Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg 67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Heterobimetallic coordination networks based on metallaporphyrins bearing four pyridine N-Oxide groups as coordinating sites ; loop_ _publ_author_name 'M Hosseini' 'Veronique Bulach' 'Emmanuel Deiters' data_e42a _database_code_depnum_ccdc_archive 'CCDC 649317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 N8 Ni O7' _chemical_formula_weight 821.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1660(8) _cell_length_b 14.8060(14) _cell_length_c 15.5049(15) _cell_angle_alpha 76.201(4) _cell_angle_beta 73.291(4) _cell_angle_gamma 77.186(4) _cell_volume 1930.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.74 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8487 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details sadabs _exptl_special_details ; No H atoms has been introduced to C43 O7 and O8 due to the disorder of these atoms. However, the missing H atoms has been introduced in the formula ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61035 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 29.70 _reflns_number_total 10850 _reflns_number_gt 7212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The unit-occupancy of O7 and the half-unit occupancy of C43 and O8 is meant to be a half methanol C7-O43 and two half-occupancy water oxygens at O7 and O8 sites ; _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^)+(0.1427P)^2^+2.4164P] 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 10850 _refine_ls_number_parameters 539 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2409 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.75274(5) 0.50966(3) 0.60518(3) 0.02036(14) Uani 1 1 d . . . N1 N 0.6910(3) 0.5670(2) 0.7174(2) 0.0235(6) Uani 1 1 d . . . N2 N 0.6116(3) 0.6148(2) 0.5470(2) 0.0253(6) Uani 1 1 d . . . N3 N 0.8194(3) 0.4544(2) 0.4915(2) 0.0261(6) Uani 1 1 d . . . N4 N 0.8776(3) 0.3991(2) 0.6673(2) 0.0259(6) Uani 1 1 d . . . C1 C 0.7370(4) 0.5313(2) 0.7977(2) 0.0242(7) Uani 1 1 d . . . C2 C 0.6708(4) 0.5951(3) 0.8613(2) 0.0267(7) Uani 1 1 d . . . H2 H 0.6861 0.5867 0.9209 0.032 Uiso 1 1 calc R . . C3 C 0.5832(4) 0.6689(3) 0.8203(3) 0.0279(7) Uani 1 1 d . . . H3 H 0.5248 0.7221 0.8456 0.033 Uiso 1 1 calc R . . C4 C 0.5953(4) 0.6514(2) 0.7307(2) 0.0256(7) Uani 1 1 d . . . C5 C 0.5095(4) 0.7083(2) 0.6702(2) 0.0238(7) Uani 1 1 d . . . C6 C 0.5132(4) 0.6877(2) 0.5866(2) 0.0250(7) Uani 1 1 d . . . C7 C 0.4215(4) 0.7437(3) 0.5251(3) 0.0285(7) Uani 1 1 d . . . H7 H 0.3458 0.7978 0.5358 0.034 Uiso 1 1 calc R . . C8 C 0.4636(4) 0.7047(3) 0.4494(3) 0.0296(8) Uani 1 1 d . . . H8 H 0.4209 0.7251 0.3976 0.036 Uiso 1 1 calc R . . C9 C 0.5861(4) 0.6261(2) 0.4620(2) 0.0259(7) Uani 1 1 d . . . C10 C 0.6705(4) 0.5737(2) 0.3947(2) 0.0249(7) Uani 1 1 d . . . C11 C 0.7836(4) 0.4949(2) 0.4084(2) 0.0252(7) Uani 1 1 d . . . C12 C 0.8768(4) 0.4419(3) 0.3391(3) 0.0278(7) Uani 1 1 d . . . H12 H 0.8768 0.4563 0.2760 0.033 Uiso 1 1 calc R . . C13 C 0.9641(4) 0.3680(3) 0.3807(2) 0.0282(7) Uani 1 1 d . . . H13 H 1.0369 0.3205 0.3523 0.034 Uiso 1 1 calc R . . C14 C 0.9260(4) 0.3747(2) 0.4762(2) 0.0257(7) Uani 1 1 d . . . C15 C 0.9849(4) 0.3079(2) 0.5432(3) 0.0257(7) Uani 1 1 d . . . C16 C 0.9565(4) 0.3184(2) 0.6331(3) 0.0275(7) Uani 1 1 d . . . C17 C 1.0081(5) 0.2482(3) 0.7057(3) 0.0323(8) Uani 1 1 d . . . H17 H 1.0614 0.1860 0.7010 0.039 Uiso 1 1 calc R . . C18 C 0.9667(5) 0.2873(3) 0.7809(3) 0.0325(8) Uani 1 1 d . . . H18 H 0.9861 0.2582 0.8390 0.039 Uiso 1 1 calc R . . C19 C 0.8871(4) 0.3818(3) 0.7569(2) 0.0261(7) Uani 1 1 d . . . C20 C 0.8273(4) 0.4442(3) 0.8176(2) 0.0262(7) Uani 1 1 d . . . C21 C 0.4090(4) 0.7963(2) 0.6976(2) 0.0273(7) Uani 1 1 d . . . C22 C 0.2489(4) 0.8091(3) 0.7139(3) 0.0327(8) Uani 1 1 d . . . H22 H 0.2015 0.7617 0.7059 0.039 Uiso 1 1 calc R . . C23 C 0.1581(5) 0.8904(3) 0.7415(3) 0.0412(10) Uani 1 1 d . . . H23 H 0.0489 0.8977 0.7534 0.049 Uiso 1 1 calc R . . N5 N 0.2231(4) 0.9591(2) 0.7516(3) 0.0431(9) Uani 1 1 d . . . O1 O 0.1340(5) 1.0360(2) 0.7775(3) 0.0623(10) Uani 1 1 d . . . C24 C 0.3783(5) 0.9485(3) 0.7362(3) 0.0416(10) Uani 1 1 d . . . H24 H 0.4234 0.9971 0.7439 0.050 Uiso 1 1 calc R . . C25 C 0.4716(5) 0.8683(3) 0.7095(3) 0.0338(8) Uani 1 1 d . . . H25 H 0.5804 0.8622 0.6990 0.041 Uiso 1 1 calc R . . C26 C 0.6367(4) 0.6024(2) 0.3027(2) 0.0255(7) Uani 1 1 d . . . C27 C 0.6433(4) 0.6937(3) 0.2511(3) 0.0310(8) Uani 1 1 d . . . H27 H 0.6690 0.7394 0.2756 0.037 Uiso 1 1 calc R . . C28 C 0.6135(4) 0.7188(3) 0.1655(3) 0.0329(8) Uani 1 1 d . . . H28 H 0.6181 0.7812 0.1320 0.039 Uiso 1 1 calc R . . N6 N 0.5779(4) 0.6549(2) 0.1294(2) 0.0314(7) Uani 1 1 d . . . O2 O 0.5551(4) 0.6754(2) 0.0464(2) 0.0431(7) Uani 1 1 d . . . C29 C 0.5685(4) 0.5653(3) 0.1782(3) 0.0301(8) Uani 1 1 d . . . H29 H 0.5413 0.5209 0.1528 0.036 Uiso 1 1 calc R . . C30 C 0.5980(4) 0.5392(3) 0.2630(3) 0.0294(7) Uani 1 1 d . . . H30 H 0.5919 0.4764 0.2954 0.035 Uiso 1 1 calc R . . C31 C 1.0804(4) 0.2179(2) 0.5172(2) 0.0269(7) Uani 1 1 d . . . C32 C 1.0293(4) 0.1633(3) 0.4734(3) 0.0319(8) Uani 1 1 d . . . H32 H 0.9324 0.1843 0.4583 0.038 Uiso 1 1 calc R . . C33 C 1.1163(5) 0.0798(3) 0.4516(3) 0.0339(8) Uani 1 1 d . . . H33 H 1.0805 0.0448 0.4203 0.041 Uiso 1 1 calc R . . N7 N 1.2542(4) 0.0469(2) 0.4747(2) 0.0327(7) Uani 1 1 d . . . O3 O 1.3335(4) -0.0350(2) 0.4572(2) 0.0460(8) Uani 1 1 d . . . C34 C 1.3087(4) 0.0984(3) 0.5158(3) 0.0331(8) Uani 1 1 d . . . H34 H 1.4058 0.0760 0.5304 0.040 Uiso 1 1 calc R . . C35 C 1.2245(4) 0.1833(3) 0.5368(3) 0.0301(8) Uani 1 1 d . . . H35 H 1.2651 0.2190 0.5651 0.036 Uiso 1 1 calc R . . C36 C 0.8648(4) 0.4159(2) 0.9089(2) 0.0263(7) Uani 1 1 d . . . C37 C 0.7530(4) 0.3979(3) 0.9904(3) 0.0359(9) Uani 1 1 d . . . H37 H 0.6490 0.4019 0.9886 0.043 Uiso 1 1 calc R . . C38 C 0.7914(4) 0.3744(3) 1.0740(3) 0.0354(9) Uani 1 1 d . . . H38 H 0.7133 0.3628 1.1290 0.042 Uiso 1 1 calc R . . N8 N 0.9388(4) 0.3677(2) 1.0781(2) 0.0307(7) Uani 1 1 d . . . O4 O 0.9701(4) 0.3506(2) 1.15859(19) 0.0427(7) Uani 1 1 d . . . C39 C 1.0503(4) 0.3807(3) 1.0000(3) 0.0343(8) Uani 1 1 d . . . H39 H 1.1547 0.3724 1.0029 0.041 Uiso 1 1 calc R . . C40 C 1.0152(4) 0.4060(3) 0.9160(3) 0.0305(8) Uani 1 1 d . . . H40 H 1.0954 0.4168 0.8619 0.037 Uiso 1 1 calc R . . C41 C 0.2597(9) 0.8943(7) 0.2731(6) 0.102(3) Uani 1 1 d D . . H41A H 0.2665 0.8284 0.2689 0.152 Uiso 1 1 calc R . . H41B H 0.2492 0.9351 0.2146 0.152 Uiso 1 1 calc R . . H41C H 0.1697 0.9116 0.3220 0.152 Uiso 1 1 calc R . . O5 O 0.3921(5) 0.9051(4) 0.2926(3) 0.0758(12) Uani 1 1 d D . . H5 H 0.3703 0.9469 0.3247 0.114 Uiso 1 1 calc R . . C42 C 0.0703(13) 0.1148(7) 0.9969(6) 0.0546(15) Uani 0.50 1 d PD . . H42A H 0.1232 0.0997 1.0464 0.082 Uiso 0.50 1 calc PR . . H42B H 0.0074 0.0664 1.0048 0.082 Uiso 0.50 1 calc PR . . H42C H 0.0036 0.1764 0.9984 0.082 Uiso 0.50 1 calc PR . . O6 O 0.1855(9) 0.1178(5) 0.9080(4) 0.0546(15) Uani 0.50 1 d PD . . H6 H 0.2523 0.0688 0.9101 0.082 Uiso 0.50 1 calc PR . . O7 O 0.1600(5) 0.1851(3) 0.2243(3) 0.0704(11) Uani 1 1 d D . . C43 C 0.2593(15) 0.1426(11) 0.1455(10) 0.086(4) Uani 0.50 1 d PD . . O8 O 0.4336(11) 0.1575(6) 0.0712(5) 0.073(2) Uani 0.50 1 d P . . 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 Ni1 0.0205(2) 0.0197(2) 0.0212(2) -0.00179(16) -0.00987(16) -0.00001(15) N1 0.0205(13) 0.0253(14) 0.0244(14) -0.0031(11) -0.0080(11) -0.0015(11) N2 0.0250(14) 0.0244(14) 0.0267(15) -0.0026(12) -0.0113(12) -0.0004(11) N3 0.0269(14) 0.0249(14) 0.0246(15) -0.0003(11) -0.0100(12) -0.0005(11) N4 0.0266(14) 0.0261(14) 0.0251(15) -0.0017(12) -0.0111(12) -0.0018(11) C1 0.0213(15) 0.0283(17) 0.0226(16) -0.0017(13) -0.0079(13) -0.0034(13) C2 0.0262(16) 0.0304(18) 0.0260(17) -0.0076(14) -0.0109(14) -0.0017(14) C3 0.0275(17) 0.0301(18) 0.0291(18) -0.0075(14) -0.0120(14) -0.0021(14) C4 0.0218(15) 0.0274(17) 0.0287(18) -0.0047(14) -0.0091(13) -0.0032(13) C5 0.0229(15) 0.0229(16) 0.0264(17) -0.0029(13) -0.0093(13) -0.0030(12) C6 0.0245(16) 0.0228(16) 0.0285(18) -0.0026(13) -0.0119(14) -0.0008(13) C7 0.0284(17) 0.0245(17) 0.0304(18) -0.0017(14) -0.0106(14) 0.0013(13) C8 0.0279(17) 0.0291(18) 0.0321(19) -0.0022(15) -0.0150(15) 0.0009(14) C9 0.0259(16) 0.0264(17) 0.0272(17) -0.0001(14) -0.0148(14) -0.0021(13) C10 0.0253(16) 0.0239(16) 0.0267(17) -0.0019(13) -0.0098(13) -0.0048(13) C11 0.0251(16) 0.0264(17) 0.0258(17) -0.0040(14) -0.0100(13) -0.0036(13) C12 0.0287(17) 0.0286(18) 0.0258(17) -0.0047(14) -0.0081(14) -0.0025(14) C13 0.0295(17) 0.0283(17) 0.0261(18) -0.0058(14) -0.0086(14) -0.0006(14) C14 0.0249(16) 0.0249(16) 0.0276(18) -0.0040(14) -0.0091(14) -0.0021(13) C15 0.0238(15) 0.0221(16) 0.0317(18) -0.0040(14) -0.0108(14) -0.0009(13) C16 0.0268(16) 0.0235(16) 0.0320(19) -0.0009(14) -0.0132(14) -0.0007(13) C17 0.0358(19) 0.0250(17) 0.037(2) -0.0033(15) -0.0187(16) 0.0032(15) C18 0.038(2) 0.0295(18) 0.0283(19) -0.0009(15) -0.0146(16) 0.0026(15) C19 0.0247(16) 0.0280(17) 0.0255(17) -0.0020(14) -0.0115(13) -0.0005(13) C20 0.0226(15) 0.0301(17) 0.0266(17) -0.0016(14) -0.0104(13) -0.0041(13) C21 0.0300(17) 0.0237(16) 0.0283(18) -0.0014(14) -0.0132(14) -0.0002(13) C22 0.0316(18) 0.0300(19) 0.037(2) -0.0045(16) -0.0138(16) -0.0014(15) C23 0.033(2) 0.037(2) 0.054(3) -0.0118(19) -0.0159(19) 0.0057(17) N5 0.049(2) 0.0287(17) 0.050(2) -0.0078(15) -0.0176(17) 0.0063(15) O1 0.070(2) 0.0326(17) 0.083(3) -0.0215(17) -0.028(2) 0.0189(16) C24 0.051(3) 0.028(2) 0.049(3) -0.0065(18) -0.018(2) -0.0075(18) C25 0.0329(19) 0.0286(18) 0.041(2) -0.0040(16) -0.0132(17) -0.0044(15) C26 0.0227(15) 0.0278(17) 0.0257(17) -0.0026(14) -0.0095(13) -0.0015(13) C27 0.0360(19) 0.0276(18) 0.0321(19) -0.0026(15) -0.0175(16) -0.0022(15) C28 0.036(2) 0.0302(19) 0.0314(19) 0.0002(15) -0.0126(16) -0.0051(15) N6 0.0283(15) 0.0420(18) 0.0248(15) -0.0025(13) -0.0124(12) -0.0042(13) O2 0.0488(17) 0.0545(19) 0.0294(15) -0.0018(13) -0.0217(13) -0.0061(14) C29 0.0278(17) 0.0356(19) 0.0305(19) -0.0053(15) -0.0115(15) -0.0077(15) C30 0.0280(17) 0.0304(18) 0.0310(19) -0.0015(15) -0.0107(15) -0.0074(14) C31 0.0262(16) 0.0243(16) 0.0290(18) -0.0049(14) -0.0082(14) -0.0002(13) C32 0.0284(17) 0.0305(18) 0.039(2) -0.0052(16) -0.0154(16) -0.0025(14) C33 0.0338(19) 0.0272(18) 0.044(2) -0.0081(16) -0.0145(17) -0.0040(15) N7 0.0356(17) 0.0242(15) 0.0380(18) -0.0040(13) -0.0143(14) 0.0009(13) O3 0.0501(18) 0.0265(14) 0.060(2) -0.0142(14) -0.0191(16) 0.0103(13) C34 0.0294(18) 0.0312(19) 0.040(2) -0.0076(16) -0.0146(16) 0.0021(15) C35 0.0295(18) 0.0260(17) 0.037(2) -0.0043(15) -0.0143(15) -0.0030(14) C36 0.0263(16) 0.0255(16) 0.0265(17) -0.0023(14) -0.0110(14) 0.0003(13) C37 0.0272(18) 0.045(2) 0.033(2) 0.0018(17) -0.0126(15) -0.0043(16) C38 0.0292(18) 0.045(2) 0.0289(19) -0.0013(17) -0.0091(15) -0.0038(16) N8 0.0341(16) 0.0328(16) 0.0285(16) -0.0026(13) -0.0169(13) -0.0033(13) O4 0.0485(17) 0.0557(19) 0.0267(14) -0.0004(13) -0.0201(13) -0.0082(14) C39 0.0301(18) 0.044(2) 0.0305(19) -0.0037(16) -0.0144(15) -0.0042(16) C40 0.0271(17) 0.037(2) 0.0287(18) -0.0032(15) -0.0106(14) -0.0052(15) C41 0.076(5) 0.144(8) 0.115(6) -0.044(6) -0.044(5) -0.032(5) O5 0.067(3) 0.092(3) 0.079(3) -0.027(3) -0.025(2) -0.014(2) C42 0.092(5) 0.037(3) 0.048(3) 0.006(2) -0.037(3) -0.027(3) O6 0.092(5) 0.037(3) 0.048(3) 0.006(2) -0.037(3) -0.027(3) O7 0.072(3) 0.074(3) 0.071(3) 0.011(2) -0.035(2) -0.031(2) C43 0.078(9) 0.095(10) 0.104(11) -0.006(9) -0.048(9) -0.033(8) O8 0.110(7) 0.058(5) 0.056(5) -0.009(4) -0.033(5) -0.008(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 Ni1 N4 1.992(3) . ? Ni1 N3 1.999(3) . ? Ni1 N1 2.000(3) . ? Ni1 N2 2.004(3) . ? N1 C1 1.377(4) . ? N1 C4 1.380(4) . ? N2 C9 1.369(4) . ? N2 C6 1.387(4) . ? N3 C14 1.376(4) . ? N3 C11 1.384(4) . ? N4 C19 1.375(4) . ? N4 C16 1.389(5) . ? C1 C20 1.388(5) . ? C1 C2 1.441(5) . ? C2 C3 1.346(5) . ? C2 H2 0.9500 . ? C3 C4 1.442(5) . ? C3 H3 0.9500 . ? C4 C5 1.401(5) . ? C5 C6 1.389(5) . ? C5 C21 1.494(5) . ? C6 C7 1.442(5) . ? C7 C8 1.351(5) . ? C7 H7 0.9500 . ? C8 C9 1.447(5) . ? C8 H8 0.9500 . ? C9 C10 1.395(5) . ? C10 C11 1.397(5) . ? C10 C26 1.489(5) . ? C11 C12 1.441(5) . ? C12 C13 1.351(5) . ? C12 H12 0.9500 . ? C13 C14 1.444(5) . ? C13 H13 0.9500 . ? C14 C15 1.394(5) . ? C15 C16 1.383(5) . ? C15 C31 1.496(5) . ? C16 C17 1.450(5) . ? C17 C18 1.345(6) . ? C17 H17 0.9500 . ? C18 C19 1.443(5) . ? C18 H18 0.9500 . ? C19 C20 1.390(5) . ? C20 C36 1.494(5) . ? C21 C25 1.388(5) . ? C21 C22 1.393(5) . ? C22 C23 1.386(5) . ? C22 H22 0.9500 . ? C23 N5 1.347(6) . ? C23 H23 0.9500 . ? N5 O1 1.320(4) . ? N5 C24 1.352(6) . ? C24 C25 1.377(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.389(5) . ? C26 C27 1.402(5) . ? C27 C28 1.379(5) . ? C27 H27 0.9500 . ? C28 N6 1.345(5) . ? C28 H28 0.9500 . ? N6 O2 1.316(4) . ? N6 C29 1.369(5) . ? C29 C30 1.366(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.396(5) . ? C31 C35 1.398(5) . ? C32 C33 1.373(5) . ? C32 H32 0.9500 . ? C33 N7 1.366(5) . ? C33 H33 0.9500 . ? N7 O3 1.313(4) . ? N7 C34 1.350(5) . ? C34 C35 1.379(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C40 1.386(5) . ? C36 C37 1.390(5) . ? C37 C38 1.385(5) . ? C37 H37 0.9500 . ? C38 N8 1.352(5) . ? C38 H38 0.9500 . ? N8 O4 1.314(4) . ? N8 C39 1.346(5) . ? C39 C40 1.377(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 O5 1.382(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O5 H5 0.8400 . ? C42 O6 1.474(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O6 H6 0.8400 . ? O7 C43 1.480(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N3 89.98(12) . . ? N4 Ni1 N1 90.14(12) . . ? N3 Ni1 N1 178.38(12) . . ? N4 Ni1 N2 175.03(12) . . ? N3 Ni1 N2 90.15(12) . . ? N1 Ni1 N2 89.88(12) . . ? C1 N1 C4 105.2(3) . . ? C1 N1 Ni1 127.2(2) . . ? C4 N1 Ni1 127.6(2) . . ? C9 N2 C6 106.0(3) . . ? C9 N2 Ni1 126.9(2) . . ? C6 N2 Ni1 127.0(2) . . ? C14 N3 C11 105.8(3) . . ? C14 N3 Ni1 126.8(2) . . ? C11 N3 Ni1 126.8(2) . . ? C19 N4 C16 105.8(3) . . ? C19 N4 Ni1 126.7(2) . . ? C16 N4 Ni1 127.0(2) . . ? N1 C1 C20 125.5(3) . . ? N1 C1 C2 110.3(3) . . ? C20 C1 C2 124.2(3) . . ? C3 C2 C1 107.3(3) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 106.8(3) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? N1 C4 C5 125.3(3) . . ? N1 C4 C3 110.4(3) . . ? C5 C4 C3 124.0(3) . . ? C6 C5 C4 123.8(3) . . ? C6 C5 C21 118.6(3) . . ? C4 C5 C21 117.6(3) . . ? N2 C6 C5 125.7(3) . . ? N2 C6 C7 109.7(3) . . ? C5 C6 C7 124.5(3) . . ? C8 C7 C6 107.1(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 107.1(3) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N2 C9 C10 125.7(3) . . ? N2 C9 C8 110.0(3) . . ? C10 C9 C8 124.2(3) . . ? C9 C10 C11 124.1(3) . . ? C9 C10 C26 118.1(3) . . ? C11 C10 C26 117.8(3) . . ? N3 C11 C10 125.0(3) . . ? N3 C11 C12 109.8(3) . . ? C10 C11 C12 125.2(3) . . ? C13 C12 C11 107.2(3) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 107.1(3) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N3 C14 C15 125.4(3) . . ? N3 C14 C13 110.0(3) . . ? C15 C14 C13 124.5(3) . . ? C16 C15 C14 124.0(3) . . ? C16 C15 C31 117.9(3) . . ? C14 C15 C31 118.2(3) . . ? C15 C16 N4 125.2(3) . . ? C15 C16 C17 125.4(3) . . ? N4 C16 C17 109.3(3) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 107.3(3) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? N4 C19 C20 126.0(3) . . ? N4 C19 C18 110.1(3) . . ? C20 C19 C18 123.8(3) . . ? C1 C20 C19 123.9(3) . . ? C1 C20 C36 118.4(3) . . ? C19 C20 C36 117.7(3) . . ? C25 C21 C22 117.1(3) . . ? C25 C21 C5 121.2(3) . . ? C22 C21 C5 121.7(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? N5 C23 C22 120.7(4) . . ? N5 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? O1 N5 C23 119.5(4) . . ? O1 N5 C24 120.6(4) . . ? C23 N5 C24 120.0(4) . . ? N5 C24 C25 120.8(4) . . ? N5 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C21 120.9(4) . . ? C24 C25 H25 119.6 . . ? C21 C25 H25 119.6 . . ? C30 C26 C27 116.3(3) . . ? C30 C26 C10 121.4(3) . . ? C27 C26 C10 122.3(3) . . ? C28 C27 C26 121.5(4) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? N6 C28 C27 120.1(4) . . ? N6 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? O2 N6 C28 121.6(3) . . ? O2 N6 C29 118.3(3) . . ? C28 N6 C29 120.0(3) . . ? C30 C29 N6 120.7(3) . . ? C30 C29 H29 119.7 . . ? N6 C29 H29 119.7 . . ? C29 C30 C26 121.3(4) . . ? C29 C30 H30 119.3 . . ? C26 C30 H30 119.3 . . ? C32 C31 C35 116.4(3) . . ? C32 C31 C15 121.7(3) . . ? C35 C31 C15 121.8(3) . . ? C33 C32 C31 121.3(3) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? N7 C33 C32 120.5(4) . . ? N7 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? O3 N7 C34 120.0(3) . . ? O3 N7 C33 120.0(3) . . ? C34 N7 C33 119.9(3) . . ? N7 C34 C35 120.5(3) . . ? N7 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C31 121.3(3) . . ? C34 C35 H35 119.4 . . ? C31 C35 H35 119.4 . . ? C40 C36 C37 116.7(3) . . ? C40 C36 C20 120.9(3) . . ? C37 C36 C20 122.4(3) . . ? C38 C37 C36 120.8(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? N8 C38 C37 120.7(4) . . ? N8 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? O4 N8 C39 121.1(3) . . ? O4 N8 C38 119.3(3) . . ? C39 N8 C38 119.6(3) . . ? N8 C39 C40 120.9(3) . . ? N8 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C36 121.1(4) . . ? C39 C40 H40 119.4 . . ? C36 C40 H40 119.4 . . ? O5 C41 H41A 109.5 . . ? O5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 O5 H5 109.5 . . ? O6 C42 H42A 109.5 . . ? O6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C42 O6 H6 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.70 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.673 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.134 # Attachment 'Hosseini_3-HgBr2.cif' data_e513a _database_code_depnum_ccdc_archive 'CCDC 649318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H24 Br4 Hg2 N8 Ni O4' _chemical_formula_weight 1460.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 15.2904(4) _cell_length_b 15.2904(4) _cell_length_c 16.7746(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3921.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6510 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 28.90 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 12.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.190 _exptl_absorpt_correction_T_max 0.380 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32721 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.02 _reflns_number_total 2870 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+36.1989P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(10) _refine_ls_number_reflns 2870 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.64748(2) 0.7500 0.6250 0.02626(8) Uani 1 2 d S . . Br1 Br 0.66493(5) 0.88698(5) 0.69787(4) 0.03627(16) Uani 1 1 d . . . Ni1 Ni 0.0000 1.0000 0.5000 0.0113(2) Uani 1 4 d S . . N1 N 0.0657(3) 0.8914(3) 0.5070(2) 0.0132(8) Uani 1 1 d . . . C1 C 0.0348(3) 0.8070(3) 0.5040(3) 0.0152(9) Uani 1 1 d . . . C2 C 0.1036(3) 0.7450(4) 0.5158(3) 0.0199(9) Uani 1 1 d . . . H2 H 0.0979 0.6831 0.5163 0.024 Uiso 1 1 calc R . . C3 C 0.1784(4) 0.7910(4) 0.5262(3) 0.0200(10) Uani 1 1 d . . . H3 H 0.2349 0.7679 0.5365 0.024 Uiso 1 1 calc R . . C4 C 0.1554(3) 0.8819(3) 0.5185(3) 0.0144(9) Uani 1 1 d . . . C5 C 0.2165(3) 0.9488(3) 0.5127(3) 0.0152(9) Uani 1 1 d . . . C6 C 0.3110(3) 0.9245(4) 0.5172(3) 0.0176(10) Uani 1 1 d . . . C7 C 0.3625(4) 0.9229(4) 0.4486(3) 0.0226(11) Uani 1 1 d . . . H7 H 0.3401 0.9448 0.3997 0.027 Uiso 1 1 calc R . . C8 C 0.4462(4) 0.8892(4) 0.4521(4) 0.0266(11) Uani 1 1 d . . . H8 H 0.4812 0.8886 0.4053 0.032 Uiso 1 1 calc R . . N2 N 0.4790(3) 0.8573(3) 0.5204(3) 0.0229(9) Uani 1 1 d . . . O1 O 0.5561(3) 0.8181(4) 0.5175(3) 0.0351(11) Uani 1 1 d . . . C9 C 0.4325(4) 0.8647(4) 0.5886(3) 0.0254(12) Uani 1 1 d . . . H9 H 0.4582 0.8469 0.6375 0.031 Uiso 1 1 calc R . . C10 C 0.3490(4) 0.8973(4) 0.5886(3) 0.0220(10) Uani 1 1 d . . . H10 H 0.3172 0.9014 0.6371 0.026 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 Hg1 0.02451(16) 0.02947(17) 0.02480(13) -0.00045(13) 0.000 0.000 Br1 0.0445(4) 0.0332(3) 0.0311(3) -0.0043(3) -0.0041(3) -0.0046(3) Ni1 0.0104(3) 0.0104(3) 0.0131(5) 0.000 0.000 0.000 N1 0.0121(18) 0.0126(18) 0.0150(18) 0.0008(15) 0.0010(14) 0.0006(14) C1 0.019(2) 0.014(2) 0.013(2) -0.0013(17) 0.0016(18) 0.0028(18) C2 0.021(2) 0.013(2) 0.026(2) 0.003(2) 0.0025(19) 0.004(2) C3 0.018(2) 0.018(2) 0.024(3) 0.000(2) -0.0016(19) 0.000(2) C4 0.012(2) 0.017(2) 0.014(2) -0.0005(16) 0.0005(16) 0.0066(18) C5 0.013(2) 0.018(2) 0.015(2) 0.0004(18) -0.0021(17) -0.0001(18) C6 0.012(2) 0.020(2) 0.021(2) -0.0006(18) -0.0008(18) -0.0005(19) C7 0.018(2) 0.029(3) 0.020(2) 0.004(2) -0.002(2) 0.002(2) C8 0.021(3) 0.034(3) 0.024(3) -0.002(2) 0.002(2) 0.007(2) N2 0.014(2) 0.025(2) 0.030(2) -0.002(2) -0.0004(17) -0.0001(19) O1 0.0150(19) 0.054(3) 0.036(3) 0.003(2) -0.0020(17) 0.015(2) C9 0.018(2) 0.036(3) 0.023(3) -0.001(2) -0.006(2) 0.004(2) C10 0.013(2) 0.031(3) 0.022(2) -0.001(2) 0.002(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Br1 2.4397(7) 14_465 ? Hg1 Br1 2.4397(7) . ? Hg1 O1 2.508(5) 14_465 ? Hg1 O1 2.508(5) . ? Ni1 N1 1.943(4) 2_575 ? Ni1 N1 1.943(4) 4_666 ? Ni1 N1 1.943(4) . ? Ni1 N1 1.943(4) 3_466 ? N1 C1 1.375(6) . ? N1 C4 1.393(6) . ? C1 C5 1.393(7) 3_466 ? C1 C2 1.430(7) . ? C2 C3 1.354(8) . ? C2 H2 0.9500 . ? C3 C4 1.439(7) . ? C3 H3 0.9500 . ? C4 C5 1.389(8) . ? C5 C1 1.393(7) 4_666 ? C5 C6 1.493(7) . ? C6 C7 1.394(8) . ? C6 C10 1.395(7) . ? C7 C8 1.380(8) . ? C7 H7 0.9500 . ? C8 N2 1.342(8) . ? C8 H8 0.9500 . ? N2 O1 1.324(6) . ? N2 C9 1.351(8) . ? C9 C10 1.370(8) . ? C9 H9 0.9500 . ? C10 H10 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 Br1 Hg1 Br1 167.44(4) 14_465 . ? Br1 Hg1 O1 93.73(13) 14_465 14_465 ? Br1 Hg1 O1 93.26(13) . 14_465 ? Br1 Hg1 O1 93.26(13) 14_465 . ? Br1 Hg1 O1 93.73(13) . . ? O1 Hg1 O1 112.3(2) 14_465 . ? N1 Ni1 N1 90.212(16) 2_575 4_666 ? N1 Ni1 N1 173.0(2) 2_575 . ? N1 Ni1 N1 90.211(15) 4_666 . ? N1 Ni1 N1 90.211(16) 2_575 3_466 ? N1 Ni1 N1 173.1(2) 4_666 3_466 ? N1 Ni1 N1 90.208(16) . 3_466 ? C1 N1 C4 104.2(4) . . ? C1 N1 Ni1 128.5(3) . . ? C4 N1 Ni1 127.3(3) . . ? N1 C1 C5 125.1(4) . 3_466 ? N1 C1 C2 111.4(5) . . ? C5 C1 C2 123.4(5) 3_466 . ? C3 C2 C1 107.1(5) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 106.5(5) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C5 C4 N1 125.2(4) . . ? C5 C4 C3 123.5(5) . . ? N1 C4 C3 110.7(5) . . ? C4 C5 C1 122.3(5) . 4_666 ? C4 C5 C6 117.7(5) . . ? C1 C5 C6 119.7(5) 4_666 . ? C7 C6 C10 117.9(5) . . ? C7 C6 C5 120.6(5) . . ? C10 C6 C5 121.4(5) . . ? C8 C7 C6 119.7(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? N2 C8 C7 121.2(5) . . ? N2 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? O1 N2 C9 122.5(5) . . ? O1 N2 C8 117.8(5) . . ? C9 N2 C8 119.7(5) . . ? N2 O1 Hg1 131.2(4) . . ? N2 C9 C10 121.4(5) . . ? N2 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C6 119.7(5) . . ? C9 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.497 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.190 # Attachment 'Hosseini_4-PbI2.cif' data_e458a _database_code_depnum_ccdc_archive 'CCDC 649319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 I4 N8 O6 Pb2 Zn' _chemical_formula_weight 1732.11 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' Zn Zn 0.2839 1.4301 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8976(3) _cell_length_b 11.5397(3) _cell_length_c 17.3986(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.1380(10) _cell_angle_gamma 90.00 _cell_volume 2431.20(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5896 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 24.41 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 9.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3410 _exptl_absorpt_correction_T_max 0.6180 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28138 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5559 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+30.6595P] 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 5559 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.23749(4) 0.23722(4) 0.48974(3) 0.04317(17) Uani 1 1 d . . . I1 I -0.43234(11) 0.17540(13) 0.35094(8) 0.0958(5) Uani 1 1 d . . . I2 I -0.1911(5) 0.4676(5) 0.4446(4) 0.0825(15) Uani 0.60 1 d P . . I3A I -0.2262(12) 0.4567(8) 0.4145(10) 0.095(5) Uani 0.25 1 d P . . I3B I -0.2917(13) 0.4274(13) 0.3562(8) 0.118(6) Uani 0.15 1 d P . . Zn1 Zn 0.0000 0.5000 0.0000 0.0161(3) Uani 1 2 d S . . N1 N -0.1084(6) 0.5095(6) 0.0632(4) 0.0184(13) Uani 1 1 d . . . N2 N 0.1020(6) 0.3938(6) 0.0903(4) 0.0183(14) Uani 1 1 d . . . C1 C -0.2057(7) 0.5705(7) 0.0410(5) 0.0185(16) Uani 1 1 d . . . C2 C -0.2589(7) 0.5512(8) 0.1006(5) 0.0231(18) Uani 1 1 d . . . H2 H -0.3271 0.5834 0.0998 0.028 Uiso 1 1 calc R . . C3 C -0.1929(7) 0.4784(8) 0.1583(5) 0.0248(18) Uani 1 1 d . . . H3 H -0.2061 0.4500 0.2053 0.030 Uiso 1 1 calc R . . C4 C -0.0987(7) 0.4524(7) 0.1341(5) 0.0190(16) Uani 1 1 d . . . C5 C -0.0136(7) 0.3729(7) 0.1753(5) 0.0212(17) Uani 1 1 d . . . C6 C 0.0781(7) 0.3466(7) 0.1541(5) 0.0218(17) Uani 1 1 d . . . C7 C 0.1620(8) 0.2618(9) 0.1961(6) 0.032(2) Uani 1 1 d . . . H7 H 0.1647 0.2167 0.2425 0.038 Uiso 1 1 calc R . . C8 C 0.2356(8) 0.2595(9) 0.1562(6) 0.030(2) Uani 1 1 d . . . H8 H 0.3002 0.2129 0.1696 0.037 Uiso 1 1 calc R . . C9 C 0.1973(7) 0.3416(7) 0.0890(5) 0.0193(16) Uani 1 1 d . . . C10 C 0.2470(7) 0.3594(7) 0.0300(5) 0.0196(16) Uani 1 1 d . . . C11 C -0.0263(7) 0.3132(8) 0.2480(5) 0.0235(18) Uani 1 1 d . . . C12 C 0.0322(8) 0.3447(9) 0.3271(5) 0.030(2) Uani 1 1 d . . . H12 H 0.0881 0.4023 0.3377 0.036 Uiso 1 1 calc R . . C13 C 0.0101(9) 0.2928(9) 0.3914(6) 0.032(2) Uani 1 1 d . . . H13 H 0.0498 0.3164 0.4460 0.039 Uiso 1 1 calc R . . N3 N -0.0669(6) 0.2094(6) 0.3777(4) 0.0203(14) Uani 1 1 d . . . O1 O -0.0911(5) 0.1626(5) 0.4394(4) 0.0273(14) Uani 1 1 d . . . C14 C -0.1220(9) 0.1730(9) 0.3016(6) 0.036(2) Uani 1 1 d . . . H14 H -0.1747 0.1124 0.2927 0.043 Uiso 1 1 calc R . . C15 C -0.1024(10) 0.2234(10) 0.2358(6) 0.041(3) Uani 1 1 d . . . H15 H -0.1412 0.1966 0.1819 0.049 Uiso 1 1 calc R . . C16 C 0.3543(7) 0.3013(8) 0.0422(6) 0.0250(18) Uani 1 1 d . . . C17 C 0.4474(9) 0.3304(11) 0.1074(7) 0.041(2) Uani 1 1 d . . . H17 H 0.4425 0.3856 0.1465 0.049 Uiso 1 1 calc R . . C18 C 0.5484(10) 0.2790(12) 0.1159(8) 0.049(3) Uani 1 1 d . . . H18 H 0.6121 0.2989 0.1612 0.059 Uiso 1 1 calc R . . N4 N 0.5564(8) 0.2025(9) 0.0614(6) 0.043(2) Uani 1 1 d . . . O2 O 0.6542(7) 0.1612(9) 0.0671(6) 0.065(3) Uani 1 1 d . . . C19 C 0.4657(11) 0.1689(10) -0.0001(8) 0.047(3) Uani 1 1 d . . . H19 H 0.4725 0.1109 -0.0368 0.057 Uiso 1 1 calc R . . C20 C 0.3640(9) 0.2150(9) -0.0117(7) 0.035(2) Uani 1 1 d . . . H20 H 0.3009 0.1891 -0.0554 0.042 Uiso 1 1 calc R . . C21 C 0.3569(17) 0.0334(17) 0.8014(13) 0.091(6) Uani 1 1 d . . . H21A H 0.3203 0.0341 0.7418 0.137 Uiso 1 1 calc R . . H21B H 0.4048 -0.0348 0.8173 0.137 Uiso 1 1 calc R . . H21C H 0.4014 0.1038 0.8185 0.137 Uiso 1 1 calc R . . O3 O 0.2791(9) 0.0295(9) 0.8383(6) 0.065(3) Uani 1 1 d . . . H3A H 0.3070 0.0009 0.8853 0.097 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 0.0472(3) 0.0484(3) 0.0459(3) 0.00468(19) 0.0314(2) 0.00726(19) I1 0.0806(8) 0.1127(10) 0.0799(8) -0.0415(7) 0.0095(6) 0.0230(7) I2 0.095(3) 0.0379(12) 0.146(4) -0.0141(17) 0.082(3) -0.0089(15) I3A 0.123(13) 0.035(5) 0.174(14) 0.050(7) 0.109(11) 0.032(6) I3B 0.139(12) 0.131(11) 0.127(9) 0.082(9) 0.099(9) 0.084(9) Zn1 0.0195(6) 0.0205(6) 0.0137(6) 0.0033(5) 0.0126(5) 0.0030(5) N1 0.023(3) 0.018(3) 0.020(3) 0.003(3) 0.014(3) 0.005(3) N2 0.019(3) 0.023(3) 0.019(3) 0.006(3) 0.014(3) 0.004(3) C1 0.022(4) 0.020(4) 0.020(4) 0.001(3) 0.015(3) 0.000(3) C2 0.024(4) 0.032(5) 0.023(4) 0.004(3) 0.020(4) 0.004(4) C3 0.028(4) 0.032(5) 0.023(4) 0.004(3) 0.019(4) 0.003(4) C4 0.026(4) 0.021(4) 0.017(4) -0.002(3) 0.017(3) -0.005(3) C5 0.029(5) 0.026(4) 0.015(4) 0.004(3) 0.015(3) 0.003(3) C6 0.026(4) 0.023(4) 0.023(4) 0.008(3) 0.017(3) 0.005(3) C7 0.033(5) 0.040(5) 0.029(5) 0.018(4) 0.020(4) 0.013(4) C8 0.026(5) 0.039(5) 0.032(5) 0.018(4) 0.018(4) 0.014(4) C9 0.019(4) 0.023(4) 0.019(4) 0.005(3) 0.010(3) 0.005(3) C10 0.018(4) 0.023(4) 0.022(4) 0.000(3) 0.012(3) 0.007(3) C11 0.029(5) 0.030(4) 0.019(4) 0.008(3) 0.017(4) 0.007(4) C12 0.031(5) 0.037(5) 0.025(4) 0.010(4) 0.011(4) -0.008(4) C13 0.036(5) 0.042(6) 0.022(4) 0.006(4) 0.013(4) -0.003(4) N3 0.024(4) 0.024(4) 0.021(3) 0.007(3) 0.018(3) 0.007(3) O1 0.042(4) 0.026(3) 0.027(3) 0.014(2) 0.028(3) 0.012(3) C14 0.046(6) 0.034(5) 0.027(5) 0.003(4) 0.013(4) -0.015(5) C15 0.059(7) 0.041(6) 0.024(5) 0.001(4) 0.015(5) -0.022(5) C16 0.025(4) 0.024(4) 0.035(5) 0.007(4) 0.021(4) 0.008(3) C17 0.031(5) 0.051(7) 0.046(6) 0.006(5) 0.020(5) 0.006(5) C18 0.031(6) 0.072(8) 0.048(7) 0.003(6) 0.019(5) 0.006(5) N4 0.034(5) 0.049(5) 0.057(6) 0.023(5) 0.030(5) 0.017(4) O2 0.042(5) 0.086(7) 0.086(7) 0.045(6) 0.048(5) 0.038(5) C19 0.057(8) 0.030(6) 0.074(8) 0.010(5) 0.045(7) 0.015(5) C20 0.035(5) 0.031(5) 0.047(6) 0.004(4) 0.023(5) 0.002(4) C21 0.093(13) 0.079(12) 0.099(14) 0.022(10) 0.030(11) 0.006(10) O3 0.082(7) 0.060(6) 0.064(6) 0.016(5) 0.040(6) 0.019(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 Pb1 O1 2.491(6) . ? Pb1 O2 2.536(8) 4_466 ? Pb1 I3A 2.878(9) . ? Pb1 I2 2.893(6) . ? Pb1 I1 2.9116(13) . ? Pb1 I3B 3.096(10) . ? Zn1 N1 2.058(6) . ? Zn1 N1 2.058(6) 3_565 ? Zn1 N2 2.068(7) . ? Zn1 N2 2.068(7) 3_565 ? Zn1 O1 2.271(6) 4_565 ? Zn1 O1 2.271(6) 2 ? N1 C4 1.364(10) . ? N1 C1 1.374(10) . ? N2 C6 1.362(10) . ? N2 C9 1.377(10) . ? C1 C10 1.418(11) 3_565 ? C1 C2 1.445(10) . ? C2 C3 1.360(13) . ? C2 H2 0.9500 . ? C3 C4 1.448(11) . ? C3 H3 0.9500 . ? C4 C5 1.421(12) . ? C5 C6 1.389(11) . ? C5 C11 1.499(11) . ? C6 C7 1.456(12) . ? C7 C8 1.356(13) . ? C7 H7 0.9500 . ? C8 C9 1.453(11) . ? C8 H8 0.9500 . ? C9 C10 1.400(11) . ? C10 C1 1.418(11) 3_565 ? C10 C16 1.486(11) . ? C11 C12 1.371(13) . ? C11 C15 1.393(14) . ? C12 C13 1.383(12) . ? C12 H12 0.9500 . ? C13 N3 1.344(13) . ? C13 H13 0.9500 . ? N3 O1 1.332(8) . ? N3 C14 1.337(12) . ? O1 Zn1 2.271(6) 2_545 ? C14 C15 1.381(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.379(15) . ? C16 C20 1.402(14) . ? C17 C18 1.393(15) . ? C17 H17 0.9500 . ? C18 N4 1.325(17) . ? C18 H18 0.9500 . ? N4 O2 1.320(11) . ? N4 C19 1.342(17) . ? O2 Pb1 2.536(8) 4_665 ? C19 C20 1.365(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 O3 1.37(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O3 H3A 0.8400 . ? 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 O1 Pb1 O2 165.6(2) . 4_466 ? O1 Pb1 I3A 88.9(3) . . ? O2 Pb1 I3A 87.6(4) 4_466 . ? O1 Pb1 I2 88.3(2) . . ? O2 Pb1 I2 85.6(3) 4_466 . ? I3A Pb1 I2 11.4(4) . . ? O1 Pb1 I1 99.55(16) . . ? O2 Pb1 I1 94.5(2) 4_466 . ? I3A Pb1 I1 90.2(3) . . ? I2 Pb1 I1 101.54(12) . . ? O1 Pb1 I3B 89.1(3) . . ? O2 Pb1 I3B 92.7(4) 4_466 . ? I3A Pb1 I3B 21.3(4) . . ? I2 Pb1 I3B 32.7(4) . . ? I1 Pb1 I3B 69.1(4) . . ? N1 Zn1 N1 180.0(2) . 3_565 ? N1 Zn1 N2 89.8(3) . . ? N1 Zn1 N2 90.2(3) 3_565 . ? N1 Zn1 N2 90.2(3) . 3_565 ? N1 Zn1 N2 89.8(3) 3_565 3_565 ? N2 Zn1 N2 180.0(3) . 3_565 ? N1 Zn1 O1 87.3(2) . 4_565 ? N1 Zn1 O1 92.7(2) 3_565 4_565 ? N2 Zn1 O1 87.4(3) . 4_565 ? N2 Zn1 O1 92.6(3) 3_565 4_565 ? N1 Zn1 O1 92.7(2) . 2 ? N1 Zn1 O1 87.3(2) 3_565 2 ? N2 Zn1 O1 92.6(3) . 2 ? N2 Zn1 O1 87.4(3) 3_565 2 ? O1 Zn1 O1 180.00(17) 4_565 2 ? C4 N1 C1 107.0(6) . . ? C4 N1 Zn1 126.1(5) . . ? C1 N1 Zn1 126.8(5) . . ? C6 N2 C9 107.0(6) . . ? C6 N2 Zn1 126.3(5) . . ? C9 N2 Zn1 125.8(5) . . ? N1 C1 C10 124.8(7) . 3_565 ? N1 C1 C2 109.4(7) . . ? C10 C1 C2 125.8(7) 3_565 . ? C3 C2 C1 107.1(7) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 106.7(7) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? N1 C4 C5 125.6(7) . . ? N1 C4 C3 109.8(7) . . ? C5 C4 C3 124.5(7) . . ? C6 C5 C4 126.0(7) . . ? C6 C5 C11 118.4(7) . . ? C4 C5 C11 115.7(7) . . ? N2 C6 C5 125.5(7) . . ? N2 C6 C7 109.9(7) . . ? C5 C6 C7 124.5(7) . . ? C8 C7 C6 106.6(8) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 107.2(8) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 125.8(7) . . ? N2 C9 C8 109.3(7) . . ? C10 C9 C8 124.8(7) . . ? C9 C10 C1 126.4(7) . 3_565 ? C9 C10 C16 117.9(7) . . ? C1 C10 C16 115.7(7) 3_565 . ? C12 C11 C15 117.8(8) . . ? C12 C11 C5 122.9(8) . . ? C15 C11 C5 119.3(8) . . ? C11 C12 C13 120.1(9) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? N3 C13 C12 120.8(9) . . ? N3 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? O1 N3 C14 118.7(8) . . ? O1 N3 C13 120.8(7) . . ? C14 N3 C13 120.6(7) . . ? N3 O1 Zn1 118.8(5) . 2_545 ? N3 O1 Pb1 124.0(5) . . ? Zn1 O1 Pb1 117.1(2) 2_545 . ? N3 C14 C15 120.1(9) . . ? N3 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C11 120.5(9) . . ? C14 C15 H15 119.8 . . ? C11 C15 H15 119.8 . . ? C17 C16 C20 118.1(9) . . ? C17 C16 C10 120.8(8) . . ? C20 C16 C10 121.2(9) . . ? C16 C17 C18 120.1(11) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N4 C18 C17 120.5(12) . . ? N4 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? O2 N4 C18 119.6(11) . . ? O2 N4 C19 120.2(11) . . ? C18 N4 C19 120.2(10) . . ? N4 O2 Pb1 118.7(6) . 4_665 ? N4 C19 C20 122.3(11) . . ? N4 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C16 118.7(11) . . ? C19 C20 H20 120.7 . . ? C16 C20 H20 120.7 . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 O3 H3A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.014 _refine_diff_density_min -2.341 _refine_diff_density_rms 0.255