# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email JPLANG@SUDA.EDU.CN _publ_section_title ; Assembly of [CunIn]-based Coordination Polymers from Cracking the 3D Framework of Bulk CuI via Flexible N-Heterocyclic Ligands ; loop_ _publ_author_name 'Jian-Ping Lang' 'Yang Chen' 'Ling-Ling Li' 'Hong-Xi Li' 'Dong Liu' ; Zhi-Gang Ren ; 'Yong Zhang' # Attachment 'JPlangCIF__revised_.cif' data_[Cu3I(m-I)(m3-I)(bpe)3]n _database_code_depnum_ccdc_archive 'CCDC 727478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Cu3 I3 N6' _chemical_formula_sum 'C36 H36 Cu3 I3 N6' _chemical_formula_weight 1124.06 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.6669(19) _cell_length_b 28.873(6) _cell_length_c 13.072(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.21(3) _cell_angle_gamma 90.00 _cell_volume 3642.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9779 _cell_measurement_theta_min 3.0402 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 4.314 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35560 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6674 _reflns_number_gt 5178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+71.2602P] 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 6674 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Cu3 Cu 1.22305(14) 0.71237(5) 0.43528(11) 0.0266(3) Uani 1 1 d . . . Cu2 Cu 0.15354(15) 0.46533(5) 0.77926(12) 0.0268(3) Uani 1 1 d . . . Cu1 Cu 0.01011(15) 0.47581(5) 1.12236(12) 0.0289(4) Uani 1 1 d . . . I1 I 0.20149(8) 0.47755(3) 0.98040(6) 0.0267(2) Uani 1 1 d . . . I3 I 1.43714(8) 0.70338(3) 0.56845(6) 0.0277(2) Uani 1 1 d . . . I2 I -0.09103(8) 0.48458(3) 0.69939(6) 0.0298(2) Uani 1 1 d . . . N1 N -0.0241(9) 0.4072(3) 1.1522(7) 0.021(2) Uani 1 1 d . . . N2 N -0.3101(9) 0.1027(3) 1.2437(7) 0.022(2) Uani 1 1 d . . . N5 N 1.1658(9) 0.7804(3) 0.4335(7) 0.025(2) Uani 1 1 d . . . N6 N 0.7687(10) 0.8176(3) 0.8015(7) 0.025(2) Uani 1 1 d . . . N3 N 0.3086(10) 0.5028(3) 0.7130(8) 0.027(2) Uani 1 1 d . . . N4 N 1.0519(9) 0.6786(3) 0.4911(7) 0.022(2) Uani 1 1 d . . . C1 C -0.1112(11) 0.3955(4) 1.2242(8) 0.022(3) Uani 1 1 d . . . H1 H -0.1538 0.4196 1.2606 0.026 Uiso 1 1 calc R . . C2 C -0.1422(11) 0.3505(4) 1.2481(9) 0.027(3) Uani 1 1 d . . . H2 H -0.2055 0.3442 1.2993 0.033 Uiso 1 1 calc R . . C3 C -0.0819(11) 0.3149(4) 1.1983(8) 0.020(2) Uani 1 1 d . . . C4 C 0.0115(12) 0.3253(4) 1.1233(10) 0.030(3) Uani 1 1 d . . . H4 H 0.0570 0.3015 1.0879 0.036 Uiso 1 1 calc R . . C5 C 0.0354(12) 0.3725(4) 1.1023(10) 0.035(3) Uani 1 1 d . . . H5 H 0.0965 0.3801 1.0504 0.042 Uiso 1 1 calc R . . C6 C -0.1136(12) 0.2644(4) 1.2238(10) 0.031(3) Uani 1 1 d . . . H6A H -0.0285 0.2457 1.2179 0.037 Uiso 1 1 calc R . . H6B H -0.1402 0.2625 1.2958 0.037 Uiso 1 1 calc R . . C7 C -0.2270(12) 0.2440(4) 1.1557(10) 0.029(3) Uani 1 1 d . . . H7A H -0.1991 0.2444 1.0839 0.035 Uiso 1 1 calc R . . H7B H -0.3115 0.2631 1.1594 0.035 Uiso 1 1 calc R . . C8 C -0.2592(11) 0.1943(3) 1.1863(8) 0.016(2) Uani 1 1 d . . . C9 C -0.3730(12) 0.1826(4) 1.2397(8) 0.022(3) Uani 1 1 d . . . H9 H -0.4367 0.2059 1.2579 0.027 Uiso 1 1 calc R . . C10 C -0.3941(11) 0.1374(4) 1.2664(9) 0.024(3) Uani 1 1 d . . . H10 H -0.4733 0.1304 1.3034 0.029 Uiso 1 1 calc R . . C11 C -0.1999(12) 0.1141(4) 1.1923(9) 0.027(3) Uani 1 1 d . . . H11 H -0.1372 0.0902 1.1763 0.033 Uiso 1 1 calc R . . C12 C -0.1702(12) 0.1593(4) 1.1602(9) 0.027(3) Uani 1 1 d . . . H12 H -0.0918 0.1656 1.1218 0.032 Uiso 1 1 calc R . . C29 C 1.1822(12) 0.8041(4) 0.5219(9) 0.027(3) Uani 1 1 d . . . H29 H 1.2434 0.7915 0.5741 0.033 Uiso 1 1 calc R . . C28 C 1.1176(12) 0.8448(4) 0.5422(9) 0.027(3) Uani 1 1 d . . . H28 H 1.1349 0.8594 0.6068 0.033 Uiso 1 1 calc R . . C27 C 1.0265(12) 0.8651(4) 0.4690(9) 0.027(3) Uani 1 1 d . . . C26 C 1.0125(12) 0.8423(4) 0.3749(9) 0.027(3) Uani 1 1 d . . . H26 H 0.9561 0.8554 0.3205 0.033 Uiso 1 1 calc R . . C25 C 1.0797(11) 0.8013(4) 0.3608(9) 0.025(3) Uani 1 1 d . . . H25 H 1.0655 0.7863 0.2963 0.030 Uiso 1 1 calc R . . C30 C 0.9416(12) 0.9064(4) 0.4897(10) 0.030(3) Uani 1 1 d . . . H30A H 0.9358 0.9266 0.4285 0.036 Uiso 1 1 calc R . . H30B H 0.9862 0.9242 0.5473 0.036 Uiso 1 1 calc R . . C31 C 0.7965(12) 0.8922(4) 0.5164(9) 0.029(3) Uani 1 1 d . . . H31A H 0.7389 0.9204 0.5197 0.034 Uiso 1 1 calc R . . H31B H 0.7558 0.8727 0.4602 0.034 Uiso 1 1 calc R . . C32 C 0.7881(11) 0.8662(4) 0.6155(9) 0.024(3) Uani 1 1 d . . . C36 C 0.8249(13) 0.8868(4) 0.7095(9) 0.031(3) Uani 1 1 d . . . H36 H 0.8582 0.9178 0.7125 0.037 Uiso 1 1 calc R . . C35 C 0.8121(12) 0.8616(4) 0.7982(9) 0.031(3) Uani 1 1 d . . . H35 H 0.8360 0.8765 0.8616 0.037 Uiso 1 1 calc R . . C34 C 0.7387(12) 0.7975(4) 0.7099(9) 0.026(3) Uani 1 1 d . . . H34 H 0.7087 0.7661 0.7085 0.031 Uiso 1 1 calc R . . C33 C 0.7497(13) 0.8204(5) 0.6183(9) 0.033(3) Uani 1 1 d . . . H33 H 0.7304 0.8042 0.5559 0.039 Uiso 1 1 calc R . . C17 C 0.4313(11) 0.5106(4) 0.7620(9) 0.027(3) Uani 1 1 d . . . H17 H 0.4458 0.4984 0.8292 0.033 Uiso 1 1 calc R . . C16 C 0.5370(11) 0.5348(4) 0.7231(9) 0.026(3) Uani 1 1 d . . . H16 H 0.6210 0.5395 0.7629 0.031 Uiso 1 1 calc R . . C15 C 0.5203(11) 0.5525(4) 0.6232(9) 0.025(3) Uani 1 1 d . . . C14 C 0.3939(11) 0.5436(4) 0.5718(9) 0.026(3) Uani 1 1 d . . . H14 H 0.3770 0.5547 0.5038 0.031 Uiso 1 1 calc R . . C13 C 0.2927(12) 0.5191(4) 0.6174(10) 0.026(3) Uani 1 1 d . . . H13 H 0.2076 0.5136 0.5795 0.032 Uiso 1 1 calc R . . C18 C 0.6344(10) 0.5782(4) 0.5713(8) 0.022(2) Uani 1 1 d . . . H18A H 0.5912 0.5989 0.5183 0.026 Uiso 1 1 calc R . . H18B H 0.6913 0.5553 0.5360 0.026 Uiso 1 1 calc R . . C19 C 0.7296(11) 0.6069(4) 0.6434(8) 0.025(3) Uani 1 1 d . . . H19A H 0.6734 0.6301 0.6784 0.030 Uiso 1 1 calc R . . H19B H 0.7732 0.5863 0.6965 0.030 Uiso 1 1 calc R . . C20 C 0.8398(11) 0.6313(4) 0.5900(8) 0.022(3) Uani 1 1 d . . . C24 C 0.8488(12) 0.6793(4) 0.5901(9) 0.024(3) Uani 1 1 d . . . H24 H 0.7822 0.6973 0.6232 0.029 Uiso 1 1 calc R . . C23 C 0.9565(11) 0.7010(4) 0.5413(8) 0.023(3) Uani 1 1 d . . . H23 H 0.9617 0.7338 0.5442 0.028 Uiso 1 1 calc R . . C21 C 0.9392(11) 0.6081(4) 0.5356(9) 0.023(3) Uani 1 1 d . . . H21 H 0.9369 0.5752 0.5319 0.028 Uiso 1 1 calc R . . C22 C 1.0402(12) 0.6318(4) 0.4871(9) 0.028(3) Uani 1 1 d . . . H22 H 1.1043 0.6148 0.4494 0.034 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 Cu3 0.0257(8) 0.0290(8) 0.0255(8) -0.0023(6) 0.0050(6) -0.0029(6) Cu2 0.0253(8) 0.0204(8) 0.0356(9) -0.0012(6) 0.0086(7) -0.0002(6) Cu1 0.0333(8) 0.0181(8) 0.0360(9) -0.0012(6) 0.0089(7) -0.0007(6) I1 0.0272(4) 0.0252(4) 0.0284(4) 0.0026(3) 0.0080(3) 0.0017(3) I3 0.0238(4) 0.0337(5) 0.0255(4) -0.0003(3) 0.0012(3) 0.0043(3) I2 0.0254(4) 0.0267(4) 0.0373(5) -0.0037(3) 0.0010(3) 0.0015(3) N1 0.022(5) 0.015(5) 0.026(5) -0.007(4) 0.002(4) 0.008(4) N2 0.019(5) 0.027(5) 0.019(5) 0.001(4) 0.002(4) -0.001(4) N5 0.020(5) 0.025(5) 0.029(6) 0.008(4) -0.003(4) -0.001(4) N6 0.025(5) 0.027(6) 0.024(6) 0.002(4) 0.005(4) 0.006(4) N3 0.023(5) 0.020(5) 0.038(6) -0.003(4) 0.005(5) 0.003(4) N4 0.014(5) 0.029(6) 0.023(5) 0.006(4) -0.002(4) -0.003(4) C1 0.020(6) 0.035(7) 0.010(6) -0.002(5) -0.003(5) -0.006(5) C2 0.017(6) 0.028(7) 0.038(7) 0.001(5) 0.004(5) -0.019(5) C3 0.021(6) 0.014(6) 0.024(6) -0.004(5) -0.007(5) -0.007(4) C4 0.032(7) 0.012(6) 0.046(8) 0.000(5) 0.005(6) -0.003(5) C5 0.020(6) 0.042(8) 0.043(8) -0.007(6) 0.010(6) -0.003(5) C6 0.019(6) 0.033(7) 0.040(8) 0.005(6) -0.007(5) -0.008(5) C7 0.030(7) 0.016(6) 0.040(8) 0.007(5) -0.011(6) -0.004(5) C8 0.025(6) 0.010(5) 0.012(5) 0.004(4) -0.011(5) -0.003(4) C9 0.032(7) 0.013(6) 0.023(6) -0.002(5) 0.002(5) 0.001(5) C10 0.013(6) 0.030(7) 0.031(7) -0.004(5) 0.002(5) 0.002(5) C11 0.025(6) 0.028(7) 0.029(7) -0.009(5) -0.001(5) 0.005(5) C12 0.029(7) 0.026(7) 0.027(7) -0.001(5) 0.012(5) -0.008(5) C29 0.025(6) 0.034(7) 0.022(6) -0.001(5) -0.002(5) -0.001(5) C28 0.033(7) 0.026(7) 0.023(6) -0.006(5) -0.004(5) 0.000(5) C27 0.024(6) 0.024(6) 0.033(7) 0.010(5) 0.015(5) -0.007(5) C26 0.023(6) 0.036(7) 0.022(6) 0.000(5) -0.001(5) 0.002(5) C25 0.023(6) 0.026(7) 0.026(7) 0.001(5) -0.006(5) -0.005(5) C30 0.040(7) 0.018(6) 0.033(7) 0.005(5) 0.005(6) -0.005(5) C31 0.036(7) 0.023(6) 0.027(7) 0.004(5) 0.000(6) 0.008(5) C32 0.025(6) 0.024(7) 0.023(6) 0.006(5) 0.003(5) 0.018(5) C36 0.038(7) 0.023(7) 0.030(7) -0.002(5) 0.006(6) 0.005(5) C35 0.031(7) 0.041(8) 0.021(7) -0.010(6) 0.009(5) 0.003(6) C34 0.038(7) 0.016(6) 0.025(7) -0.005(5) 0.016(5) -0.001(5) C33 0.033(7) 0.049(9) 0.017(6) 0.003(6) 0.014(5) 0.006(6) C17 0.018(6) 0.033(7) 0.031(7) 0.000(5) -0.005(5) 0.012(5) C16 0.017(6) 0.030(7) 0.030(7) 0.002(5) -0.001(5) 0.002(5) C15 0.013(6) 0.030(7) 0.031(7) 0.003(5) 0.008(5) 0.001(5) C14 0.020(6) 0.038(7) 0.020(6) 0.003(5) 0.004(5) 0.000(5) C13 0.023(6) 0.019(6) 0.039(7) -0.001(5) 0.013(5) -0.002(5) C18 0.012(5) 0.035(7) 0.020(6) 0.005(5) 0.004(5) -0.006(5) C19 0.017(6) 0.038(7) 0.020(6) 0.011(5) 0.003(5) 0.000(5) C20 0.025(6) 0.024(6) 0.018(6) -0.002(5) -0.002(5) -0.002(5) C24 0.027(6) 0.020(6) 0.027(7) -0.004(5) 0.008(5) -0.001(5) C23 0.019(6) 0.028(6) 0.022(6) 0.004(5) 0.005(5) 0.000(5) C21 0.026(6) 0.017(6) 0.026(6) 0.008(5) 0.008(5) 0.000(5) C22 0.020(6) 0.029(7) 0.036(7) -0.010(5) 0.007(5) 0.004(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 Cu3 N6 2.022(9) 4_675 ? Cu3 N5 2.040(9) . ? Cu3 N4 2.086(9) . ? Cu3 I3 2.6414(18) . ? Cu2 N2 2.052(9) 4_665 ? Cu2 N3 2.077(10) . ? Cu2 I2 2.5908(18) . ? Cu2 I1 2.6676(18) . ? Cu2 Cu1 2.697(2) 3_567 ? Cu1 N1 2.049(9) . ? Cu1 I2 2.6728(18) 3_567 ? Cu1 I1 2.6932(18) . ? Cu1 Cu2 2.697(2) 3_567 ? Cu1 I1 2.7374(18) 3_567 ? I1 Cu1 2.7374(18) 3_567 ? I2 Cu1 2.6728(18) 3_567 ? N1 C5 1.342(14) . ? N1 C1 1.341(14) . ? N2 C11 1.333(14) . ? N2 C10 1.335(14) . ? N2 Cu2 2.052(9) 4_566 ? N5 C29 1.344(14) . ? N5 C25 1.368(14) . ? N6 C35 1.338(15) . ? N6 C34 1.348(14) . ? N6 Cu3 2.022(9) 4_576 ? N3 C13 1.337(15) . ? N3 C17 1.335(14) . ? N4 C23 1.330(14) . ? N4 C22 1.356(15) . ? C1 C2 1.373(15) . ? C1 H1 0.9500 . ? C2 C3 1.364(16) . ? C2 H2 0.9500 . ? C3 C4 1.403(16) . ? C3 C6 1.532(15) . ? C4 C5 1.412(17) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.494(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.527(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.377(15) . ? C8 C12 1.381(15) . ? C9 C10 1.369(15) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.405(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C29 C28 1.365(16) . ? C29 H29 0.9500 . ? C28 C27 1.393(16) . ? C28 H28 0.9500 . ? C27 C26 1.394(16) . ? C27 C30 1.480(16) . ? C26 C25 1.369(16) . ? C26 H26 0.9500 . ? C25 H25 0.9500 . ? C30 C31 1.520(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.503(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.375(17) . ? C32 C36 1.394(16) . ? C36 C35 1.381(16) . ? C36 H36 0.9500 . ? C35 H35 0.9500 . ? C34 C33 1.377(16) . ? C34 H34 0.9500 . ? C33 H33 0.9500 . ? C17 C16 1.359(16) . ? C17 H17 0.9500 . ? C16 C15 1.404(16) . ? C16 H16 0.9500 . ? C15 C14 1.385(15) . ? C15 C18 1.520(14) . ? C14 C13 1.370(15) . ? C14 H14 0.9500 . ? C13 H13 0.9500 . ? C18 C19 1.526(15) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.483(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.390(15) . ? C20 C21 1.398(15) . ? C24 C23 1.399(15) . ? C24 H24 0.9500 . ? C23 H23 0.9500 . ? C21 C22 1.377(15) . ? C21 H21 0.9500 . ? C22 H22 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 N6 Cu3 N5 118.3(4) 4_675 . ? N6 Cu3 N4 108.5(4) 4_675 . ? N5 Cu3 N4 103.5(4) . . ? N6 Cu3 I3 109.1(3) 4_675 . ? N5 Cu3 I3 107.7(3) . . ? N4 Cu3 I3 109.3(2) . . ? N2 Cu2 N3 105.5(4) 4_665 . ? N2 Cu2 I2 106.1(2) 4_665 . ? N3 Cu2 I2 112.6(3) . . ? N2 Cu2 I1 109.1(3) 4_665 . ? N3 Cu2 I1 104.6(3) . . ? I2 Cu2 I1 118.23(6) . . ? N2 Cu2 Cu1 145.4(3) 4_665 3_567 ? N3 Cu2 Cu1 109.1(3) . 3_567 ? I2 Cu2 Cu1 60.69(5) . 3_567 ? I1 Cu2 Cu1 61.36(5) . 3_567 ? N1 Cu1 I2 106.9(3) . 3_567 ? N1 Cu1 I1 105.9(3) . . ? I2 Cu1 I1 114.45(6) 3_567 . ? N1 Cu1 Cu2 114.4(3) . 3_567 ? I2 Cu1 Cu2 57.69(5) 3_567 3_567 ? I1 Cu1 Cu2 139.53(7) . 3_567 ? N1 Cu1 I1 116.4(3) . 3_567 ? I2 Cu1 I1 113.05(6) 3_567 3_567 ? I1 Cu1 I1 100.13(5) . 3_567 ? Cu2 Cu1 I1 58.79(5) 3_567 3_567 ? Cu2 I1 Cu1 126.05(6) . . ? Cu2 I1 Cu1 59.84(5) . 3_567 ? Cu1 I1 Cu1 79.87(6) . 3_567 ? Cu2 I2 Cu1 61.62(5) . 3_567 ? C5 N1 C1 117.1(10) . . ? C5 N1 Cu1 123.4(8) . . ? C1 N1 Cu1 119.4(7) . . ? C11 N2 C10 116.0(10) . . ? C11 N2 Cu2 120.2(8) . 4_566 ? C10 N2 Cu2 123.7(8) . 4_566 ? C29 N5 C25 114.3(10) . . ? C29 N5 Cu3 117.4(8) . . ? C25 N5 Cu3 125.9(8) . . ? C35 N6 C34 115.7(10) . . ? C35 N6 Cu3 121.2(8) . 4_576 ? C34 N6 Cu3 122.5(8) . 4_576 ? C13 N3 C17 116.1(10) . . ? C13 N3 Cu2 121.8(8) . . ? C17 N3 Cu2 122.1(8) . . ? C23 N4 C22 116.4(10) . . ? C23 N4 Cu3 122.1(8) . . ? C22 N4 Cu3 121.2(8) . . ? N1 C1 C2 123.5(11) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 120.0(11) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.8(10) . . ? C2 C3 C6 121.2(11) . . ? C4 C3 C6 120.0(10) . . ? C3 C4 C5 117.4(11) . . ? C3 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? N1 C5 C4 123.2(12) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C6 C3 113.3(9) . . ? C7 C6 H6A 108.9 . . ? C3 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? C3 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 111.6(9) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C12 118.2(10) . . ? C9 C8 C7 122.9(10) . . ? C12 C8 C7 118.9(10) . . ? C10 C9 C8 119.8(10) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 123.9(11) . . ? N2 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N2 C11 C12 124.3(11) . . ? N2 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C8 C12 C11 117.6(10) . . ? C8 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? N5 C29 C28 124.9(11) . . ? N5 C29 H29 117.5 . . ? C28 C29 H29 117.5 . . ? C29 C28 C27 120.5(11) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C26 C27 C28 115.7(11) . . ? C26 C27 C30 120.9(11) . . ? C28 C27 C30 123.3(11) . . ? C25 C26 C27 120.3(11) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? N5 C25 C26 124.2(11) . . ? N5 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C27 C30 C31 110.7(9) . . ? C27 C30 H30A 109.5 . . ? C31 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 115.3(10) . . ? C32 C31 H31A 108.4 . . ? C30 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C30 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C36 116.3(11) . . ? C33 C32 C31 122.1(11) . . ? C36 C32 C31 121.5(11) . . ? C35 C36 C32 119.0(11) . . ? C35 C36 H36 120.5 . . ? C32 C36 H36 120.5 . . ? N6 C35 C36 124.8(11) . . ? N6 C35 H35 117.6 . . ? C36 C35 H35 117.6 . . ? N6 C34 C33 122.8(11) . . ? N6 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C32 C33 C34 121.3(12) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? N3 C17 C16 125.1(11) . . ? N3 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? C17 C16 C15 119.0(11) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C14 C15 C16 115.9(10) . . ? C14 C15 C18 121.1(10) . . ? C16 C15 C18 123.0(10) . . ? C13 C14 C15 121.1(11) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? N3 C13 C14 122.8(11) . . ? N3 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C18 C19 114.7(9) . . ? C15 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? C15 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 113.0(9) . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C24 C20 C21 115.7(10) . . ? C24 C20 C19 121.2(10) . . ? C21 C20 C19 123.0(10) . . ? C20 C24 C23 119.6(11) . . ? C20 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? N4 C23 C24 124.2(11) . . ? N4 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C22 C21 C20 121.4(10) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? N4 C22 C21 122.6(10) . . ? N4 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.071 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.200 #===END data_{[CuI(bbbm)1.5].0.25MeCN}n _database_code_depnum_ccdc_archive 'CCDC 727479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Cu I N6 0.25(C2 H3 N)' _chemical_formula_sum 'C27.50 H27.75 Cu I N6.25' _chemical_formula_weight 636.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 hexagonal _symmetry_space_group_name_H-M 'P -3 c 1 ' _symmetry_space_group_name_Hall '-P 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' _cell_length_a 13.989(2) _cell_length_b 13.989(2) _cell_length_c 16.395(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2778.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6649 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1271.0 _exptl_absorpt_coefficient_mu 1.924 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.681 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23589 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.34 _reflns_number_total 1695 _reflns_number_gt 1425 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+41.6380P] 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 1695 _refine_ls_number_parameters 112 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 0.3333 0.6667 0.07407(10) 0.0516(6) Uani 1 3 d S . . I1 I 0.3333 0.6667 0.23449(6) 0.0617(4) Uani 1 3 d S . . N1 N 0.3587(6) 0.5452(7) 0.0208(4) 0.0474(18) Uani 1 1 d . . . N2 N 0.3883(7) 0.4553(7) -0.0785(4) 0.051(2) Uani 1 1 d . . . C1 C 0.3317(8) 0.4425(8) 0.0484(5) 0.046(2) Uani 1 1 d . . . C2 C 0.2917(10) 0.3928(10) 0.1244(6) 0.064(3) Uani 1 1 d . . . H2A H 0.2811 0.4309 0.1666 0.077 Uiso 1 1 calc R . . C3 C 0.2689(14) 0.2862(12) 0.1346(8) 0.104(5) Uani 1 1 d . . . H3A H 0.2393 0.2502 0.1838 0.125 Uiso 1 1 calc R . . C4 C 0.2896(16) 0.2309(13) 0.0718(8) 0.116(6) Uani 1 1 d . . . H4A H 0.2762 0.1597 0.0811 0.139 Uiso 1 1 calc R . . C5 C 0.3282(13) 0.2776(12) -0.0019(7) 0.093(5) Uani 1 1 d . . . H5A H 0.3397 0.2391 -0.0434 0.112 Uiso 1 1 calc R . . C6 C 0.3502(9) 0.3845(9) -0.0137(5) 0.054(3) Uani 1 1 d . . . C7 C 0.3933(7) 0.5494(8) -0.0543(5) 0.048(2) Uani 1 1 d . . . H7A H 0.4187 0.6113 -0.0875 0.058 Uiso 1 1 calc R . . C8 C 0.4220(9) 0.4336(9) -0.1587(5) 0.062(3) Uani 1 1 d . . . H8A H 0.4678 0.4005 -0.1506 0.074 Uiso 1 1 calc R . . H8B H 0.4655 0.5029 -0.1873 0.074 Uiso 1 1 calc R . . C9 C 0.3227(8) 0.3572(9) -0.2104(5) 0.055(3) Uani 1 1 d . . . H9A H 0.2818 0.3941 -0.2242 0.066 Uiso 1 1 calc R . . H9B H 0.2743 0.2917 -0.1790 0.066 Uiso 1 1 calc R . . N3 N 0.0000 0.0000 0.210(5) 0.19(6) Uiso 0.25 3 d SPD . . C10 C 0.0000 0.0000 0.141(4) 0.10(3) Uiso 0.25 3 d SPD . . C11 C 0.0000 0.0000 0.048(4) 0.09(3) Uiso 0.25 3 d SPD . . 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 0.0616(8) 0.0616(8) 0.0318(9) 0.000 0.000 0.0308(4) I1 0.0786(6) 0.0786(6) 0.0279(5) 0.000 0.000 0.0393(3) N1 0.052(5) 0.059(5) 0.036(4) -0.007(3) -0.001(3) 0.031(4) N2 0.059(5) 0.063(5) 0.038(4) -0.006(4) 0.001(4) 0.035(4) C1 0.055(6) 0.048(6) 0.034(4) -0.003(4) -0.013(4) 0.025(5) C2 0.094(8) 0.075(8) 0.037(5) -0.010(5) -0.005(5) 0.052(7) C3 0.175(16) 0.092(10) 0.057(7) 0.014(7) -0.002(9) 0.076(11) C4 0.22(2) 0.096(11) 0.071(9) 0.000(8) -0.014(10) 0.111(13) C5 0.169(15) 0.108(11) 0.053(7) -0.031(7) -0.032(8) 0.107(11) C6 0.067(7) 0.071(7) 0.043(5) -0.018(5) -0.011(5) 0.050(6) C7 0.055(6) 0.058(6) 0.034(4) -0.001(4) 0.001(4) 0.030(5) C8 0.066(7) 0.079(8) 0.041(5) -0.018(5) 0.003(5) 0.037(6) C9 0.057(6) 0.070(7) 0.039(5) -0.009(5) -0.001(4) 0.031(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 Cu1 N1 2.093(7) 3_565 ? Cu1 N1 2.093(7) 2_665 ? Cu1 N1 2.093(7) . ? Cu1 I1 2.630(2) . ? N1 C7 1.314(10) . ? N1 C1 1.366(11) . ? N2 C7 1.342(12) . ? N2 C6 1.367(12) . ? N2 C8 1.478(10) . ? C1 C2 1.401(12) . ? C1 C6 1.403(12) . ? C2 C3 1.369(16) . ? C2 H2A 0.9300 . ? C3 C4 1.404(18) . ? C3 H3A 0.9300 . ? C4 C5 1.351(18) . ? C4 H4A 0.9300 . ? C5 C6 1.381(16) . ? C5 H5A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.518(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C9 1.544(17) 4_554 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N3 C10 1.14(2) . ? N3 N3 1.31(15) 4 ? C10 C11 1.52(2) . ? C11 C11 1.57(15) 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 N1 Cu1 N1 103.8(2) 3_565 2_665 ? N1 Cu1 N1 103.8(2) 3_565 . ? N1 Cu1 N1 103.8(2) 2_665 . ? N1 Cu1 I1 114.7(2) 3_565 . ? N1 Cu1 I1 114.7(2) 2_665 . ? N1 Cu1 I1 114.7(2) . . ? C7 N1 C1 105.0(8) . . ? C7 N1 Cu1 124.2(7) . . ? C1 N1 Cu1 130.2(6) . . ? C7 N2 C6 106.9(7) . . ? C7 N2 C8 126.7(8) . . ? C6 N2 C8 126.3(8) . . ? N1 C1 C2 130.4(9) . . ? N1 C1 C6 109.6(8) . . ? C2 C1 C6 120.1(9) . . ? C3 C2 C1 117.9(10) . . ? C3 C2 H2A 121.1 . . ? C1 C2 H2A 121.1 . . ? C2 C3 C4 120.7(12) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 122.2(13) . . ? C5 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? C4 C5 C6 117.9(11) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? N2 C6 C5 133.5(9) . . ? N2 C6 C1 105.2(8) . . ? C5 C6 C1 121.3(10) . . ? N1 C7 N2 113.3(8) . . ? N1 C7 H7A 123.4 . . ? N2 C7 H7A 123.4 . . ? N2 C8 C9 111.6(8) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C9 111.8(7) . 4_554 ? C8 C9 H9A 109.3 . . ? C9 C9 H9A 109.3 4_554 . ? C8 C9 H9B 109.3 . . ? C9 C9 H9B 109.3 4_554 . ? H9A C9 H9B 107.9 . . ? C10 N3 N3 180.000(7) . 4 ? N3 C10 C11 180.000(11) . . ? C10 C11 C11 180.000(1) . 7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 N1 C7 74.8(6) 3_565 . . . ? N1 Cu1 N1 C7 -33.5(7) 2_665 . . . ? I1 Cu1 N1 C7 -159.3(7) . . . . ? N1 Cu1 N1 C1 -95.7(9) 3_565 . . . ? N1 Cu1 N1 C1 156.0(8) 2_665 . . . ? I1 Cu1 N1 C1 30.2(8) . . . . ? C7 N1 C1 C2 179.1(10) . . . . ? Cu1 N1 C1 C2 -9.1(15) . . . . ? C7 N1 C1 C6 -0.7(10) . . . . ? Cu1 N1 C1 C6 171.1(6) . . . . ? N1 C1 C2 C3 178.4(12) . . . . ? C6 C1 C2 C3 -1.8(17) . . . . ? C1 C2 C3 C4 3(2) . . . . ? C2 C3 C4 C5 -3(3) . . . . ? C3 C4 C5 C6 2(3) . . . . ? C7 N2 C6 C5 180.0(13) . . . . ? C8 N2 C6 C5 -2.3(19) . . . . ? C7 N2 C6 C1 1.0(10) . . . . ? C8 N2 C6 C1 178.8(9) . . . . ? C4 C5 C6 N2 -179.6(13) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? N1 C1 C6 N2 -0.2(11) . . . . ? C2 C1 C6 N2 180.0(9) . . . . ? N1 C1 C6 C5 -179.3(10) . . . . ? C2 C1 C6 C5 0.9(16) . . . . ? C1 N1 C7 N2 1.4(11) . . . . ? Cu1 N1 C7 N2 -171.1(6) . . . . ? C6 N2 C7 N1 -1.6(11) . . . . ? C8 N2 C7 N1 -179.3(8) . . . . ? C7 N2 C8 C9 -106.8(11) . . . . ? C6 N2 C8 C9 75.9(13) . . . . ? N2 C8 C9 C9 -172.9(9) . . . 4_554 ? N3 N3 C10 C11 0.0 4 . . . ? N3 C10 C11 C11 0.0 . . . 7 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.804 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.089 #===END data_[Cu4(m3-I)4(bbbt)2]n _database_code_depnum_ccdc_archive 'CCDC 727480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H8 Cu I N3' _chemical_formula_sum 'C8 H8 Cu I N3' _chemical_formula_weight 336.61 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 tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 13.4355(19) _cell_length_b 13.4355(19) _cell_length_c 10.724(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1935.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3555 _cell_measurement_theta_min 3.0324 _cell_measurement_theta_max 27.4778 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 5.399 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1552 _exptl_absorpt_correction_T_max 0.1732 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4684 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2214 _reflns_number_gt 1538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+148.0000P] 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 2214 _refine_ls_number_parameters 128 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2428 _refine_ls_wR_factor_gt 0.2308 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.65974(13) 0.80098(15) 1.16238(18) 0.0306(5) Uani 1 1 d . . . I1 I 0.67858(10) 0.61423(10) 1.11048(13) 0.0500(4) Uani 1 1 d . . . N1 N 0.5458(8) 0.8457(8) 1.0558(11) 0.020(2) Uani 1 1 d . . . N2 N 0.4552(9) 0.8504(9) 1.0991(12) 0.026(3) Uani 1 1 d . . . N3 N 0.3958(8) 0.8801(8) 1.0060(12) 0.023(2) Uani 1 1 d . . . C1 C 0.5457(9) 0.8725(9) 0.9324(12) 0.019(2) Uani 1 1 d . . . C2 C 0.6227(11) 0.8788(10) 0.8451(13) 0.026(3) Uani 1 1 d . . . H2 H 0.6889 0.8641 0.8665 0.031 Uiso 1 1 calc R . . C3 C 0.5967(12) 0.9077(11) 0.7267(14) 0.031(3) Uani 1 1 d . . . H3 H 0.6463 0.9118 0.6649 0.038 Uiso 1 1 calc R . . C4 C 0.4989(13) 0.9311(11) 0.6958(14) 0.033(3) Uani 1 1 d . . . H4 H 0.4844 0.9512 0.6139 0.040 Uiso 1 1 calc R . . C5 C 0.4235(12) 0.9257(10) 0.7805(14) 0.031(3) Uani 1 1 d . . . H5 H 0.3577 0.9420 0.7588 0.037 Uiso 1 1 calc R . . C6 C 0.4478(10) 0.8953(8) 0.8994(12) 0.019(3) Uani 1 1 d . . . C7 C 0.2874(10) 0.8889(11) 1.0272(18) 0.034(4) Uani 1 1 d . . . C8 C 0.244(2) 0.788(2) 1.065(4) 0.029(7) Uani 0.48(4) 1 d PU . . C8A C 0.235(2) 0.800(2) 0.983(4) 0.032(7) Uani 0.52(4) 1 d PU . . 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 0.0238(9) 0.0406(11) 0.0272(9) 0.0061(8) -0.0052(8) 0.0018(7) I1 0.0501(8) 0.0532(8) 0.0468(8) -0.0099(6) 0.0032(6) -0.0043(6) N1 0.015(5) 0.021(5) 0.024(6) -0.003(5) 0.000(4) -0.002(4) N2 0.023(6) 0.027(6) 0.029(7) 0.002(5) 0.003(5) -0.002(5) N3 0.013(5) 0.021(5) 0.035(7) 0.003(5) -0.003(5) 0.001(4) C1 0.021(6) 0.013(6) 0.021(6) -0.002(5) -0.007(5) -0.002(4) C2 0.033(7) 0.018(6) 0.025(7) -0.011(6) -0.002(6) -0.002(5) C3 0.044(9) 0.028(7) 0.022(7) -0.006(6) 0.010(6) -0.003(6) C4 0.051(10) 0.028(7) 0.020(7) 0.002(6) -0.004(7) 0.000(7) C5 0.038(8) 0.020(7) 0.035(8) -0.004(6) -0.015(7) 0.004(6) C6 0.024(6) 0.008(5) 0.024(7) -0.004(5) -0.008(5) -0.001(5) C7 0.015(6) 0.023(7) 0.065(11) 0.001(7) -0.001(7) 0.004(5) C8 0.014(11) 0.026(12) 0.047(18) -0.009(13) 0.003(14) -0.001(10) C8A 0.017(11) 0.022(12) 0.057(19) 0.002(13) -0.009(14) 0.000(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.003(11) . ? Cu1 I1 2.515(2) 2_665 ? Cu1 I1 2.526(2) 7_578 ? Cu1 I1 2.583(2) . ? Cu1 Cu1 2.722(3) 7_578 ? Cu1 Cu1 2.722(3) 8_758 ? Cu1 Cu1 2.786(4) 2_665 ? I1 Cu1 2.515(2) 2_665 ? I1 Cu1 2.526(2) 8_758 ? N1 N2 1.305(15) . ? N1 C1 1.372(17) . ? N2 N3 1.338(16) . ? N3 C6 1.355(18) . ? N3 C7 1.479(17) . ? C1 C6 1.396(17) . ? C1 C2 1.398(19) . ? C2 C3 1.37(2) . ? C2 H2 0.9400 . ? C3 C4 1.39(2) . ? C3 H3 0.9400 . ? C4 C5 1.36(2) . ? C4 H4 0.9400 . ? C5 C6 1.38(2) . ? C5 H5 0.9400 . ? C7 C8A 1.47(3) . ? C7 C8 1.54(4) . ? C8A C8 1.50(4) 2_565 ? 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 I1 113.4(3) . 2_665 ? N1 Cu1 I1 109.4(3) . 7_578 ? I1 Cu1 I1 111.91(8) 2_665 7_578 ? N1 Cu1 I1 104.1(3) . . ? I1 Cu1 I1 107.92(8) 2_665 . ? I1 Cu1 I1 109.70(8) 7_578 . ? N1 Cu1 Cu1 150.3(3) . 7_578 ? I1 Cu1 Cu1 57.52(6) 2_665 7_578 ? I1 Cu1 Cu1 58.81(9) 7_578 7_578 ? I1 Cu1 Cu1 105.59(7) . 7_578 ? N1 Cu1 Cu1 138.7(3) . 8_758 ? I1 Cu1 Cu1 107.52(6) 2_665 8_758 ? I1 Cu1 Cu1 57.12(8) 7_578 8_758 ? I1 Cu1 Cu1 56.81(6) . 8_758 ? Cu1 Cu1 Cu1 61.54(8) 7_578 8_758 ? N1 Cu1 Cu1 144.4(3) . 2_665 ? I1 Cu1 Cu1 58.04(7) 2_665 2_665 ? I1 Cu1 Cu1 105.32(5) 7_578 2_665 ? I1 Cu1 Cu1 55.72(7) . 2_665 ? Cu1 Cu1 Cu1 59.23(4) 7_578 2_665 ? Cu1 Cu1 Cu1 59.23(4) 8_758 2_665 ? Cu1 I1 Cu1 65.36(7) 2_665 8_758 ? Cu1 I1 Cu1 66.23(7) 2_665 . ? Cu1 I1 Cu1 64.39(7) 8_758 . ? N2 N1 C1 109.2(11) . . ? N2 N1 Cu1 121.6(9) . . ? C1 N1 Cu1 129.1(9) . . ? N1 N2 N3 107.7(11) . . ? N2 N3 C6 111.6(10) . . ? N2 N3 C7 119.7(12) . . ? C6 N3 C7 128.6(12) . . ? N1 C1 C6 107.7(12) . . ? N1 C1 C2 131.4(12) . . ? C6 C1 C2 121.0(13) . . ? C3 C2 C1 116.7(14) . . ? C3 C2 H2 121.7 . . ? C1 C2 H2 121.7 . . ? C2 C3 C4 121.6(14) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 122.1(14) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 117.1(14) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? N3 C6 C5 134.7(13) . . ? N3 C6 C1 103.8(11) . . ? C5 C6 C1 121.5(13) . . ? C8A C7 N3 111.2(16) . . ? C8A C7 C8 35.0(16) . . ? N3 C7 C8 110.3(15) . . ? C7 C8A C8 111(2) . 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 I1 Cu1 147.5(3) . . . 2_665 ? I1 Cu1 I1 Cu1 26.68(10) 2_665 . . 2_665 ? I1 Cu1 I1 Cu1 -95.48(7) 7_578 . . 2_665 ? Cu1 Cu1 I1 Cu1 -33.60(11) 7_578 . . 2_665 ? Cu1 Cu1 I1 Cu1 -72.90(6) 8_758 . . 2_665 ? N1 Cu1 I1 Cu1 -139.6(3) . . . 8_758 ? I1 Cu1 I1 Cu1 99.59(8) 2_665 . . 8_758 ? I1 Cu1 I1 Cu1 -22.58(8) 7_578 . . 8_758 ? Cu1 Cu1 I1 Cu1 39.31(10) 7_578 . . 8_758 ? Cu1 Cu1 I1 Cu1 72.90(6) 2_665 . . 8_758 ? I1 Cu1 N1 N2 -146.9(9) 2_665 . . . ? I1 Cu1 N1 N2 -21.1(11) 7_578 . . . ? I1 Cu1 N1 N2 96.1(10) . . . . ? Cu1 Cu1 N1 N2 -81.8(12) 7_578 . . . ? Cu1 Cu1 N1 N2 40.8(12) 8_758 . . . ? Cu1 Cu1 N1 N2 145.8(8) 2_665 . . . ? I1 Cu1 N1 C1 35.2(11) 2_665 . . . ? I1 Cu1 N1 C1 160.9(10) 7_578 . . . ? I1 Cu1 N1 C1 -81.9(11) . . . . ? Cu1 Cu1 N1 C1 100.3(11) 7_578 . . . ? Cu1 Cu1 N1 C1 -137.1(9) 8_758 . . . ? Cu1 Cu1 N1 C1 -32.2(14) 2_665 . . . ? C1 N1 N2 N3 -0.1(14) . . . . ? Cu1 N1 N2 N3 -178.5(8) . . . . ? N1 N2 N3 C6 0.0(15) . . . . ? N1 N2 N3 C7 178.0(11) . . . . ? N2 N1 C1 C6 0.2(14) . . . . ? Cu1 N1 C1 C6 178.4(8) . . . . ? N2 N1 C1 C2 -179.6(13) . . . . ? Cu1 N1 C1 C2 -1(2) . . . . ? N1 C1 C2 C3 179.4(13) . . . . ? C6 C1 C2 C3 -0.4(18) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? N2 N3 C6 C5 -179.5(14) . . . . ? C7 N3 C6 C5 3(2) . . . . ? N2 N3 C6 C1 0.1(14) . . . . ? C7 N3 C6 C1 -177.6(12) . . . . ? C4 C5 C6 N3 -179.4(14) . . . . ? C4 C5 C6 C1 1.1(19) . . . . ? N1 C1 C6 N3 -0.2(13) . . . . ? C2 C1 C6 N3 179.6(11) . . . . ? N1 C1 C6 C5 179.5(11) . . . . ? C2 C1 C6 C5 -0.7(18) . . . . ? N2 N3 C7 C8A -98(2) . . . . ? C6 N3 C7 C8A 80(2) . . . . ? N2 N3 C7 C8 -60(2) . . . . ? C6 N3 C7 C8 117(2) . . . . ? N3 C7 C8A C8 70(3) . . . 2_565 ? C8 C7 C8A C8 -25(3) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.423 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.360 #===END data_[Cu4(m3-I)4(pbbm)2]n _database_code_depnum_ccdc_archive 'CCDC 727481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H40 Cu4 I4 N8' _chemical_formula_sum 'C38 H40 Cu4 I4 N8' _chemical_formula_weight 1370.58 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.635(2) _cell_length_b 11.673(2) _cell_length_c 15.624(3) _cell_angle_alpha 90.322(7) _cell_angle_beta 91.196(7) _cell_angle_gamma 91.947(7) _cell_volume 2120.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6084 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 4.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.611 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20856 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7743 _reflns_number_gt 5089 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0410P)^2^+12.4572P] 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 7683 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 I1 I 0.91665(8) 0.91526(7) 0.37125(6) 0.0477(3) Uani 1 1 d . . . I2 I 0.56093(8) 0.89333(8) 0.23621(6) 0.0536(3) Uani 1 1 d . . . I3 I 0.66880(8) 0.60562(8) 0.40034(6) 0.0521(3) Uani 1 1 d . . . I4 I 0.85648(9) 0.67289(9) 0.15570(7) 0.0614(3) Uani 1 1 d . . . Cu1 Cu 0.65556(16) 0.68558(15) 0.24280(12) 0.0590(5) Uani 1 1 d . . . Cu2 Cu 0.85841(15) 0.70114(14) 0.32955(13) 0.0581(5) Uani 1 1 d . . . Cu3 Cu 0.79041(16) 0.87137(15) 0.22207(12) 0.0578(5) Uani 1 1 d . . . Cu4 Cu 0.69672(15) 0.85291(17) 0.37128(12) 0.0603(5) Uani 1 1 d . . . N1 N 0.6029(10) 0.8874(10) 0.4749(7) 0.055(3) Uani 1 1 d . . . N2 N 0.4689(10) 0.8040(10) 0.5554(8) 0.055(3) Uani 1 1 d . . . N3 N -0.0399(9) 0.5831(9) 0.6036(7) 0.047(3) Uani 1 1 d . . . N4 N 0.0201(9) 0.4099(9) 0.6341(7) 0.049(3) Uani 1 1 d . . . N5 N 0.5519(11) 0.5777(10) 0.1740(8) 0.056(3) Uani 1 1 d . . . N6 N 0.3995(10) 0.5146(9) 0.0947(7) 0.048(3) Uani 1 1 d . . . N7 N -0.0391(10) 0.1274(10) 0.0837(8) 0.055(3) Uani 1 1 d . . . N8 N -0.1543(10) -0.0096(9) 0.1412(7) 0.046(3) Uani 1 1 d . . . C1 C 0.6437(12) 0.8859(11) 0.5603(10) 0.049(4) Uani 1 1 d . . . C2 C 0.7463(13) 0.9265(14) 0.5973(10) 0.063(4) Uani 1 1 d . . . H2 H 0.8036 0.9618 0.5652 0.075 Uiso 1 1 calc R . . C3 C 0.7588(16) 0.9121(15) 0.6835(12) 0.077(5) Uani 1 1 d . . . H3 H 0.8251 0.9423 0.7106 0.093 Uiso 1 1 calc R . . C4 C 0.6780(17) 0.8550(19) 0.7330(12) 0.091(6) Uani 1 1 d . . . H4 H 0.6930 0.8442 0.7910 0.110 Uiso 1 1 calc R . . C5 C 0.5754(15) 0.8141(15) 0.6967(11) 0.072(5) Uani 1 1 d . . . H5 H 0.5192 0.7775 0.7292 0.087 Uiso 1 1 calc R . . C6 C 0.5600(13) 0.8303(12) 0.6094(10) 0.053(4) Uani 1 1 d . . . C7 C 0.5001(13) 0.8377(13) 0.4768(10) 0.060(4) Uani 1 1 d . . . H7 H 0.4532 0.8269 0.4282 0.072 Uiso 1 1 calc R . . C8 C 0.3592(12) 0.7463(13) 0.5761(11) 0.065(4) Uani 1 1 d . . . H8A H 0.3738 0.6821 0.6134 0.078 Uiso 1 1 calc R . . H8B H 0.3227 0.7164 0.5238 0.078 Uiso 1 1 calc R . . C9 C 0.2803(12) 0.8241(12) 0.6185(11) 0.064(4) Uani 1 1 d . . . H9A H 0.2668 0.8887 0.5812 0.076 Uiso 1 1 calc R . . H9B H 0.3172 0.8537 0.6707 0.076 Uiso 1 1 calc R . . C10 C 0.1631(11) 0.7669(12) 0.6410(9) 0.050(4) Uani 1 1 d . . . H10A H 0.1757 0.6930 0.6671 0.061 Uiso 1 1 calc R . . H10B H 0.1253 0.8142 0.6823 0.061 Uiso 1 1 calc R . . C11 C 0.0842(12) 0.7499(12) 0.5609(10) 0.058(4) Uani 1 1 d . . . H11A H 0.0790 0.8230 0.5320 0.070 Uiso 1 1 calc R . . H11B H 0.1202 0.6975 0.5221 0.070 Uiso 1 1 calc R . . C12 C -0.0348(11) 0.7048(11) 0.5777(10) 0.053(4) Uani 1 1 d . . . H12A H -0.0674 0.7507 0.6224 0.064 Uiso 1 1 calc R . . H12B H -0.0819 0.7133 0.5263 0.064 Uiso 1 1 calc R . . C13 C -0.1347(10) 0.5195(11) 0.6286(8) 0.040(3) Uani 1 1 d . . . C14 C -0.2484(13) 0.5477(13) 0.6347(9) 0.061(4) Uani 1 1 d . . . H14 H -0.2737 0.6203 0.6213 0.073 Uiso 1 1 calc R . . C15 C -0.3238(13) 0.4591(17) 0.6627(10) 0.072(5) Uani 1 1 d . . . H15 H -0.4015 0.4734 0.6683 0.087 Uiso 1 1 calc R . . C16 C -0.2861(14) 0.3545(16) 0.6814(10) 0.065(4) Uani 1 1 d . . . H16 H -0.3394 0.2987 0.6989 0.079 Uiso 1 1 calc R . . C17 C -0.1732(13) 0.3255(12) 0.6761(9) 0.056(4) Uani 1 1 d . . . H17 H -0.1488 0.2526 0.6892 0.067 Uiso 1 1 calc R . . C18 C -0.0972(11) 0.4134(11) 0.6495(9) 0.048(3) Uani 1 1 d . . . C19 C 0.0483(12) 0.5121(12) 0.6070(11) 0.061(4) Uani 1 1 d . . . H19 H 0.1226 0.5338 0.5914 0.073 Uiso 1 1 calc R . . C20 C 0.5694(14) 0.4615(12) 0.1511(10) 0.058(4) Uani 1 1 d . . . C21 C 0.6586(14) 0.3913(14) 0.1696(11) 0.068(4) Uani 1 1 d . . . H21 H 0.7204 0.4159 0.2045 0.082 Uiso 1 1 calc R . . C22 C 0.6531(16) 0.2859(15) 0.1353(12) 0.080(5) Uani 1 1 d . . . H22 H 0.7137 0.2377 0.1460 0.096 Uiso 1 1 calc R . . C23 C 0.5621(19) 0.2458(15) 0.0852(13) 0.086(6) Uani 1 1 d . . . H23 H 0.5625 0.1715 0.0634 0.104 Uiso 1 1 calc R . . C24 C 0.4723(16) 0.3117(15) 0.0669(11) 0.074(5) Uani 1 1 d . . . H24 H 0.4108 0.2844 0.0328 0.089 Uiso 1 1 calc R . . C25 C 0.4747(13) 0.4262(12) 0.1021(9) 0.054(4) Uani 1 1 d . . . C26 C 0.4517(12) 0.6013(12) 0.1390(9) 0.053(4) Uani 1 1 d . . . H26 H 0.4194 0.6727 0.1444 0.064 Uiso 1 1 calc R . . C27 C 0.2834(12) 0.5146(14) 0.0611(11) 0.069(5) Uani 1 1 d . . . H27A H 0.2823 0.4909 0.0015 0.083 Uiso 1 1 calc R . . H27B H 0.2548 0.5915 0.0642 0.083 Uiso 1 1 calc R . . C28 C 0.2011(13) 0.429(2) 0.1145(12) 0.112(8) Uani 1 1 d . . . H28A H 0.2274 0.3512 0.1094 0.134 Uiso 1 1 calc R . . H28B H 0.2046 0.4503 0.1746 0.134 Uiso 1 1 calc R . . C29 C 0.0890(16) 0.4332(16) 0.0841(14) 0.098(6) Uani 1 1 d . . . H29A H 0.0891 0.4357 0.0220 0.117 Uiso 1 1 calc R . . H29B H 0.0560 0.5033 0.1043 0.117 Uiso 1 1 calc R . . C30 C 0.0134(15) 0.3309(15) 0.1120(12) 0.085(6) Uani 1 1 d . . . H30A H 0.0126 0.3300 0.1741 0.101 Uiso 1 1 calc R . . H30B H -0.0647 0.3424 0.0917 0.101 Uiso 1 1 calc R . . C31 C 0.0494(13) 0.2160(14) 0.0811(11) 0.069(5) Uani 1 1 d . . . H31A H 0.0749 0.2234 0.0227 0.083 Uiso 1 1 calc R . . H31B H 0.1144 0.1927 0.1159 0.083 Uiso 1 1 calc R . . C32 C -0.1237(12) 0.1039(11) 0.0259(9) 0.048(3) Uani 1 1 d . . . C33 C -0.1470(15) 0.1467(15) -0.0577(11) 0.073(5) Uani 1 1 d . . . H33 H -0.0997 0.2032 -0.0817 0.087 Uiso 1 1 calc R . . C34 C -0.2386(17) 0.1031(14) -0.1002(11) 0.075(5) Uani 1 1 d . . . H34 H -0.2557 0.1316 -0.1543 0.091 Uiso 1 1 calc R . . C35 C -0.3116(15) 0.0151(15) -0.0667(12) 0.077(5) Uani 1 1 d . . . H35 H -0.3742 -0.0133 -0.0992 0.093 Uiso 1 1 calc R . . C36 C -0.2907(14) -0.0280(13) 0.0128(10) 0.064(4) Uani 1 1 d . . . H36 H -0.3372 -0.0863 0.0353 0.077 Uiso 1 1 calc R . . C37 C -0.1973(12) 0.0187(11) 0.0585(8) 0.045(3) Uani 1 1 d . . . C38 C -0.0630(13) 0.0602(14) 0.1512(10) 0.062(4) Uani 1 1 d . . . H38 H -0.0184 0.0627 0.2013 0.074 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 I1 0.0450(5) 0.0419(5) 0.0559(6) 0.0006(4) -0.0050(4) -0.0007(4) I2 0.0457(6) 0.0541(6) 0.0610(6) 0.0035(5) -0.0079(5) 0.0062(4) I3 0.0462(6) 0.0486(5) 0.0619(6) 0.0097(5) 0.0076(5) 0.0029(4) I4 0.0630(7) 0.0624(6) 0.0593(7) -0.0107(5) 0.0215(5) -0.0032(5) Cu1 0.0540(11) 0.0553(11) 0.0668(13) -0.0054(9) -0.0043(10) -0.0069(9) Cu2 0.0499(11) 0.0456(10) 0.0792(14) 0.0064(9) 0.0011(10) 0.0061(8) Cu3 0.0579(12) 0.0566(11) 0.0585(12) 0.0112(9) 0.0026(9) -0.0051(9) Cu4 0.0483(11) 0.0802(13) 0.0530(12) -0.0042(10) 0.0071(9) 0.0056(9) N1 0.057(8) 0.063(8) 0.047(8) -0.013(6) -0.003(6) 0.003(6) N2 0.047(7) 0.059(8) 0.061(8) 0.002(6) 0.015(7) 0.016(6) N3 0.034(6) 0.050(7) 0.057(7) 0.006(6) 0.001(5) 0.007(5) N4 0.044(7) 0.041(7) 0.061(8) 0.005(6) 0.000(6) 0.006(5) N5 0.057(8) 0.055(8) 0.055(8) 0.002(6) 0.003(6) -0.008(6) N6 0.051(7) 0.044(7) 0.048(7) -0.013(5) 0.000(6) -0.017(6) N7 0.045(7) 0.063(8) 0.056(8) 0.015(6) -0.006(6) -0.011(6) N8 0.057(7) 0.040(6) 0.041(7) 0.005(5) -0.006(6) -0.002(5) C1 0.046(9) 0.036(7) 0.066(10) -0.007(7) 0.006(8) 0.019(6) C2 0.049(10) 0.088(12) 0.052(10) -0.015(9) 0.004(8) 0.018(8) C3 0.074(12) 0.082(12) 0.075(13) -0.053(10) -0.014(10) 0.014(10) C4 0.070(13) 0.144(19) 0.062(12) 0.007(12) -0.008(11) 0.037(13) C5 0.069(12) 0.089(13) 0.061(11) -0.001(9) 0.018(9) 0.021(10) C6 0.053(10) 0.053(9) 0.054(10) 0.003(7) 0.011(8) 0.019(7) C7 0.047(9) 0.082(11) 0.049(10) -0.014(8) -0.006(8) -0.004(8) C8 0.048(9) 0.068(10) 0.078(11) -0.001(9) 0.017(8) -0.001(8) C9 0.049(9) 0.055(9) 0.088(12) -0.022(8) 0.020(9) 0.002(7) C10 0.040(8) 0.046(8) 0.064(10) -0.008(7) 0.003(7) -0.009(6) C11 0.048(9) 0.050(9) 0.078(11) 0.008(8) 0.001(8) 0.010(7) C12 0.046(8) 0.042(8) 0.073(10) 0.013(7) 0.001(8) 0.009(6) C13 0.026(7) 0.059(9) 0.036(7) 0.008(6) 0.002(6) 0.006(6) C14 0.064(10) 0.058(10) 0.061(10) 0.009(8) -0.002(8) 0.016(8) C15 0.038(9) 0.112(15) 0.067(11) 0.013(11) -0.002(8) 0.004(10) C16 0.050(10) 0.094(13) 0.052(10) -0.002(9) 0.008(8) -0.016(9) C17 0.056(10) 0.053(9) 0.059(10) 0.010(7) 0.011(8) -0.007(7) C18 0.030(7) 0.051(8) 0.064(10) 0.006(7) 0.012(7) 0.012(6) C19 0.037(8) 0.047(9) 0.098(13) 0.004(8) 0.000(8) 0.006(7) C20 0.067(11) 0.048(9) 0.057(10) -0.002(7) 0.011(8) -0.017(8) C21 0.059(11) 0.067(11) 0.079(12) 0.000(9) -0.010(9) 0.008(9) C22 0.074(13) 0.069(12) 0.099(14) -0.013(11) 0.034(11) 0.006(10) C23 0.102(16) 0.053(11) 0.103(16) -0.021(10) 0.029(13) -0.014(11) C24 0.080(13) 0.081(12) 0.061(11) -0.015(9) 0.016(10) -0.013(10) C25 0.053(9) 0.052(9) 0.058(10) -0.022(8) 0.017(8) -0.006(7) C26 0.044(9) 0.049(8) 0.068(10) -0.007(8) 0.014(8) -0.003(7) C27 0.050(10) 0.074(11) 0.082(12) -0.022(9) -0.003(9) -0.016(8) C28 0.031(9) 0.22(3) 0.085(14) -0.045(15) 0.001(9) -0.035(12) C29 0.083(14) 0.083(13) 0.127(18) -0.015(13) 0.006(13) -0.004(11) C30 0.078(13) 0.086(13) 0.088(13) -0.013(11) 0.022(11) -0.032(10) C31 0.050(9) 0.080(12) 0.076(12) 0.007(9) 0.016(9) -0.020(8) C32 0.050(9) 0.042(8) 0.052(9) 0.009(7) 0.007(7) -0.003(6) C33 0.068(11) 0.076(12) 0.074(12) 0.002(10) 0.007(10) -0.003(9) C34 0.113(16) 0.060(11) 0.052(10) 0.003(8) -0.008(10) -0.002(10) C35 0.061(11) 0.078(12) 0.093(14) -0.027(11) -0.027(10) 0.025(9) C36 0.072(11) 0.053(9) 0.066(11) 0.001(8) -0.022(9) -0.009(8) C37 0.052(9) 0.042(8) 0.041(8) -0.013(6) -0.002(7) 0.007(7) C38 0.047(9) 0.078(11) 0.062(10) 0.003(9) -0.001(8) 0.001(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 I1 Cu4 2.636(2) . ? I1 Cu2 2.642(2) . ? I1 Cu3 2.765(2) . ? I2 Cu4 2.664(2) . ? I2 Cu1 2.699(2) . ? I2 Cu3 2.704(2) . ? I3 Cu1 2.641(2) . ? I3 Cu2 2.698(2) . ? I3 Cu4 2.933(2) . ? I4 Cu3 2.676(2) . ? I4 Cu2 2.734(2) . ? I4 Cu1 2.737(2) . ? Cu1 N5 2.005(12) . ? Cu1 Cu3 2.658(2) . ? Cu1 Cu2 2.697(3) . ? Cu1 Cu4 2.815(3) . ? Cu2 N4 2.025(11) 2_666 ? Cu2 Cu4 2.714(3) . ? Cu2 Cu3 2.736(3) . ? Cu3 N8 1.983(11) 1_665 ? Cu3 Cu4 2.601(3) . ? Cu4 N1 2.018(12) . ? N1 C7 1.312(17) . ? N1 C1 1.407(17) . ? N2 C7 1.345(18) . ? N2 C6 1.366(18) . ? N2 C8 1.466(17) . ? N3 C19 1.341(16) . ? N3 C13 1.374(15) . ? N3 C12 1.479(16) . ? N4 C19 1.302(17) . ? N4 C18 1.392(15) . ? N4 Cu2 2.025(11) 2_666 ? N5 C26 1.316(17) . ? N5 C20 1.424(18) . ? N6 C26 1.343(16) . ? N6 C25 1.379(18) . ? N6 C27 1.439(17) . ? N7 C32 1.342(17) . ? N7 C38 1.346(18) . ? N7 C31 1.435(17) . ? N8 C38 1.323(17) . ? N8 C37 1.422(16) . ? N8 Cu3 1.983(11) 1_445 ? C1 C2 1.383(19) . ? C1 C6 1.397(19) . ? C2 C3 1.36(2) . ? C2 H2 0.9300 . ? C3 C4 1.39(3) . ? C3 H3 0.9300 . ? C4 C5 1.38(2) . ? C4 H4 0.9300 . ? C5 C6 1.39(2) . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.477(19) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.546(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.543(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.494(18) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.367(17) . ? C13 C14 1.378(18) . ? C14 C15 1.41(2) . ? C14 H14 0.9300 . ? C15 C16 1.34(2) . ? C15 H15 0.9300 . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 C18 1.402(18) . ? C17 H17 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.37(2) . ? C20 C25 1.38(2) . ? C21 C22 1.34(2) . ? C21 H21 0.9300 . ? C22 C23 1.37(2) . ? C22 H22 0.9300 . ? C23 C24 1.35(2) . ? C23 H23 0.9300 . ? C24 C25 1.44(2) . ? C24 H24 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.61(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.38(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.53(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.50(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C37 1.395(18) . ? C32 C33 1.43(2) . ? C33 C34 1.33(2) . ? C33 H33 0.9300 . ? C34 C35 1.42(2) . ? C34 H34 0.9300 . ? C35 C36 1.36(2) . ? C35 H35 0.9300 . ? C36 C37 1.382(18) . ? C36 H36 0.9300 . ? C38 H38 0.9300 . ? 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 Cu4 I1 Cu2 61.89(6) . . ? Cu4 I1 Cu3 57.51(6) . . ? Cu2 I1 Cu3 60.74(6) . . ? Cu4 I2 Cu1 63.33(6) . . ? Cu4 I2 Cu3 57.96(6) . . ? Cu1 I2 Cu3 58.95(6) . . ? Cu1 I3 Cu2 60.67(6) . . ? Cu1 I3 Cu4 60.41(6) . . ? Cu2 I3 Cu4 57.45(5) . . ? Cu3 I4 Cu2 60.74(6) . . ? Cu3 I4 Cu1 58.81(6) . . ? Cu2 I4 Cu1 59.07(6) . . ? N5 Cu1 I3 107.7(3) . . ? N5 Cu1 Cu3 140.0(3) . . ? I3 Cu1 Cu3 112.20(8) . . ? N5 Cu1 Cu2 143.1(4) . . ? I3 Cu1 Cu2 60.72(6) . . ? Cu3 Cu1 Cu2 61.43(7) . . ? N5 Cu1 I2 106.9(4) . . ? I3 Cu1 I2 112.36(7) . . ? Cu3 Cu1 I2 60.64(6) . . ? Cu2 Cu1 I2 109.82(7) . . ? N5 Cu1 I4 101.2(4) . . ? I3 Cu1 I4 113.63(7) . . ? Cu3 Cu1 I4 59.44(6) . . ? Cu2 Cu1 I4 60.40(6) . . ? I2 Cu1 I4 113.95(7) . . ? N5 Cu1 Cu4 152.4(4) . . ? I3 Cu1 Cu4 64.94(6) . . ? Cu3 Cu1 Cu4 56.65(7) . . ? Cu2 Cu1 Cu4 58.95(7) . . ? I2 Cu1 Cu4 57.73(6) . . ? I4 Cu1 Cu4 105.98(7) . . ? N4 Cu2 I1 112.3(3) 2_666 . ? N4 Cu2 Cu1 135.7(3) 2_666 . ? I1 Cu2 Cu1 111.92(7) . . ? N4 Cu2 I3 101.4(3) 2_666 . ? I1 Cu2 I3 117.99(7) . . ? Cu1 Cu2 I3 58.61(6) . . ? N4 Cu2 Cu4 149.8(3) 2_666 . ? I1 Cu2 Cu4 58.96(6) . . ? Cu1 Cu2 Cu4 62.70(7) . . ? I3 Cu2 Cu4 65.62(6) . . ? N4 Cu2 I4 101.2(3) 2_666 . ? I1 Cu2 I4 110.43(7) . . ? Cu1 Cu2 I4 60.52(6) . . ? I3 Cu2 I4 111.91(7) . . ? Cu4 Cu2 I4 108.96(8) . . ? N4 Cu2 Cu3 148.8(3) 2_666 . ? I1 Cu2 Cu3 61.86(6) . . ? Cu1 Cu2 Cu3 58.59(7) . . ? I3 Cu2 Cu3 108.08(7) . . ? Cu4 Cu2 Cu3 57.01(7) . . ? I4 Cu2 Cu3 58.58(6) . . ? N8 Cu3 Cu4 140.3(3) 1_665 . ? N8 Cu3 Cu1 146.1(3) 1_665 . ? Cu4 Cu3 Cu1 64.72(7) . . ? N8 Cu3 I4 105.0(3) 1_665 . ? Cu4 Cu3 I4 114.34(8) . . ? Cu1 Cu3 I4 61.74(6) . . ? N8 Cu3 I2 107.3(3) 1_665 . ? Cu4 Cu3 I2 60.23(6) . . ? Cu1 Cu3 I2 60.42(6) . . ? I4 Cu3 I2 115.80(7) . . ? N8 Cu3 Cu2 144.1(3) 1_665 . ? Cu4 Cu3 Cu2 61.08(7) . . ? Cu1 Cu3 Cu2 59.98(7) . . ? I4 Cu3 Cu2 60.68(6) . . ? I2 Cu3 Cu2 108.50(7) . . ? N8 Cu3 I1 104.5(3) 1_665 . ? Cu4 Cu3 I1 58.76(6) . . ? Cu1 Cu3 I1 109.32(8) . . ? I4 Cu3 I1 108.48(7) . . ? I2 Cu3 I1 114.68(7) . . ? Cu2 Cu3 I1 57.40(6) . . ? N1 Cu4 Cu3 161.3(4) . . ? N1 Cu4 I1 119.3(3) . . ? Cu3 Cu4 I1 63.72(6) . . ? N1 Cu4 I2 105.7(3) . . ? Cu3 Cu4 I2 61.81(6) . . ? I1 Cu4 I2 120.64(8) . . ? N1 Cu4 Cu2 136.5(4) . . ? Cu3 Cu4 Cu2 61.91(7) . . ? I1 Cu4 Cu2 59.15(6) . . ? I2 Cu4 Cu2 110.36(8) . . ? N1 Cu4 Cu1 129.2(3) . . ? Cu3 Cu4 Cu1 58.63(7) . . ? I1 Cu4 Cu1 108.45(7) . . ? I2 Cu4 Cu1 58.94(6) . . ? Cu2 Cu4 Cu1 58.36(7) . . ? N1 Cu4 I3 91.2(3) . . ? Cu3 Cu4 I3 105.12(8) . . ? I1 Cu4 I3 110.43(7) . . ? I2 Cu4 I3 104.77(7) . . ? Cu2 Cu4 I3 56.93(6) . . ? Cu1 Cu4 I3 54.65(6) . . ? C7 N1 C1 104.9(13) . . ? C7 N1 Cu4 116.0(10) . . ? C1 N1 Cu4 125.3(9) . . ? C7 N2 C6 106.7(12) . . ? C7 N2 C8 125.3(13) . . ? C6 N2 C8 127.9(13) . . ? C19 N3 C13 106.0(11) . . ? C19 N3 C12 126.5(11) . . ? C13 N3 C12 127.5(11) . . ? C19 N4 C18 104.7(11) . . ? C19 N4 Cu2 121.1(9) . 2_666 ? C18 N4 Cu2 132.3(9) . 2_666 ? C26 N5 C20 104.8(12) . . ? C26 N5 Cu1 126.4(10) . . ? C20 N5 Cu1 128.7(11) . . ? C26 N6 C25 104.1(12) . . ? C26 N6 C27 125.0(13) . . ? C25 N6 C27 130.1(11) . . ? C32 N7 C38 105.3(11) . . ? C32 N7 C31 128.3(12) . . ? C38 N7 C31 125.9(13) . . ? C38 N8 C37 103.1(12) . . ? C38 N8 Cu3 127.1(10) . 1_445 ? C37 N8 Cu3 129.8(9) . 1_445 ? C2 C1 C6 120.9(15) . . ? C2 C1 N1 131.2(14) . . ? C6 C1 N1 107.9(13) . . ? C3 C2 C1 116.4(16) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? C2 C3 C4 123.6(17) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 120.4(17) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 116.8(17) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 121.6 . . ? N2 C6 C5 131.4(15) . . ? N2 C6 C1 106.7(13) . . ? C5 C6 C1 121.9(16) . . ? N1 C7 N2 113.7(13) . . ? N1 C7 H7 123.2 . . ? N2 C7 H7 123.2 . . ? N2 C8 C9 112.2(12) . . ? N2 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 113.9(12) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 111.7(12) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 115.3(13) . . ? C12 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? N3 C12 C11 113.6(11) . . ? N3 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? N3 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C18 C13 N3 106.6(11) . . ? C18 C13 C14 122.3(12) . . ? N3 C13 C14 131.1(13) . . ? C13 C14 C15 115.6(14) . . ? C13 C14 H14 122.2 . . ? C15 C14 H14 122.2 . . ? C16 C15 C14 121.5(15) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 123.5(15) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C16 C17 C18 115.5(14) . . ? C16 C17 H17 122.2 . . ? C18 C17 H17 122.2 . . ? C13 C18 N4 109.0(11) . . ? C13 C18 C17 121.6(12) . . ? N4 C18 C17 129.3(12) . . ? N4 C19 N3 113.6(13) . . ? N4 C19 H19 123.2 . . ? N3 C19 H19 123.2 . . ? C21 C20 C25 122.8(14) . . ? C21 C20 N5 130.9(15) . . ? C25 C20 N5 106.2(14) . . ? C22 C21 C20 117.2(16) . . ? C22 C21 H21 121.4 . . ? C20 C21 H21 121.4 . . ? C21 C22 C23 123.0(18) . . ? C21 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C24 C23 C22 121.3(17) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 117.7(16) . . ? C23 C24 H24 121.2 . . ? C25 C24 H24 121.2 . . ? C20 C25 N6 109.7(12) . . ? C20 C25 C24 117.9(15) . . ? N6 C25 C24 132.3(15) . . ? N5 C26 N6 115.1(13) . . ? N5 C26 H26 122.5 . . ? N6 C26 H26 122.5 . . ? N6 C27 C28 110.8(14) . . ? N6 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 110.2(18) . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C28 C29 C30 113.0(19) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 115.5(14) . . ? C31 C30 H30A 108.4 . . ? C29 C30 H30A 108.4 . . ? C31 C30 H30B 108.4 . . ? C29 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? N7 C31 C30 114.5(13) . . ? N7 C31 H31A 108.6 . . ? C30 C31 H31A 108.6 . . ? N7 C31 H31B 108.6 . . ? C30 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? N7 C32 C37 108.9(12) . . ? N7 C32 C33 132.5(13) . . ? C37 C32 C33 118.6(14) . . ? C34 C33 C32 117.7(16) . . ? C34 C33 H33 121.1 . . ? C32 C33 H33 121.1 . . ? C33 C34 C35 123.0(16) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C36 C35 C34 120.5(16) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 117.1(15) . . ? C35 C36 H36 121.5 . . ? C37 C36 H36 121.5 . . ? C36 C37 C32 123.2(14) . . ? C36 C37 N8 129.5(14) . . ? C32 C37 N8 107.3(12) . . ? N8 C38 N7 115.3(13) . . ? N8 C38 H38 122.3 . . ? N7 C38 H38 122.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu2 I3 Cu1 N5 141.6(4) . . . . ? Cu4 I3 Cu1 N5 -151.4(4) . . . . ? Cu2 I3 Cu1 Cu3 -34.81(8) . . . . ? Cu4 I3 Cu1 Cu3 32.20(8) . . . . ? Cu4 I3 Cu1 Cu2 67.01(6) . . . . ? Cu2 I3 Cu1 I2 -100.93(8) . . . . ? Cu4 I3 Cu1 I2 -33.92(6) . . . . ? Cu2 I3 Cu1 I4 30.30(7) . . . . ? Cu4 I3 Cu1 I4 97.31(8) . . . . ? Cu2 I3 Cu1 Cu4 -67.01(6) . . . . ? Cu4 I2 Cu1 N5 154.7(4) . . . . ? Cu3 I2 Cu1 N5 -138.3(4) . . . . ? Cu4 I2 Cu1 I3 36.72(7) . . . . ? Cu3 I2 Cu1 I3 103.73(8) . . . . ? Cu4 I2 Cu1 Cu3 -67.01(7) . . . . ? Cu4 I2 Cu1 Cu2 -28.83(8) . . . . ? Cu3 I2 Cu1 Cu2 38.18(8) . . . . ? Cu4 I2 Cu1 I4 -94.35(8) . . . . ? Cu3 I2 Cu1 I4 -27.34(7) . . . . ? Cu3 I2 Cu1 Cu4 67.01(7) . . . . ? Cu3 I4 Cu1 N5 142.1(4) . . . . ? Cu2 I4 Cu1 N5 -145.6(4) . . . . ? Cu3 I4 Cu1 I3 -102.75(9) . . . . ? Cu2 I4 Cu1 I3 -30.41(7) . . . . ? Cu2 I4 Cu1 Cu3 72.34(7) . . . . ? Cu3 I4 Cu1 Cu2 -72.34(7) . . . . ? Cu3 I4 Cu1 I2 27.70(7) . . . . ? Cu2 I4 Cu1 I2 100.04(8) . . . . ? Cu3 I4 Cu1 Cu4 -33.58(7) . . . . ? Cu2 I4 Cu1 Cu4 38.76(7) . . . . ? Cu4 I1 Cu2 N4 -147.5(4) . . . 2_666 ? Cu3 I1 Cu2 N4 146.0(4) . . . 2_666 ? Cu4 I1 Cu2 Cu1 34.98(8) . . . . ? Cu3 I1 Cu2 Cu1 -31.52(8) . . . . ? Cu4 I1 Cu2 I3 -30.06(7) . . . . ? Cu3 I1 Cu2 I3 -96.56(9) . . . . ? Cu3 I1 Cu2 Cu4 -66.50(7) . . . . ? Cu4 I1 Cu2 I4 100.39(8) . . . . ? Cu3 I1 Cu2 I4 33.89(7) . . . . ? Cu4 I1 Cu2 Cu3 66.50(7) . . . . ? N5 Cu1 Cu2 N4 -7.4(8) . . . 2_666 ? I3 Cu1 Cu2 N4 73.0(5) . . . 2_666 ? Cu3 Cu1 Cu2 N4 -144.0(5) . . . 2_666 ? I2 Cu1 Cu2 N4 178.2(5) . . . 2_666 ? I4 Cu1 Cu2 N4 -74.9(5) . . . 2_666 ? Cu4 Cu1 Cu2 N4 149.7(5) . . . 2_666 ? N5 Cu1 Cu2 I1 169.3(6) . . . . ? I3 Cu1 Cu2 I1 -110.30(8) . . . . ? Cu3 Cu1 Cu2 I1 32.69(8) . . . . ? I2 Cu1 Cu2 I1 -5.14(11) . . . . ? I4 Cu1 Cu2 I1 101.81(8) . . . . ? Cu4 Cu1 Cu2 I1 -33.56(8) . . . . ? N5 Cu1 Cu2 I3 -80.4(6) . . . . ? Cu3 Cu1 Cu2 I3 143.00(8) . . . . ? I2 Cu1 Cu2 I3 105.16(8) . . . . ? I4 Cu1 Cu2 I3 -147.88(7) . . . . ? Cu4 Cu1 Cu2 I3 76.74(7) . . . . ? N5 Cu1 Cu2 Cu4 -157.2(6) . . . . ? I3 Cu1 Cu2 Cu4 -76.74(7) . . . . ? Cu3 Cu1 Cu2 Cu4 66.25(8) . . . . ? I2 Cu1 Cu2 Cu4 28.42(8) . . . . ? I4 Cu1 Cu2 Cu4 135.37(8) . . . . ? N5 Cu1 Cu2 I4 67.5(6) . . . . ? I3 Cu1 Cu2 I4 147.88(7) . . . . ? Cu3 Cu1 Cu2 I4 -69.12(7) . . . . ? I2 Cu1 Cu2 I4 -106.96(8) . . . . ? Cu4 Cu1 Cu2 I4 -135.37(8) . . . . ? N5 Cu1 Cu2 Cu3 136.6(6) . . . . ? I3 Cu1 Cu2 Cu3 -143.00(8) . . . . ? I2 Cu1 Cu2 Cu3 -37.84(8) . . . . ? I4 Cu1 Cu2 Cu3 69.12(7) . . . . ? Cu4 Cu1 Cu2 Cu3 -66.25(8) . . . . ? Cu1 I3 Cu2 N4 -137.0(3) . . . 2_666 ? Cu4 I3 Cu2 N4 151.2(3) . . . 2_666 ? Cu1 I3 Cu2 I1 99.85(9) . . . . ? Cu4 I3 Cu2 I1 28.11(7) . . . . ? Cu4 I3 Cu2 Cu1 -71.74(7) . . . . ? Cu1 I3 Cu2 Cu4 71.74(7) . . . . ? Cu1 I3 Cu2 I4 -29.92(7) . . . . ? Cu4 I3 Cu2 I4 -101.66(8) . . . . ? Cu1 I3 Cu2 Cu3 32.70(8) . . . . ? Cu4 I3 Cu2 Cu3 -39.03(7) . . . . ? Cu3 I4 Cu2 N4 -154.3(3) . . . 2_666 ? Cu1 I4 Cu2 N4 136.6(3) . . . 2_666 ? Cu3 I4 Cu2 I1 -35.18(7) . . . . ? Cu1 I4 Cu2 I1 -104.31(8) . . . . ? Cu3 I4 Cu2 Cu1 69.13(7) . . . . ? Cu3 I4 Cu2 I3 98.41(8) . . . . ? Cu1 I4 Cu2 I3 29.28(7) . . . . ? Cu3 I4 Cu2 Cu4 27.83(7) . . . . ? Cu1 I4 Cu2 Cu4 -41.30(8) . . . . ? Cu1 I4 Cu2 Cu3 -69.13(7) . . . . ? N5 Cu1 Cu3 N8 4.7(8) . . . 1_665 ? I3 Cu1 Cu3 N8 179.4(6) . . . 1_665 ? Cu2 Cu1 Cu3 N8 144.9(6) . . . 1_665 ? I2 Cu1 Cu3 N8 -76.6(6) . . . 1_665 ? I4 Cu1 Cu3 N8 74.2(6) . . . 1_665 ? Cu4 Cu1 Cu3 N8 -145.3(6) . . . 1_665 ? N5 Cu1 Cu3 Cu4 150.1(6) . . . . ? I3 Cu1 Cu3 Cu4 -35.29(8) . . . . ? Cu2 Cu1 Cu3 Cu4 -69.83(8) . . . . ? I2 Cu1 Cu3 Cu4 68.70(6) . . . . ? I4 Cu1 Cu3 Cu4 -140.47(8) . . . . ? N5 Cu1 Cu3 I4 -69.5(6) . . . . ? I3 Cu1 Cu3 I4 105.18(8) . . . . ? Cu2 Cu1 Cu3 I4 70.64(7) . . . . ? I2 Cu1 Cu3 I4 -150.83(7) . . . . ? Cu4 Cu1 Cu3 I4 140.47(8) . . . . ? N5 Cu1 Cu3 I2 81.4(6) . . . . ? I3 Cu1 Cu3 I2 -104.00(8) . . . . ? Cu2 Cu1 Cu3 I2 -138.54(8) . . . . ? I4 Cu1 Cu3 I2 150.83(7) . . . . ? Cu4 Cu1 Cu3 I2 -68.70(6) . . . . ? N5 Cu1 Cu3 Cu2 -140.1(6) . . . . ? I3 Cu1 Cu3 Cu2 34.54(8) . . . . ? I2 Cu1 Cu3 Cu2 138.54(8) . . . . ? I4 Cu1 Cu3 Cu2 -70.64(7) . . . . ? Cu4 Cu1 Cu3 Cu2 69.83(8) . . . . ? N5 Cu1 Cu3 I1 -170.6(6) . . . . ? I3 Cu1 Cu3 I1 4.05(11) . . . . ? Cu2 Cu1 Cu3 I1 -30.49(7) . . . . ? I2 Cu1 Cu3 I1 108.05(8) . . . . ? I4 Cu1 Cu3 I1 -101.12(8) . . . . ? Cu4 Cu1 Cu3 I1 39.35(7) . . . . ? Cu2 I4 Cu3 N8 144.2(3) . . . 1_665 ? Cu1 I4 Cu3 N8 -146.2(3) . . . 1_665 ? Cu2 I4 Cu3 Cu4 -30.37(8) . . . . ? Cu1 I4 Cu3 Cu4 39.17(8) . . . . ? Cu2 I4 Cu3 Cu1 -69.55(7) . . . . ? Cu2 I4 Cu3 I2 -97.63(8) . . . . ? Cu1 I4 Cu3 I2 -28.09(7) . . . . ? Cu1 I4 Cu3 Cu2 69.55(7) . . . . ? Cu2 I4 Cu3 I1 32.95(6) . . . . ? Cu1 I4 Cu3 I1 102.49(8) . . . . ? Cu4 I2 Cu3 N8 -138.6(3) . . . 1_665 ? Cu1 I2 Cu3 N8 145.3(3) . . . 1_665 ? Cu1 I2 Cu3 Cu4 -76.05(8) . . . . ? Cu4 I2 Cu3 Cu1 76.05(8) . . . . ? Cu4 I2 Cu3 I4 104.53(9) . . . . ? Cu1 I2 Cu3 I4 28.48(7) . . . . ? Cu4 I2 Cu3 Cu2 38.85(8) . . . . ? Cu1 I2 Cu3 Cu2 -37.20(8) . . . . ? Cu4 I2 Cu3 I1 -23.03(7) . . . . ? Cu1 I2 Cu3 I1 -99.08(8) . . . . ? N4 Cu2 Cu3 N8 -19.1(9) 2_666 . . 1_665 ? I1 Cu2 Cu3 N8 67.9(5) . . . 1_665 ? Cu1 Cu2 Cu3 N8 -146.7(6) . . . 1_665 ? I3 Cu2 Cu3 N8 -179.5(5) . . . 1_665 ? Cu4 Cu2 Cu3 N8 137.4(6) . . . 1_665 ? I4 Cu2 Cu3 N8 -74.4(5) . . . 1_665 ? N4 Cu2 Cu3 Cu4 -156.5(6) 2_666 . . . ? I1 Cu2 Cu3 Cu4 -69.51(7) . . . . ? Cu1 Cu2 Cu3 Cu4 75.86(8) . . . . ? I3 Cu2 Cu3 Cu4 43.14(8) . . . . ? I4 Cu2 Cu3 Cu4 148.24(8) . . . . ? N4 Cu2 Cu3 Cu1 127.6(6) 2_666 . . . ? I1 Cu2 Cu3 Cu1 -145.37(8) . . . . ? I3 Cu2 Cu3 Cu1 -32.71(7) . . . . ? Cu4 Cu2 Cu3 Cu1 -75.86(8) . . . . ? I4 Cu2 Cu3 Cu1 72.39(7) . . . . ? N4 Cu2 Cu3 I4 55.2(6) 2_666 . . . ? I1 Cu2 Cu3 I4 142.24(7) . . . . ? Cu1 Cu2 Cu3 I4 -72.39(7) . . . . ? I3 Cu2 Cu3 I4 -105.10(8) . . . . ? Cu4 Cu2 Cu3 I4 -148.24(8) . . . . ? N4 Cu2 Cu3 I2 165.0(6) 2_666 . . . ? I1 Cu2 Cu3 I2 -107.98(8) . . . . ? Cu1 Cu2 Cu3 I2 37.39(7) . . . . ? I3 Cu2 Cu3 I2 4.68(10) . . . . ? Cu4 Cu2 Cu3 I2 -38.47(7) . . . . ? I4 Cu2 Cu3 I2 109.78(8) . . . . ? N4 Cu2 Cu3 I1 -87.0(6) 2_666 . . . ? Cu1 Cu2 Cu3 I1 145.37(8) . . . . ? I3 Cu2 Cu3 I1 112.66(8) . . . . ? Cu4 Cu2 Cu3 I1 69.51(7) . . . . ? I4 Cu2 Cu3 I1 -142.24(7) . . . . ? Cu4 I1 Cu3 N8 140.6(3) . . . 1_665 ? Cu2 I1 Cu3 N8 -145.9(3) . . . 1_665 ? Cu2 I1 Cu3 Cu4 73.53(7) . . . . ? Cu4 I1 Cu3 Cu1 -42.10(8) . . . . ? Cu2 I1 Cu3 Cu1 31.43(8) . . . . ? Cu4 I1 Cu3 I4 -107.79(8) . . . . ? Cu2 I1 Cu3 I4 -34.25(7) . . . . ? Cu4 I1 Cu3 I2 23.40(7) . . . . ? Cu2 I1 Cu3 I2 96.93(8) . . . . ? Cu4 I1 Cu3 Cu2 -73.53(7) . . . . ? N8 Cu3 Cu4 N1 29.8(12) 1_665 . . . ? Cu1 Cu3 Cu4 N1 -120.4(11) . . . . ? I4 Cu3 Cu4 N1 -158.3(11) . . . . ? I2 Cu3 Cu4 N1 -51.4(11) . . . . ? Cu2 Cu3 Cu4 N1 171.4(11) . . . . ? I1 Cu3 Cu4 N1 104.1(11) . . . . ? N8 Cu3 Cu4 I1 -74.2(5) 1_665 . . . ? Cu1 Cu3 Cu4 I1 135.59(8) . . . . ? I4 Cu3 Cu4 I1 97.61(8) . . . . ? I2 Cu3 Cu4 I1 -155.44(7) . . . . ? Cu2 Cu3 Cu4 I1 67.37(6) . . . . ? N8 Cu3 Cu4 I2 81.2(5) 1_665 . . . ? Cu1 Cu3 Cu4 I2 -68.97(6) . . . . ? I4 Cu3 Cu4 I2 -106.95(8) . . . . ? Cu2 Cu3 Cu4 I2 -137.19(8) . . . . ? I1 Cu3 Cu4 I2 155.44(7) . . . . ? N8 Cu3 Cu4 Cu2 -141.6(5) 1_665 . . . ? Cu1 Cu3 Cu4 Cu2 68.22(7) . . . . ? I4 Cu3 Cu4 Cu2 30.24(8) . . . . ? I2 Cu3 Cu4 Cu2 137.19(8) . . . . ? I1 Cu3 Cu4 Cu2 -67.37(6) . . . . ? N8 Cu3 Cu4 Cu1 150.2(5) 1_665 . . . ? I4 Cu3 Cu4 Cu1 -37.98(8) . . . . ? I2 Cu3 Cu4 Cu1 68.97(6) . . . . ? Cu2 Cu3 Cu4 Cu1 -68.22(7) . . . . ? I1 Cu3 Cu4 Cu1 -135.59(8) . . . . ? N8 Cu3 Cu4 I3 -179.9(5) 1_665 . . . ? Cu1 Cu3 Cu4 I3 29.93(7) . . . . ? I4 Cu3 Cu4 I3 -8.04(10) . . . . ? I2 Cu3 Cu4 I3 98.91(7) . . . . ? Cu2 Cu3 Cu4 I3 -38.29(7) . . . . ? I1 Cu3 Cu4 I3 -105.66(7) . . . . ? Cu2 I1 Cu4 N1 129.4(4) . . . . ? Cu3 I1 Cu4 N1 -159.1(4) . . . . ? Cu2 I1 Cu4 Cu3 -71.53(7) . . . . ? Cu2 I1 Cu4 I2 -96.73(10) . . . . ? Cu3 I1 Cu4 I2 -25.21(7) . . . . ? Cu3 I1 Cu4 Cu2 71.53(7) . . . . ? Cu2 I1 Cu4 Cu1 -32.49(8) . . . . ? Cu3 I1 Cu4 Cu1 39.04(7) . . . . ? Cu2 I1 Cu4 I3 25.74(7) . . . . ? Cu3 I1 Cu4 I3 97.27(8) . . . . ? Cu1 I2 Cu4 N1 -126.6(4) . . . . ? Cu3 I2 Cu4 N1 164.9(4) . . . . ? Cu1 I2 Cu4 Cu3 68.49(7) . . . . ? Cu1 I2 Cu4 I1 94.16(9) . . . . ? Cu3 I2 Cu4 I1 25.67(8) . . . . ? Cu1 I2 Cu4 Cu2 28.74(8) . . . . ? Cu3 I2 Cu4 Cu2 -39.75(8) . . . . ? Cu3 I2 Cu4 Cu1 -68.49(7) . . . . ? Cu1 I2 Cu4 I3 -30.99(6) . . . . ? Cu3 I2 Cu4 I3 -99.48(8) . . . . ? N4 Cu2 Cu4 N1 -20.2(8) 2_666 . . . ? I1 Cu2 Cu4 N1 -101.4(5) . . . . ? Cu1 Cu2 Cu4 N1 115.3(5) . . . . ? I3 Cu2 Cu4 N1 49.5(5) . . . . ? I4 Cu2 Cu4 N1 155.6(5) . . . . ? Cu3 Cu2 Cu4 N1 -176.0(5) . . . . ? N4 Cu2 Cu4 Cu3 155.8(6) 2_666 . . . ? I1 Cu2 Cu4 Cu3 74.59(7) . . . . ? Cu1 Cu2 Cu4 Cu3 -68.64(8) . . . . ? I3 Cu2 Cu4 Cu3 -134.46(8) . . . . ? I4 Cu2 Cu4 Cu3 -28.35(7) . . . . ? N4 Cu2 Cu4 I1 81.2(6) 2_666 . . . ? Cu1 Cu2 Cu4 I1 -143.24(8) . . . . ? I3 Cu2 Cu4 I1 150.95(7) . . . . ? I4 Cu2 Cu4 I1 -102.95(7) . . . . ? Cu3 Cu2 Cu4 I1 -74.59(7) . . . . ? N4 Cu2 Cu4 I2 -164.5(6) 2_666 . . . ? I1 Cu2 Cu4 I2 114.30(8) . . . . ? Cu1 Cu2 Cu4 I2 -28.94(8) . . . . ? I3 Cu2 Cu4 I2 -94.75(8) . . . . ? I4 Cu2 Cu4 I2 11.35(10) . . . . ? Cu3 Cu2 Cu4 I2 39.71(7) . . . . ? N4 Cu2 Cu4 Cu1 -135.6(6) 2_666 . . . ? I1 Cu2 Cu4 Cu1 143.24(8) . . . . ? I3 Cu2 Cu4 Cu1 -65.82(6) . . . . ? I4 Cu2 Cu4 Cu1 40.29(7) . . . . ? Cu3 Cu2 Cu4 Cu1 68.64(8) . . . . ? N4 Cu2 Cu4 I3 -69.8(6) 2_666 . . . ? I1 Cu2 Cu4 I3 -150.95(7) . . . . ? Cu1 Cu2 Cu4 I3 65.82(6) . . . . ? I4 Cu2 Cu4 I3 106.11(7) . . . . ? Cu3 Cu2 Cu4 I3 134.46(8) . . . . ? N5 Cu1 Cu4 N1 23.1(9) . . . . ? I3 Cu1 Cu4 N1 -57.1(5) . . . . ? Cu3 Cu1 Cu4 N1 159.1(5) . . . . ? Cu2 Cu1 Cu4 N1 -126.7(5) . . . . ? I2 Cu1 Cu4 N1 85.3(5) . . . . ? I4 Cu1 Cu4 N1 -166.1(5) . . . . ? N5 Cu1 Cu4 Cu3 -136.0(8) . . . . ? I3 Cu1 Cu4 Cu3 143.80(8) . . . . ? Cu2 Cu1 Cu4 Cu3 74.21(8) . . . . ? I2 Cu1 Cu4 Cu3 -73.82(7) . . . . ? I4 Cu1 Cu4 Cu3 34.76(8) . . . . ? N5 Cu1 Cu4 I1 -177.4(8) . . . . ? I3 Cu1 Cu4 I1 102.39(8) . . . . ? Cu3 Cu1 Cu4 I1 -41.41(8) . . . . ? Cu2 Cu1 Cu4 I1 32.80(7) . . . . ? I2 Cu1 Cu4 I1 -115.23(8) . . . . ? I4 Cu1 Cu4 I1 -6.65(10) . . . . ? N5 Cu1 Cu4 I2 -62.2(8) . . . . ? I3 Cu1 Cu4 I2 -142.38(7) . . . . ? Cu3 Cu1 Cu4 I2 73.82(7) . . . . ? Cu2 Cu1 Cu4 I2 148.03(8) . . . . ? I4 Cu1 Cu4 I2 108.58(8) . . . . ? N5 Cu1 Cu4 Cu2 149.8(8) . . . . ? I3 Cu1 Cu4 Cu2 69.60(6) . . . . ? Cu3 Cu1 Cu4 Cu2 -74.21(8) . . . . ? I2 Cu1 Cu4 Cu2 -148.03(8) . . . . ? I4 Cu1 Cu4 Cu2 -39.45(7) . . . . ? N5 Cu1 Cu4 I3 80.2(8) . . . . ? Cu3 Cu1 Cu4 I3 -143.80(8) . . . . ? Cu2 Cu1 Cu4 I3 -69.60(6) . . . . ? I2 Cu1 Cu4 I3 142.38(7) . . . . ? I4 Cu1 Cu4 I3 -109.04(8) . . . . ? Cu1 I3 Cu4 N1 139.4(3) . . . . ? Cu2 I3 Cu4 N1 -148.4(4) . . . . ? Cu1 I3 Cu4 Cu3 -31.49(8) . . . . ? Cu2 I3 Cu4 Cu3 40.71(8) . . . . ? Cu1 I3 Cu4 I1 -98.61(8) . . . . ? Cu2 I3 Cu4 I1 -26.42(7) . . . . ? Cu1 I3 Cu4 I2 32.74(6) . . . . ? Cu2 I3 Cu4 I2 104.94(8) . . . . ? Cu1 I3 Cu4 Cu2 -72.20(7) . . . . ? Cu2 I3 Cu4 Cu1 72.20(7) . . . . ? Cu3 Cu4 N1 C7 96.8(15) . . . . ? I1 Cu4 N1 C7 -169.0(10) . . . . ? I2 Cu4 N1 C7 51.1(12) . . . . ? Cu2 Cu4 N1 C7 -94.3(12) . . . . ? Cu1 Cu4 N1 C7 -11.4(13) . . . . ? I3 Cu4 N1 C7 -54.7(11) . . . . ? Cu3 Cu4 N1 C1 -129.3(11) . . . . ? I1 Cu4 N1 C1 -35.1(12) . . . . ? I2 Cu4 N1 C1 -175.0(10) . . . . ? Cu2 Cu4 N1 C1 39.7(13) . . . . ? Cu1 Cu4 N1 C1 122.5(10) . . . . ? I3 Cu4 N1 C1 79.3(11) . . . . ? I3 Cu1 N5 C26 115.4(11) . . . . ? Cu3 Cu1 N5 C26 -69.8(13) . . . . ? Cu2 Cu1 N5 C26 179.9(9) . . . . ? I2 Cu1 N5 C26 -5.6(12) . . . . ? I4 Cu1 N5 C26 -125.1(11) . . . . ? Cu4 Cu1 N5 C26 45.8(16) . . . . ? I3 Cu1 N5 C20 -65.7(12) . . . . ? Cu3 Cu1 N5 C20 109.1(11) . . . . ? Cu2 Cu1 N5 C20 -1.1(15) . . . . ? I2 Cu1 N5 C20 173.4(11) . . . . ? I4 Cu1 N5 C20 53.8(12) . . . . ? Cu4 Cu1 N5 C20 -135.2(10) . . . . ? C7 N1 C1 C2 -179.6(14) . . . . ? Cu4 N1 C1 C2 42(2) . . . . ? C7 N1 C1 C6 1.6(15) . . . . ? Cu4 N1 C1 C6 -136.4(10) . . . . ? C6 C1 C2 C3 -2(2) . . . . ? N1 C1 C2 C3 179.5(14) . . . . ? C1 C2 C3 C4 3(2) . . . . ? C2 C3 C4 C5 -3(3) . . . . ? C3 C4 C5 C6 2(3) . . . . ? C7 N2 C6 C5 -179.6(16) . . . . ? C8 N2 C6 C5 -2(2) . . . . ? C7 N2 C6 C1 2.9(15) . . . . ? C8 N2 C6 C1 -179.3(13) . . . . ? C4 C5 C6 N2 -177.6(15) . . . . ? C4 C5 C6 C1 0(2) . . . . ? C2 C1 C6 N2 178.3(12) . . . . ? N1 C1 C6 N2 -2.8(14) . . . . ? C2 C1 C6 C5 0(2) . . . . ? N1 C1 C6 C5 179.4(13) . . . . ? C1 N1 C7 N2 0.3(17) . . . . ? Cu4 N1 C7 N2 142.8(10) . . . . ? C6 N2 C7 N1 -2.1(17) . . . . ? C8 N2 C7 N1 -179.9(13) . . . . ? C7 N2 C8 C9 -104.6(17) . . . . ? C6 N2 C8 C9 78.0(19) . . . . ? N2 C8 C9 C10 179.6(13) . . . . ? C8 C9 C10 C11 -75.4(18) . . . . ? C9 C10 C11 C12 -174.7(12) . . . . ? C19 N3 C12 C11 -5(2) . . . . ? C13 N3 C12 C11 175.4(13) . . . . ? C10 C11 C12 N3 -71.1(16) . . . . ? C19 N3 C13 C18 2.5(15) . . . . ? C12 N3 C13 C18 -177.8(13) . . . . ? C19 N3 C13 C14 -177.9(15) . . . . ? C12 N3 C13 C14 2(2) . . . . ? C18 C13 C14 C15 -1(2) . . . . ? N3 C13 C14 C15 179.6(14) . . . . ? C13 C14 C15 C16 0(2) . . . . ? C14 C15 C16 C17 1(3) . . . . ? C15 C16 C17 C18 0(2) . . . . ? N3 C13 C18 N4 -2.4(16) . . . . ? C14 C13 C18 N4 178.1(13) . . . . ? N3 C13 C18 C17 -178.6(13) . . . . ? C14 C13 C18 C17 2(2) . . . . ? C19 N4 C18 C13 1.3(16) . . . . ? Cu2 N4 C18 C13 165.4(10) 2_666 . . . ? C19 N4 C18 C17 177.1(15) . . . . ? Cu2 N4 C18 C17 -19(2) 2_666 . . . ? C16 C17 C18 C13 -1(2) . . . . ? C16 C17 C18 N4 -176.7(14) . . . . ? C18 N4 C19 N3 0.4(18) . . . . ? Cu2 N4 C19 N3 -166.0(9) 2_666 . . . ? C13 N3 C19 N4 -1.9(17) . . . . ? C12 N3 C19 N4 178.5(13) . . . . ? C26 N5 C20 C21 -180.0(16) . . . . ? Cu1 N5 C20 C21 1(2) . . . . ? C26 N5 C20 C25 0.6(15) . . . . ? Cu1 N5 C20 C25 -178.6(10) . . . . ? C25 C20 C21 C22 2(2) . . . . ? N5 C20 C21 C22 -177.0(15) . . . . ? C20 C21 C22 C23 -2(3) . . . . ? C21 C22 C23 C24 1(3) . . . . ? C22 C23 C24 C25 0(3) . . . . ? C21 C20 C25 N6 179.8(14) . . . . ? N5 C20 C25 N6 -0.7(16) . . . . ? C21 C20 C25 C24 -2(2) . . . . ? N5 C20 C25 C24 177.5(12) . . . . ? C26 N6 C25 C20 0.6(16) . . . . ? C27 N6 C25 C20 -169.9(14) . . . . ? C26 N6 C25 C24 -177.2(16) . . . . ? C27 N6 C25 C24 12(3) . . . . ? C23 C24 C25 C20 1(2) . . . . ? C23 C24 C25 N6 178.6(16) . . . . ? C20 N5 C26 N6 -0.2(16) . . . . ? Cu1 N5 C26 N6 178.9(9) . . . . ? C25 N6 C26 N5 -0.2(16) . . . . ? C27 N6 C26 N5 170.9(13) . . . . ? C26 N6 C27 C28 -108.4(16) . . . . ? C25 N6 C27 C28 60(2) . . . . ? N6 C27 C28 C29 177.4(16) . . . . ? C27 C28 C29 C30 162.8(16) . . . . ? C28 C29 C30 C31 -62(2) . . . . ? C32 N7 C31 C30 83(2) . . . . ? C38 N7 C31 C30 -87(2) . . . . ? C29 C30 C31 N7 -161.1(16) . . . . ? C38 N7 C32 C37 -1.8(16) . . . . ? C31 N7 C32 C37 -173.7(14) . . . . ? C38 N7 C32 C33 179.8(16) . . . . ? C31 N7 C32 C33 8(3) . . . . ? N7 C32 C33 C34 178.6(16) . . . . ? C37 C32 C33 C34 0(2) . . . . ? C32 C33 C34 C35 -1(3) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C34 C35 C36 C37 1(2) . . . . ? C35 C36 C37 C32 -2(2) . . . . ? C35 C36 C37 N8 -179.1(13) . . . . ? N7 C32 C37 C36 -177.2(13) . . . . ? C33 C32 C37 C36 1(2) . . . . ? N7 C32 C37 N8 0.5(15) . . . . ? C33 C32 C37 N8 179.1(12) . . . . ? C38 N8 C37 C36 178.6(15) . . . . ? Cu3 N8 C37 C36 1(2) 1_445 . . . ? C38 N8 C37 C32 1.0(14) . . . . ? Cu3 N8 C37 C32 -176.3(9) 1_445 . . . ? C37 N8 C38 N7 -2.3(17) . . . . ? Cu3 N8 C38 N7 175.1(10) 1_445 . . . ? C32 N7 C38 N8 2.7(18) . . . . ? C31 N7 C38 N8 174.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.818 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.197 #===END