 calc PR A 2 C42B C -0.384(3) 0.250(2) 1.1297(15) 0.130(7) Uiso 0.389(5) 1 d PD A 2 H42D H -0.3207 0.2477 1.1404 0.195 Uiso 0.389(5) 1 calc PR A 2 H42E H -0.3952 0.1943 1.1470 0.195 Uiso 0.389(5) 1 calc PR A 2 H42F H -0.4480 0.2943 1.1596 0.195 Uiso 0.389(5) 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 0.0281(3) 0.0398(4) 0.0448(4) 0.0091(3) -0.0200(3) -0.0152(3) Cu2 0.0253(3) 0.0436(4) 0.0316(4) -0.0073(3) -0.0121(3) -0.0102(3) Cu3 0.0282(3) 0.0351(4) 0.0437(4) -0.0032(3) -0.0178(3) -0.0104(3) Cu4 0.0246(3) 0.0344(4) 0.0557(5) -0.0066(3) -0.0165(3) -0.0090(3) Cu5 0.0541(5) 0.0329(4) 0.0375(4) -0.0028(3) -0.0246(4) 0.0018(3) Cu6 0.0653(6) 0.0287(4) 0.0388(4) -0.0062(3) -0.0090(4) -0.0053(4) Cu7 0.0480(5) 0.0425(4) 0.0298(4) -0.0101(3) -0.0094(3) 0.0070(4) Cu8 0.0654(5) 0.0427(4) 0.0268(4) -0.0118(3) -0.0178(4) -0.0013(4) I1 0.02956(19) 0.0483(2) 0.0376(2) -0.00695(17) -0.01346(16) -0.01535(16) I2 0.03525(19) 0.0410(2) 0.03174(19) 0.01146(15) -0.01778(15) -0.02163(16) I3 0.02225(18) 0.0587(3) 0.0572(3) -0.0311(2) -0.00586(17) -0.01322(17) I4 0.03017(19) 0.0331(2) 0.0628(3) 0.00800(18) -0.02532(18) -0.01075(16) I5 0.0483(2) 0.0333(2) 0.0326(2) -0.00966(15) -0.01344(17) 0.00382(17) I6 0.0443(2) 0.0361(2) 0.0335(2) -0.00570(15) -0.01943(17) 0.00018(17) I7 0.0653(3) 0.0412(2) 0.0274(2) -0.00732(16) -0.01924(19) 0.0125(2) I8 0.0522(3) 0.0406(2) 0.0324(2) -0.01606(16) -0.01119(18) -0.00146(18) N1 0.025(2) 0.044(3) 0.037(3) 0.010(2) -0.010(2) -0.018(2) N2 0.024(2) 0.030(2) 0.024(2) -0.0008(17) -0.0098(17) -0.0065(18) N3 0.028(2) 0.032(2) 0.021(2) -0.0017(18) -0.0080(18) 0.0007(19) N4 0.053(3) 0.039(3) 0.026(2) -0.006(2) -0.018(2) 0.000(2) N5 0.029(2) 0.038(3) 0.028(2) -0.0024(19) -0.0110(19) -0.011(2) N6 0.034(2) 0.036(3) 0.028(2) -0.0037(19) -0.018(2) -0.011(2) N7 0.042(3) 0.029(2) 0.028(2) -0.0051(19) -0.015(2) -0.008(2) N8 0.061(4) 0.027(3) 0.042(3) -0.007(2) -0.018(3) -0.005(2) N9 0.025(2) 0.029(2) 0.031(2) -0.0061(18) -0.0093(18) -0.0083(18) N10 0.026(2) 0.024(2) 0.033(2) -0.0040(18) -0.0126(19) -0.0078(18) N11 0.022(2) 0.022(2) 0.035(2) -0.0076(18) -0.0099(18) -0.0026(17) N12 0.023(2) 0.029(2) 0.053(3) -0.007(2) -0.017(2) -0.0057(19) N13 0.020(2) 0.028(2) 0.047(3) -0.002(2) -0.017(2) -0.0062(18) N14 0.018(2) 0.031(2) 0.049(3) -0.002(2) -0.016(2) -0.0060(18) N15 0.034(3) 0.034(3) 0.030(2) -0.003(2) -0.011(2) -0.004(2) N16 0.039(3) 0.027(2) 0.031(3) -0.0049(19) -0.012(2) 0.002(2) C1 0.030(3) 0.057(4) 0.085(6) 0.040(4) -0.019(3) -0.022(3) C2 0.032(3) 0.052(4) 0.060(4) 0.031(3) -0.009(3) -0.012(3) C7 0.035(3) 0.038(3) 0.030(3) -0.012(2) -0.018(2) 0.008(2) C8 0.047(3) 0.025(3) 0.032(3) -0.003(2) -0.018(3) -0.006(2) C9 0.041(3) 0.023(3) 0.026(3) -0.002(2) -0.012(2) -0.003(2) C10 0.037(3) 0.026(3) 0.030(3) -0.003(2) -0.017(2) 0.005(2) C11 0.041(4) 0.064(5) 0.039(4) -0.022(3) -0.019(3) 0.012(3) C12 0.048(4) 0.073(5) 0.035(4) -0.023(3) -0.010(3) 0.004(4) C13 0.026(3) 0.050(4) 0.033(3) -0.013(3) -0.002(2) -0.011(3) C14 0.043(4) 0.050(4) 0.029(3) -0.010(3) -0.005(3) -0.013(3) C19 0.053(4) 0.033(3) 0.038(3) -0.004(2) -0.030(3) -0.006(3) C20 0.058(4) 0.032(3) 0.046(4) -0.010(3) -0.016(3) -0.003(3) C21 0.050(4) 0.036(3) 0.045(4) -0.011(3) -0.015(3) -0.007(3) C22 0.055(4) 0.032(3) 0.031(3) -0.005(2) -0.027(3) -0.008(3) C23 0.052(4) 0.028(3) 0.054(4) -0.012(3) -0.016(3) -0.001(3) C24 0.062(5) 0.034(3) 0.056(4) -0.013(3) -0.011(4) -0.008(3) C25 0.027(3) 0.035(3) 0.030(3) 0.001(2) -0.015(2) -0.006(2) C26 0.029(3) 0.033(3) 0.028(3) 0.000(2) -0.012(2) -0.006(2) C27 0.030(3) 0.052(4) 0.047(4) 0.006(3) -0.022(3) -0.013(3) C28 0.038(4) 0.093(7) 0.094(7) -0.023(6) -0.021(4) 0.006(4) C29 0.057(6) 0.148(11) 0.073(7) -0.022(7) -0.014(5) 0.002(6) C30 0.136(12) 0.130(12) 0.116(11) -0.066(9) -0.035(9) 0.058(9) C31 0.031(3) 0.025(3) 0.036(3) -0.006(2) -0.010(2) -0.009(2) C32 0.031(3) 0.031(3) 0.032(3) 0.001(2) -0.009(2) 0.001(2) C33 0.030(3) 0.039(3) 0.024(3) 0.000(2) -0.011(2) -0.005(2) C34 0.030(3) 0.019(2) 0.033(3) -0.004(2) -0.009(2) -0.006(2) C35 0.035(3) 0.047(4) 0.037(3) -0.001(3) -0.018(3) 0.007(3) C36 0.045(4) 0.047(4) 0.034(3) -0.006(3) -0.021(3) 0.003(3) C37 0.029(3) 0.035(3) 0.064(4) -0.013(3) -0.020(3) -0.008(2) C38 0.026(3) 0.041(3) 0.057(4) -0.019(3) -0.016(3) -0.005(2) C43 0.019(2) 0.042(3) 0.034(3) 0.002(2) -0.011(2) -0.008(2) C44 0.049(4) 0.037(3) 0.062(4) 0.006(3) -0.030(3) -0.019(3) C45 0.032(3) 0.043(4) 0.063(4) 0.002(3) -0.024(3) -0.014(3) C46 0.019(2) 0.036(3) 0.026(3) -0.003(2) -0.004(2) -0.004(2) C47 0.022(2) 0.033(3) 0.025(3) -0.005(2) -0.005(2) -0.006(2) C48 0.033(3) 0.030(3) 0.025(3) -0.006(2) -0.014(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 N1 2.024(5) . ? Cu1 N13 2.106(5) 1_655 ? Cu1 I1 2.6221(9) . ? Cu1 I2 2.6328(8) . ? Cu2 N5 2.037(5) . ? Cu2 N2 2.132(4) . ? Cu2 I2 2.5929(8) . ? Cu2 I3 2.6116(8) . ? Cu3 N9 2.055(5) . ? Cu3 N6 2.105(5) . ? Cu3 I4 2.5992(8) . ? Cu3 I3 2.6528(8) . ? Cu4 N12 2.057(5) . ? Cu4 N10 2.104(4) . ? Cu4 I1 2.6231(8) 1_455 ? Cu4 I4 2.6589(8) . ? Cu5 N15 2.045(5) . ? Cu5 I8 2.6320(9) . ? Cu5 Cu7 2.6639(11) . ? Cu5 Cu8 2.6802(11) . ? Cu5 I6 2.7153(10) . ? Cu5 Cu6 2.7503(11) . ? Cu5 I5 2.7653(9) . ? Cu6 N8 2.021(6) 1_465 ? Cu6 Cu7 2.6048(13) . ? Cu6 Cu8 2.6215(13) . ? Cu6 I5 2.6286(9) . ? Cu6 I8 2.6780(9) . ? Cu6 I7 2.7132(11) . ? Cu7 N16 2.022(5) 2_367 ? Cu7 I7 2.6417(9) . ? Cu7 I6 2.6737(10) . ? Cu7 Cu8 2.7540(11) . ? Cu7 I8 2.7827(11) . ? Cu8 N4 2.041(5) 2_466 ? Cu8 I6 2.6601(10) . ? Cu8 I5 2.7084(11) . ? Cu8 I7 2.7637(9) . ? I1 Cu4 2.6230(8) 1_655 ? N1 N2 1.322(6) . ? N1 C1 1.362(8) . ? N2 N3 1.338(6) . ? N3 C2 1.348(8) . ? N3 C7 1.451(7) . ? N4 C8 1.331(8) . ? N4 C12 1.337(9) . ? N4 Cu8 2.041(5) 2_466 ? N5 N6 1.325(6) . ? N5 C13 1.350(7) . ? N6 N7 1.349(6) . ? N7 C14 1.338(8) . ? N7 C19 1.464(7) . ? N8 C24 1.323(8) . ? N8 C20 1.335(9) . ? N8 Cu6 2.021(6) 1_645 ? N9 N10 1.321(6) . ? N9 C25 1.361(7) . ? N10 N11 1.349(6) . ? N11 C26 1.332(7) . ? N11 C31 1.468(7) . ? N12 N13 1.322(6) . ? N12 C37 1.341(8) . ? N13 N14 1.324(7) . ? N13 Cu1 2.106(5) 1_455 ? N14 C38 1.341(7) . ? N14 C43 1.476(6) . ? N15 C48 1.336(7) . ? N15 C44 1.342(8) . ? N16 C32 1.328(7) . ? N16 C36 1.339(8) . ? N16 Cu7 2.022(5) 2_367 ? C1 C2 1.369(9) . ? C1 C3B 1.474(12) . ? C1 C3 1.622(11) . ? C7 C10 1.503(8) . ? C8 C9 1.388(8) . ? C9 C10 1.390(8) . ? C10 C11 1.382(9) . ? C11 C12 1.378(9) . ? C13 C14 1.361(8) . ? C13 C15B 1.488(15) . ? C13 C15 1.515(11) . ? C19 C22 1.506(8) . ? C20 C21 1.371(9) . ? C21 C22 1.382(9) . ? C22 C23 1.377(9) . ? C23 C24 1.401(10) . ? C25 C26 1.364(8) . ? C25 C27 1.498(7) . ? C27 C28 1.501(10) . ? C28 C29 1.482(11) . ? C29 C30 1.558(13) . ? C31 C34 1.513(7) . ? C32 C33 1.389(8) . ? C33 C34 1.369(7) . ? C34 C35 1.387(8) . ? C35 C36 1.378(9) . ? C37 C38 1.380(8) . ? C37 C39B 1.513(13) . ? C37 C39 1.519(11) . ? C43 C46 1.511(7) . ? C44 C45 1.390(9) . ? C45 C46 1.384(8) . ? C46 C47 1.380(7) . ? C47 C48 1.374(7) . ? N1S C1S 1.142(14) . ? C1S C2S 1.491(15) . ? N1SB C1SB 1.118(17) . ? C1SB C2SB 1.489(18) . ? C3 C4 1.550(13) . ? C4 C5 1.533(15) . ? C5 C6 1.543(18) . ? C15 C16 1.483(15) . ? C16 C17 1.522(16) . ? C17 C18 1.542(17) . ? C39 C40 1.497(15) . ? C40 C41 1.481(15) . ? C41 C42 1.571(16) . ? C3B C4B 1.567(16) . ? C4B C5B 1.533(17) . ? C5B C6B 1.555(19) . ? C15B C16B 1.594(17) . ? C16B C17B 1.480(15) . ? C17B C18B 1.499(15) . ? C39B C40B 1.534(17) . ? C40B C41B 1.510(17) . ? C41B C42B 1.518(18) . ? 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 N13 108.7(2) . 1_655 ? N1 Cu1 I1 111.97(15) . . ? N13 Cu1 I1 103.58(12) 1_655 . ? N1 Cu1 I2 104.15(13) . . ? N13 Cu1 I2 114.34(13) 1_655 . ? I1 Cu1 I2 114.25(3) . . ? N5 Cu2 N2 100.54(18) . . ? N5 Cu2 I2 118.74(14) . . ? N2 Cu2 I2 101.43(11) . . ? N5 Cu2 I3 105.86(13) . . ? N2 Cu2 I3 115.12(12) . . ? I2 Cu2 I3 114.60(3) . . ? N9 Cu3 N6 112.69(18) . . ? N9 Cu3 I4 106.91(12) . . ? N6 Cu3 I4 114.62(12) . . ? N9 Cu3 I3 106.52(13) . . ? N6 Cu3 I3 101.68(12) . . ? I4 Cu3 I3 114.24(3) . . ? N12 Cu4 N10 118.07(19) . . ? N12 Cu4 I1 105.49(13) . 1_455 ? N10 Cu4 I1 110.24(12) . 1_455 ? N12 Cu4 I4 104.12(14) . . ? N10 Cu4 I4 104.20(12) . . ? I1 Cu4 I4 114.96(3) 1_455 . ? N15 Cu5 I8 105.25(14) . . ? N15 Cu5 Cu7 143.52(14) . . ? I8 Cu5 Cu7 63.39(3) . . ? N15 Cu5 Cu8 142.98(14) . . ? I8 Cu5 Cu8 111.66(3) . . ? Cu7 Cu5 Cu8 62.04(3) . . ? N15 Cu5 I6 105.73(15) . . ? I8 Cu5 I6 117.85(3) . . ? Cu7 Cu5 I6 59.60(3) . . ? Cu8 Cu5 I6 59.07(3) . . ? N15 Cu5 Cu6 149.48(15) . . ? I8 Cu5 Cu6 59.63(3) . . ? Cu7 Cu5 Cu6 57.49(3) . . ? Cu8 Cu5 Cu6 57.71(3) . . ? I6 Cu5 Cu6 104.78(3) . . ? N15 Cu5 I5 108.76(14) . . ? I8 Cu5 I5 104.32(3) . . ? Cu7 Cu5 I5 107.67(3) . . ? Cu8 Cu5 I5 59.63(3) . . ? I6 Cu5 I5 114.36(3) . . ? Cu6 Cu5 I5 56.92(2) . . ? N8 Cu6 Cu7 135.57(17) 1_465 . ? N8 Cu6 Cu8 146.82(16) 1_465 . ? Cu7 Cu6 Cu8 63.60(3) . . ? N8 Cu6 I5 110.57(17) 1_465 . ? Cu7 Cu6 I5 113.77(4) . . ? Cu8 Cu6 I5 62.11(3) . . ? N8 Cu6 I8 101.07(16) 1_465 . ? Cu7 Cu6 I8 63.55(3) . . ? Cu8 Cu6 I8 112.07(4) . . ? I5 Cu6 I8 106.90(3) . . ? N8 Cu6 I7 101.23(17) 1_465 . ? Cu7 Cu6 I7 59.53(3) . . ? Cu8 Cu6 I7 62.38(3) . . ? I5 Cu6 I7 118.23(3) . . ? I8 Cu6 I7 117.21(3) . . ? N8 Cu6 Cu5 148.98(17) 1_465 . ? Cu7 Cu6 Cu5 59.59(3) . . ? Cu8 Cu6 Cu5 59.80(3) . . ? I5 Cu6 Cu5 61.83(3) . . ? I8 Cu6 Cu5 57.99(3) . . ? I7 Cu6 Cu5 108.69(4) . . ? N16 Cu7 Cu6 137.81(15) 2_367 . ? N16 Cu7 I7 109.31(14) 2_367 . ? Cu6 Cu7 I7 62.28(3) . . ? N16 Cu7 Cu5 136.46(14) 2_367 . ? Cu6 Cu7 Cu5 62.92(3) . . ? I7 Cu7 Cu5 113.60(3) . . ? N16 Cu7 I6 111.44(15) 2_367 . ? Cu6 Cu7 I6 110.22(3) . . ? I7 Cu7 I6 108.54(3) . . ? Cu5 Cu7 I6 61.16(3) . . ? N16 Cu7 Cu8 158.05(16) 2_367 . ? Cu6 Cu7 Cu8 58.50(3) . . ? I7 Cu7 Cu8 61.58(3) . . ? Cu5 Cu7 Cu8 59.27(3) . . ? I6 Cu7 Cu8 58.67(3) . . ? N16 Cu7 I8 96.84(15) 2_367 . ? Cu6 Cu7 I8 59.50(3) . . ? I7 Cu7 I8 116.05(4) . . ? Cu5 Cu7 I8 57.74(3) . . ? I6 Cu7 I8 114.14(3) . . ? Cu8 Cu7 I8 105.09(4) . . ? N4 Cu8 Cu6 140.33(16) 2_466 . ? N4 Cu8 I6 109.41(16) 2_466 . ? Cu6 Cu8 I6 110.13(3) . . ? N4 Cu8 Cu5 145.23(15) 2_466 . ? Cu6 Cu8 Cu5 62.49(3) . . ? I6 Cu8 Cu5 61.12(3) . . ? N4 Cu8 I5 103.85(17) 2_466 . ? Cu6 Cu8 I5 59.07(3) . . ? I6 Cu8 I5 118.17(3) . . ? Cu5 Cu8 I5 61.75(3) . . ? N4 Cu8 Cu7 149.04(17) 2_466 . ? Cu6 Cu8 Cu7 57.91(3) . . ? I6 Cu8 Cu7 59.16(3) . . ? Cu5 Cu8 Cu7 58.69(3) . . ? I5 Cu8 Cu7 106.73(4) . . ? N4 Cu8 I7 105.51(14) 2_466 . ? Cu6 Cu8 I7 60.44(3) . . ? I6 Cu8 I7 105.40(3) . . ? Cu5 Cu8 I7 109.26(3) . . ? I5 Cu8 I7 113.81(4) . . ? Cu7 Cu8 I7 57.21(2) . . ? Cu1 I1 Cu4 85.46(3) . 1_655 ? Cu2 I2 Cu1 86.87(2) . . ? Cu2 I3 Cu3 84.67(2) . . ? Cu3 I4 Cu4 83.85(2) . . ? Cu6 I5 Cu8 58.81(3) . . ? Cu6 I5 Cu5 61.25(3) . . ? Cu8 I5 Cu5 58.62(2) . . ? Cu8 I6 Cu7 62.17(3) . . ? Cu8 I6 Cu5 59.80(3) . . ? Cu7 I6 Cu5 59.24(3) . . ? Cu7 I7 Cu6 58.20(3) . . ? Cu7 I7 Cu8 61.21(2) . . ? Cu6 I7 Cu8 57.19(3) . . ? Cu5 I8 Cu6 62.38(3) . . ? Cu5 I8 Cu7 58.86(3) . . ? Cu6 I8 Cu7 56.94(3) . . ? N2 N1 C1 109.9(5) . . ? N2 N1 Cu1 121.7(3) . . ? C1 N1 Cu1 128.4(4) . . ? N1 N2 N3 106.9(4) . . ? N1 N2 Cu2 124.4(3) . . ? N3 N2 Cu2 128.5(3) . . ? N2 N3 C2 110.3(5) . . ? N2 N3 C7 120.8(5) . . ? C2 N3 C7 128.7(5) . . ? C8 N4 C12 117.1(5) . . ? C8 N4 Cu8 122.7(4) . 2_466 ? C12 N4 Cu8 119.8(4) . 2_466 ? N6 N5 C13 109.2(5) . . ? N6 N5 Cu2 121.1(4) . . ? C13 N5 Cu2 128.3(4) . . ? N5 N6 N7 106.8(4) . . ? N5 N6 Cu3 121.5(3) . . ? N7 N6 Cu3 131.1(3) . . ? C14 N7 N6 110.1(5) . . ? C14 N7 C19 129.2(5) . . ? N6 N7 C19 120.7(5) . . ? C24 N8 C20 117.7(6) . . ? C24 N8 Cu6 117.4(5) . 1_645 ? C20 N8 Cu6 124.5(4) . 1_645 ? N10 N9 C25 109.1(4) . . ? N10 N9 Cu3 122.1(3) . . ? C25 N9 Cu3 128.9(4) . . ? N9 N10 N11 106.9(4) . . ? N9 N10 Cu4 121.5(3) . . ? N11 N10 Cu4 131.5(3) . . ? C26 N11 N10 110.4(4) . . ? C26 N11 C31 127.5(5) . . ? N10 N11 C31 122.0(4) . . ? N13 N12 C37 109.5(5) . . ? N13 N12 Cu4 121.8(4) . . ? C37 N12 Cu4 128.7(4) . . ? N12 N13 N14 106.8(4) . . ? N12 N13 Cu1 123.1(4) . 1_455 ? N14 N13 Cu1 130.0(3) . 1_455 ? N13 N14 C38 111.4(4) . . ? N13 N14 C43 121.7(5) . . ? C38 N14 C43 126.8(5) . . ? C48 N15 C44 117.3(5) . . ? C48 N15 Cu5 120.9(4) . . ? C44 N15 Cu5 121.8(4) . . ? C32 N16 C36 117.0(5) . . ? C32 N16 Cu7 117.6(4) . 2_367 ? C36 N16 Cu7 125.1(4) . 2_367 ? N1 C1 C2 106.6(6) . . ? N1 C1 C3B 121.8(7) . . ? C2 C1 C3B 125.2(8) . . ? N1 C1 C3 120.9(6) . . ? C2 C1 C3 129.9(7) . . ? C3B C1 C3 36.6(7) . . ? N3 C2 C1 106.3(5) . . ? N3 C7 C10 115.0(5) . . ? N4 C8 C9 123.3(6) . . ? C8 C9 C10 119.1(5) . . ? C11 C10 C9 117.5(5) . . ? C11 C10 C7 124.8(6) . . ? C9 C10 C7 117.6(5) . . ? C12 C11 C10 119.5(7) . . ? N4 C12 C11 123.4(6) . . ? N5 C13 C14 107.8(5) . . ? N5 C13 C15B 126.2(10) . . ? C14 C13 C15B 125.2(10) . . ? N5 C13 C15 119.5(7) . . ? C14 C13 C15 132.0(7) . . ? C15B C13 C15 15.9(9) . . ? N7 C14 C13 106.2(5) . . ? N7 C19 C22 111.7(5) . . ? N8 C20 C21 123.3(6) . . ? C20 C21 C22 119.3(7) . . ? C23 C22 C21 117.9(6) . . ? C23 C22 C19 119.6(6) . . ? C21 C22 C19 122.4(6) . . ? C22 C23 C24 119.0(6) . . ? N8 C24 C23 122.7(7) . . ? N9 C25 C26 107.4(4) . . ? N9 C25 C27 123.0(5) . . ? C26 C25 C27 129.6(5) . . ? N11 C26 C25 106.3(5) . . ? C25 C27 C28 113.3(6) . . ? C29 C28 C27 114.7(8) . . ? C28 C29 C30 112.8(9) . . ? N11 C31 C34 112.7(4) . . ? N16 C32 C33 123.2(5) . . ? C34 C33 C32 119.3(5) . . ? C33 C34 C35 118.3(5) . . ? C33 C34 C31 119.5(5) . . ? C35 C34 C31 122.2(5) . . ? C36 C35 C34 118.6(5) . . ? N16 C36 C35 123.6(6) . . ? N12 C37 C38 107.6(5) . . ? N12 C37 C39B 120.1(8) . . ? C38 C37 C39B 131.3(8) . . ? N12 C37 C39 124.6(7) . . ? C38 C37 C39 127.0(7) . . ? C39B C37 C39 16.8(7) . . ? N14 C38 C37 104.6(5) . . ? N14 C43 C46 114.1(4) . . ? N15 C44 C45 122.3(6) . . ? C46 C45 C44 119.8(6) . . ? C47 C46 C45 117.5(5) . . ? C47 C46 C43 119.0(5) . . ? C45 C46 C43 123.3(5) . . ? C48 C47 C46 119.5(5) . . ? N15 C48 C47 123.6(5) . . ? N1S C1S C2S 176(2) . . ? N1SB C1SB C2SB 173(3) . . ? C4 C3 C1 115.0(8) . . ? C5 C4 C3 109.1(11) . . ? C4 C5 C6 108.9(17) . . ? C16 C15 C13 117.9(11) . . ? C15 C16 C17 113.5(14) . . ? C16 C17 C18 113.7(18) . . ? C40 C39 C37 118.8(11) . . ? C41 C40 C39 107.3(13) . . ? C40 C41 C42 110.7(14) . . ? C1 C3B C4B 104.2(11) . . ? C5B C4B C3B 119.6(17) . . ? C4B C5B C6B 108.4(17) . . ? C13 C15B C16B 100.6(14) . . ? C17B C16B C15B 126(2) . . ? C16B C17B C18B 138(3) . . ? C37 C39B C40B 104.9(13) . . ? C41B C40B C39B 101.1(16) . . ? C40B C41B C42B 106.7(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.469 _refine_diff_density_min -1.724 _refine_diff_density_rms 0.149 #===END data_9294 _database_code_depnum_ccdc_archive 'CCDC 738740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 Cu8 I8 N16' _chemical_formula_weight 2444.78 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' I I -0.4742 1.8119 '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 14.4297(19) _cell_length_b 16.937(2) _cell_length_c 17.684(2) _cell_angle_alpha 76.127(2) _cell_angle_beta 66.663(2) _cell_angle_gamma 65.040(2) _cell_volume 3584.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8321 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.60 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 5.817 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1060 _exptl_absorpt_correction_T_max 0.4964 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45151 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16358 _reflns_number_gt 13859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+99.6409P] 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 16358 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.85533(9) 0.77665(8) 0.69067(8) 0.0199(3) Uani 1 1 d . . . Cu2 Cu 0.60276(10) 0.75565(8) 0.72762(8) 0.0186(2) Uani 1 1 d . . . Cu3 Cu 0.37225(10) 0.74424(8) 0.70157(8) 0.0190(3) Uani 1 1 d . . . Cu4 Cu 0.12158(10) 0.75417(9) 0.68274(8) 0.0208(3) Uani 1 1 d . . . Cu5 Cu 0.39465(10) 0.70307(8) 1.14030(8) 0.0200(3) Uani 1 1 d . . . Cu6 Cu 0.42673(10) 0.82356(8) 1.18053(8) 0.0210(3) Uani 1 1 d . . . Cu7 Cu 0.46137(10) 0.66403(8) 1.26620(8) 0.0204(3) Uani 1 1 d . . . Cu8 Cu 0.26476(10) 0.78111(9) 1.29137(8) 0.0202(3) Uani 1 1 d . . . I1 I 0.92358(5) 0.85373(5) 0.75841(4) 0.02505(16) Uani 1 1 d . . . I2 I 0.76141(5) 0.66577(4) 0.78558(5) 0.02355(15) Uani 1 1 d . . . I3 I 0.58162(5) 0.67467(5) 0.62934(5) 0.02501(16) Uani 1 1 d . . . I4 I 0.25602(5) 0.84007(4) 0.60860(4) 0.02081(14) Uani 1 1 d . . . I5 I 0.59867(5) 0.68891(4) 1.11129(4) 0.01931(14) Uani 1 1 d . . . I6 I 0.24234(5) 0.86687(4) 1.14723(4) 0.01871(14) Uani 1 1 d . . . I7 I 0.30082(5) 0.61577(4) 1.27581(4) 0.01776(13) Uani 1 1 d . . . I8 I 0.40650(5) 0.80534(4) 1.34021(4) 0.01939(14) Uani 1 1 d . . . N1 N 1.4516(7) 0.4343(6) 0.6696(5) 0.0195(17) Uani 1 1 d . . . N2 N 1.1674(6) 0.6493(5) 0.5427(5) 0.0181(17) Uani 1 1 d . . . N3 N 1.0939(7) 0.6976(6) 0.6046(5) 0.0178(17) Uani 1 1 d . . . N4 N 0.9968(6) 0.7041(6) 0.6088(5) 0.0177(17) Uani 1 1 d . . . N5 N 1.1213(7) 0.8344(6) 0.3801(6) 0.0192(17) Uani 1 1 d . . . N6 N 0.7375(7) 0.9387(5) 0.5926(5) 0.0179(17) Uani 1 1 d . . . N7 N 0.7358(7) 0.8660(5) 0.6418(5) 0.0184(17) Uani 1 1 d . . . N8 N 0.6404(6) 0.8606(5) 0.6582(5) 0.0165(16) Uani 1 1 d . . . N9 N 0.5405(7) 1.0665(6) 0.8622(6) 0.0215(18) Uani 1 1 d . . . N10 N 0.4110(7) 0.8241(5) 0.8863(5) 0.0161(16) Uani 1 1 d . . . N11 N 0.4476(6) 0.7939(5) 0.8117(5) 0.0143(15) Uani 1 1 d . . . N12 N 0.3605(6) 0.7995(5) 0.7977(5) 0.0145(15) Uani 1 1 d . . . N13 N 0.4073(7) 0.6505(6) 1.0444(5) 0.0204(18) Uani 1 1 d . . . N14 N 0.3167(7) 0.5885(5) 0.8167(5) 0.0185(17) Uani 1 1 d . . . N15 N 0.2904(6) 0.6575(5) 0.7616(5) 0.0157(16) Uani 1 1 d . . . N16 N 0.1970(7) 0.6627(6) 0.7589(5) 0.0184(17) Uani 1 1 d . . . C1 C 1.4796(8) 0.5032(6) 0.6300(6) 0.019(2) Uani 1 1 d . . . H1 H 1.5403 0.5074 0.6354 0.022 Uiso 1 1 calc R . . C2 C 1.4248(8) 0.5692(6) 0.5811(6) 0.019(2) Uani 1 1 d . . . H2 H 1.4469 0.6174 0.5551 0.023 Uiso 1 1 calc R . . C3 C 1.3376(7) 0.5628(7) 0.5715(6) 0.0174(19) Uani 1 1 d . . . C4 C 1.3084(8) 0.4912(8) 0.6111(7) 0.026(2) Uani 1 1 d . . . H4 H 1.2487 0.4853 0.6058 0.031 Uiso 1 1 calc R . . C5 C 1.3663(9) 0.4290(8) 0.6579(8) 0.031(3) Uani 1 1 d . . . H5 H 1.3462 0.3798 0.6834 0.037 Uiso 1 1 calc R . . C6 C 1.2818(7) 0.6338(7) 0.5174(6) 0.019(2) Uani 1 1 d . . . H6A H 1.2899 0.6886 0.5187 0.023 Uiso 1 1 calc R . . H6B H 1.3176 0.6177 0.4597 0.023 Uiso 1 1 calc R . . C7 C 1.1177(8) 0.6258(7) 0.5052(7) 0.022(2) Uani 1 1 d . . . H7 H 1.1514 0.5924 0.4588 0.027 Uiso 1 1 calc R . . C8 C 1.0086(9) 0.6606(7) 0.5484(7) 0.024(2) Uani 1 1 d . . . C9 C 0.9142(9) 0.6609(9) 0.5331(8) 0.031(3) Uani 1 1 d . . . H9A H 0.8582 0.7207 0.5375 0.037 Uiso 1 1 calc R . . H9B H 0.8823 0.6214 0.5763 0.037 Uiso 1 1 calc R . . C10 C 0.9455(10) 0.6316(10) 0.4471(8) 0.037(3) Uani 1 1 d . . . H10A H 0.9862 0.6661 0.4046 0.045 Uiso 1 1 calc R . . H10B H 0.9945 0.5694 0.4455 0.045 Uiso 1 1 calc R . . C11 C 0.8491(11) 0.6421(11) 0.4251(9) 0.045(3) Uani 1 1 d . . . H11A H 0.8052 0.6111 0.4693 0.054 Uiso 1 1 calc R . . H11B H 0.8756 0.6149 0.3731 0.054 Uiso 1 1 calc R . . C12 C 0.7776(15) 0.7380(11) 0.4145(11) 0.057(5) Uani 1 1 d . . . H12A H 0.8234 0.7706 0.3754 0.069 Uiso 1 1 calc R . . H12B H 0.7439 0.7632 0.4684 0.069 Uiso 1 1 calc R . . C13 C 0.6879(16) 0.7498(13) 0.3819(13) 0.066(5) Uani 1 1 d . . . H13A H 0.6565 0.7049 0.4101 0.100 Uiso 1 1 calc R . . H13B H 0.7188 0.7441 0.3223 0.100 Uiso 1 1 calc R . . H13C H 0.6311 0.8079 0.3927 0.100 Uiso 1 1 calc R . . C14 C 1.1190(7) 0.8478(6) 0.4522(6) 0.0166(19) Uani 1 1 d . . . H14 H 1.1862 0.8274 0.4615 0.020 Uiso 1 1 calc R . . C15 C 1.0264(8) 0.8890(7) 0.5141(6) 0.0178(19) Uani 1 1 d . . . H15 H 1.0302 0.8970 0.5640 0.021 Uiso 1 1 calc R . . C16 C 0.9267(8) 0.9187(6) 0.5019(6) 0.0180(19) Uani 1 1 d . . . C17 C 0.9266(9) 0.9031(8) 0.4289(7) 0.025(2) Uani 1 1 d . . . H17 H 0.8599 0.9203 0.4195 0.030 Uiso 1 1 calc R . . C18 C 1.0249(8) 0.8619(9) 0.3685(7) 0.029(3) Uani 1 1 d . . . H18 H 1.0238 0.8530 0.3179 0.035 Uiso 1 1 calc R . . C19 C 0.8261(8) 0.9698(7) 0.5670(6) 0.0181(19) Uani 1 1 d . . . H19A H 0.8448 0.9668 0.6160 0.022 Uiso 1 1 calc R . . H19B H 0.8012 1.0319 0.5452 0.022 Uiso 1 1 calc R . . C20 C 0.6424(8) 0.9814(7) 0.5771(6) 0.019(2) Uani 1 1 d . . . H20 H 0.6227 1.0347 0.5438 0.023 Uiso 1 1 calc R . . C21 C 0.5805(8) 0.9308(7) 0.6199(6) 0.019(2) Uani 1 1 d . . . C22 C 0.4644(8) 0.9510(7) 0.6334(7) 0.021(2) Uani 1 1 d . . . H22A H 0.4525 0.8957 0.6412 0.026 Uiso 1 1 calc R . . H22B H 0.4466 0.9856 0.5840 0.026 Uiso 1 1 calc R . . C23 C 0.3888(8) 1.0029(8) 0.7101(7) 0.025(2) Uani 1 1 d . . . H23A H 0.4013 0.9654 0.7602 0.029 Uiso 1 1 calc R . . H23B H 0.4074 1.0543 0.7052 0.029 Uiso 1 1 calc R . . C24 C 0.2696(9) 1.0338(8) 0.7204(7) 0.028(2) Uani 1 1 d . . . H24A H 0.2513 0.9828 0.7233 0.033 Uiso 1 1 calc R . . H24B H 0.2562 1.0733 0.6714 0.033 Uiso 1 1 calc R . . C25 C 0.1965(9) 1.0817(9) 0.7978(8) 0.036(3) Uani 1 1 d . . . H25A H 0.2184 1.1304 0.7962 0.043 Uiso 1 1 calc R . . H25B H 0.2076 1.0410 0.8467 0.043 Uiso 1 1 calc R . . C26 C 0.0756(9) 1.1187(9) 0.8082(8) 0.037(3) Uani 1 1 d . . . H26A H 0.0614 1.1672 0.7660 0.055 Uiso 1 1 calc R . . H26B H 0.0327 1.1398 0.8632 0.055 Uiso 1 1 calc R . . H26C H 0.0554 1.0727 0.8021 0.055 Uiso 1 1 calc R . . C27 C 0.4423(8) 1.0634(7) 0.9102(7) 0.023(2) Uani 1 1 d . . . H27 H 0.3850 1.1162 0.9300 0.028 Uiso 1 1 calc R . . C28 C 0.4208(8) 0.9870(7) 0.9319(7) 0.025(2) Uani 1 1 d . . . H28 H 0.3505 0.9879 0.9666 0.029 Uiso 1 1 calc R . . C29 C 0.5018(8) 0.9099(7) 0.9030(6) 0.019(2) Uani 1 1 d . . . C30 C 0.6027(8) 0.9112(7) 0.8563(7) 0.023(2) Uani 1 1 d . . . H30 H 0.6612 0.8586 0.8375 0.027 Uiso 1 1 calc R . . C31 C 0.6197(9) 0.9907(7) 0.8359(8) 0.029(3) Uani 1 1 d . . . H31 H 0.6899 0.9907 0.8022 0.035 Uiso 1 1 calc R . . C32 C 0.4846(8) 0.8255(7) 0.9230(6) 0.019(2) Uani 1 1 d . . . H32A H 0.5554 0.7776 0.9030 0.023 Uiso 1 1 calc R . . H32B H 0.4549 0.8146 0.9838 0.023 Uiso 1 1 calc R . . C33 C 0.3012(8) 0.8517(7) 0.9183(6) 0.019(2) Uani 1 1 d . . . H33 H 0.2556 0.8773 0.9690 0.023 Uiso 1 1 calc R . . C34 C 0.2697(8) 0.8348(7) 0.8621(6) 0.019(2) Uani 1 1 d . . . C35 C 0.1586(8) 0.8454(8) 0.8674(7) 0.027(2) Uani 1 1 d . . . H35A H 0.1586 0.7880 0.8638 0.033 Uiso 1 1 calc R . . H35B H 0.1402 0.8853 0.8201 0.033 Uiso 1 1 calc R . . C36 C 0.0720(9) 0.8826(9) 0.9489(8) 0.031(3) Uani 1 1 d . . . H36A H 0.0970 0.8486 0.9957 0.038 Uiso 1 1 calc R . . H36B H 0.0634 0.9440 0.9481 0.038 Uiso 1 1 calc R . . C37 C -0.0375(9) 0.8796(10) 0.9624(8) 0.037(3) Uani 1 1 d . . . H37A H -0.0928 0.9132 1.0099 0.045 Uiso 1 1 calc R . . H37B H -0.0587 0.9083 0.9128 0.045 Uiso 1 1 calc R . . C38 C -0.0369(12) 0.7872(11) 0.9788(9) 0.047(4) Uani 1 1 d . . . H38A H -0.0045 0.7553 1.0225 0.057 Uiso 1 1 calc R . . H38B H 0.0091 0.7565 0.9280 0.057 Uiso 1 1 calc R . . C39 C -0.1512(13) 0.7856(15) 1.0060(12) 0.067(5) Uani 1 1 d . . . H39A H -0.1935 0.8073 1.0608 0.101 Uiso 1 1 calc R . . H39B H -0.1460 0.7256 1.0082 0.101 Uiso 1 1 calc R . . H39C H -0.1870 0.8230 0.9662 0.101 Uiso 1 1 calc R . . C40 C 0.5002(8) 0.6181(7) 0.9807(6) 0.0189(19) Uani 1 1 d . . . H40 H 0.5658 0.6154 0.9837 0.023 Uiso 1 1 calc R . . C41 C 0.5059(8) 0.5888(6) 0.9119(6) 0.019(2) Uani 1 1 d . . . H41 H 0.5735 0.5665 0.8695 0.022 Uiso 1 1 calc R . . C42 C 0.4113(8) 0.5925(6) 0.9059(6) 0.0172(19) Uani 1 1 d . . . C43 C 0.3168(9) 0.6243(8) 0.9700(7) 0.027(2) Uani 1 1 d . . . H43 H 0.2505 0.6271 0.9682 0.032 Uiso 1 1 calc R . . C44 C 0.3173(8) 0.6520(7) 1.0368(7) 0.024(2) Uani 1 1 d . . . H44 H 0.2503 0.6735 1.0800 0.029 Uiso 1 1 calc R . . C45 C 0.4208(9) 0.5601(7) 0.8310(7) 0.024(2) Uani 1 1 d . . . H45A H 0.4717 0.5808 0.7821 0.029 Uiso 1 1 calc R . . H45B H 0.4522 0.4954 0.8363 0.029 Uiso 1 1 calc R . . C46 C 0.2436(9) 0.5523(7) 0.8475(7) 0.025(2) Uani 1 1 d . . . H46 H 0.2443 0.5034 0.8874 0.030 Uiso 1 1 calc R . . C47 C 0.1657(9) 0.5987(7) 0.8109(7) 0.022(2) Uani 1 1 d . . . C48 C 0.0663(13) 0.5851(10) 0.8204(9) 0.044(4) Uani 1 1 d . . . H48A H 0.0664 0.5803 0.7656 0.052 Uiso 1 1 calc R . . H48B H 0.0010 0.6354 0.8452 0.052 Uiso 1 1 calc R . . C49 C 0.0641(16) 0.4992(13) 0.8775(11) 0.064(5) Uani 1 1 d . . . H49A H 0.1366 0.4528 0.8583 0.077 Uiso 1 1 calc R . . H49B H 0.0514 0.5093 0.9343 0.077 Uiso 1 1 calc R . . C50 C -0.0192(15) 0.4661(13) 0.8813(12) 0.064(5) Uani 1 1 d . . . H50A H -0.0907 0.5147 0.8923 0.077 Uiso 1 1 calc R . . H50B H -0.0251 0.4204 0.9280 0.077 Uiso 1 1 calc R . . C51 C 0.0074(18) 0.4281(15) 0.8019(13) 0.075(6) Uani 1 1 d . . . H51A H 0.0064 0.4747 0.7557 0.090 Uiso 1 1 calc R . . H51B H 0.0810 0.3822 0.7880 0.090 Uiso 1 1 calc R . . C52 C -0.0740(18) 0.3897(14) 0.8129(15) 0.078(6) Uani 1 1 d . . . H52A H -0.0654 0.3381 0.8528 0.116 Uiso 1 1 calc R . . H52B H -0.0625 0.3728 0.7597 0.116 Uiso 1 1 calc R . . H52C H -0.1474 0.4332 0.8333 0.116 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 0.0113(5) 0.0250(6) 0.0226(6) -0.0042(5) -0.0047(5) -0.0057(5) Cu2 0.0139(5) 0.0222(6) 0.0213(6) 0.0002(5) -0.0063(5) -0.0089(5) Cu3 0.0142(5) 0.0255(6) 0.0194(6) -0.0050(5) -0.0053(5) -0.0081(5) Cu4 0.0144(6) 0.0292(7) 0.0207(6) -0.0006(5) -0.0074(5) -0.0091(5) Cu5 0.0218(6) 0.0232(6) 0.0169(6) -0.0032(5) -0.0058(5) -0.0100(5) Cu6 0.0196(6) 0.0188(6) 0.0235(6) -0.0012(5) -0.0037(5) -0.0099(5) Cu7 0.0188(6) 0.0195(6) 0.0225(6) 0.0010(5) -0.0105(5) -0.0049(5) Cu8 0.0151(6) 0.0260(7) 0.0171(6) -0.0042(5) -0.0029(5) -0.0065(5) I1 0.0152(3) 0.0360(4) 0.0255(4) -0.0136(3) -0.0052(3) -0.0065(3) I2 0.0161(3) 0.0232(3) 0.0295(4) 0.0047(3) -0.0099(3) -0.0070(3) I3 0.0141(3) 0.0333(4) 0.0303(4) -0.0149(3) -0.0008(3) -0.0109(3) I4 0.0226(3) 0.0261(3) 0.0197(3) 0.0048(3) -0.0113(3) -0.0141(3) I5 0.0139(3) 0.0192(3) 0.0219(3) -0.0029(2) -0.0031(2) -0.0055(2) I6 0.0160(3) 0.0214(3) 0.0165(3) -0.0006(2) -0.0062(2) -0.0047(2) I7 0.0161(3) 0.0210(3) 0.0165(3) -0.0003(2) -0.0043(2) -0.0088(2) I8 0.0155(3) 0.0246(3) 0.0196(3) -0.0058(2) -0.0048(2) -0.0077(2) N1 0.022(4) 0.017(4) 0.015(4) 0.003(3) -0.005(3) -0.007(3) N2 0.012(4) 0.018(4) 0.020(4) -0.001(3) -0.003(3) -0.004(3) N3 0.015(4) 0.025(4) 0.012(4) -0.002(3) -0.006(3) -0.006(3) N4 0.010(4) 0.024(4) 0.020(4) 0.000(3) -0.006(3) -0.007(3) N5 0.017(4) 0.020(4) 0.024(4) -0.005(3) -0.007(3) -0.008(3) N6 0.014(4) 0.018(4) 0.021(4) -0.003(3) -0.005(3) -0.005(3) N7 0.019(4) 0.016(4) 0.018(4) -0.004(3) -0.002(3) -0.007(3) N8 0.012(4) 0.018(4) 0.019(4) 0.000(3) -0.007(3) -0.004(3) N9 0.023(4) 0.022(4) 0.024(5) -0.001(4) -0.009(4) -0.011(4) N10 0.019(4) 0.021(4) 0.013(4) 0.000(3) -0.008(3) -0.009(3) N11 0.018(4) 0.015(4) 0.012(4) 0.000(3) -0.005(3) -0.009(3) N12 0.010(3) 0.022(4) 0.015(4) -0.002(3) -0.002(3) -0.009(3) N13 0.018(4) 0.019(4) 0.022(4) 0.000(3) -0.001(3) -0.010(3) N14 0.019(4) 0.014(4) 0.019(4) 0.001(3) -0.008(3) -0.004(3) N15 0.016(4) 0.015(4) 0.016(4) -0.005(3) -0.005(3) -0.004(3) N16 0.019(4) 0.021(4) 0.021(4) -0.005(3) -0.010(3) -0.008(3) C1 0.019(5) 0.018(5) 0.021(5) -0.006(4) -0.009(4) -0.003(4) C2 0.018(5) 0.015(5) 0.021(5) -0.003(4) -0.004(4) -0.005(4) C3 0.010(4) 0.021(5) 0.014(4) -0.005(4) 0.002(3) -0.003(4) C4 0.014(5) 0.036(6) 0.031(6) 0.007(5) -0.010(4) -0.016(4) C5 0.026(6) 0.036(7) 0.038(7) 0.008(5) -0.014(5) -0.021(5) C6 0.009(4) 0.026(5) 0.021(5) -0.001(4) -0.005(4) -0.006(4) C7 0.020(5) 0.027(5) 0.020(5) -0.010(4) -0.010(4) -0.002(4) C8 0.019(5) 0.028(6) 0.023(5) -0.007(4) -0.004(4) -0.010(4) C9 0.020(5) 0.043(7) 0.031(6) -0.013(5) -0.010(5) -0.008(5) C10 0.027(6) 0.051(8) 0.034(7) -0.016(6) -0.007(5) -0.012(6) C11 0.034(7) 0.074(10) 0.044(8) -0.002(7) -0.017(6) -0.032(7) C12 0.075(11) 0.074(11) 0.062(10) 0.031(9) -0.055(9) -0.051(10) C13 0.076(12) 0.078(12) 0.075(12) 0.031(10) -0.056(11) -0.048(10) C14 0.010(4) 0.021(5) 0.023(5) 0.003(4) -0.009(4) -0.009(4) C15 0.018(5) 0.025(5) 0.011(4) 0.002(4) -0.005(4) -0.011(4) C16 0.017(5) 0.018(5) 0.020(5) 0.002(4) -0.003(4) -0.013(4) C17 0.018(5) 0.039(6) 0.020(5) 0.000(5) -0.006(4) -0.013(5) C18 0.015(5) 0.056(8) 0.020(5) -0.010(5) -0.008(4) -0.011(5) C19 0.013(4) 0.019(5) 0.019(5) -0.004(4) 0.001(4) -0.009(4) C20 0.013(4) 0.021(5) 0.023(5) 0.002(4) -0.008(4) -0.006(4) C21 0.017(5) 0.019(5) 0.020(5) -0.003(4) -0.007(4) -0.004(4) C22 0.017(5) 0.025(5) 0.022(5) 0.000(4) -0.008(4) -0.007(4) C23 0.012(4) 0.030(6) 0.028(6) -0.002(4) -0.007(4) -0.004(4) C24 0.019(5) 0.034(6) 0.031(6) -0.006(5) -0.011(5) -0.006(5) C25 0.022(6) 0.049(8) 0.034(7) -0.010(6) -0.012(5) -0.006(5) C26 0.020(5) 0.049(8) 0.033(7) -0.013(6) -0.007(5) -0.002(5) C27 0.016(5) 0.019(5) 0.024(5) 0.000(4) 0.004(4) -0.007(4) C28 0.016(5) 0.031(6) 0.025(5) -0.004(4) -0.002(4) -0.011(4) C29 0.023(5) 0.022(5) 0.013(4) 0.004(4) -0.010(4) -0.009(4) C30 0.016(5) 0.021(5) 0.028(6) -0.005(4) -0.002(4) -0.008(4) C31 0.020(5) 0.024(6) 0.041(7) -0.011(5) -0.002(5) -0.008(4) C32 0.024(5) 0.024(5) 0.017(5) 0.004(4) -0.014(4) -0.012(4) C33 0.017(5) 0.022(5) 0.019(5) -0.008(4) -0.005(4) -0.005(4) C34 0.015(4) 0.026(5) 0.017(5) -0.004(4) -0.002(4) -0.011(4) C35 0.014(5) 0.040(7) 0.026(6) -0.016(5) -0.002(4) -0.006(4) C36 0.017(5) 0.046(7) 0.033(6) -0.024(6) -0.001(5) -0.009(5) C37 0.016(5) 0.062(9) 0.030(6) -0.024(6) 0.001(5) -0.008(5) C38 0.041(8) 0.073(11) 0.030(7) -0.004(7) -0.002(6) -0.032(8) C39 0.038(8) 0.118(16) 0.061(11) -0.020(11) -0.002(8) -0.048(10) C40 0.019(5) 0.020(5) 0.017(5) 0.001(4) -0.007(4) -0.008(4) C41 0.018(5) 0.016(5) 0.014(5) -0.002(4) 0.002(4) -0.005(4) C42 0.025(5) 0.012(4) 0.012(4) 0.003(3) -0.008(4) -0.004(4) C43 0.017(5) 0.037(6) 0.028(6) -0.013(5) -0.007(4) -0.006(4) C44 0.014(5) 0.033(6) 0.024(5) -0.008(4) -0.001(4) -0.009(4) C45 0.022(5) 0.022(5) 0.026(5) -0.003(4) -0.015(4) 0.000(4) C46 0.029(6) 0.023(5) 0.027(6) 0.004(4) -0.013(5) -0.015(5) C47 0.031(6) 0.026(5) 0.019(5) 0.003(4) -0.010(4) -0.020(5) C48 0.061(9) 0.064(9) 0.040(7) 0.016(7) -0.034(7) -0.049(8) C49 0.081(13) 0.089(13) 0.051(10) 0.013(9) -0.022(9) -0.068(12) C50 0.061(11) 0.079(13) 0.071(12) 0.015(10) -0.033(9) -0.044(10) C51 0.090(15) 0.086(14) 0.071(13) -0.024(11) -0.015(11) -0.054(12) C52 0.078(14) 0.076(14) 0.092(16) -0.013(12) -0.016(12) -0.049(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 2.041(8) . ? Cu1 N7 2.089(9) . ? Cu1 I1 2.6228(14) . ? Cu1 I2 2.6486(15) . ? Cu2 N8 2.050(8) . ? Cu2 N11 2.059(8) . ? Cu2 I2 2.6034(14) . ? Cu2 I3 2.6289(14) . ? Cu3 N12 2.048(8) . ? Cu3 N15 2.098(8) . ? Cu3 I4 2.5996(14) . ? Cu3 I3 2.6091(14) . ? Cu4 N16 2.034(9) . ? Cu4 N3 2.094(8) 1_455 ? Cu4 I1 2.6046(14) 1_455 ? Cu4 I4 2.6555(14) . ? Cu5 N13 2.011(9) . ? Cu5 Cu6 2.5768(18) . ? Cu5 Cu7 2.6031(18) . ? Cu5 I7 2.6800(14) . ? Cu5 I5 2.6933(15) . ? Cu5 I6 2.7104(15) . ? Cu5 Cu8 2.8342(18) . ? Cu6 N9 2.012(9) 2_677 ? Cu6 Cu8 2.6333(18) . ? Cu6 I5 2.6482(14) . ? Cu6 I8 2.6755(15) . ? Cu6 Cu7 2.7099(18) . ? Cu6 I6 2.7113(15) . ? Cu7 N1 2.024(9) 2_767 ? Cu7 Cu8 2.6180(18) . ? Cu7 I8 2.6740(15) . ? Cu7 I7 2.6987(14) . ? Cu7 I5 2.7311(15) . ? Cu8 N5 2.022(9) 1_456 ? Cu8 I6 2.6820(15) . ? Cu8 I7 2.6861(15) . ? Cu8 I8 2.7158(14) . ? I1 Cu4 2.6047(14) 1_655 ? N1 C1 1.341(13) . ? N1 C5 1.367(14) . ? N1 Cu7 2.024(9) 2_767 ? N2 N3 1.330(12) . ? N2 C7 1.362(13) . ? N2 C6 1.449(12) . ? N3 N4 1.331(11) . ? N3 Cu4 2.094(8) 1_655 ? N4 C8 1.357(14) . ? N5 C14 1.333(13) . ? N5 C18 1.352(13) . ? N5 Cu8 2.022(9) 1_654 ? N6 N7 1.330(12) . ? N6 C20 1.359(12) . ? N6 C19 1.454(12) . ? N7 N8 1.328(11) . ? N8 C21 1.352(13) . ? N9 C31 1.340(14) . ? N9 C27 1.349(13) . ? N9 Cu6 2.012(9) 2_677 ? N10 N11 1.352(11) . ? N10 C33 1.357(13) . ? N10 C32 1.457(12) . ? N11 N12 1.337(11) . ? N12 C34 1.361(12) . ? N13 C44 1.347(13) . ? N13 C40 1.359(13) . ? N14 C46 1.309(14) . ? N14 N15 1.354(12) . ? N14 C45 1.478(13) . ? N15 N16 1.332(11) . ? N16 C47 1.354(13) . ? C1 C2 1.398(14) . ? C2 C3 1.386(14) . ? C3 C4 1.390(15) . ? C3 C6 1.501(14) . ? C4 C5 1.370(16) . ? C7 C8 1.374(14) . ? C8 C9 1.488(15) . ? C9 C10 1.548(17) . ? C10 C11 1.517(17) . ? C11 C12 1.53(2) . ? C12 C13 1.54(2) . ? C14 C15 1.375(14) . ? C15 C16 1.397(14) . ? C16 C17 1.381(15) . ? C16 C19 1.508(13) . ? C17 C18 1.400(15) . ? C20 C21 1.379(14) . ? C21 C22 1.489(13) . ? C22 C23 1.547(15) . ? C23 C24 1.517(14) . ? C24 C25 1.521(17) . ? C25 C26 1.533(16) . ? C27 C28 1.387(15) . ? C28 C29 1.376(15) . ? C29 C30 1.367(14) . ? C29 C32 1.488(14) . ? C30 C31 1.407(15) . ? C33 C34 1.369(14) . ? C34 C35 1.503(14) . ? C35 C36 1.544(15) . ? C36 C37 1.523(16) . ? C37 C38 1.52(2) . ? C38 C39 1.534(19) . ? C40 C41 1.382(14) . ? C41 C42 1.385(14) . ? C42 C43 1.372(14) . ? C42 C45 1.489(14) . ? C43 C44 1.376(15) . ? C46 C47 1.374(15) . ? C47 C48 1.485(15) . ? C48 C49 1.57(2) . ? C49 C50 1.50(2) . ? C50 C51 1.53(3) . ? C51 C52 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N7 116.6(3) . . ? N4 Cu1 I1 102.0(2) . . ? N7 Cu1 I1 112.2(2) . . ? N4 Cu1 I2 106.2(2) . . ? N7 Cu1 I2 101.9(2) . . ? I1 Cu1 I2 118.42(5) . . ? N8 Cu2 N11 111.8(3) . . ? N8 Cu2 I2 104.8(2) . . ? N11 Cu2 I2 117.4(2) . . ? N8 Cu2 I3 107.0(2) . . ? N11 Cu2 I3 100.4(2) . . ? I2 Cu2 I3 115.28(5) . . ? N12 Cu3 N15 102.8(3) . . ? N12 Cu3 I4 118.0(2) . . ? N15 Cu3 I4 99.1(2) . . ? N12 Cu3 I3 102.5(2) . . ? N15 Cu3 I3 116.7(2) . . ? I4 Cu3 I3 117.46(5) . . ? N16 Cu4 N3 112.0(3) . 1_455 ? N16 Cu4 I1 114.3(2) . 1_455 ? N3 Cu4 I1 100.2(2) 1_455 1_455 ? N16 Cu4 I4 101.5(2) . . ? N3 Cu4 I4 115.8(2) 1_455 . ? I1 Cu4 I4 113.59(5) 1_455 . ? N13 Cu5 Cu6 144.1(2) . . ? N13 Cu5 Cu7 141.9(3) . . ? Cu6 Cu5 Cu7 63.09(5) . . ? N13 Cu5 I7 105.4(2) . . ? Cu6 Cu5 I7 110.48(5) . . ? Cu7 Cu5 I7 61.42(4) . . ? N13 Cu5 I5 104.0(2) . . ? Cu6 Cu5 I5 60.28(4) . . ? Cu7 Cu5 I5 62.05(4) . . ? I7 Cu5 I5 118.52(5) . . ? N13 Cu5 I6 108.3(3) . . ? Cu6 Cu5 I6 61.64(4) . . ? Cu7 Cu5 I6 109.60(5) . . ? I7 Cu5 I6 103.11(5) . . ? I5 Cu5 I6 116.77(5) . . ? N13 Cu5 Cu8 149.3(2) . . ? Cu6 Cu5 Cu8 58.01(5) . . ? Cu7 Cu5 Cu8 57.38(5) . . ? I7 Cu5 Cu8 58.22(4) . . ? I5 Cu5 Cu8 106.70(5) . . ? I6 Cu5 Cu8 57.80(4) . . ? N9 Cu6 Cu5 144.0(3) 2_677 . ? N9 Cu6 Cu8 136.3(3) 2_677 . ? Cu5 Cu6 Cu8 65.90(5) . . ? N9 Cu6 I5 109.3(3) 2_677 . ? Cu5 Cu6 I5 62.04(4) . . ? Cu8 Cu6 I5 114.24(6) . . ? N9 Cu6 I8 102.9(3) 2_677 . ? Cu5 Cu6 I8 113.03(6) . . ? Cu8 Cu6 I8 61.53(4) . . ? I5 Cu6 I8 106.88(5) . . ? N9 Cu6 Cu7 151.4(3) 2_677 . ? Cu5 Cu6 Cu7 58.93(5) . . ? Cu8 Cu6 Cu7 58.66(5) . . ? I5 Cu6 Cu7 61.28(4) . . ? I8 Cu6 Cu7 59.54(4) . . ? N9 Cu6 I6 101.6(3) 2_677 . ? Cu5 Cu6 I6 61.60(4) . . ? Cu8 Cu6 I6 60.22(4) . . ? I5 Cu6 I6 118.32(5) . . ? I8 Cu6 I6 116.39(5) . . ? Cu7 Cu6 I6 106.45(5) . . ? N1 Cu7 Cu5 144.4(3) 2_767 . ? N1 Cu7 Cu8 139.2(3) 2_767 . ? Cu5 Cu7 Cu8 65.75(5) . . ? N1 Cu7 I8 103.3(3) 2_767 . ? Cu5 Cu7 I8 112.23(5) . . ? Cu8 Cu7 I8 61.74(4) . . ? N1 Cu7 I7 104.9(3) 2_767 . ? Cu5 Cu7 I7 60.69(4) . . ? Cu8 Cu7 I7 60.67(4) . . ? I8 Cu7 I7 117.93(5) . . ? N1 Cu7 Cu6 149.0(3) 2_767 . ? Cu5 Cu7 Cu6 57.98(5) . . ? Cu8 Cu7 Cu6 59.21(5) . . ? I8 Cu7 Cu6 59.59(4) . . ? I7 Cu7 Cu6 105.98(5) . . ? N1 Cu7 I5 108.5(2) 2_767 . ? Cu5 Cu7 I5 60.60(4) . . ? Cu8 Cu7 I5 112.02(5) . . ? I8 Cu7 I5 104.58(5) . . ? I7 Cu7 I5 116.54(5) . . ? Cu6 Cu7 I5 58.25(4) . . ? N5 Cu8 Cu7 143.6(3) 1_456 . ? N5 Cu8 Cu6 140.3(2) 1_456 . ? Cu7 Cu8 Cu6 62.13(5) . . ? N5 Cu8 I6 106.3(3) 1_456 . ? Cu7 Cu8 I6 110.03(5) . . ? Cu6 Cu8 I6 61.33(4) . . ? N5 Cu8 I7 111.1(2) 1_456 . ? Cu7 Cu8 I7 61.15(4) . . ? Cu6 Cu8 I7 108.57(5) . . ? I6 Cu8 I7 103.71(5) . . ? N5 Cu8 I8 102.4(2) 1_456 . ? Cu7 Cu8 I8 60.14(4) . . ? Cu6 Cu8 I8 60.00(4) . . ? I6 Cu8 I8 116.02(5) . . ? I7 Cu8 I8 116.91(5) . . ? N5 Cu8 Cu5 153.2(2) 1_456 . ? Cu7 Cu8 Cu5 56.87(5) . . ? Cu6 Cu8 Cu5 56.09(5) . . ? I6 Cu8 Cu5 58.78(4) . . ? I7 Cu8 Cu5 58.01(4) . . ? I8 Cu8 Cu5 104.23(5) . . ? Cu4 I1 Cu1 88.43(4) 1_655 . ? Cu2 I2 Cu1 86.42(4) . . ? Cu3 I3 Cu2 87.47(4) . . ? Cu3 I4 Cu4 89.28(4) . . ? Cu6 I5 Cu5 57.68(4) . . ? Cu6 I5 Cu7 60.48(4) . . ? Cu5 I5 Cu7 57.35(4) . . ? Cu8 I6 Cu5 63.41(4) . . ? Cu8 I6 Cu6 58.45(4) . . ? Cu5 I6 Cu6 56.76(4) . . ? Cu5 I7 Cu8 63.76(4) . . ? Cu5 I7 Cu7 57.89(4) . . ? Cu8 I7 Cu7 58.18(4) . . ? Cu7 I8 Cu6 60.87(4) . . ? Cu7 I8 Cu8 58.11(4) . . ? Cu6 I8 Cu8 58.47(4) . . ? C1 N1 C5 116.3(9) . . ? C1 N1 Cu7 122.7(7) . 2_767 ? C5 N1 Cu7 120.7(7) . 2_767 ? N3 N2 C7 110.3(8) . . ? N3 N2 C6 121.9(8) . . ? C7 N2 C6 127.5(9) . . ? N2 N3 N4 107.4(8) . . ? N2 N3 Cu4 127.6(6) . 1_655 ? N4 N3 Cu4 125.0(6) . 1_655 ? N3 N4 C8 109.4(8) . . ? N3 N4 Cu1 123.0(7) . . ? C8 N4 Cu1 127.5(7) . . ? C14 N5 C18 117.0(9) . . ? C14 N5 Cu8 120.2(6) . 1_654 ? C18 N5 Cu8 122.7(7) . 1_654 ? N7 N6 C20 110.3(8) . . ? N7 N6 C19 123.1(8) . . ? C20 N6 C19 126.4(9) . . ? N8 N7 N6 107.5(8) . . ? N8 N7 Cu1 124.5(6) . . ? N6 N7 Cu1 127.9(6) . . ? N7 N8 C21 109.3(8) . . ? N7 N8 Cu2 121.8(6) . . ? C21 N8 Cu2 128.8(7) . . ? C31 N9 C27 116.8(9) . . ? C31 N9 Cu6 117.9(7) . 2_677 ? C27 N9 Cu6 125.1(7) . 2_677 ? N11 N10 C33 110.6(8) . . ? N11 N10 C32 121.8(8) . . ? C33 N10 C32 127.6(8) . . ? N12 N11 N10 106.4(7) . . ? N12 N11 Cu2 124.3(6) . . ? N10 N11 Cu2 129.1(6) . . ? N11 N12 C34 109.4(8) . . ? N11 N12 Cu3 122.4(6) . . ? C34 N12 Cu3 127.6(6) . . ? C44 N13 C40 114.9(9) . . ? C44 N13 Cu5 119.6(7) . . ? C40 N13 Cu5 125.3(7) . . ? C46 N14 N15 111.5(9) . . ? C46 N14 C45 128.6(9) . . ? N15 N14 C45 119.8(8) . . ? N16 N15 N14 105.3(8) . . ? N16 N15 Cu3 127.4(6) . . ? N14 N15 Cu3 127.2(6) . . ? N15 N16 C47 110.1(8) . . ? N15 N16 Cu4 122.1(7) . . ? C47 N16 Cu4 127.8(7) . . ? N1 C1 C2 123.8(9) . . ? C3 C2 C1 118.5(9) . . ? C2 C3 C4 118.4(9) . . ? C2 C3 C6 117.2(9) . . ? C4 C3 C6 124.3(9) . . ? C5 C4 C3 119.6(10) . . ? N1 C5 C4 123.3(10) . . ? N2 C6 C3 112.8(8) . . ? N2 C7 C8 105.6(9) . . ? N4 C8 C7 107.3(9) . . ? N4 C8 C9 122.3(9) . . ? C7 C8 C9 130.2(10) . . ? C8 C9 C10 112.5(10) . . ? C11 C10 C9 113.9(11) . . ? C10 C11 C12 112.1(12) . . ? C11 C12 C13 112.4(14) . . ? N5 C14 C15 124.7(9) . . ? C14 C15 C16 118.5(9) . . ? C17 C16 C15 117.9(9) . . ? C17 C16 C19 123.5(9) . . ? C15 C16 C19 118.5(9) . . ? C16 C17 C18 119.8(10) . . ? N5 C18 C17 122.0(10) . . ? N6 C19 C16 113.7(8) . . ? N6 C20 C21 105.3(9) . . ? N8 C21 C20 107.5(9) . . ? N8 C21 C22 123.3(9) . . ? C20 C21 C22 128.8(9) . . ? C21 C22 C23 111.2(9) . . ? C24 C23 C22 112.9(9) . . ? C23 C24 C25 112.0(9) . . ? C24 C25 C26 113.8(10) . . ? N9 C27 C28 123.3(10) . . ? C29 C28 C27 119.6(10) . . ? C30 C29 C28 118.0(10) . . ? C30 C29 C32 119.3(10) . . ? C28 C29 C32 122.7(10) . . ? C29 C30 C31 119.9(10) . . ? N9 C31 C30 122.4(10) . . ? N10 C32 C29 113.0(8) . . ? N10 C33 C34 105.5(8) . . ? N12 C34 C33 108.0(8) . . ? N12 C34 C35 122.5(9) . . ? C33 C34 C35 129.4(9) . . ? C34 C35 C36 111.4(9) . . ? C37 C36 C35 112.3(9) . . ? C38 C37 C36 113.0(11) . . ? C37 C38 C39 112.3(14) . . ? N13 C40 C41 124.5(9) . . ? C40 C41 C42 118.8(9) . . ? C43 C42 C41 117.5(9) . . ? C43 C42 C45 125.2(10) . . ? C41 C42 C45 117.3(9) . . ? C42 C43 C44 120.5(10) . . ? N13 C44 C43 123.8(10) . . ? N14 C45 C42 114.0(9) . . ? N14 C46 C47 106.7(9) . . ? N16 C47 C46 106.4(9) . . ? N16 C47 C48 123.4(10) . . ? C46 C47 C48 130.2(10) . . ? C47 C48 C49 108.6(12) . . ? C50 C49 C48 115.9(15) . . ? C49 C50 C51 113.1(16) . . ? C52 C51 C50 109.9(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.845 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.302 #===END data_8621 _database_code_depnum_ccdc_archive 'CCDC 738741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H17 Cu2 I2 N6 O0.50' _chemical_formula_weight 658.22 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9089(4) _cell_length_b 16.0244(8) _cell_length_c 13.7163(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.8060(10) _cell_angle_gamma 90.00 _cell_volume 1901.56(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5154 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.44 _exptl_crystal_description BLOCK _exptl_crystal_colour PALE _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 5.496 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4061 _exptl_absorpt_correction_T_max 0.6095 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13298 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4364 _reflns_number_gt 3928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.5153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4364 _refine_ls_number_parameters 234 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.23384(5) 0.50210(3) 0.19538(3) 0.01509(10) Uani 1 1 d . . . Cu2 Cu -0.03609(5) 0.54266(3) 0.07823(3) 0.01757(10) Uani 1 1 d . . . I1 I -0.22755(2) 0.427901(13) -0.018920(15) 0.01454(7) Uani 1 1 d . . . I2 I 0.00725(2) 0.524449(14) 0.278158(16) 0.01819(7) Uani 1 1 d . . . N1 N 0.3324(3) 0.38614(17) 0.1981(2) 0.0146(6) Uani 1 1 d . . . N2 N 0.4889(3) 0.37885(17) 0.2115(2) 0.0154(6) Uani 1 1 d . . . N3 N 0.4306(3) 0.54737(17) 0.2995(2) 0.0141(5) Uani 1 1 d . . . N4 N 0.4381(3) 0.58603(16) 0.3853(2) 0.0147(6) Uani 1 1 d . . . N5 N 0.5801(3) 0.57132(16) 0.4423(2) 0.0136(6) Uani 1 1 d . . . N6 N 0.8493(3) 0.84606(17) 0.5533(2) 0.0159(6) Uani 1 1 d . . . C1 C 0.2802(4) 0.3086(2) 0.2031(2) 0.0166(7) Uani 1 1 d . . . C2 C 0.4040(4) 0.2523(2) 0.2200(2) 0.0178(7) Uani 1 1 d . . . H2 H 0.3978 0.1934 0.2265 0.021 Uiso 1 1 calc R . . C3 C 0.5359(4) 0.2982(2) 0.2257(2) 0.0177(7) Uani 1 1 d . . . C4 C 0.1130(4) 0.2916(2) 0.1911(3) 0.0205(7) Uani 1 1 d . . . H4A H 0.0754 0.3227 0.2421 0.031 Uiso 1 1 calc R . . H4B H 0.0973 0.2317 0.1993 0.031 Uiso 1 1 calc R . . H4C H 0.0559 0.3092 0.1241 0.031 Uiso 1 1 calc R . . C5 C 0.7018(4) 0.2736(2) 0.2424(3) 0.0292(9) Uani 1 1 d . . . H5A H 0.7389 0.2868 0.1825 0.044 Uiso 1 1 calc R . . H5B H 0.7120 0.2135 0.2557 0.044 Uiso 1 1 calc R . . H5C H 0.7633 0.3042 0.3001 0.044 Uiso 1 1 calc R . . C6 C 0.5826(4) 0.4550(2) 0.2162(3) 0.0162(7) Uani 1 1 d . . . H6A H 0.5486 0.4866 0.1527 0.019 Uiso 1 1 calc R . . H6B H 0.6925 0.4396 0.2241 0.019 Uiso 1 1 calc R . . C7 C 0.5667(4) 0.5084(2) 0.3021(2) 0.0145(7) Uani 1 1 d . . . C8 C 0.6638(4) 0.5239(2) 0.3943(3) 0.0159(7) Uani 1 1 d . . . H8 H 0.7672 0.5053 0.4186 0.019 Uiso 1 1 calc R . . C9 C 0.6254(4) 0.6079(2) 0.5437(2) 0.0174(7) Uani 1 1 d . . . H9A H 0.6974 0.5694 0.5884 0.021 Uiso 1 1 calc R . . H9B H 0.5324 0.6141 0.5707 0.021 Uiso 1 1 calc R . . C10 C 0.9287(4) 0.7744(2) 0.5597(2) 0.0185(7) Uani 1 1 d . . . H10 H 1.0376 0.7770 0.5682 0.022 Uiso 1 1 calc R . . C11 C 0.8594(4) 0.6968(2) 0.5545(3) 0.0189(7) Uani 1 1 d . . . H11 H 0.9196 0.6475 0.5581 0.023 Uiso 1 1 calc R . . C12 C 0.7020(4) 0.6918(2) 0.5441(2) 0.0150(7) Uani 1 1 d . . . C13 C 0.6180(4) 0.7651(2) 0.5359(2) 0.0183(7) Uani 1 1 d . . . H13 H 0.5090 0.7638 0.5269 0.022 Uiso 1 1 calc R . . C14 C 0.6955(4) 0.8404(2) 0.5411(2) 0.0166(7) Uani 1 1 d . . . H14 H 0.6371 0.8905 0.5358 0.020 Uiso 1 1 calc R . . O1W O 0.2143(8) 0.6612(5) 0.4925(6) 0.0518(18) Uani 0.50 1 d PD . . H1WA H 0.124(6) 0.658(8) 0.455(8) 0.078 Uiso 0.50 1 d PD . . H1WB H 0.269(11) 0.646(8) 0.453(7) 0.078 Uiso 0.50 1 d PD . . 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 0.0122(2) 0.0161(2) 0.0164(2) 0.00055(16) 0.00213(16) 0.00122(15) Cu2 0.0163(2) 0.0149(2) 0.0203(2) 0.00076(16) 0.00190(16) 0.00339(16) I1 0.01464(11) 0.01403(11) 0.01508(11) 0.00121(8) 0.00384(8) 0.00006(8) I2 0.01364(11) 0.02422(13) 0.01730(12) 0.00094(8) 0.00489(8) 0.00100(9) N1 0.0096(12) 0.0177(14) 0.0160(13) 0.0010(11) 0.0020(10) 0.0002(11) N2 0.0133(13) 0.0149(13) 0.0175(14) -0.0017(11) 0.0026(11) -0.0006(11) N3 0.0151(14) 0.0129(13) 0.0151(13) -0.0003(11) 0.0051(11) -0.0029(11) N4 0.0153(14) 0.0130(13) 0.0154(13) -0.0010(11) 0.0029(11) -0.0024(11) N5 0.0141(13) 0.0124(13) 0.0138(13) 0.0005(10) 0.0022(10) -0.0028(10) N6 0.0184(14) 0.0156(14) 0.0127(13) 0.0006(11) 0.0018(11) -0.0019(11) C1 0.0217(17) 0.0180(16) 0.0096(15) -0.0022(12) 0.0027(13) -0.0034(14) C2 0.0241(18) 0.0124(15) 0.0157(16) 0.0005(13) 0.0023(13) 0.0028(14) C3 0.0245(18) 0.0143(16) 0.0147(16) -0.0008(13) 0.0052(13) 0.0035(14) C4 0.0233(18) 0.0181(17) 0.0210(17) -0.0004(14) 0.0068(14) -0.0072(14) C5 0.0215(19) 0.027(2) 0.036(2) -0.0026(17) 0.0008(16) 0.0074(16) C6 0.0139(16) 0.0157(16) 0.0205(17) -0.0015(13) 0.0072(13) -0.0027(13) C7 0.0127(15) 0.0139(15) 0.0171(16) 0.0032(13) 0.0038(13) -0.0019(12) C8 0.0138(16) 0.0137(15) 0.0193(17) 0.0012(13) 0.0025(13) -0.0010(12) C9 0.0214(17) 0.0167(16) 0.0139(16) 0.0004(13) 0.0042(13) -0.0067(14) C10 0.0118(15) 0.0216(18) 0.0203(17) 0.0054(14) 0.0001(13) -0.0021(13) C11 0.0202(17) 0.0147(16) 0.0208(17) 0.0032(13) 0.0031(14) -0.0001(14) C12 0.0182(16) 0.0171(16) 0.0084(14) -0.0015(12) 0.0005(12) -0.0047(13) C13 0.0168(16) 0.0235(17) 0.0153(16) -0.0016(14) 0.0053(13) -0.0042(14) C14 0.0161(16) 0.0170(16) 0.0172(16) -0.0021(13) 0.0050(13) 0.0013(13) O1W 0.045(4) 0.063(5) 0.050(4) 0.009(4) 0.019(3) 0.022(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 2.052(3) . ? Cu1 N3 2.108(3) . ? Cu1 I2 2.5664(5) . ? Cu1 Cu2 2.6350(6) . ? Cu1 I1 2.6561(5) 3_565 ? Cu2 N6 2.043(3) 4_475 ? Cu2 I1 2.6424(5) . ? Cu2 I2 2.6924(5) . ? Cu2 I1 2.7042(5) 3_565 ? Cu2 Cu2 2.7472(9) 3_565 ? I1 Cu1 2.6561(5) 3_565 ? I1 Cu2 2.7042(5) 3_565 ? N1 C1 1.335(4) . ? N1 N2 1.367(4) . ? N2 C3 1.358(4) . ? N2 C6 1.471(4) . ? N3 N4 1.318(4) . ? N3 C7 1.356(4) . ? N4 N5 1.340(4) . ? N5 C8 1.342(4) . ? N5 C9 1.474(4) . ? N6 C10 1.341(4) . ? N6 C14 1.344(4) . ? N6 Cu2 2.043(3) 4_676 ? C1 C2 1.400(5) . ? C1 C4 1.484(5) . ? C2 C3 1.374(5) . ? C3 C5 1.494(5) . ? C6 C7 1.491(5) . ? C7 C8 1.373(5) . ? C9 C12 1.507(4) . ? C10 C11 1.382(5) . ? C11 C12 1.377(5) . ? C12 C13 1.383(5) . ? C13 C14 1.383(5) . ? 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 N3 90.93(10) . . ? N1 Cu1 I2 119.77(8) . . ? N3 Cu1 I2 105.48(8) . . ? N1 Cu1 Cu2 123.98(7) . . ? N3 Cu1 Cu2 144.94(8) . . ? I2 Cu1 Cu2 62.331(15) . . ? N1 Cu1 I1 108.37(8) . 3_565 ? N3 Cu1 I1 107.78(8) . 3_565 ? I2 Cu1 I1 119.767(16) . 3_565 ? Cu2 Cu1 I1 61.472(14) . 3_565 ? N6 Cu2 Cu1 131.63(8) 4_475 . ? N6 Cu2 I1 106.65(8) 4_475 . ? Cu1 Cu2 I1 121.415(18) . . ? N6 Cu2 I2 102.09(8) 4_475 . ? Cu1 Cu2 I2 57.586(13) . . ? I1 Cu2 I2 110.891(17) . . ? N6 Cu2 I1 103.45(8) 4_475 3_565 ? Cu1 Cu2 I1 59.648(14) . 3_565 ? I1 Cu2 I1 118.176(17) . 3_565 ? I2 Cu2 I1 113.677(16) . 3_565 ? N6 Cu2 Cu2 120.31(8) 4_475 3_565 ? Cu1 Cu2 Cu2 90.23(2) . 3_565 ? I1 Cu2 Cu2 60.194(16) . 3_565 ? I2 Cu2 Cu2 137.59(2) . 3_565 ? I1 Cu2 Cu2 57.982(16) 3_565 3_565 ? Cu2 I1 Cu1 92.082(14) . 3_565 ? Cu2 I1 Cu2 61.825(17) . 3_565 ? Cu1 I1 Cu2 58.880(13) 3_565 3_565 ? Cu1 I2 Cu2 60.084(13) . . ? C1 N1 N2 105.7(3) . . ? C1 N1 Cu1 133.8(2) . . ? N2 N1 Cu1 119.9(2) . . ? C3 N2 N1 111.7(3) . . ? C3 N2 C6 129.1(3) . . ? N1 N2 C6 119.0(3) . . ? N4 N3 C7 109.7(3) . . ? N4 N3 Cu1 128.6(2) . . ? C7 N3 Cu1 117.0(2) . . ? N3 N4 N5 106.1(3) . . ? N4 N5 C8 111.8(3) . . ? N4 N5 C9 119.2(3) . . ? C8 N5 C9 129.0(3) . . ? C10 N6 C14 117.2(3) . . ? C10 N6 Cu2 120.2(2) . 4_676 ? C14 N6 Cu2 122.3(2) . 4_676 ? N1 C1 C2 109.8(3) . . ? N1 C1 C4 121.2(3) . . ? C2 C1 C4 129.1(3) . . ? C3 C2 C1 107.1(3) . . ? N2 C3 C2 105.7(3) . . ? N2 C3 C5 122.3(3) . . ? C2 C3 C5 132.0(3) . . ? N2 C6 C7 110.6(3) . . ? N3 C7 C8 107.7(3) . . ? N3 C7 C6 119.7(3) . . ? C8 C7 C6 132.3(3) . . ? N5 C8 C7 104.6(3) . . ? N5 C9 C12 112.3(3) . . ? N6 C10 C11 123.0(3) . . ? C12 C11 C10 119.3(3) . . ? C11 C12 C13 118.5(3) . . ? C11 C12 C9 120.1(3) . . ? C13 C12 C9 121.5(3) . . ? C12 C13 C14 118.9(3) . . ? N6 C14 C13 123.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB N4 0.85(2) 2.17(4) 2.998(7) 165(11) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.989 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.137 #===END