# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 891591' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C20 H10 Cu I N4)(I3 Pb)(C1.5 H3.5 N0.5 O0.5)(H2 O)' _chemical_formula_sum 'C21.50 H20.50 Cu I4 N4.50 O Pb' _chemical_formula_weight 1136.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pb Pb -3.3944 10.1111 '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 triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.860(5) _cell_length_b 14.713(5) _cell_length_c 7.995(3) _cell_angle_alpha 104.946(3) _cell_angle_beta 82.3390(10) _cell_angle_gamma 68.821(3) _cell_volume 1626.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4570 _cell_measurement_theta_min 2.6568 _cell_measurement_theta_max 27.4855 _exptl_crystal_description sheet _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 9.636 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4458 _exptl_absorpt_correction_T_max 0.6444 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Ultrax-Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11996 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5724 _reflns_number_gt 4617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5724 _refine_ls_number_parameters 334 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.066 _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 Pb1 Pb 0.5000 0.5000 0.0000 0.03946(8) Uani 1 2 d S . . Pb2 Pb 0.5000 0.5000 -0.5000 0.03999(8) Uani 1 2 d S . . I1 I 0.48660(3) 0.32866(3) 0.17213(5) 0.05451(11) Uani 1 1 d . . . I2 I 0.36377(3) 0.67489(3) 0.36752(5) 0.05152(12) Uani 1 1 d . . . I3 I 0.33676(3) 0.50168(3) -0.20546(5) 0.04656(10) Uani 1 1 d . . . I4 I -0.04768(3) 0.73384(3) 1.04930(6) 0.05952(11) Uani 1 1 d . . . Cu1 Cu -0.02210(5) 0.77055(4) 0.74078(9) 0.03931(17) Uani 1 1 d . . . C11 C 0.1472(5) 0.6136(4) 0.4219(8) 0.0577(19) Uani 1 1 d . . . H11A H 0.1834 0.6431 0.4776 0.069 Uiso 1 1 calc R . . C12 C 0.1889(6) 0.5348(5) 0.2596(9) 0.068(2) Uani 1 1 d . . . H12A H 0.2523 0.5113 0.2075 0.082 Uiso 1 1 calc R . . C13 C 0.1364(5) 0.4921(4) 0.1774(8) 0.060(2) Uani 1 1 d . . . H13A H 0.1628 0.4403 0.0664 0.072 Uiso 1 1 calc R . . C14 C 0.0444(5) 0.5258(4) 0.2586(7) 0.0513(17) Uani 1 1 d . . . H14A H 0.0087 0.4943 0.2060 0.062 Uiso 1 1 calc R . . C15 C 0.0040(4) 0.6061(4) 0.4178(7) 0.0413(15) Uani 1 1 d . . . C16 C -0.0950(4) 0.6503(4) 0.5133(7) 0.0404(14) Uani 1 1 d . . . C17 C -0.1597(5) 0.6169(4) 0.4544(8) 0.0559(17) Uani 1 1 d . . . H17A H -0.1423 0.5645 0.3454 0.067 Uiso 1 1 calc R . . C18 C -0.2473(5) 0.6598(5) 0.5534(10) 0.0683(19) Uani 1 1 d . . . H18A H -0.2907 0.6359 0.5150 0.082 Uiso 1 1 calc R . . C19 C -0.2741(5) 0.7391(5) 0.7122(10) 0.065(2) Uani 1 1 d . . . H19A H -0.3355 0.7704 0.7812 0.078 Uiso 1 1 calc R . . C20 C -0.2083(4) 0.7705(4) 0.7653(9) 0.0512(16) Uani 1 1 d . . . H20A H -0.2253 0.8239 0.8728 0.061 Uiso 1 1 calc R . . C21 C 0.1545(4) 0.7655(4) 0.8292(8) 0.0476(16) Uani 1 1 d . . . H21A H 0.1635 0.7010 0.8382 0.057 Uiso 1 1 calc R . . C22 C 0.2223(4) 0.8006(5) 0.8564(9) 0.0547(18) Uani 1 1 d . . . H22A H 0.2766 0.7600 0.8801 0.066 Uiso 1 1 calc R . . C23 C 0.2088(5) 0.8942(5) 0.8480(8) 0.0600(19) Uani 1 1 d . . . H23A H 0.2539 0.9195 0.8677 0.072 Uiso 1 1 calc R . . C24 C 0.1278(4) 0.9542(4) 0.8101(8) 0.0495(16) Uani 1 1 d . . . H24A H 0.1176 1.0196 0.8047 0.059 Uiso 1 1 calc R . . C25 C 0.0638(4) 0.9137(4) 0.7811(7) 0.0355(13) Uani 1 1 d . . . C26 C -0.0248(4) 0.9681(4) 0.7353(7) 0.0372(14) Uani 1 1 d . . . C27 C -0.0533(5) 1.0676(4) 0.7256(8) 0.0494(17) Uani 1 1 d . . . H27A H -0.0166 1.1042 0.7474 0.059 Uiso 1 1 calc R . . C28 C -0.1358(5) 1.1101(4) 0.6837(9) 0.0557(19) Uani 1 1 d . . . H28A H -0.1555 1.1761 0.6752 0.067 Uiso 1 1 calc R . . C29 C -0.1898(5) 1.0566(4) 0.6540(9) 0.0579(19) Uani 1 1 d . . . H29A H -0.2467 1.0855 0.6267 0.069 Uiso 1 1 calc R . . C30 C -0.1582(4) 0.9594(4) 0.6655(9) 0.0532(17) Uani 1 1 d . . . H30A H -0.1947 0.9226 0.6434 0.064 Uiso 1 1 calc R . . C31 C -0.4676(7) 0.8221(10) 0.3446(19) 0.177(9) Uani 0.50 1 d PDU . . H31A H -0.4420 0.7871 0.2182 0.265 Uiso 0.50 1 calc PR . . H31B H -0.5270 0.8782 0.3656 0.265 Uiso 0.50 1 calc PR . . H31C H -0.4755 0.7745 0.4010 0.265 Uiso 0.50 1 calc PR . . C32 C -0.3379(9) 0.8249(14) 0.2691(13) 0.186(9) Uani 0.50 1 d PD . . H32A H -0.2918 0.8498 0.2998 0.279 Uiso 0.50 1 calc PR . . H32B H -0.3610 0.8493 0.1768 0.279 Uiso 0.50 1 calc PR . . H32C H -0.3101 0.7507 0.2271 0.279 Uiso 0.50 1 calc PR . . C33 C -0.4188(7) 0.9143(9) 0.5855(10) 0.121(6) Uani 0.50 1 d PDU . . H33A H -0.4650 0.9210 0.6787 0.145 Uiso 0.50 1 calc PR . . N11 N 0.0558(3) 0.6493(3) 0.5023(6) 0.0431(12) Uani 1 1 d . . . N12 N -0.1208(3) 0.7274(3) 0.6690(6) 0.0417(12) Uani 1 1 d . . . N21 N 0.0763(3) 0.8188(3) 0.7907(6) 0.0378(12) Uani 1 1 d . . . N22 N -0.0784(3) 0.9144(3) 0.7063(6) 0.0401(12) Uani 1 1 d . . . N31 N -0.4085(5) 0.8596(6) 0.4137(10) 0.050(3) Uani 0.50 1 d PD . . O31 O -0.3586(7) 0.9585(8) 0.6143(19) 0.110(4) Uani 0.50 1 d PD . . O1W O -0.3869(7) 1.0237(7) 0.9690(15) 0.137(6) Uani 0.50 1 d PD . . H1WA H -0.3431(16) 0.995(2) 1.013(4) 0.206 Uiso 0.50 1 d PD . . H1WB H -0.365(2) 1.053(2) 0.908(5) 0.206 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 Pb1 0.03574(16) 0.05013(14) 0.03179(15) 0.01683(11) -0.00836(12) -0.01474(13) Pb2 0.03761(16) 0.04938(15) 0.03234(15) 0.01662(11) -0.00899(12) -0.01508(13) I1 0.0623(2) 0.05945(19) 0.0545(2) 0.02143(16) -0.01572(19) -0.03697(18) I2 0.0386(2) 0.0500(2) 0.0469(2) 0.01476(16) -0.00293(18) -0.00098(17) I3 0.03503(19) 0.05950(19) 0.0462(2) 0.01906(16) -0.01101(16) -0.01937(16) I4 0.0859(3) 0.05923(19) 0.0603(2) 0.03125(16) -0.0323(2) -0.04682(18) Cu1 0.0335(3) 0.0336(3) 0.0484(4) 0.0092(3) -0.0110(3) -0.0140(3) C11 0.052(4) 0.055(3) 0.054(4) 0.012(3) 0.006(3) -0.020(3) C12 0.067(5) 0.058(3) 0.058(4) 0.011(3) 0.017(4) -0.018(3) C13 0.079(5) 0.046(3) 0.034(3) 0.005(2) 0.001(3) -0.014(3) C14 0.077(4) 0.042(3) 0.038(3) 0.014(2) -0.019(3) -0.026(3) C15 0.055(3) 0.034(2) 0.038(3) 0.017(2) -0.010(3) -0.020(2) C16 0.047(3) 0.036(2) 0.051(3) 0.022(2) -0.020(3) -0.024(2) C17 0.070(4) 0.059(3) 0.055(4) 0.021(3) -0.033(3) -0.038(3) C18 0.069(4) 0.092(4) 0.078(4) 0.036(3) -0.037(3) -0.057(3) C19 0.041(3) 0.073(4) 0.089(5) 0.031(3) -0.015(3) -0.030(3) C20 0.043(3) 0.055(3) 0.057(4) 0.014(3) -0.013(3) -0.025(3) C21 0.037(3) 0.040(3) 0.056(4) 0.009(2) -0.014(3) -0.010(2) C22 0.032(3) 0.057(3) 0.058(4) 0.005(3) -0.008(3) -0.010(3) C23 0.049(3) 0.077(4) 0.051(4) 0.001(3) -0.006(3) -0.039(3) C24 0.052(3) 0.055(3) 0.047(3) 0.010(2) -0.007(3) -0.035(3) C25 0.032(3) 0.043(2) 0.027(3) 0.004(2) -0.002(2) -0.017(2) C26 0.038(3) 0.035(2) 0.032(3) 0.011(2) -0.001(2) -0.012(2) C27 0.060(4) 0.040(3) 0.045(3) 0.012(2) -0.009(3) -0.020(3) C28 0.056(4) 0.043(3) 0.061(4) 0.028(3) -0.013(3) -0.005(3) C29 0.056(4) 0.048(3) 0.069(4) 0.024(3) -0.032(3) -0.012(3) C30 0.044(3) 0.052(3) 0.064(4) 0.022(3) -0.022(3) -0.016(3) C31 0.183(16) 0.069(9) 0.248(16) 0.075(10) -0.015(13) -0.017(10) C32 0.085(15) 0.272(14) 0.242(16) 0.236(12) -0.016(12) -0.023(14) C33 0.118(9) 0.099(7) 0.138(8) 0.074(6) -0.046(7) -0.007(6) N11 0.044(3) 0.040(2) 0.046(3) 0.0125(19) -0.008(2) -0.020(2) N12 0.040(2) 0.043(2) 0.042(3) 0.0111(19) -0.010(2) -0.0180(19) N21 0.030(2) 0.0305(19) 0.047(3) 0.0097(18) -0.011(2) -0.0069(18) N22 0.042(2) 0.036(2) 0.042(2) 0.0122(18) -0.018(2) -0.0138(19) N31 0.069(6) 0.024(4) 0.058(6) 0.012(4) -0.046(5) -0.011(4) O31 0.068(6) 0.108(7) 0.191(11) 0.074(7) -0.082(7) -0.044(6) O1W 0.120(11) 0.060(6) 0.145(11) -0.041(7) 0.053(9) -0.023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I2 3.2115(8) 2_665 ? Pb1 I2 3.2115(8) . ? Pb1 I1 3.2238(9) . ? Pb1 I1 3.2238(9) 2_665 ? Pb1 I3 3.2420(9) . ? Pb1 I3 3.2420(9) 2_665 ? Pb2 I1 3.2247(8) 1_554 ? Pb2 I1 3.2247(8) 2_665 ? Pb2 I2 3.2265(8) 2_665 ? Pb2 I2 3.2265(8) 1_554 ? Pb2 I3 3.2476(9) . ? Pb2 I3 3.2476(9) 2_664 ? I1 Pb2 3.2247(8) 1_556 ? I2 Pb2 3.2265(8) 1_556 ? I4 Cu1 2.6682(11) . ? Cu1 N21 1.980(5) . ? Cu1 N12 1.988(5) . ? Cu1 N22 2.086(4) . ? Cu1 N11 2.090(4) . ? C11 N11 1.349(8) . ? C11 C12 1.381(8) . ? C11 H11A 0.9300 . ? C12 C13 1.353(11) . ? C12 H12A 0.9300 . ? C13 C14 1.362(10) . ? C13 H13A 0.9300 . ? C14 C15 1.373(7) . ? C14 H14A 0.9300 . ? C15 N11 1.357(8) . ? C15 C16 1.468(8) . ? C16 N12 1.344(6) . ? C16 C17 1.375(9) . ? C17 C18 1.331(9) . ? C17 H17A 0.9300 . ? C18 C19 1.374(9) . ? C18 H18A 0.9300 . ? C19 C20 1.361(9) . ? C19 H19A 0.9300 . ? C20 N12 1.321(7) . ? C20 H20A 0.9300 . ? C21 N21 1.331(7) . ? C21 C22 1.369(9) . ? C21 H21A 0.9300 . ? C22 C23 1.336(9) . ? C22 H22A 0.9300 . ? C23 C24 1.395(9) . ? C23 H23A 0.9300 . ? C24 C25 1.367(8) . ? C24 H24A 0.9300 . ? C25 N21 1.361(7) . ? C25 C26 1.491(8) . ? C26 N22 1.359(7) . ? C26 C27 1.394(7) . ? C27 C28 1.361(9) . ? C27 H27A 0.9300 . ? C28 C29 1.362(10) . ? C28 H28A 0.9300 . ? C29 C30 1.367(8) . ? C29 H29A 0.9300 . ? C30 N22 1.326(8) . ? C30 H30A 0.9300 . ? C31 N31 1.356(8) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N31 1.338(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O31 1.350(9) . ? C33 N31 1.355(7) . ? C33 H33A 0.9300 . ? O1W H1WA 0.847(10) . ? O1W H1WB 0.850(10) . ? 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 I2 Pb1 I2 180.00(2) 2_665 . ? I2 Pb1 I1 91.68(3) 2_665 . ? I2 Pb1 I1 88.32(3) . . ? I2 Pb1 I1 88.32(3) 2_665 2_665 ? I2 Pb1 I1 91.68(3) . 2_665 ? I1 Pb1 I1 180.000(6) . 2_665 ? I2 Pb1 I3 84.13(2) 2_665 . ? I2 Pb1 I3 95.87(2) . . ? I1 Pb1 I3 95.059(17) . . ? I1 Pb1 I3 84.941(17) 2_665 . ? I2 Pb1 I3 95.87(2) 2_665 2_665 ? I2 Pb1 I3 84.13(2) . 2_665 ? I1 Pb1 I3 84.941(17) . 2_665 ? I1 Pb1 I3 95.059(17) 2_665 2_665 ? I3 Pb1 I3 180.0 . 2_665 ? I1 Pb2 I1 180.0 1_554 2_665 ? I1 Pb2 I2 91.96(3) 1_554 2_665 ? I1 Pb2 I2 88.04(3) 2_665 2_665 ? I1 Pb2 I2 88.04(3) 1_554 1_554 ? I1 Pb2 I2 91.96(3) 2_665 1_554 ? I2 Pb2 I2 180.00(2) 2_665 1_554 ? I1 Pb2 I3 95.17(2) 1_554 . ? I1 Pb2 I3 84.83(2) 2_665 . ? I2 Pb2 I3 83.80(2) 2_665 . ? I2 Pb2 I3 96.20(2) 1_554 . ? I1 Pb2 I3 84.83(2) 1_554 2_664 ? I1 Pb2 I3 95.17(2) 2_665 2_664 ? I2 Pb2 I3 96.20(2) 2_665 2_664 ? I2 Pb2 I3 83.80(2) 1_554 2_664 ? I3 Pb2 I3 180.000(1) . 2_664 ? Pb1 I1 Pb2 76.62(3) . 1_556 ? Pb1 I2 Pb2 76.77(2) . 1_556 ? Pb1 I3 Pb2 76.05(3) . . ? N21 Cu1 N12 174.0(2) . . ? N21 Cu1 N22 80.39(18) . . ? N12 Cu1 N22 95.31(19) . . ? N21 Cu1 N11 98.16(18) . . ? N12 Cu1 N11 79.67(18) . . ? N22 Cu1 N11 113.47(18) . . ? N21 Cu1 I4 93.75(14) . . ? N12 Cu1 I4 92.14(14) . . ? N22 Cu1 I4 125.86(12) . . ? N11 Cu1 I4 120.63(13) . . ? N11 C11 C12 122.3(7) . . ? N11 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 119.1(7) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C14 119.4(6) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? N11 C15 C14 120.9(6) . . ? N11 C15 C16 114.4(4) . . ? C14 C15 C16 124.7(6) . . ? N12 C16 C17 119.9(5) . . ? N12 C16 C15 115.8(5) . . ? C17 C16 C15 124.4(5) . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 120.4(7) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C18 118.0(6) . . ? C20 C19 H19A 121.0 . . ? C18 C19 H19A 121.0 . . ? N12 C20 C19 122.0(6) . . ? N12 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? N21 C21 C22 123.4(6) . . ? N21 C21 H21A 118.3 . . ? C22 C21 H21A 118.3 . . ? C23 C22 C21 118.7(6) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 120.5(6) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 117.8(6) . . ? C25 C24 H24A 121.1 . . ? C23 C24 H24A 121.1 . . ? N21 C25 C24 122.3(5) . . ? N21 C25 C26 114.1(5) . . ? C24 C25 C26 123.5(5) . . ? N22 C26 C27 121.2(5) . . ? N22 C26 C25 115.1(4) . . ? C27 C26 C25 123.7(5) . . ? C28 C27 C26 118.8(6) . . ? C28 C27 H27A 120.6 . . ? C26 C27 H27A 120.6 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C28 C29 C30 118.2(6) . . ? C28 C29 H29A 120.9 . . ? C30 C29 H29A 120.9 . . ? N22 C30 C29 123.9(6) . . ? N22 C30 H30A 118.1 . . ? C29 C30 H30A 118.1 . . ? N31 C31 H31A 109.5 . . ? N31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O31 C33 N31 116.5(10) . . ? O31 C33 H33A 121.8 . . ? N31 C33 H33A 121.8 . . ? C11 N11 C15 117.9(5) . . ? C11 N11 Cu1 128.5(4) . . ? C15 N11 Cu1 113.4(4) . . ? C20 N12 C16 119.8(5) . . ? C20 N12 Cu1 123.5(4) . . ? C16 N12 Cu1 116.6(4) . . ? C21 N21 C25 117.3(5) . . ? C21 N21 Cu1 125.5(4) . . ? C25 N21 Cu1 117.2(4) . . ? C30 N22 C26 117.6(5) . . ? C30 N22 Cu1 129.2(4) . . ? C26 N22 Cu1 113.1(4) . . ? C32 N31 C33 130.4(9) . . ? C32 N31 C31 101.3(11) . . ? C33 N31 C31 128.3(8) . . ? H1WA O1W H1WB 104(2) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.695 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.170 data_2 _database_code_depnum_ccdc_archive 'CCDC 891592' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Cu I N4, I3 Pb' _chemical_formula_sum 'C20 H16 Cu I4 N4 Pb' _chemical_formula_weight 1090.70 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' Pb Pb -3.3944 10.1111 '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 _symmetry_space_group_name_hall '-P 2ybc' 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 17.943(6) _cell_length_b 19.378(6) _cell_length_c 7.853(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.009(5) _cell_angle_gamma 90.00 _cell_volume 2720.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6349 _cell_measurement_theta_min 2.2789 _cell_measurement_theta_max 27.4855 _exptl_crystal_description column _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 11.517 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4593 _exptl_absorpt_correction_T_max 0.5967 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Ultrax-Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17959 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5002 _reflns_number_gt 3595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5002 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Pb1 Pb 0.627612(14) 0.749517(13) 0.26670(3) 0.04745(9) Uani 1 1 d . . . I2 I 0.50832(3) 0.68223(2) -0.00800(6) 0.06029(14) Uani 1 1 d . . . I3 I 0.75958(3) 0.69112(2) 0.04390(5) 0.05749(14) Uani 1 1 d . . . I1 I 0.61225(3) 0.61740(2) 0.52603(6) 0.05741(14) Uani 1 1 d . . . Cu1 Cu 1.17121(4) 0.59258(4) 0.66798(10) 0.0521(2) Uani 1 1 d . . . I4 I 1.11320(4) 0.62399(3) 0.94903(7) 0.0925(2) Uani 1 1 d . . . N11 N 1.0818(3) 0.6259(3) 0.5240(7) 0.0505(13) Uani 1 1 d . . . N12 N 1.1459(3) 0.5032(3) 0.5184(7) 0.0527(14) Uani 1 1 d . . . C13 C 0.9545(4) 0.6639(5) 0.3251(11) 0.081(3) Uani 1 1 d . . . H13A H 0.9116 0.6771 0.2578 0.097 Uiso 1 1 calc R . . C12 C 0.9873(5) 0.7077(4) 0.4413(12) 0.083(3) Uani 1 1 d . . . H12A H 0.9671 0.7513 0.4557 0.099 Uiso 1 1 calc R . . C110 C 1.1841(4) 0.4448(4) 0.5156(11) 0.073(2) Uani 1 1 d . . . H11A H 1.2232 0.4376 0.5995 0.088 Uiso 1 1 calc R . . C16 C 1.0896(4) 0.5137(4) 0.3968(9) 0.0544(18) Uani 1 1 d . . . C14 C 0.9850(4) 0.5993(5) 0.3066(9) 0.073(2) Uani 1 1 d . . . H14A H 0.9624 0.5684 0.2276 0.088 Uiso 1 1 calc R . . C18 C 1.1095(6) 0.4047(5) 0.2693(12) 0.093(3) Uani 1 1 d . . . H18A H 1.0968 0.3720 0.1849 0.112 Uiso 1 1 calc R . . C15 C 1.0503(4) 0.5804(4) 0.4073(8) 0.0520(17) Uani 1 1 d . . . C11 C 1.0508(4) 0.6876(4) 0.5386(10) 0.069(2) Uani 1 1 d . . . H11B H 1.0731 0.7185 0.6181 0.083 Uiso 1 1 calc R . . C19 C 1.1682(5) 0.3931(4) 0.3920(13) 0.093(3) Uani 1 1 d . . . H19A H 1.1962 0.3527 0.3927 0.112 Uiso 1 1 calc R . . C17 C 1.0711(4) 0.4640(5) 0.2747(9) 0.074(2) Uani 1 1 d . . . H17A H 1.0310 0.4719 0.1939 0.089 Uiso 1 1 calc R . . N21 N 1.2470(3) 0.6365(2) 0.5208(6) 0.0664(16) Uani 1 1 d G . . C21 C 1.2313(3) 0.6788(3) 0.3793(7) 0.105(3) Uani 1 1 d G . . H21A H 1.1824 0.6930 0.3490 0.126 Uiso 1 1 calc R . . C22 C 1.2886(5) 0.7000(3) 0.2832(7) 0.162(6) Uani 1 1 d G . . H22A H 1.2781 0.7283 0.1885 0.195 Uiso 1 1 calc R . . C23 C 1.3617(4) 0.6788(4) 0.3285(10) 0.184(8) Uani 1 1 d G . . H23A H 1.4001 0.6929 0.2642 0.221 Uiso 1 1 calc R . . C24 C 1.3774(2) 0.6365(4) 0.4700(11) 0.162(6) Uani 1 1 d G . . H24A H 1.4263 0.6223 0.5003 0.194 Uiso 1 1 calc R . . C25 C 1.3201(3) 0.6153(3) 0.5661(8) 0.094(3) Uani 1 1 d G . . N22 N 1.2634(3) 0.5572(3) 0.7867(8) 0.084(2) Uani 1 1 d G . . C26 C 1.3287(4) 0.5710(3) 0.7095(7) 0.107(4) Uani 1 1 d G . . C27 C 1.3960(3) 0.5418(3) 0.7746(10) 0.172(7) Uani 1 1 d G . . H27A H 1.4397 0.5510 0.7229 0.206 Uiso 1 1 calc R . . C28 C 1.3981(3) 0.4989(3) 0.9167(11) 0.221(10) Uani 1 1 d G . . H28A H 1.4432 0.4794 0.9603 0.265 Uiso 1 1 calc R . . C29 C 1.3329(5) 0.4851(3) 0.9939(8) 0.219(10) Uani 1 1 d G . . H29A H 1.3343 0.4564 1.0890 0.263 Uiso 1 1 calc R . . C210 C 1.2655(4) 0.5143(3) 0.9288(8) 0.138(5) Uani 1 1 d G . . H21B H 1.2219 0.5051 0.9804 0.165 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 Pb1 0.05214(18) 0.05838(17) 0.03207(14) -0.00147(11) 0.00500(12) -0.00137(12) I2 0.0580(3) 0.0739(3) 0.0497(3) -0.0047(2) 0.0085(2) -0.0185(2) I3 0.0565(3) 0.0665(3) 0.0489(3) -0.0029(2) 0.0016(2) 0.0153(2) I1 0.0648(3) 0.0534(3) 0.0542(3) -0.0011(2) 0.0058(2) -0.0003(2) Cu1 0.0449(5) 0.0473(5) 0.0632(5) 0.0102(4) -0.0002(4) 0.0019(4) I4 0.1063(5) 0.1081(5) 0.0659(3) -0.0069(3) 0.0220(3) -0.0126(4) N11 0.052(3) 0.044(3) 0.055(3) 0.008(3) 0.003(3) -0.001(3) N12 0.045(4) 0.039(3) 0.075(4) -0.001(3) 0.012(3) -0.004(3) C13 0.049(5) 0.109(8) 0.082(6) 0.050(6) -0.012(4) 0.008(5) C12 0.065(6) 0.082(6) 0.102(7) 0.029(6) 0.008(5) 0.013(5) C110 0.053(5) 0.054(5) 0.114(7) 0.001(5) 0.014(5) 0.001(4) C16 0.045(4) 0.069(5) 0.051(4) 0.000(4) 0.018(4) -0.016(4) C14 0.058(5) 0.104(7) 0.057(5) 0.025(5) -0.001(4) -0.025(5) C18 0.103(8) 0.088(7) 0.093(7) -0.035(6) 0.031(6) -0.042(6) C15 0.046(4) 0.069(5) 0.042(4) 0.016(4) 0.011(3) -0.007(4) C11 0.061(5) 0.050(5) 0.094(6) 0.015(4) -0.008(5) 0.012(4) C19 0.095(7) 0.053(5) 0.138(9) -0.039(6) 0.050(6) -0.013(5) C17 0.070(6) 0.093(7) 0.061(5) -0.008(5) 0.016(4) -0.017(5) N21 0.052(4) 0.069(4) 0.080(4) -0.018(3) 0.015(3) -0.021(3) C21 0.110(8) 0.120(8) 0.089(7) 0.005(6) 0.034(6) -0.054(6) C22 0.161(12) 0.217(13) 0.119(9) -0.006(9) 0.067(9) -0.097(11) C23 0.145(13) 0.250(18) 0.174(14) -0.087(12) 0.108(11) -0.102(12) C24 0.075(8) 0.224(15) 0.193(14) -0.088(12) 0.049(9) -0.056(8) C25 0.048(5) 0.088(7) 0.149(9) -0.076(6) 0.020(6) -0.019(5) N22 0.069(5) 0.054(4) 0.120(6) 0.005(4) -0.036(4) 0.011(3) C26 0.059(6) 0.046(5) 0.206(12) -0.058(6) -0.051(7) 0.014(4) C27 0.070(7) 0.097(9) 0.328(19) -0.099(10) -0.098(9) 0.030(6) C28 0.164(14) 0.086(9) 0.37(2) -0.074(12) -0.197(15) 0.031(9) C29 0.205(15) 0.063(7) 0.35(2) 0.032(9) -0.215(15) -0.004(8) C210 0.150(10) 0.067(6) 0.178(11) 0.013(7) -0.093(9) 0.001(6) _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 Pb1 I2 3.1816(8) 4_576 ? Pb1 I2 3.1826(8) . ? Pb1 I1 3.1949(9) 4_575 ? Pb1 I3 3.2668(9) . ? Pb1 I3 3.2816(8) 4_576 ? Pb1 I1 3.2978(9) . ? I2 Pb1 3.1816(8) 4_575 ? I3 Pb1 3.2816(8) 4_575 ? I1 Pb1 3.1949(9) 4_576 ? Cu1 N22 1.951(4) . ? Cu1 N11 1.988(5) . ? Cu1 N21 2.046(4) . ? Cu1 N12 2.119(5) . ? Cu1 I4 2.5935(12) . ? N11 C11 1.328(7) . ? N11 C15 1.358(8) . ? N12 C16 1.343(8) . ? N12 C110 1.325(8) . ? C13 C12 1.343(10) . ? C13 C14 1.379(10) . ? C13 H13A 0.9300 . ? C12 C11 1.372(10) . ? C12 H12A 0.9300 . ? C110 C19 1.407(10) . ? C110 H11A 0.9300 . ? C16 C17 1.378(9) . ? C16 C15 1.478(9) . ? C14 C15 1.404(9) . ? C14 H14A 0.9300 . ? C18 C17 1.343(11) . ? C18 C19 1.383(12) . ? C18 H18A 0.9300 . ? C11 H11B 0.9300 . ? C19 H19A 0.9300 . ? C17 H17A 0.9300 . ? N21 C21 1.3900 . ? N21 C25 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.414(8) . ? N22 C26 1.3900 . ? N22 C210 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9300 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C210 1.3900 . ? C29 H29A 0.9300 . ? C210 H21B 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 I2 Pb1 I2 95.85(3) 4_576 . ? I2 Pb1 I1 88.05(2) 4_576 4_575 ? I2 Pb1 I1 84.92(2) . 4_575 ? I2 Pb1 I3 174.953(15) 4_576 . ? I2 Pb1 I3 88.35(3) . . ? I1 Pb1 I3 89.54(2) 4_575 . ? I2 Pb1 I3 88.10(3) 4_576 4_576 ? I2 Pb1 I3 175.473(15) . 4_576 ? I1 Pb1 I3 97.44(2) 4_575 4_576 ? I3 Pb1 I3 87.82(3) . 4_576 ? I2 Pb1 I1 83.26(2) 4_576 . ? I2 Pb1 I1 90.75(2) . . ? I1 Pb1 I1 169.858(18) 4_575 . ? I3 Pb1 I1 99.52(2) . . ? I3 Pb1 I1 87.53(2) 4_576 . ? Pb1 I2 Pb1 76.19(2) 4_575 . ? Pb1 I3 Pb1 73.68(2) . 4_575 ? Pb1 I1 Pb1 74.41(3) 4_576 . ? N22 Cu1 N11 173.9(2) . . ? N22 Cu1 N21 80.7(3) . . ? N11 Cu1 N21 95.0(2) . . ? N22 Cu1 N12 96.3(2) . . ? N11 Cu1 N12 80.0(2) . . ? N21 Cu1 N12 98.46(18) . . ? N22 Cu1 I4 93.60(19) . . ? N11 Cu1 I4 92.51(16) . . ? N21 Cu1 I4 136.01(12) . . ? N12 Cu1 I4 125.53(14) . . ? C11 N11 C15 119.3(6) . . ? C11 N11 Cu1 124.5(5) . . ? C15 N11 Cu1 116.2(4) . . ? C16 N12 C110 118.4(6) . . ? C16 N12 Cu1 112.5(4) . . ? C110 N12 Cu1 128.4(5) . . ? C12 C13 C14 119.3(8) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C13 C12 C11 119.5(8) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? N12 C110 C19 123.1(8) . . ? N12 C110 H11A 118.4 . . ? C19 C110 H11A 118.4 . . ? N12 C16 C17 120.6(7) . . ? N12 C16 C15 115.2(6) . . ? C17 C16 C15 124.2(8) . . ? C15 C14 C13 119.8(8) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C17 C18 C19 118.5(8) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N11 C15 C14 119.2(7) . . ? N11 C15 C16 115.6(6) . . ? C14 C15 C16 125.1(7) . . ? N11 C11 C12 122.8(8) . . ? N11 C11 H11B 118.6 . . ? C12 C11 H11B 118.6 . . ? C18 C19 C110 117.5(8) . . ? C18 C19 H19A 121.3 . . ? C110 C19 H19A 121.3 . . ? C18 C17 C16 121.9(8) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C21 N21 C25 120.0 . . ? C21 N21 Cu1 126.8(4) . . ? C25 N21 Cu1 113.0(4) . . ? N21 C21 C22 120.0 . . ? N21 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 N21 120.0 . . ? C24 C25 C26 125.3(5) . . ? N21 C25 C26 114.7(5) . . ? C26 N22 C210 120.0 . . ? C26 N22 Cu1 115.8(4) . . ? C210 N22 Cu1 123.8(4) . . ? C27 C26 N22 120.0 . . ? C27 C26 C25 124.8(5) . . ? N22 C26 C25 115.2(5) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C210 120.0 . . ? C28 C29 H29A 120.0 . . ? C210 C29 H29A 120.0 . . ? C29 C210 N22 120.0 . . ? C29 C210 H21B 120.0 . . ? N22 C210 H21B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.183 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.130 data_3 _database_code_depnum_ccdc_archive 'CCDC 891593' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Cu N6, I6 Pb2' _chemical_formula_sum 'C30 H24 Cu I6 N6 Pb2' _chemical_formula_weight 1707.87 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' Pb Pb -3.3944 10.1111 '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/c' _symmetry_space_group_name_hall '-P 2ybc' 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 17.604(6) _cell_length_b 14.926(5) _cell_length_c 16.292(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.311(5) _cell_angle_gamma 90.00 _cell_volume 4129(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8881 _cell_measurement_theta_min 1.8810 _cell_measurement_theta_max 33.3515 _exptl_crystal_description spicule _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_coefficient_mu 13.160 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3011 _exptl_absorpt_correction_T_max 0.6211 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Ultrax-Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30722 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7653 _reflns_number_gt 5890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0871P)^2^+6.6955P] 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 7653 _refine_ls_number_parameters 406 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.003 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 Pb1 Pb 0.240692(17) 0.233584(19) 0.226104(17) 0.04283(8) Uani 1 1 d . . . Pb2 Pb 0.238470(17) 0.244362(18) 0.477074(18) 0.04372(8) Uani 1 1 d . . . I1 I 0.31648(4) 0.09521(4) 0.10967(4) 0.06389(17) Uani 1 1 d . . . I2 I 0.32834(3) 0.38259(3) 0.13617(3) 0.05594(15) Uani 1 1 d . . . I3 I 0.09065(3) 0.24928(4) 0.06161(4) 0.05871(17) Uani 1 1 d . . . I4 I 0.16689(3) 0.08819(4) 0.33723(4) 0.06076(17) Uani 1 1 d . . . I5 I 0.16276(3) 0.37781(3) 0.31776(3) 0.05463(15) Uani 1 1 d . . . I6 I 0.38572(3) 0.23693(3) 0.39637(3) 0.04433(13) Uani 1 1 d . . . Cu1 Cu 0.75060(5) 0.26115(5) 0.55573(6) 0.0389(2) Uani 1 1 d . . . C10 C 0.6775(5) 0.4379(5) 0.5943(5) 0.057(2) Uani 1 1 d . . . H10A H 0.7255 0.4648 0.5959 0.069 Uiso 1 1 calc R . . C11 C 0.6171(5) 0.4904(5) 0.6032(6) 0.071(3) Uani 1 1 d . . . H11A H 0.6245 0.5517 0.6120 0.085 Uiso 1 1 calc R . . C12 C 0.5444(5) 0.4526(5) 0.5994(5) 0.059(3) Uani 1 1 d . . . H12A H 0.5029 0.4882 0.6054 0.071 Uiso 1 1 calc R . . C13 C 0.5341(4) 0.3599(5) 0.5862(4) 0.048(2) Uani 1 1 d . . . H13A H 0.4854 0.3331 0.5814 0.058 Uiso 1 1 calc R . . C14 C 0.5999(4) 0.3085(5) 0.5805(4) 0.043(2) Uani 1 1 d . . . C15 C 0.5998(4) 0.2094(5) 0.5761(4) 0.0385(19) Uani 1 1 d . . . C16 C 0.5405(4) 0.1565(5) 0.5882(5) 0.050(2) Uani 1 1 d . . . H16A H 0.4949 0.1830 0.5955 0.060 Uiso 1 1 calc R . . C17 C 0.5467(5) 0.0652(5) 0.5897(5) 0.064(3) Uani 1 1 d . . . H17A H 0.5088 0.0286 0.6030 0.077 Uiso 1 1 calc R . . C18 C 0.6147(5) 0.0295(5) 0.5697(6) 0.071(3) Uani 1 1 d . . . H18A H 0.6210 -0.0322 0.5671 0.085 Uiso 1 1 calc R . . C19 C 0.6708(5) 0.0855(5) 0.5544(6) 0.064(3) Uani 1 1 d . . . H19A H 0.7147 0.0610 0.5412 0.077 Uiso 1 1 calc R . . C20 C 0.6165(6) 0.3347(6) 0.3670(6) 0.071(3) Uani 1 1 d . . . H20A H 0.6151 0.3936 0.3853 0.086 Uiso 1 1 calc R . . C21 C 0.5502(5) 0.3020(6) 0.3113(5) 0.063(3) Uani 1 1 d . . . H21A H 0.5055 0.3371 0.2915 0.076 Uiso 1 1 calc R . . C22 C 0.5532(6) 0.2153(7) 0.2862(6) 0.079(3) Uani 1 1 d . . . H22A H 0.5083 0.1889 0.2514 0.095 Uiso 1 1 calc R . . C23 C 0.6218(5) 0.1661(7) 0.3115(5) 0.069(3) Uani 1 1 d . . . H23A H 0.6249 0.1089 0.2900 0.083 Uiso 1 1 calc R . . C24 C 0.6875(4) 0.2047(5) 0.3712(5) 0.048(2) Uani 1 1 d . . . C25 C 0.7635(4) 0.1568(5) 0.4039(5) 0.048(2) Uani 1 1 d . . . C26 C 0.7924(5) 0.0949(5) 0.3564(6) 0.068(3) Uani 1 1 d . . . H26A H 0.7639 0.0817 0.3011 0.082 Uiso 1 1 calc R . . C27 C 0.8630(6) 0.0533(6) 0.3911(7) 0.087(3) Uani 1 1 d . . . H27A H 0.8825 0.0105 0.3604 0.104 Uiso 1 1 calc R . . C28 C 0.9046(6) 0.0767(6) 0.4730(7) 0.098(4) Uani 1 1 d . . . H28A H 0.9537 0.0518 0.4978 0.118 Uiso 1 1 calc R . . C29 C 0.8716(5) 0.1373(6) 0.5164(6) 0.071(3) Uani 1 1 d . . . H29A H 0.8990 0.1515 0.5719 0.085 Uiso 1 1 calc R . . C30 C 0.8361(5) 0.4130(5) 0.5098(6) 0.070(2) Uani 1 1 d . . . H30A H 0.7954 0.4115 0.4601 0.084 Uiso 1 1 calc R . . C31 C 0.8924(5) 0.4782(6) 0.5195(7) 0.088(3) Uani 1 1 d . . . H31A H 0.8887 0.5228 0.4788 0.106 Uiso 1 1 calc R . . C32 C 0.9569(6) 0.4759(6) 0.5939(7) 0.105(3) Uani 1 1 d . . . H32A H 0.9968 0.5185 0.6024 0.127 Uiso 1 1 calc R . . C33 C 0.9588(5) 0.4089(7) 0.6531(7) 0.098(3) Uani 1 1 d . . . H33A H 1.0019 0.4040 0.7003 0.118 Uiso 1 1 calc R . . C34 C 0.8973(4) 0.3492(6) 0.6426(6) 0.065(3) Uani 1 1 d U . . C35 C 0.8904(5) 0.2780(6) 0.7060(6) 0.069(3) Uani 1 1 d . . . C36 C 0.9472(8) 0.2682(7) 0.7822(8) 0.119(5) Uani 1 1 d . . . H36A H 0.9893 0.3079 0.7966 0.142 Uiso 1 1 calc R . . C37 C 0.9422(7) 0.2078(10) 0.8300(9) 0.141(6) Uani 1 1 d . . . H37A H 0.9838 0.1970 0.8776 0.170 Uiso 1 1 calc R . . C38 C 0.8728(7) 0.1525(8) 0.8146(6) 0.111(4) Uani 1 1 d . . . H38A H 0.8654 0.1109 0.8542 0.133 Uiso 1 1 calc R . . C39 C 0.8177(7) 0.1649(7) 0.7372(6) 0.085(4) Uani 1 1 d . . . H39A H 0.7737 0.1279 0.7222 0.102 Uiso 1 1 calc R . . N11 N 0.6707(3) 0.3488(3) 0.5831(4) 0.0398(16) Uani 1 1 d . . . N12 N 0.6645(4) 0.1742(3) 0.5577(4) 0.0432(17) Uani 1 1 d . . . N21 N 0.6834(4) 0.2886(4) 0.3975(5) 0.056(2) Uani 1 1 d . . . N22 N 0.8019(3) 0.1776(4) 0.4833(4) 0.0482(18) Uani 1 1 d . . . N31 N 0.8380(4) 0.3510(4) 0.5701(4) 0.0542(19) Uani 1 1 d . . . N32 N 0.8269(4) 0.2287(5) 0.6843(5) 0.057(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.04307(15) 0.04901(15) 0.03576(15) -0.00544(11) 0.00924(12) 0.00224(12) Pb2 0.04315(15) 0.05029(15) 0.03816(16) 0.00100(12) 0.01151(12) -0.00081(12) I1 0.0721(3) 0.0506(3) 0.0734(3) -0.0053(3) 0.0271(3) 0.0169(3) I2 0.0554(3) 0.0518(3) 0.0625(3) -0.0084(2) 0.0190(2) -0.0078(2) I3 0.0346(3) 0.0902(4) 0.0488(3) -0.0034(3) 0.0066(2) -0.0012(3) I4 0.0470(3) 0.0482(3) 0.0779(4) 0.0045(3) 0.0003(3) -0.0049(2) I5 0.0643(3) 0.0503(3) 0.0515(3) -0.0011(2) 0.0191(2) 0.0157(2) I6 0.0363(2) 0.0483(2) 0.0463(3) 0.0021(2) 0.0072(2) -0.0021(2) Cu1 0.0276(4) 0.0353(4) 0.0508(5) -0.0067(3) 0.0053(4) -0.0002(3) C10 0.052(4) 0.041(4) 0.081(5) -0.008(4) 0.021(4) -0.007(4) C11 0.076(5) 0.034(4) 0.118(6) 0.013(4) 0.051(5) 0.023(4) C12 0.061(5) 0.049(4) 0.066(5) -0.002(4) 0.013(4) 0.020(4) C13 0.032(4) 0.064(5) 0.045(4) -0.001(4) 0.006(3) 0.004(3) C14 0.033(4) 0.046(4) 0.044(4) -0.002(3) -0.002(3) 0.006(3) C15 0.022(3) 0.046(4) 0.041(4) -0.007(3) -0.002(3) 0.002(3) C16 0.040(4) 0.045(4) 0.064(5) -0.005(4) 0.013(3) -0.014(3) C17 0.055(5) 0.057(5) 0.072(6) -0.001(4) 0.006(4) -0.022(4) C18 0.079(6) 0.032(4) 0.098(6) 0.012(4) 0.018(5) -0.017(4) C19 0.050(5) 0.050(4) 0.089(6) 0.003(4) 0.013(4) 0.007(4) C20 0.070(6) 0.063(5) 0.078(6) 0.006(5) 0.014(5) -0.006(5) C21 0.043(5) 0.084(6) 0.061(5) 0.001(5) 0.010(4) 0.002(4) C22 0.052(6) 0.125(8) 0.054(5) -0.006(6) 0.001(5) -0.013(6) C23 0.056(5) 0.091(6) 0.057(5) -0.006(5) 0.008(4) -0.009(5) C24 0.040(4) 0.053(4) 0.048(4) -0.006(4) 0.008(3) -0.002(3) C25 0.051(4) 0.048(4) 0.051(4) -0.012(3) 0.023(3) -0.008(3) C26 0.067(5) 0.048(4) 0.096(6) -0.027(4) 0.031(5) -0.001(4) C27 0.071(6) 0.068(5) 0.125(7) -0.042(5) 0.034(5) 0.017(5) C28 0.073(6) 0.092(6) 0.122(8) -0.040(6) 0.012(6) 0.047(5) C29 0.053(5) 0.079(5) 0.075(6) -0.027(5) 0.007(4) 0.018(4) C30 0.065(4) 0.062(5) 0.103(6) -0.030(4) 0.058(4) -0.033(4) C31 0.087(6) 0.064(5) 0.139(7) -0.023(5) 0.074(5) -0.026(5) C32 0.081(5) 0.073(5) 0.191(9) -0.072(6) 0.084(6) -0.035(5) C33 0.038(5) 0.112(6) 0.138(8) -0.085(6) 0.012(5) -0.012(5) C34 0.011(3) 0.082(5) 0.099(6) -0.048(4) 0.011(3) -0.008(3) C35 0.035(4) 0.079(5) 0.079(6) -0.039(4) -0.008(4) 0.023(4) C36 0.104(9) 0.085(7) 0.111(9) -0.022(6) -0.070(7) 0.017(6) C37 0.077(7) 0.178(12) 0.122(10) -0.052(9) -0.055(7) 0.063(8) C38 0.123(8) 0.151(9) 0.054(6) 0.022(6) 0.015(6) 0.092(7) C39 0.089(7) 0.099(7) 0.061(6) 0.015(5) 0.009(5) 0.030(6) N11 0.036(3) 0.030(3) 0.052(3) -0.001(3) 0.010(3) -0.003(2) N12 0.044(3) 0.026(3) 0.053(3) -0.002(3) 0.000(3) -0.003(2) N21 0.039(3) 0.038(3) 0.089(5) -0.007(3) 0.014(3) 0.002(3) N22 0.032(3) 0.048(3) 0.063(4) -0.007(3) 0.009(3) 0.010(3) N31 0.035(3) 0.049(3) 0.080(4) -0.018(3) 0.019(3) -0.015(3) N32 0.038(4) 0.068(4) 0.058(4) -0.004(3) 0.003(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I5 3.1349(9) . ? Pb1 I3 3.2366(10) . ? Pb1 I6 3.2366(10) . ? Pb1 I2 3.2660(9) . ? Pb1 I4 3.3042(9) . ? Pb1 I1 3.3137(9) . ? Pb2 I6 3.2032(11) . ? Pb2 I3 3.2511(11) 4_566 ? Pb2 I2 3.2629(9) 4_566 ? Pb2 I5 3.2639(9) . ? Pb2 I4 3.2704(9) . ? Pb2 I1 3.2741(9) 4_566 ? I1 Pb2 3.2741(9) 4_565 ? I2 Pb2 3.2629(9) 4_565 ? I3 Pb2 3.2511(11) 4_565 ? Cu1 N12 2.002(6) . ? Cu1 N31 2.008(6) . ? Cu1 N11 2.054(6) . ? Cu1 N22 2.081(6) . ? Cu1 N32 2.222(7) . ? C10 N11 1.343(9) . ? C10 C11 1.360(11) . ? C10 H10A 0.9300 . ? C11 C12 1.384(12) . ? C11 H11A 0.9300 . ? C12 C13 1.405(11) . ? C12 H12A 0.9300 . ? C13 C14 1.413(10) . ? C13 H13A 0.9300 . ? C14 N11 1.375(9) . ? C14 C15 1.481(10) . ? C15 N12 1.357(9) . ? C15 C16 1.364(10) . ? C16 C17 1.367(11) . ? C16 H16A 0.9300 . ? C17 C18 1.425(13) . ? C17 H17A 0.9300 . ? C18 C19 1.367(12) . ? C18 H18A 0.9300 . ? C19 N12 1.331(9) . ? C19 H19A 0.9300 . ? C20 N21 1.341(11) . ? C20 C21 1.366(12) . ? C20 H20A 0.9300 . ? C21 C22 1.362(14) . ? C21 H21A 0.9300 . ? C22 C23 1.380(13) . ? C22 H22A 0.9300 . ? C23 C24 1.422(11) . ? C23 H23A 0.9300 . ? C24 N21 1.331(10) . ? C24 C25 1.486(10) . ? C25 N22 1.327(9) . ? C25 C26 1.385(11) . ? C26 C27 1.371(12) . ? C26 H26A 0.9300 . ? C27 C28 1.386(14) . ? C27 H27A 0.9300 . ? C28 C29 1.369(13) . ? C28 H28A 0.9300 . ? C29 N22 1.345(10) . ? C29 H29A 0.9300 . ? C30 N31 1.344(11) . ? C30 C31 1.368(12) . ? C30 H30A 0.9300 . ? C31 C32 1.425(14) . ? C31 H31A 0.9300 . ? C32 C33 1.385(15) . ? C32 H32A 0.9300 . ? C33 C34 1.377(12) . ? C33 H33A 0.9300 . ? C34 N31 1.354(10) . ? C34 C35 1.509(13) . ? C35 N32 1.307(11) . ? C35 C36 1.381(13) . ? C36 C37 1.209(19) . ? C36 H36A 0.9300 . ? C37 C38 1.440(18) . ? C37 H37A 0.9300 . ? C38 C39 1.386(13) . ? C38 H38A 0.9300 . ? C39 N32 1.323(12) . ? C39 H39A 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 I5 Pb1 I3 88.89(3) . . ? I5 Pb1 I6 85.79(3) . . ? I3 Pb1 I6 174.350(17) . . ? I5 Pb1 I2 93.67(3) . . ? I3 Pb1 I2 87.60(3) . . ? I6 Pb1 I2 90.85(3) . . ? I5 Pb1 I4 84.56(3) . . ? I3 Pb1 I4 98.53(3) . . ? I6 Pb1 I4 82.87(3) . . ? I2 Pb1 I4 173.573(16) . . ? I5 Pb1 I1 173.538(17) . . ? I3 Pb1 I1 86.27(3) . . ? I6 Pb1 I1 98.89(3) . . ? I2 Pb1 I1 81.85(3) . . ? I4 Pb1 I1 100.39(3) . . ? I6 Pb2 I3 179.152(16) . 4_566 ? I6 Pb2 I2 91.77(3) . 4_566 ? I3 Pb2 I2 87.41(3) 4_566 4_566 ? I6 Pb2 I5 84.23(2) . . ? I3 Pb2 I5 96.58(2) 4_566 . ? I2 Pb2 I5 175.289(18) 4_566 . ? I6 Pb2 I4 83.92(2) . . ? I3 Pb2 I4 96.41(2) 4_566 . ? I2 Pb2 I4 98.99(3) 4_566 . ? I5 Pb2 I4 83.09(3) . . ? I6 Pb2 I1 92.99(2) . 4_566 ? I3 Pb2 I1 86.69(2) 4_566 4_566 ? I2 Pb2 I1 82.51(3) 4_566 4_566 ? I5 Pb2 I1 95.19(3) . 4_566 ? I4 Pb2 I1 176.594(19) . 4_566 ? Pb2 I1 Pb1 76.10(3) 4_565 . ? Pb2 I2 Pb1 76.91(3) 4_565 . ? Pb1 I3 Pb2 77.49(3) . 4_565 ? Pb2 I4 Pb1 77.21(3) . . ? Pb1 I5 Pb2 79.72(3) . . ? Pb2 I6 Pb1 79.14(3) . . ? N12 Cu1 N31 172.4(3) . . ? N12 Cu1 N11 81.1(2) . . ? N31 Cu1 N11 95.5(2) . . ? N12 Cu1 N22 93.7(2) . . ? N31 Cu1 N22 91.9(3) . . ? N11 Cu1 N22 158.4(2) . . ? N12 Cu1 N32 96.6(2) . . ? N31 Cu1 N32 77.4(3) . . ? N11 Cu1 N32 102.2(2) . . ? N22 Cu1 N32 99.2(2) . . ? N11 C10 C11 122.7(8) . . ? N11 C10 H10A 118.7 . . ? C11 C10 H10A 118.7 . . ? C10 C11 C12 120.0(7) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 119.3(8) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 118.0(7) . . ? C14 C13 H13A 121.0 . . ? C12 C13 H13A 121.0 . . ? N11 C14 C13 120.9(6) . . ? N11 C14 C15 115.4(6) . . ? C13 C14 C15 123.7(7) . . ? N12 C15 C16 121.8(6) . . ? N12 C15 C14 114.0(6) . . ? C16 C15 C14 124.2(7) . . ? C15 C16 C17 121.3(8) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C16 C17 C18 115.9(8) . . ? C16 C17 H17A 122.1 . . ? C18 C17 H17A 122.1 . . ? C19 C18 C17 120.3(8) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? N12 C19 C18 121.9(8) . . ? N12 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? N21 C20 C21 125.0(9) . . ? N21 C20 H20A 117.5 . . ? C21 C20 H20A 117.5 . . ? C20 C21 C22 116.5(8) . . ? C20 C21 H21A 121.7 . . ? C22 C21 H21A 121.7 . . ? C21 C22 C23 121.0(9) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C22 C23 C24 118.6(9) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? N21 C24 C23 119.8(7) . . ? N21 C24 C25 117.2(6) . . ? C23 C24 C25 122.9(7) . . ? N22 C25 C26 122.1(7) . . ? N22 C25 C24 114.6(6) . . ? C26 C25 C24 123.3(7) . . ? C27 C26 C25 119.9(8) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 118.2(9) . . ? C26 C27 H27A 120.9 . . ? C28 C27 H27A 120.9 . . ? C29 C28 C27 118.4(9) . . ? C29 C28 H28A 120.8 . . ? C27 C28 H28A 120.8 . . ? N22 C29 C28 123.7(8) . . ? N22 C29 H29A 118.2 . . ? C28 C29 H29A 118.2 . . ? N31 C30 C31 121.9(8) . . ? N31 C30 H30A 119.1 . . ? C31 C30 H30A 119.1 . . ? C30 C31 C32 118.1(9) . . ? C30 C31 H31A 121.0 . . ? C32 C31 H31A 120.9 . . ? C33 C32 C31 118.5(9) . . ? C33 C32 H32A 120.8 . . ? C31 C32 H32A 120.8 . . ? C32 C33 C34 120.5(9) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? N31 C34 C33 119.7(9) . . ? N31 C34 C35 115.3(7) . . ? C33 C34 C35 125.0(8) . . ? N32 C35 C36 123.3(10) . . ? N32 C35 C34 115.4(7) . . ? C36 C35 C34 121.3(9) . . ? C37 C36 C35 119.9(12) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 121.2(11) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C39 C38 C37 116.1(11) . . ? C39 C38 H38A 121.9 . . ? C37 C38 H38A 122.0 . . ? N32 C39 C38 120.8(10) . . ? N32 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C10 N11 C14 119.1(6) . . ? C10 N11 Cu1 128.2(5) . . ? C14 N11 Cu1 112.4(4) . . ? C19 N12 C15 118.5(7) . . ? C19 N12 Cu1 124.9(6) . . ? C15 N12 Cu1 115.9(4) . . ? C24 N21 C20 118.8(7) . . ? C25 N22 C29 117.6(7) . . ? C25 N22 Cu1 120.4(5) . . ? C29 N22 Cu1 121.8(5) . . ? C34 N31 C30 121.1(7) . . ? C34 N31 Cu1 118.6(6) . . ? C30 N31 Cu1 120.3(5) . . ? C35 N32 C39 118.2(8) . . ? C35 N32 Cu1 113.2(6) . . ? C39 N32 Cu1 128.6(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.305 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.173