Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrea Bencini' _publ_contact_author_address ; Department of Chemistry, Polo Scientifico, University of Florence via della Lastruccia 3 I-50019 Sesto Fiorentino, Firenze, Italy ; _publ_contact_author_email andrea.bencini@unifi.it _publ_section_title ; Coordination features of a terpyridine-containing polyamine receptor. Effect of protonation on the photophysical properties of the complexes ; loop_ _publ_author_name 'Andrea Bencini' 'Carla Bazzicalupi' A.Bianchi 'Lucia Borsari' 'Andrea Danesi' 'Claudia Giorgi' ; P.Mariani ; F.Pina 'Samuele Santarelli' 'Barbara Valtancoli' data_[H5L]Br5.2H2O _database_code_depnum_ccdc_archive 'CCDC 613191' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 N7 +5, (Br -1)5, (H2 O)2' _chemical_formula_sum 'C26 H44 Br5 N7 O2' _chemical_formula_weight 886.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.645(2) _cell_length_b 15.062(3) _cell_length_c 16.524(4) _cell_angle_alpha 75.695(9) _cell_angle_beta 77.65(1) _cell_angle_gamma 82.034(9) _cell_volume 1793.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 7.046 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'crossed Gobels mirrors' _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5697 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 55.18 _reflns_number_total 3512 _reflns_number_gt 1857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart\Bruker CCD' _computing_cell_refinement 'Saint\Bruker CCD' _computing_data_reduction 'Saint\Bruker CCD' _computing_structure_solution 'SIR97 (Altomare 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _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. Colourless single crystals of [H5L]Br5 . 2H2O were analyzed by means of X-ray crystallography. The intensities of some reflections were monitored during data collections to check the stability of the crystal: no loss of intensity was observed. The integrated intensities were corrected for Lorentz and polarization effects and empirical absorption correction was applied by means of SADABS program. The structure were solved by direct methods (SIR97). Refinement was performed by means of full-matrix least-squares using SHELX-97 program. All the non hydrogen atoms were anisotropically refined while the hydrogen atoms linked to carbon atoms were introduced in calculated position and their coordinates were refined according to the linked atoms. Four of the five acidic protons were introduced in calculated position on the secondary nitrogens. The remaining fifth proton was not localized in the final DF map and thus not introduced in the calculation. ; _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^)+(0.2000P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3512 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.625 _refine_ls_restrained_S_all 0.625 _refine_ls_shift/su_max 0.003 _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 Br1 Br -0.54446(16) -0.60446(8) 0.83249(8) 0.0677(5) Uani 1 1 d . . . Br2 Br 0.32059(17) -0.34528(9) 0.90097(8) 0.0724(5) Uani 1 1 d . . . Br3 Br 0.2872(2) -0.41772(9) 0.45623(8) 0.0796(5) Uani 1 1 d . . . Br4 Br 0.05631(16) -0.80997(8) 0.86520(8) 0.0673(5) Uani 1 1 d . . . Br5 Br -0.10231(18) -0.20451(10) 0.71327(9) 0.0842(5) Uani 1 1 d . . . N7 N 0.3265(10) -0.2001(5) 0.7254(5) 0.049(2) Uani 1 1 d . . . H7A H 0.2103 -0.1862 0.7206 0.058 Uiso 1 1 calc R . . H7B H 0.3349 -0.2532 0.7646 0.058 Uiso 1 1 calc R . . N5 N -0.1232(11) -0.6034(5) 0.8244(6) 0.054(2) Uani 1 1 d . . . H5A H -0.0627 -0.6591 0.8370 0.065 Uiso 1 1 calc R . . H5B H -0.2412 -0.6116 0.8386 0.065 Uiso 1 1 calc R . . N4 N -0.2685(12) -0.3086(5) 0.9132(6) 0.055(2) Uani 1 1 d . . . H4A H -0.3867 -0.3147 0.9206 0.065 Uiso 1 1 calc R . . H4B H -0.2319 -0.2808 0.8584 0.065 Uiso 1 1 calc R . . N6 N 0.3752(11) -0.4630(5) 0.6521(5) 0.055(2) Uani 1 1 d . . . H6A H 0.3882 -0.4599 0.5961 0.066 Uiso 1 1 calc R . . H6B H 0.4355 -0.5158 0.6748 0.066 Uiso 1 1 calc R . . C10 C 0.4385(18) -0.2129(8) 0.6397(7) 0.067(3) Uani 1 1 d . . . H10A H 0.4243 -0.1569 0.5966 0.080 Uiso 1 1 calc R . . H10B H 0.5647 -0.2249 0.6438 0.080 Uiso 1 1 calc R . . N1 N 0.1610(12) -0.0027(6) 0.7276(6) 0.054(2) Uani 1 1 d . . . N3 N -0.3108(13) -0.0889(6) 0.8949(6) 0.062(3) Uani 1 1 d . . . N2 N -0.1779(12) 0.0463(5) 0.7789(6) 0.051(2) Uani 1 1 d . . . C14 C -0.0842(13) -0.5462(6) 0.8802(6) 0.041(3) Uani 1 1 d . . . H14A H -0.1124 -0.5788 0.9392 0.049 Uiso 1 1 calc R . . H14B H 0.0429 -0.5373 0.8668 0.049 Uiso 1 1 calc R . . C15 C 0.3877(15) -0.1268(6) 0.7537(7) 0.052(3) Uani 1 1 d . . . H15A H 0.5177 -0.1352 0.7465 0.062 Uiso 1 1 calc R . . H15B H 0.3400 -0.1331 0.8140 0.062 Uiso 1 1 calc R . . C16 C -0.5493(16) -0.1627(6) 0.9971(6) 0.049(3) Uani 1 1 d . . . H16 H -0.5869 -0.2137 1.0389 0.059 Uiso 1 1 calc R . . C17 C 0.1206(16) -0.5616(6) 0.6953(7) 0.058(3) Uani 1 1 d . . . H17A H 0.1466 -0.5738 0.6388 0.070 Uiso 1 1 calc R . . H17B H 0.1885 -0.6089 0.7307 0.070 Uiso 1 1 calc R . . C18 C -0.3774(15) -0.1626(8) 0.9541(7) 0.055(3) Uani 1 1 d . . . C19 C -0.3500(18) 0.0615(7) 0.8133(7) 0.062(3) Uani 1 1 d . . . C20 C -0.0843(16) 0.1093(7) 0.7143(7) 0.055(3) Uani 1 1 d . . . C21 C 0.1082(15) 0.0833(7) 0.6871(7) 0.055(3) Uani 1 1 d . . . C23 C 0.4592(14) -0.3848(6) 0.6634(6) 0.050(3) Uani 1 1 d . . . H23A H 0.5879 -0.3918 0.6429 0.060 Uiso 1 1 calc R . . H23B H 0.4388 -0.3844 0.7233 0.060 Uiso 1 1 calc R . . C24 C 0.3339(16) -0.0305(8) 0.7078(7) 0.060(3) Uani 1 1 d . . . C25 C 0.1852(16) -0.4667(7) 0.6900(7) 0.062(3) Uani 1 1 d . . . H25A H 0.1152 -0.4187 0.6563 0.075 Uiso 1 1 calc R . . H25B H 0.1653 -0.4553 0.7467 0.075 Uiso 1 1 calc R . . C26 C -0.4333(16) -0.0143(7) 0.8789(8) 0.055(3) Uani 1 1 d . . . C27 C -0.1758(18) 0.1936(7) 0.6827(8) 0.071(4) Uani 1 1 d . . . H27 H -0.1190 0.2369 0.6378 0.085 Uiso 1 1 calc R . . C28 C -0.1729(15) -0.4007(7) 0.9293(7) 0.056(3) Uani 1 1 d . . . H28A H -0.0464 -0.3950 0.9255 0.067 Uiso 1 1 calc R . . H28B H -0.2196 -0.4335 0.9866 0.067 Uiso 1 1 calc R . . C29 C -0.0796(16) -0.5684(7) 0.7312(8) 0.064(3) Uani 1 1 d . . . H29A H -0.1428 -0.5078 0.7167 0.077 Uiso 1 1 calc R . . H29B H -0.1239 -0.6086 0.7040 0.077 Uiso 1 1 calc R . . C30 C 0.4648(18) 0.0211(9) 0.6482(8) 0.071(4) Uani 1 1 d . . . H30 H 0.5838 -0.0027 0.6353 0.086 Uiso 1 1 calc R . . C31 C -0.4397(17) 0.1462(7) 0.7838(7) 0.059(3) Uani 1 1 d . . . H31 H -0.5596 0.1593 0.8074 0.071 Uiso 1 1 calc R . . C32 C 0.3785(17) -0.2932(7) 0.6141(7) 0.059(3) Uani 1 1 d . . . H32A H 0.4183 -0.2882 0.5535 0.071 Uiso 1 1 calc R . . H32B H 0.2483 -0.2911 0.6266 0.071 Uiso 1 1 calc R . . C33 C -0.2440(16) -0.2479(7) 0.9672(7) 0.058(3) Uani 1 1 d . . . H33A H -0.1221 -0.2300 0.9519 0.070 Uiso 1 1 calc R . . H33B H -0.2648 -0.2802 1.0265 0.070 Uiso 1 1 calc R . . C36 C -0.6686(16) -0.0857(8) 0.9779(7) 0.063(3) Uani 1 1 d . . . H36 H -0.7881 -0.0852 1.0055 0.076 Uiso 1 1 calc R . . C40 C -0.1916(15) -0.4543(7) 0.8686(8) 0.062(3) Uani 1 1 d . . . H40A H -0.1531 -0.4193 0.8112 0.074 Uiso 1 1 calc R . . H40B H -0.3174 -0.4635 0.8752 0.074 Uiso 1 1 calc R . . C42 C -0.6067(16) -0.0093(7) 0.9166(7) 0.063(3) Uani 1 1 d . . . H42 H -0.6832 0.0433 0.9024 0.076 Uiso 1 1 calc R . . C48 C 0.224(2) 0.1395(8) 0.6304(9) 0.085(4) Uani 1 1 d . . . H48 H 0.1824 0.1986 0.6049 0.102 Uiso 1 1 calc R . . C49 C 0.404(2) 0.1100(9) 0.6101(9) 0.085(4) Uani 1 1 d . . . H49 H 0.4832 0.1488 0.5716 0.102 Uiso 1 1 calc R . . C52 C -0.3516(18) 0.2105(7) 0.7198(8) 0.068(4) Uani 1 1 d . . . H52 H -0.4129 0.2672 0.7011 0.082 Uiso 1 1 calc R . . O1 O 0.846(2) -0.3561(11) 0.5132(10) 0.214(7) Uani 1 1 d . . . O2 O 0.916(3) 0.0160(17) 0.5041(18) 0.157(9) Uani 0.60 1 d P . . O3 O 0.876(4) 0.091(2) 0.5050(16) 0.108(9) Uani 0.40 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 Br1 0.0567(8) 0.0677(8) 0.0732(10) -0.0059(7) -0.0124(7) -0.0042(6) Br2 0.0605(9) 0.0818(9) 0.0683(10) -0.0073(7) -0.0089(7) -0.0072(7) Br3 0.0888(11) 0.0836(9) 0.0593(10) -0.0145(8) -0.0154(8) 0.0154(8) Br4 0.0623(9) 0.0513(7) 0.0861(11) -0.0175(7) -0.0144(7) 0.0070(6) Br5 0.0581(9) 0.1050(11) 0.0807(11) -0.0089(9) -0.0099(8) -0.0040(7) N7 0.036(5) 0.046(5) 0.055(6) -0.001(4) -0.006(4) 0.002(4) N5 0.053(6) 0.049(5) 0.052(7) 0.009(5) -0.013(5) -0.003(4) N4 0.056(6) 0.047(5) 0.062(6) -0.013(5) -0.015(5) 0.004(4) N6 0.045(6) 0.047(5) 0.063(6) -0.015(5) 0.007(5) 0.000(4) C10 0.098(10) 0.071(7) 0.032(7) -0.012(6) -0.001(6) -0.026(7) N1 0.052(6) 0.051(6) 0.065(7) -0.028(5) -0.007(5) -0.005(5) N3 0.078(7) 0.049(6) 0.052(7) -0.013(5) -0.004(5) 0.008(5) N2 0.049(6) 0.047(5) 0.052(6) -0.012(5) 0.007(5) -0.009(4) C14 0.040(6) 0.036(5) 0.039(7) 0.002(5) 0.000(5) -0.007(4) C15 0.056(7) 0.044(6) 0.052(7) -0.016(6) 0.007(6) -0.013(5) C16 0.072(9) 0.036(6) 0.037(7) -0.007(5) -0.003(6) -0.004(6) C17 0.087(10) 0.039(6) 0.044(7) -0.007(5) -0.010(6) -0.002(6) C18 0.044(8) 0.073(8) 0.047(8) -0.026(7) 0.010(6) -0.005(6) C19 0.092(10) 0.038(6) 0.048(8) -0.009(6) -0.010(7) 0.012(7) C20 0.074(9) 0.045(6) 0.052(8) -0.017(6) -0.024(7) 0.001(6) C21 0.066(9) 0.038(6) 0.060(8) -0.018(6) -0.009(7) 0.004(6) C23 0.056(7) 0.051(6) 0.032(7) 0.003(5) -0.005(5) -0.001(5) C24 0.048(8) 0.072(8) 0.067(9) -0.040(7) 0.006(6) -0.010(6) C25 0.076(9) 0.048(6) 0.066(8) -0.024(6) -0.018(7) 0.010(6) C26 0.058(8) 0.044(6) 0.073(9) -0.028(6) -0.019(7) 0.006(6) C27 0.084(10) 0.051(7) 0.070(9) -0.011(7) -0.014(8) 0.009(7) C28 0.057(7) 0.060(7) 0.051(8) -0.027(6) -0.005(6) 0.008(6) C29 0.071(9) 0.046(6) 0.081(10) -0.024(7) -0.012(7) -0.005(6) C30 0.073(9) 0.083(9) 0.062(9) -0.036(8) 0.012(7) -0.026(8) C31 0.081(9) 0.049(7) 0.043(8) 0.001(6) -0.013(6) -0.013(6) C32 0.091(9) 0.053(7) 0.031(7) -0.006(6) -0.013(6) -0.001(6) C33 0.070(8) 0.052(6) 0.060(8) -0.013(6) -0.028(6) 0.001(6) C36 0.054(8) 0.072(8) 0.055(9) -0.013(7) 0.002(6) 0.001(7) C40 0.055(8) 0.048(6) 0.071(9) -0.006(6) -0.006(6) 0.012(5) C42 0.055(9) 0.050(7) 0.067(9) 0.003(7) -0.005(7) 0.015(6) C48 0.088(12) 0.049(7) 0.088(11) 0.008(7) 0.023(8) -0.008(7) C49 0.107(13) 0.063(9) 0.075(10) -0.008(8) -0.005(9) -0.006(8) C52 0.084(10) 0.038(6) 0.072(9) -0.010(6) 0.001(8) 0.004(6) O1 0.158(14) 0.241(17) 0.171(13) 0.013(12) 0.034(10) 0.018(12) O2 0.13(2) 0.133(19) 0.21(2) -0.071(18) 0.00(2) -0.01(2) O3 0.11(2) 0.13(2) 0.091(19) -0.034(18) 0.006(16) -0.06(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 N7 C15 1.466(12) . ? N7 C10 1.531(12) . ? N5 C29 1.479(14) . ? N5 C14 1.504(12) . ? N4 C28 1.466(12) . ? N4 C33 1.480(13) . ? N6 C25 1.456(13) . ? N6 C23 1.485(12) . ? C10 C32 1.530(14) . ? N1 C24 1.326(13) . ? N1 C21 1.353(12) . ? N3 C18 1.362(13) . ? N3 C26 1.370(13) . ? N2 C19 1.329(14) . ? N2 C20 1.383(13) . ? C14 C40 1.500(12) . ? C15 C24 1.507(15) . ? C16 C18 1.354(14) . ? C16 C36 1.387(14) . ? C17 C29 1.526(16) . ? C17 C25 1.552(14) . ? C18 C33 1.526(14) . ? C19 C31 1.390(14) . ? C19 C26 1.475(16) . ? C20 C27 1.399(14) . ? C20 C21 1.471(15) . ? C21 C48 1.359(15) . ? C23 C32 1.540(13) . ? C24 C30 1.411(15) . ? C26 C42 1.339(15) . ? C27 C52 1.370(16) . ? C28 C40 1.474(15) . ? C30 C49 1.394(17) . ? C31 C52 1.371(14) . ? C36 C42 1.394(14) . ? C48 C49 1.379(18) . ? O2 O3 1.14(3) . ? O2 O2 1.30(4) 2_756 ? 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 C15 N7 C10 111.5(8) . . ? C29 N5 C14 118.0(8) . . ? C28 N4 C33 115.5(8) . . ? C25 N6 C23 115.0(7) . . ? C32 C10 N7 110.3(9) . . ? C24 N1 C21 116.2(9) . . ? C18 N3 C26 115.0(10) . . ? C19 N2 C20 123.8(9) . . ? C40 C14 N5 111.6(9) . . ? N7 C15 C24 114.9(9) . . ? C18 C16 C36 119.2(10) . . ? C29 C17 C25 114.0(8) . . ? C16 C18 N3 123.6(10) . . ? C16 C18 C33 121.6(11) . . ? N3 C18 C33 114.9(9) . . ? N2 C19 C31 118.0(11) . . ? N2 C19 C26 117.3(9) . . ? C31 C19 C26 124.6(11) . . ? C27 C20 N2 118.3(11) . . ? C27 C20 C21 125.1(11) . . ? N2 C20 C21 116.5(9) . . ? C48 C21 N1 122.6(11) . . ? C48 C21 C20 124.7(11) . . ? N1 C21 C20 112.7(10) . . ? N6 C23 C32 110.2(9) . . ? N1 C24 C30 125.9(11) . . ? N1 C24 C15 114.7(10) . . ? C30 C24 C15 119.4(10) . . ? N6 C25 C17 111.5(8) . . ? C42 C26 N3 125.4(11) . . ? C42 C26 C19 123.5(10) . . ? N3 C26 C19 111.1(11) . . ? C52 C27 C20 118.0(12) . . ? C40 C28 N4 112.3(9) . . ? N5 C29 C17 114.4(10) . . ? C49 C30 C24 115.5(12) . . ? C52 C31 C19 120.0(11) . . ? C10 C32 C23 109.6(9) . . ? N4 C33 C18 108.7(8) . . ? C16 C36 C42 119.1(11) . . ? C28 C40 C14 113.1(10) . . ? C26 C42 C36 117.8(10) . . ? C21 C48 C49 120.7(12) . . ? C48 C49 C30 119.1(13) . . ? C31 C52 C27 121.8(11) . . ? O3 O2 O2 120(4) . 2_756 ? _diffrn_measured_fraction_theta_max 0.775 _diffrn_reflns_theta_full 55.18 _diffrn_measured_fraction_theta_full 0.775 _refine_diff_density_max 0.603 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.128 #===END data_[CdHL(H2O)2](ClO4)3 _database_code_depnum_ccdc_archive 'CCDC 613192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C26 H40 Cd N7 O2 +3), (Cl O4 -1)3 ; _chemical_formula_sum 'C26 H40 Cd Cl3 N7 O14' _chemical_formula_weight 893.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.026(1) _cell_length_b 11.965(1) _cell_length_c 15.417(1) _cell_angle_alpha 75.701(3) _cell_angle_beta 78.955(4) _cell_angle_gamma 84.782(4) _cell_volume 1757.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5912 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 20.97 _reflns_number_total 3292 _reflns_number_gt 3030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart\Bruker CCD' _computing_cell_refinement 'Saint\Bruker CCD' _computing_data_reduction 'Saint\Bruker CCD' _computing_structure_solution 'SIR97 (Altomare 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _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. Colourless single crystal of [CdHL(H2O)2](ClO4)3 was analyzed by means of X-ray crystallography. The intensities of some reflections were monitored during data collection to check the stability of the crystal: no loss of intensity was observed. The integrated intensities were corrected for Lorentz and polarization effects and empirical absorption correction was applied by means of SADABS program. The structure were solved by direct methods (SIR97). Refinement was performed by means of full-matrix least-squares using SHELX-97 program. All the non hydrogen atoms were anisotropically refined while the hydrogen atoms linked to carbon atoms were introduced in calculated position and their coordinates were refined according to the linked atoms. Disorder affects a perchlorate anion and some carbon atoms in the ligand molecule which gives rise to high displacement parameter. In particular, double positions were seen for the O31, O32 and O34 oxygens belonging to the perchlorate and the C19 carbon atom of the ligand (population parameter 0.7 - 0.3). DF map carried out at the end of refined did not allow the localization of acidic proton. ; _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^)+(0.1692P)^2^+0.8433P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3292 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 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 Cd1 Cd 0.15521(5) 0.16256(5) 0.67056(4) 0.0444(4) Uani 1 1 d . . . O1 O 0.3592(7) 0.0929(7) 0.5892(5) 0.075(2) Uani 1 1 d . . . O2 O -0.0508(6) 0.2345(6) 0.7539(5) 0.0672(19) Uani 1 1 d . . . C1 C 0.2404(10) 0.4048(9) 0.5318(6) 0.055(3) Uani 1 1 d . . . C2 C 0.2491(11) 0.4996(9) 0.4589(7) 0.068(3) Uani 1 1 d . . . H2 H 0.3081 0.5580 0.4522 0.082 Uiso 1 1 calc R . . C3 C 0.1661(14) 0.5034(11) 0.3968(9) 0.086(4) Uani 1 1 d . . . H3 H 0.1713 0.5640 0.3454 0.104 Uiso 1 1 calc R . . C4 C 0.0764(14) 0.4197(11) 0.4097(7) 0.078(4) Uani 1 1 d . . . H4A H 0.0209 0.4234 0.3671 0.094 Uiso 1 1 calc R . . C5 C 0.0674(10) 0.3288(8) 0.4860(6) 0.055(3) Uani 1 1 d . . . N1 N 0.1531(7) 0.3247(6) 0.5435(5) 0.0473(18) Uani 1 1 d . . . C6 C -0.0250(9) 0.2338(9) 0.5061(6) 0.051(2) Uani 1 1 d . . . C7 C -0.1298(12) 0.2342(12) 0.4590(8) 0.079(3) Uani 1 1 d . . . H7A H -0.1455 0.2968 0.4120 0.094 Uiso 1 1 calc R . . C8 C -0.2094(12) 0.1410(13) 0.4828(9) 0.083(4) Uani 1 1 d . . . H8 H -0.2787 0.1398 0.4507 0.100 Uiso 1 1 calc R . . C9 C -0.1891(11) 0.0491(11) 0.5533(8) 0.072(3) Uani 1 1 d . . . H9 H -0.2434 -0.0144 0.5697 0.086 Uiso 1 1 calc R . . C10 C -0.0834(9) 0.0549(9) 0.5995(6) 0.053(2) Uani 1 1 d . . . N2 N -0.0037(7) 0.1453(7) 0.5752(5) 0.0494(19) Uani 1 1 d . . . C11 C -0.0466(10) -0.0397(8) 0.6741(7) 0.057(3) Uani 1 1 d . . . C12 C -0.1121(13) -0.1400(12) 0.7032(9) 0.081(4) Uani 1 1 d . . . H12 H -0.1880 -0.1499 0.6799 0.098 Uiso 1 1 calc R . . C13 C -0.0629(17) -0.2284(11) 0.7690(9) 0.097(4) Uani 1 1 d . . . H13 H -0.1035 -0.2993 0.7882 0.116 Uiso 1 1 calc R . . C14 C 0.0478(15) -0.2091(10) 0.8057(8) 0.084(4) Uani 1 1 d . . . H14 H 0.0831 -0.2665 0.8492 0.100 Uiso 1 1 calc R . . C15 C 0.1027(11) -0.1020(9) 0.7750(7) 0.060(3) Uani 1 1 d . . . N3 N 0.0582(8) -0.0214(6) 0.7120(5) 0.0474(19) Uani 1 1 d . . . C16 C 0.2228(11) -0.0782(9) 0.8109(7) 0.068(3) Uani 1 1 d . . . H16A H 0.2171 -0.1213 0.8736 0.082 Uiso 1 1 calc R . . H16B H 0.3052 -0.1048 0.7760 0.082 Uiso 1 1 calc R . . N4 N 0.2313(9) 0.0470(8) 0.8065(5) 0.064(2) Uani 1 1 d . . . H4 H 0.3205 0.0608 0.8020 0.076 Uiso 1 1 calc R . . C17 C 0.1562(12) 0.0818(9) 0.8877(6) 0.069(3) Uani 1 1 d . . . H17A H 0.0618 0.0630 0.8960 0.083 Uiso 1 1 calc R . . H17B H 0.1589 0.1649 0.8779 0.083 Uiso 1 1 calc R . . C18 C 0.2132(19) 0.0229(11) 0.9765(8) 0.105(5) Uani 1 1 d . . . H18A H 0.1760 -0.0532 1.0022 0.126 Uiso 0.70 1 d P . . H18B H 0.3117 0.0116 0.9626 0.126 Uiso 0.70 1 d P . . H18C H 0.1353 0.0197 1.0087 0.126 Uiso 0.30 1 d P . . H18D H 0.2369 -0.0566 0.9735 0.126 Uiso 0.30 1 d P . . C19 C 0.1763(19) 0.0953(15) 1.0426(11) 0.079(5) Uani 0.70 1 d P . . H19A H 0.0841 0.1201 1.0460 0.095 Uiso 0.70 1 d P . . H19B H 0.1900 0.0466 1.1024 0.095 Uiso 0.70 1 d P . . C19' C 0.312(4) 0.056(3) 1.000(2) 0.059(9) Uani 0.30 1 d P . . H19C H 0.3880 0.0542 0.9587 0.070 Uiso 0.30 1 d P . . H19D H 0.3204 0.0032 1.0600 0.070 Uiso 0.30 1 d P . . N5 N 0.2683(15) 0.1924(10) 1.0181(7) 0.117(5) Uani 1 1 d . . . H5A H 0.2150 0.2514 1.0361 0.140 Uiso 0.70 1 d P . . H5B H 0.1921 0.1980 1.0594 0.140 Uiso 0.30 1 d P . . C20 C 0.3952(18) 0.1881(11) 1.0539(9) 0.113(5) Uani 1 1 d . . . H20A H 0.4664 0.1465 1.0207 0.136 Uiso 1 1 calc R . . H20B H 0.3815 0.1474 1.1174 0.136 Uiso 1 1 calc R . . C21 C 0.4378(12) 0.3100(11) 1.0442(8) 0.079(3) Uani 1 1 d . . . H21A H 0.3646 0.3518 1.0757 0.095 Uiso 1 1 calc R . . H21B H 0.5166 0.3062 1.0729 0.095 Uiso 1 1 calc R . . C22 C 0.4715(11) 0.3750(11) 0.9465(8) 0.075(3) Uani 1 1 d . . . H22A H 0.5115 0.4470 0.9436 0.090 Uiso 1 1 calc R . . H22B H 0.5383 0.3298 0.9134 0.090 Uiso 1 1 calc R . . N6 N 0.3480(8) 0.4004(7) 0.9023(5) 0.0540(19) Uani 1 1 d . . . H6 H 0.2872 0.4444 0.9325 0.065 Uiso 1 1 d . . . C23 C 0.3801(10) 0.4646(8) 0.8065(7) 0.060(3) Uani 1 1 d . . . H23A H 0.4442 0.4181 0.7729 0.072 Uiso 1 1 calc R . . H23B H 0.4238 0.5347 0.8037 0.072 Uiso 1 1 calc R . . C24 C 0.2541(10) 0.4968(8) 0.7601(7) 0.059(3) Uani 1 1 d . . . H24A H 0.1858 0.5356 0.7975 0.071 Uiso 1 1 calc R . . H24B H 0.2798 0.5509 0.7021 0.071 Uiso 1 1 calc R . . C25 C 0.1912(9) 0.3942(8) 0.7439(6) 0.050(2) Uani 1 1 d . . . H25A H 0.1566 0.3452 0.8028 0.060 Uiso 1 1 calc R . . H25B H 0.1136 0.4233 0.7144 0.060 Uiso 1 1 calc R . . N7 N 0.2778(7) 0.3215(6) 0.6898(5) 0.0463(18) Uani 1 1 d . . . H7 H 0.3466 0.2895 0.7202 0.056 Uiso 1 1 calc R . . C26 C 0.3410(11) 0.3860(9) 0.5964(7) 0.063(3) Uani 1 1 d . . . H26A H 0.4209 0.3425 0.5739 0.076 Uiso 1 1 calc R . . H26B H 0.3695 0.4600 0.5996 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.4759(3) 0.2508(2) 0.34778(17) 0.0664(8) Uani 1 1 d . . . O11 O 0.5105(11) 0.3253(9) 0.3978(7) 0.120(3) Uani 1 1 d . . . O12 O 0.4450(18) 0.1450(12) 0.3997(8) 0.194(7) Uani 1 1 d . . . O13 O 0.3832(15) 0.3058(12) 0.2936(12) 0.191(6) Uani 1 1 d . . . O14 O 0.5903(17) 0.2488(12) 0.2843(11) 0.206(8) Uani 1 1 d . . . Cl2 Cl -0.4037(2) 0.1546(2) 0.75013(17) 0.0633(7) Uani 1 1 d . . . O21 O -0.5139(8) 0.1860(7) 0.8124(5) 0.086(2) Uani 1 1 d . . . O22 O -0.4493(10) 0.0589(9) 0.7235(7) 0.115(3) Uani 1 1 d . . . O23 O -0.3730(11) 0.2463(9) 0.6767(7) 0.133(4) Uani 1 1 d . . . O24 O -0.2869(9) 0.1130(9) 0.7871(7) 0.120(4) Uani 1 1 d . . . Cl3 Cl 0.8746(3) 0.3964(3) -0.05781(18) 0.0715(8) Uani 1 1 d . . . O31A O 0.876(3) 0.484(2) -0.1295(17) 0.148(9) Uani 0.70 1 d P . . O31B O 0.891(10) 0.517(6) -0.082(4) 0.20(3) Uani 0.30 1 d P . . O32A O 0.842(3) 0.2923(17) -0.0740(13) 0.114(5) Uani 0.70 1 d P . . O32B O 0.827(4) 0.383(7) -0.133(4) 0.140(18) Uani 0.30 1 d P . . O33 O 0.7812(10) 0.4084(9) 0.0208(7) 0.115(3) Uani 1 1 d . . . O34A O 1.010(3) 0.374(3) -0.038(2) 0.115(11) Uani 0.70 1 d P . . O34B O 0.975(7) 0.326(7) -0.044(5) 0.16(4) Uani 0.30 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 Cd1 0.0475(5) 0.0417(6) 0.0427(5) -0.0097(3) -0.0095(3) 0.0067(3) O1 0.062(5) 0.086(6) 0.061(4) -0.009(4) 0.006(3) 0.027(4) O2 0.046(4) 0.083(5) 0.078(5) -0.039(4) -0.004(3) 0.008(3) C1 0.055(6) 0.053(7) 0.047(6) -0.015(5) 0.008(4) 0.015(5) C2 0.075(7) 0.052(8) 0.064(7) -0.003(6) -0.002(6) 0.015(5) C3 0.097(10) 0.059(10) 0.075(9) 0.010(6) 0.006(7) 0.029(7) C4 0.108(10) 0.066(10) 0.050(7) -0.010(6) -0.014(6) 0.041(8) C5 0.071(7) 0.049(7) 0.040(6) -0.007(5) -0.019(5) 0.033(5) N1 0.055(5) 0.036(5) 0.044(5) -0.005(3) -0.004(4) 0.011(4) C6 0.044(6) 0.070(8) 0.042(6) -0.026(5) -0.009(4) 0.018(5) C7 0.077(8) 0.105(11) 0.062(7) -0.035(7) -0.030(6) 0.033(7) C8 0.063(8) 0.118(12) 0.087(9) -0.049(9) -0.031(6) 0.010(7) C9 0.059(7) 0.088(10) 0.086(9) -0.051(8) -0.015(6) 0.000(6) C10 0.052(6) 0.060(7) 0.050(6) -0.030(5) 0.005(5) 0.004(5) N2 0.042(4) 0.060(6) 0.049(5) -0.022(4) -0.011(3) 0.015(4) C11 0.062(7) 0.043(7) 0.069(7) -0.032(5) 0.008(5) -0.011(5) C12 0.088(9) 0.083(10) 0.077(9) -0.039(7) 0.012(6) -0.026(7) C13 0.152(13) 0.052(10) 0.083(10) -0.021(7) 0.008(9) -0.032(8) C14 0.137(11) 0.043(9) 0.060(7) -0.006(6) -0.001(7) -0.001(7) C15 0.084(8) 0.034(7) 0.062(7) -0.015(5) -0.011(6) 0.012(5) N3 0.066(5) 0.027(5) 0.045(5) -0.007(4) -0.003(4) 0.003(4) C16 0.088(8) 0.052(8) 0.062(7) -0.015(5) -0.017(6) 0.025(5) N4 0.066(6) 0.065(7) 0.056(5) -0.002(4) -0.017(4) -0.006(4) C17 0.119(9) 0.043(7) 0.044(6) -0.004(5) -0.014(6) -0.006(6) C18 0.209(17) 0.058(9) 0.042(7) 0.000(6) -0.043(9) 0.037(9) C19 0.099(14) 0.074(13) 0.063(11) -0.010(8) -0.026(9) 0.004(10) C19' 0.09(3) 0.06(2) 0.041(19) -0.010(15) -0.045(19) -0.006(18) N5 0.195(13) 0.091(9) 0.075(7) 0.014(6) -0.064(8) -0.070(9) C20 0.205(17) 0.058(10) 0.095(10) -0.005(7) -0.088(11) -0.007(9) C21 0.085(8) 0.090(10) 0.073(8) -0.028(7) -0.029(6) -0.005(6) C22 0.071(7) 0.086(9) 0.078(8) -0.026(6) -0.030(6) -0.001(6) N6 0.060(5) 0.053(5) 0.047(5) -0.014(4) -0.008(4) 0.010(4) C23 0.079(7) 0.042(6) 0.069(7) -0.020(5) -0.023(5) -0.006(5) C24 0.076(7) 0.043(7) 0.063(6) -0.020(5) -0.015(5) 0.009(5) C25 0.051(6) 0.042(6) 0.053(6) -0.007(4) -0.011(4) 0.010(4) N7 0.042(4) 0.045(5) 0.052(5) -0.016(4) -0.008(3) 0.007(3) C26 0.070(7) 0.051(7) 0.069(7) -0.018(5) -0.003(5) -0.008(5) Cl1 0.0649(17) 0.070(2) 0.0585(16) -0.0132(14) -0.0041(13) 0.0040(13) O11 0.141(9) 0.114(8) 0.117(8) -0.050(6) -0.020(6) -0.013(6) O12 0.336(19) 0.146(11) 0.102(8) 0.033(8) -0.059(10) -0.149(12) O13 0.195(13) 0.147(12) 0.258(16) -0.013(11) -0.155(13) 0.004(9) O14 0.236(16) 0.134(11) 0.207(15) -0.084(10) 0.119(13) -0.016(10) Cl2 0.0478(15) 0.0687(19) 0.0702(17) -0.0137(13) -0.0107(12) 0.0064(11) O21 0.073(5) 0.103(7) 0.082(5) -0.039(5) 0.008(4) 0.004(4) O22 0.097(7) 0.122(8) 0.136(8) -0.063(7) 0.002(6) -0.012(5) O23 0.135(9) 0.102(8) 0.105(8) 0.042(6) 0.025(6) 0.003(6) O24 0.073(6) 0.116(8) 0.159(9) 0.013(6) -0.055(6) 0.004(5) Cl3 0.079(2) 0.070(2) 0.065(2) -0.0252(16) -0.0042(14) 0.0056(15) O31A 0.20(2) 0.11(2) 0.090(16) 0.041(13) 0.002(14) 0.021(16) O31B 0.37(10) 0.10(5) 0.12(5) -0.02(4) -0.03(5) -0.03(4) O32A 0.170(18) 0.077(13) 0.104(13) -0.051(9) -0.007(11) -0.004(11) O32B 0.13(3) 0.20(6) 0.13(4) -0.10(4) -0.06(3) 0.03(3) O33 0.113(7) 0.123(8) 0.112(7) -0.066(6) 0.015(6) 0.014(5) O34A 0.076(12) 0.17(3) 0.103(13) -0.049(17) -0.015(8) -0.004(14) O34B 0.16(7) 0.14(6) 0.11(4) 0.00(4) 0.02(5) 0.14(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 Cd1 N3 2.378(7) . ? Cd1 O1 2.382(6) . ? Cd1 N1 2.395(7) . ? Cd1 N2 2.419(7) . ? Cd1 N4 2.424(8) . ? Cd1 O2 2.422(6) . ? Cd1 N7 2.461(7) . ? C1 N1 1.313(12) . ? C1 C2 1.382(14) . ? C1 C26 1.515(14) . ? C2 C3 1.374(17) . ? C3 C4 1.360(18) . ? C4 C5 1.386(15) . ? C5 N1 1.337(12) . ? C5 C6 1.467(14) . ? C6 N2 1.339(12) . ? C6 C7 1.385(14) . ? C7 C8 1.365(18) . ? C8 C9 1.373(17) . ? C9 C10 1.401(14) . ? C10 N2 1.338(12) . ? C10 C11 1.477(14) . ? C11 N3 1.354(12) . ? C11 C12 1.356(15) . ? C12 C13 1.399(18) . ? C13 C14 1.400(18) . ? C14 C15 1.378(15) . ? C15 N3 1.304(12) . ? C15 C16 1.494(15) . ? C16 N4 1.492(13) . ? N4 C17 1.464(13) . ? C17 C18 1.565(15) . ? C18 C19' 1.25(3) . ? C18 C19 1.47(2) . ? C19 N5 1.48(2) . ? C19 C19' 1.48(4) . ? C19' N5 1.72(4) . ? N5 C20 1.472(18) . ? C20 C21 1.522(17) . ? C21 C22 1.504(16) . ? C22 N6 1.498(12) . ? N6 C23 1.476(12) . ? C23 C24 1.542(13) . ? C24 C25 1.522(12) . ? C25 N7 1.466(11) . ? N7 C26 1.504(12) . ? Cl1 O12 1.347(10) . ? Cl1 O14 1.360(12) . ? Cl1 O13 1.382(11) . ? Cl1 O11 1.417(10) . ? Cl2 O23 1.376(8) . ? Cl2 O24 1.398(8) . ? Cl2 O21 1.407(8) . ? Cl2 O22 1.445(9) . ? Cl3 O34B 1.27(4) . ? Cl3 O31A 1.323(18) . ? Cl3 O32B 1.39(3) . ? Cl3 O32A 1.405(14) . ? Cl3 O31B 1.42(7) . ? Cl3 O33 1.412(9) . ? Cl3 O34A 1.44(2) . ? O31A O31B 0.95(5) . ? O31A O32B 1.37(6) . ? O32A O32B 1.25(7) . ? O32A O34B 1.61(8) . ? O34A O34B 0.73(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 N3 Cd1 O1 92.6(3) . . ? N3 Cd1 N1 133.7(3) . . ? O1 Cd1 N1 88.0(2) . . ? N3 Cd1 N2 67.0(3) . . ? O1 Cd1 N2 99.9(2) . . ? N1 Cd1 N2 67.3(3) . . ? N3 Cd1 N4 70.2(3) . . ? O1 Cd1 N4 86.0(3) . . ? N1 Cd1 N4 155.7(3) . . ? N2 Cd1 N4 136.9(3) . . ? N3 Cd1 O2 87.8(2) . . ? O1 Cd1 O2 179.4(2) . . ? N1 Cd1 O2 92.0(2) . . ? N2 Cd1 O2 80.7(2) . . ? N4 Cd1 O2 93.8(3) . . ? N3 Cd1 N7 156.6(3) . . ? O1 Cd1 N7 90.1(3) . . ? N1 Cd1 N7 69.6(2) . . ? N2 Cd1 N7 135.3(3) . . ? N4 Cd1 N7 86.8(3) . . ? O2 Cd1 N7 89.3(2) . . ? N1 C1 C2 121.8(10) . . ? N1 C1 C26 118.1(9) . . ? C2 C1 C26 119.9(10) . . ? C3 C2 C1 116.7(11) . . ? C4 C3 C2 120.8(11) . . ? C3 C4 C5 120.3(11) . . ? N1 C5 C4 117.6(10) . . ? N1 C5 C6 117.6(8) . . ? C4 C5 C6 124.7(10) . . ? C1 N1 C5 122.7(8) . . ? C1 N1 Cd1 117.8(6) . . ? C5 N1 Cd1 119.5(6) . . ? N2 C6 C7 120.9(10) . . ? N2 C6 C5 115.5(7) . . ? C7 C6 C5 123.5(10) . . ? C8 C7 C6 118.8(12) . . ? C9 C8 C7 121.2(10) . . ? C8 C9 C10 117.3(11) . . ? N2 C10 C9 121.5(10) . . ? N2 C10 C11 115.3(8) . . ? C9 C10 C11 123.1(10) . . ? C6 N2 C10 120.2(8) . . ? C6 N2 Cd1 119.5(6) . . ? C10 N2 Cd1 119.6(6) . . ? N3 C11 C12 121.2(11) . . ? N3 C11 C10 116.2(8) . . ? C12 C11 C10 122.6(11) . . ? C11 C12 C13 118.6(12) . . ? C12 C13 C14 119.4(11) . . ? C15 C14 C13 117.5(11) . . ? N3 C15 C14 122.5(10) . . ? N3 C15 C16 118.0(9) . . ? C14 C15 C16 119.5(10) . . ? C15 N3 C11 120.7(8) . . ? C15 N3 Cd1 118.9(7) . . ? C11 N3 Cd1 120.3(6) . . ? N4 C16 C15 112.5(8) . . ? C17 N4 C16 113.2(8) . . ? C17 N4 Cd1 110.9(6) . . ? C16 N4 Cd1 109.9(6) . . ? N4 C17 C18 113.7(10) . . ? C19' C18 C19 65.4(19) . . ? C19' C18 C17 125(2) . . ? C19 C18 C17 109.6(11) . . ? C18 C19 N5 109.7(15) . . ? C18 C19 C19' 50.1(14) . . ? N5 C19 C19' 71.1(17) . . ? C18 C19' C19 64.5(19) . . ? C18 C19' N5 107(2) . . ? C19 C19' N5 54.4(15) . . ? C19 N5 C20 123.5(11) . . ? C19 N5 C19' 54.5(14) . . ? C20 N5 C19' 88.6(14) . . ? N5 C20 C21 109.9(10) . . ? C22 C21 C20 112.5(10) . . ? N6 C22 C21 111.7(9) . . ? C23 N6 C22 112.1(8) . . ? N6 C23 C24 113.5(8) . . ? C25 C24 C23 114.2(8) . . ? N7 C25 C24 118.0(7) . . ? C25 N7 C26 114.1(7) . . ? C25 N7 Cd1 112.6(5) . . ? C26 N7 Cd1 107.2(5) . . ? N7 C26 C1 110.5(8) . . ? O12 Cl1 O14 112.6(10) . . ? O12 Cl1 O13 116.3(9) . . ? O14 Cl1 O13 100.9(11) . . ? O12 Cl1 O11 112.8(7) . . ? O14 Cl1 O11 102.0(8) . . ? O13 Cl1 O11 110.5(9) . . ? O23 Cl2 O24 109.9(6) . . ? O23 Cl2 O21 110.0(6) . . ? O24 Cl2 O21 114.5(6) . . ? O23 Cl2 O22 111.4(7) . . ? O24 Cl2 O22 105.9(6) . . ? O21 Cl2 O22 105.0(5) . . ? O34B Cl3 O31A 124(4) . . ? O34B Cl3 O32B 110(4) . . ? O31A Cl3 O32B 61(3) . . ? O34B Cl3 O32A 74(4) . . ? O31A Cl3 O32A 113.1(16) . . ? O32B Cl3 O32A 53(3) . . ? O34B Cl3 O31B 121(5) . . ? O31A Cl3 O31B 40(2) . . ? O32B Cl3 O31B 100(4) . . ? O32A Cl3 O31B 153(3) . . ? O34B Cl3 O33 115(3) . . ? O31A Cl3 O33 115.8(12) . . ? O32B Cl3 O33 119.6(19) . . ? O32A Cl3 O33 104.2(8) . . ? O31B Cl3 O33 90(3) . . ? O34B Cl3 O34A 31(5) . . ? O31A Cl3 O34A 108.6(18) . . ? O32B Cl3 O34A 129(2) . . ? O32A Cl3 O34A 104.2(14) . . ? O31B Cl3 O34A 92(4) . . ? O33 Cl3 O34A 110.2(14) . . ? O31B O31A Cl3 75(5) . . ? O31B O31A O32B 135(6) . . ? Cl3 O31A O32B 62(2) . . ? O31A O31B Cl3 64(4) . . ? O32B O32A Cl3 63(2) . . ? O32B O32A O34B 98(3) . . ? Cl3 O32A O34B 49(2) . . ? O32A O32B Cl3 64(2) . . ? O32A O32B O31A 120(3) . . ? Cl3 O32B O31A 57.3(17) . . ? O34B O34A Cl3 62(5) . . ? O34A O34B Cl3 88(6) . . ? O34A O34B O32A 144(7) . . ? Cl3 O34B O32A 57(3) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 20.97 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 1.682 _refine_diff_density_min -1.461 _refine_diff_density_rms 0.152 #===END data_[PbHLBr](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 613193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C26 H36 N7 Br Pb +2, (Cl O4 -1)2 ; _chemical_formula_sum 'C26 H36 Br Cl2 N7 O8 Pb' _chemical_formula_weight 932.62 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' Cl Cl 0.1484 0.1585 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 13.005(3) _cell_length_b 14.517(4) _cell_length_c 17.229(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.84(2) _cell_angle_gamma 90.00 _cell_volume 3252(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 6.638 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur3-Oxford Diffraction' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12836 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.4211 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 27.34 _reflns_number_total 5803 _reflns_number_gt 1329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD - Oxford Diffraction' _computing_cell_refinement 'CrysAlis Red - Oxford Diffraction' _computing_data_reduction 'CrysAlis Red - Oxford Diffraction' _computing_structure_solution 'SIR97 (Altomare 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _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. Colourless single crystal of [PbHLBr](ClO4)2 was analyzed by means of X-ray crystallography. The intensities of some reflections were monitored during data collection to check the stability of the crystal: no loss of intensity was observed. The integrated intensities were corrected for Lorentz and polarization effects and empirical absorption correction was applied by means of SADABS program. The structure were solved by direct methods (SIR97). Refinement was performed by means of full-matrix least-squares using SHELX-97 program. All the non hydrogen atoms were anisotropically refined while the hydrogen atoms linked to carbon atoms were introduced in calculated position and their coordinates were refined according to the linked atoms. DF map carried out at the end of refined did not allow the localization of acidic proton. ; _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^)+(0.0325P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5803 _refine_ls_number_parameters 406 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2477 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 0.633 _refine_ls_restrained_S_all 0.633 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.63325(5) 0.15861(4) 0.64624(4) 0.0721(3) Uani 1 1 d . . . Br2 Br 0.84022(11) 0.17611(10) 0.61700(10) 0.0881(6) Uani 1 1 d . . . Cl1 Cl 1.0270(5) -0.1194(4) 0.7845(4) 0.0921(16) Uani 1 1 d . . . Cl2 Cl 0.4110(5) 0.0855(4) 0.8906(4) 0.1108(18) Uani 1 1 d . . . N1 N 0.6195(7) 0.2828(8) 0.5349(9) 0.055(4) Uani 1 1 d . . . N4 N 0.7211(9) 0.0564(8) 0.7619(7) 0.075(4) Uani 1 1 d . . . H4A H 0.7866 0.0433 0.7477 0.090 Uiso 1 1 calc R . . C12 C 0.6293(10) -0.1500(12) 0.5427(11) 0.073(5) Uani 1 1 d . . . H12 H 0.6149 -0.1746 0.4939 0.088 Uiso 1 1 calc R . . C11 C 0.6385(11) -0.0567(14) 0.5507(13) 0.067(6) Uani 1 1 d . . . N3 N 0.6502(9) -0.0194(8) 0.6234(11) 0.068(4) Uani 1 1 d . . . C14 C 0.6531(11) -0.1680(14) 0.6805(11) 0.076(5) Uani 1 1 d . . . H14 H 0.6600 -0.2037 0.7251 0.092 Uiso 1 1 calc R . . O11 O 1.1000(10) -0.1117(7) 0.7264(7) 0.138(5) Uani 1 1 d . . . O12 O 0.9835(9) -0.2066(8) 0.7829(6) 0.124(5) Uani 1 1 d . . . O13 O 0.9481(11) -0.0537(9) 0.7709(7) 0.153(6) Uani 1 1 d . . . C1 C 0.6189(10) 0.3740(13) 0.5551(10) 0.056(5) Uani 1 1 d . . . C2 C 0.6116(11) 0.4419(12) 0.5003(13) 0.081(6) Uani 1 1 d . . . H2 H 0.6137 0.5034 0.5153 0.097 Uiso 1 1 calc R . . O21 O 0.3163(10) 0.0451(8) 0.9128(9) 0.173(6) Uani 1 1 d . . . C13 C 0.6408(12) -0.2077(12) 0.6043(16) 0.097(7) Uani 1 1 d . . . H13 H 0.6408 -0.2713 0.5974 0.116 Uiso 1 1 calc R . . C6 C 0.6187(11) 0.1600(13) 0.4415(13) 0.067(5) Uani 1 1 d . . . N7 N 0.6703(10) 0.3354(8) 0.6924(10) 0.097(4) Uani 1 1 d . . . H7A H 0.7384 0.3447 0.6836 0.116 Uiso 1 1 calc R . . C4 C 0.6043(11) 0.3261(15) 0.4047(11) 0.088(6) Uani 1 1 d . . . H4 H 0.6000 0.3096 0.3526 0.105 Uiso 1 1 calc R . . C16 C 0.6644(11) -0.0317(11) 0.7662(11) 0.086(6) Uani 1 1 d . . . H16A H 0.5968 -0.0214 0.7877 0.103 Uiso 1 1 calc R . . H16B H 0.7012 -0.0746 0.7996 0.103 Uiso 1 1 calc R . . C26 C 0.6193(12) 0.3952(10) 0.6415(11) 0.092(6) Uani 1 1 d . . . H26A H 0.6491 0.4560 0.6486 0.110 Uiso 1 1 calc R . . H26B H 0.5483 0.3991 0.6577 0.110 Uiso 1 1 calc R . . C18 C 0.7660(10) 0.0567(11) 0.9089(10) 0.084(6) Uani 1 1 d . . . H18A H 0.7211 0.0045 0.9177 0.101 Uiso 1 1 calc R . . H18B H 0.8341 0.0328 0.8986 0.101 Uiso 1 1 calc R . . C17 C 0.7271(11) 0.1091(9) 0.8374(9) 0.080(5) Uani 1 1 d . . . H17A H 0.6590 0.1325 0.8484 0.095 Uiso 1 1 calc R . . H17B H 0.7716 0.1619 0.8299 0.095 Uiso 1 1 calc R . . N2 N 0.6283(9) 0.1009(11) 0.5030(9) 0.067(4) Uani 1 1 d . . . O14 O 1.0680(11) -0.0990(10) 0.8573(9) 0.178(6) Uani 1 1 d . . . O23 O 0.4193(14) 0.1679(10) 0.9272(10) 0.263(11) Uani 1 1 d . . . C3 C 0.6011(12) 0.4196(15) 0.4227(13) 0.094(6) Uani 1 1 d . . . H3 H 0.5923 0.4644 0.3847 0.113 Uiso 1 1 calc R . . N5 N 0.6681(10) 0.1405(9) 1.0056(9) 0.090(4) Uani 1 1 d . . . H5 H 0.6310 0.0862 1.0094 0.108 Uiso 1 1 d . . . C25 C 0.6582(15) 0.3514(10) 0.7726(11) 0.107(7) Uani 1 1 d . . . H25A H 0.6708 0.4165 0.7816 0.129 Uiso 1 1 calc R . . H25B H 0.7125 0.3180 0.7996 0.129 Uiso 1 1 calc R . . C5 C 0.6138(11) 0.2539(15) 0.4604(11) 0.063(5) Uani 1 1 d . . . C23 C 0.5527(13) 0.3493(11) 0.8942(13) 0.099(6) Uani 1 1 d . . . H23A H 0.4856 0.3302 0.9120 0.118 Uiso 1 1 calc R . . H23B H 0.5571 0.4156 0.9006 0.118 Uiso 1 1 calc R . . C24 C 0.5596(14) 0.3278(10) 0.8108(14) 0.111(7) Uani 1 1 d . . . H24A H 0.5045 0.3600 0.7837 0.134 Uiso 1 1 calc R . . H24B H 0.5476 0.2624 0.8041 0.134 Uiso 1 1 calc R . . C7 C 0.6249(11) 0.1300(13) 0.3661(12) 0.075(5) Uani 1 1 d . . . H7 H 0.6280 0.1715 0.3250 0.090 Uiso 1 1 calc R . . O22 O 0.4929(10) 0.0281(11) 0.9148(8) 0.181(7) Uani 1 1 d . . . C15 C 0.6539(12) -0.0722(14) 0.6823(12) 0.073(6) Uani 1 1 d . . . O24 O 0.4193(12) 0.0991(11) 0.8095(10) 0.204(8) Uani 1 1 d . . . C19 C 0.7709(13) 0.1136(11) 0.9802(9) 0.095(6) Uani 1 1 d . . . H19A H 0.8111 0.1685 0.9703 0.114 Uiso 1 1 calc R . . H19B H 0.8051 0.0791 1.0212 0.114 Uiso 1 1 calc R . . N6 N 0.6308(10) 0.3067(8) 0.9438(10) 0.088(5) Uani 1 1 d . . . H6A H 0.6936 0.3298 0.9301 0.106 Uiso 1 1 d . . . C10 C 0.6278(11) 0.0124(15) 0.4873(11) 0.069(5) Uani 1 1 d . . . C22 C 0.6087(11) 0.3376(9) 1.0329(12) 0.084(6) Uani 1 1 d . . . H22A H 0.6142 0.4038 1.0397 0.101 Uiso 1 1 calc R . . H22B H 0.5419 0.3168 1.0501 0.101 Uiso 1 1 calc R . . C21 C 0.6951(13) 0.2872(15) 1.0734(10) 0.120(7) Uani 1 1 d . . . H21A H 0.7091 0.3153 1.1235 0.144 Uiso 1 1 calc R . . H21B H 0.7569 0.2913 1.0428 0.144 Uiso 1 1 calc R . . C8 C 0.6266(12) 0.0360(16) 0.3535(11) 0.095(6) Uani 1 1 d . . . H8 H 0.6224 0.0140 0.3029 0.114 Uiso 1 1 calc R . . C20 C 0.6649(13) 0.1837(13) 1.0846(11) 0.123(7) Uani 1 1 d . . . H20A H 0.7132 0.1535 1.1197 0.148 Uiso 1 1 calc R . . H20B H 0.5965 0.1788 1.1059 0.148 Uiso 1 1 calc R . . C9 C 0.6334(12) -0.0198(12) 0.4076(13) 0.076(6) Uani 1 1 d U . . H9 H 0.6421 -0.0821 0.3973 0.091 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 0.0822(5) 0.0618(4) 0.0723(5) -0.0010(5) 0.0006(3) 0.0027(5) Br2 0.0770(12) 0.0854(13) 0.1017(15) 0.0133(11) -0.0059(11) 0.0143(10) Cl1 0.123(5) 0.072(4) 0.081(5) -0.007(3) 0.011(4) -0.010(4) Cl2 0.097(5) 0.104(5) 0.131(6) -0.003(4) 0.001(5) -0.015(4) N1 0.030(7) 0.032(8) 0.102(13) -0.020(8) -0.008(8) 0.001(6) N4 0.099(10) 0.071(9) 0.057(10) -0.002(8) 0.023(8) -0.003(8) C12 0.073(11) 0.020(10) 0.126(18) -0.019(12) -0.019(11) -0.002(10) C11 0.039(10) 0.092(18) 0.070(17) -0.027(15) 0.016(11) 0.005(11) N3 0.082(10) 0.051(9) 0.072(13) 0.024(10) 0.019(10) 0.018(8) C14 0.084(12) 0.060(14) 0.085(16) 0.043(12) -0.016(11) 0.014(11) O11 0.192(13) 0.099(9) 0.124(11) -0.005(8) 0.080(11) -0.019(8) O12 0.186(13) 0.084(8) 0.103(11) -0.009(8) 0.039(9) -0.039(8) O13 0.200(14) 0.143(12) 0.115(12) -0.033(9) -0.031(10) 0.065(11) C1 0.028(9) 0.100(16) 0.039(13) -0.027(12) -0.011(8) 0.010(10) C2 0.072(12) 0.082(14) 0.087(17) 0.047(14) -0.014(13) 0.035(10) O21 0.113(11) 0.145(12) 0.260(18) 0.067(11) -0.023(11) -0.032(9) C13 0.045(11) 0.062(15) 0.18(3) 0.012(17) 0.016(15) 0.013(10) C6 0.069(11) 0.035(12) 0.097(18) -0.006(15) -0.014(12) 0.021(11) N7 0.130(13) 0.072(10) 0.088(13) 0.039(10) 0.012(11) -0.018(9) C4 0.072(12) 0.092(16) 0.099(17) 0.008(16) -0.006(11) 0.003(12) C16 0.068(12) 0.071(13) 0.119(19) 0.056(13) 0.018(12) 0.005(10) C26 0.124(15) 0.061(11) 0.092(17) 0.028(13) 0.015(13) 0.043(11) C18 0.063(12) 0.130(16) 0.060(14) 0.038(13) 0.004(11) 0.013(11) C17 0.119(14) 0.070(11) 0.050(13) -0.027(10) 0.031(11) 0.014(10) N2 0.060(9) 0.046(10) 0.095(13) -0.033(10) -0.021(8) 0.001(8) O14 0.189(14) 0.234(16) 0.110(13) -0.042(12) -0.023(11) -0.054(11) O23 0.39(3) 0.126(12) 0.28(2) -0.154(13) 0.148(18) -0.080(14) C3 0.062(12) 0.13(2) 0.094(19) 0.010(16) -0.010(13) 0.006(13) N5 0.090(11) 0.093(11) 0.087(12) -0.015(9) 0.004(10) -0.036(9) C25 0.18(2) 0.092(14) 0.054(15) 0.057(12) 0.040(14) 0.011(14) C5 0.048(11) 0.097(18) 0.044(14) -0.004(14) 0.014(11) 0.005(11) C23 0.079(14) 0.093(14) 0.12(2) -0.018(15) 0.013(14) 0.016(12) C24 0.138(19) 0.065(13) 0.13(2) 0.014(14) 0.024(17) 0.013(12) C7 0.081(12) 0.062(15) 0.082(16) 0.022(12) 0.004(11) -0.008(10) O22 0.101(11) 0.305(19) 0.137(14) 0.042(13) -0.002(10) 0.039(12) C15 0.091(13) 0.070(15) 0.058(16) 0.017(13) 0.033(12) 0.031(11) O24 0.214(17) 0.28(2) 0.113(14) 0.025(13) 0.005(13) -0.004(13) C19 0.108(17) 0.146(17) 0.031(13) -0.015(11) -0.010(12) -0.002(13) N6 0.092(11) 0.060(10) 0.111(14) -0.033(9) -0.021(10) 0.006(8) C10 0.061(12) 0.084(15) 0.060(15) 0.000(14) -0.022(10) -0.018(11) C22 0.052(11) 0.023(8) 0.18(2) -0.047(12) -0.020(12) 0.009(9) C21 0.092(16) 0.16(2) 0.109(17) -0.075(15) -0.006(13) -0.042(15) C8 0.103(14) 0.101(16) 0.081(17) -0.049(14) -0.028(12) -0.023(14) C20 0.133(17) 0.126(18) 0.111(19) -0.037(15) 0.051(14) -0.052(14) C9 0.066(9) 0.071(9) 0.090(10) -0.018(8) -0.018(8) 0.020(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 N2 2.606(13) . ? Pb1 N3 2.624(12) . ? Pb1 N1 2.637(13) . ? Pb1 N7 2.728(12) . ? Pb1 N4 2.722(11) . ? Pb1 Br2 2.7572(17) . ? Cl1 O14 1.387(13) . ? Cl1 O12 1.386(10) . ? Cl1 O11 1.395(10) . ? Cl1 O13 1.418(12) . ? Cl2 O23 1.356(11) . ? Cl2 O24 1.416(14) . ? Cl2 O21 1.422(12) . ? Cl2 O22 1.411(13) . ? N1 C5 1.351(16) . ? N1 C1 1.369(16) . ? N4 C16 1.479(14) . ? N4 C17 1.510(14) . ? C12 C11 1.367(18) . ? C12 C13 1.36(2) . ? C11 N3 1.371(17) . ? C11 C10 1.49(2) . ? N3 C15 1.272(16) . ? C14 C15 1.392(18) . ? C14 C13 1.440(19) . ? C1 C2 1.367(17) . ? C1 C26 1.521(18) . ? C2 C3 1.380(19) . ? C6 C7 1.375(19) . ? C6 N2 1.368(17) . ? C6 C5 1.40(2) . ? N7 C26 1.394(15) . ? N7 C25 1.413(16) . ? C4 C3 1.394(19) . ? C4 C5 1.425(19) . ? C16 C15 1.566(19) . ? C18 C19 1.481(17) . ? C18 C17 1.528(16) . ? N2 C10 1.313(17) . ? N5 C19 1.466(16) . ? N5 C20 1.501(17) . ? C25 C24 1.490(18) . ? C23 C24 1.47(2) . ? C23 N6 1.456(17) . ? C7 C8 1.383(18) . ? N6 C22 1.629(18) . ? C10 C9 1.454(19) . ? C22 C21 1.503(18) . ? C21 C20 1.565(17) . ? C8 C9 1.236(19) . ? 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 N2 Pb1 N3 62.8(5) . . ? N2 Pb1 N1 62.0(5) . . ? N3 Pb1 N1 124.7(5) . . ? N2 Pb1 N7 125.5(5) . . ? N3 Pb1 N7 162.9(5) . . ? N1 Pb1 N7 65.1(5) . . ? N2 Pb1 N4 121.5(4) . . ? N3 Pb1 N4 62.5(5) . . ? N1 Pb1 N4 158.2(3) . . ? N7 Pb1 N4 103.2(4) . . ? N2 Pb1 Br2 82.4(3) . . ? N3 Pb1 Br2 88.8(3) . . ? N1 Pb1 Br2 82.0(2) . . ? N7 Pb1 Br2 78.3(3) . . ? N4 Pb1 Br2 77.5(2) . . ? O14 Cl1 O12 111.4(9) . . ? O14 Cl1 O11 112.0(9) . . ? O12 Cl1 O11 109.9(7) . . ? O14 Cl1 O13 105.9(9) . . ? O12 Cl1 O13 108.5(9) . . ? O11 Cl1 O13 109.0(8) . . ? O23 Cl2 O24 109.2(11) . . ? O23 Cl2 O21 107.6(10) . . ? O24 Cl2 O21 113.6(10) . . ? O23 Cl2 O22 109.2(12) . . ? O24 Cl2 O22 107.8(10) . . ? O21 Cl2 O22 109.3(9) . . ? C5 N1 C1 122.8(16) . . ? C5 N1 Pb1 118.7(12) . . ? C1 N1 Pb1 118.5(12) . . ? C16 N4 C17 114.5(12) . . ? C16 N4 Pb1 107.7(9) . . ? C17 N4 Pb1 111.8(9) . . ? C11 C12 C13 121.6(19) . . ? C12 C11 N3 119.5(18) . . ? C12 C11 C10 126(2) . . ? N3 C11 C10 114.3(17) . . ? C15 N3 C11 119.5(17) . . ? C15 N3 Pb1 118.4(13) . . ? C11 N3 Pb1 121.2(12) . . ? C15 C14 C13 114.9(17) . . ? C2 C1 N1 121.5(16) . . ? C2 C1 C26 122.0(18) . . ? N1 C1 C26 116.4(16) . . ? C3 C2 C1 120.3(19) . . ? C12 C13 C14 118.3(18) . . ? C7 C6 N2 121.9(16) . . ? C7 C6 C5 122.0(19) . . ? N2 C6 C5 116(2) . . ? C26 N7 C25 116.9(15) . . ? C26 N7 Pb1 108.8(11) . . ? C25 N7 Pb1 114.7(10) . . ? C3 C4 C5 124.6(19) . . ? N4 C16 C15 108.4(13) . . ? N7 C26 C1 118.9(15) . . ? C19 C18 C17 113.6(13) . . ? N4 C17 C18 117.0(12) . . ? C10 N2 C6 117.0(17) . . ? C10 N2 Pb1 120.6(13) . . ? C6 N2 Pb1 122.2(12) . . ? C2 C3 C4 116(2) . . ? C19 N5 C20 114.8(13) . . ? N7 C25 C24 120.2(17) . . ? N1 C5 C4 114.5(17) . . ? N1 C5 C6 121.3(19) . . ? C4 C5 C6 124.2(19) . . ? C24 C23 N6 115.5(15) . . ? C23 C24 C25 116.6(16) . . ? C8 C7 C6 117.5(17) . . ? N3 C15 C14 125.8(17) . . ? N3 C15 C16 120.8(18) . . ? C14 C15 C16 113.4(18) . . ? C18 C19 N5 111.6(14) . . ? C23 N6 C22 107.8(14) . . ? N2 C10 C9 120.6(17) . . ? N2 C10 C11 120.6(18) . . ? C9 C10 C11 118.1(19) . . ? C21 C22 N6 99.3(12) . . ? C22 C21 C20 109.7(14) . . ? C9 C8 C7 122.0(19) . . ? N5 C20 C21 106.2(13) . . ? C8 C9 C10 119.9(19) . . ? _diffrn_measured_fraction_theta_max 0.788 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.788 _refine_diff_density_max 1.266 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.116 #===END