# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2144 data_banoam _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H38 Ba Cl2 N6 O10' _chemical_formula_weight 682.76 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' 'Ba' 'Ba' -0.3244 2.2819 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4020(10) _cell_length_b 14.365(2) _cell_length_c 19.363(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.504(2) _cell_angle_gamma 90.00 _cell_volume 2598.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3233 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 23.255 _exptl_crystal_description 'Irregular plate' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.794 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 26513 _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.95 _reflns_number_total 6259 _reflns_number_gt 3553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0149P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Placed geometrically' _refine_ls_hydrogen_treatment 'Riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6259 _refine_ls_number_parameters 322 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.816 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba Ba 0.09750(2) 0.756146(18) 0.083242(12) 0.02075(7) Uani 1 1 d . A . N1 N 0.3362(4) 0.8894(2) 0.09832(17) 0.0236(8) Uani 1 1 d . . . C2 C 0.4382(4) 0.8582(3) 0.1574(2) 0.0299(10) Uani 1 1 d . . . H2A H 0.5107 0.9076 0.1686 0.036 Uiso 1 1 calc R . . H2B H 0.4888 0.8021 0.1432 0.036 Uiso 1 1 calc R . . C3 C 0.3693(5) 0.8357(3) 0.2223(2) 0.0301(12) Uani 1 1 d . . . H3A H 0.4453 0.8292 0.2618 0.036 Uiso 1 1 calc R . . H3B H 0.3074 0.8884 0.2327 0.036 Uiso 1 1 calc R . . N4 N 0.2824(3) 0.7495(2) 0.21679(14) 0.0232(7) Uani 1 1 d . . . C5 C 0.3795(5) 0.6687(3) 0.2232(2) 0.0278(11) Uani 1 1 d . . . H5A H 0.4148 0.6595 0.2729 0.033 Uiso 1 1 calc R . . H5B H 0.4633 0.6824 0.1982 0.033 Uiso 1 1 calc R . . C6 C 0.3102(5) 0.5796(3) 0.1948(2) 0.0305(11) Uani 1 1 d . . . H6A H 0.3793 0.5279 0.2046 0.037 Uiso 1 1 calc R . . H6B H 0.2265 0.5662 0.2199 0.037 Uiso 1 1 calc R . . N7 N 0.2625(3) 0.5810(2) 0.11914(18) 0.0236(8) Uani 1 1 d . . . C8 C 0.3877(4) 0.5794(3) 0.0800(2) 0.0327(11) Uani 1 1 d . . . H8A H 0.4402 0.5203 0.0902 0.039 Uiso 1 1 calc R . . H8B H 0.4526 0.6310 0.0966 0.039 Uiso 1 1 calc R . . C9 C 0.3522(5) 0.5882(3) 0.0033(2) 0.0315(11) Uani 1 1 d . . . H9A H 0.4413 0.5956 -0.0189 0.038 Uiso 1 1 calc R . . H9B H 0.3032 0.5310 -0.0154 0.038 Uiso 1 1 calc R . . O10 O 0.2616(3) 0.66680(19) -0.01234(14) 0.0294(7) Uani 1 1 d . . . C11 C 0.2776(5) 0.7046(3) -0.0790(2) 0.0374(12) Uani 1 1 d . . . H11A H 0.2586 0.6559 -0.1150 0.045 Uiso 1 1 calc R . . H11B H 0.3767 0.7274 -0.0800 0.045 Uiso 1 1 calc R . . C12 C 0.1735(5) 0.7836(3) -0.0934(2) 0.0365(12) Uani 1 1 d . . . H12A H 0.1919 0.8148 -0.1370 0.044 Uiso 1 1 calc R . . H12B H 0.0750 0.7583 -0.1000 0.044 Uiso 1 1 calc R . . O13 O 0.1837(3) 0.85078(19) -0.03828(15) 0.0328(8) Uani 1 1 d . . . C14 C 0.3144(5) 0.9030(3) -0.0311(2) 0.0324(11) Uani 1 1 d . . . H14A H 0.2917 0.9703 -0.0313 0.039 Uiso 1 1 calc R . . H14B H 0.3673 0.8901 -0.0715 0.039 Uiso 1 1 calc R . . C15 C 0.4085(4) 0.8794(3) 0.0348(2) 0.0288(11) Uani 1 1 d . . . H15A H 0.4422 0.8144 0.0317 0.035 Uiso 1 1 calc R . . H15B H 0.4936 0.9204 0.0387 0.035 Uiso 1 1 calc R . . C1A C 0.2949(5) 0.9870(3) 0.1096(2) 0.0342(11) Uani 1 1 d . . . H1A1 H 0.3600 1.0286 0.0872 0.041 Uiso 1 1 calc R . . H1A2 H 0.3080 1.0002 0.1601 0.041 Uiso 1 1 calc R . . C2A C 0.1401(5) 1.0096(3) 0.0811(3) 0.0411(13) Uani 1 1 d . . . H2A1 H 0.1189 1.0752 0.0918 0.049 Uiso 1 1 calc R . . H2A2 H 0.1284 1.0023 0.0299 0.049 Uiso 1 1 calc R . . N3A N 0.0407(4) 0.9495(2) 0.11080(19) 0.0377(10) Uani 1 1 d . . . H3A1 H -0.0511 0.9640 0.0924 0.045 Uiso 1 1 calc R . . H3A2 H 0.0477 0.9590 0.1580 0.045 Uiso 1 1 calc R . . C1B C 0.1931(4) 0.7459(3) 0.27550(19) 0.0336(10) Uani 1 1 d . . . H1B1 H 0.2522 0.7667 0.3183 0.040 Uiso 1 1 calc R . . H1B2 H 0.1655 0.6804 0.2826 0.040 Uiso 1 1 calc R . . C2B C 0.0594(5) 0.8043(3) 0.2658(2) 0.0341(11) Uani 1 1 d . . . H2B1 H 0.0131 0.8037 0.3092 0.041 Uiso 1 1 calc R . . H2B2 H 0.0853 0.8694 0.2561 0.041 Uiso 1 1 calc R . . N3B N -0.0413(3) 0.7697(2) 0.20858(16) 0.0339(9) Uani 1 1 d . . . H3B1 H -0.1183 0.8094 0.2013 0.041 Uiso 1 1 calc R . . H3B2 H -0.0746 0.7121 0.2198 0.041 Uiso 1 1 calc R . . C1C C 0.1746(5) 0.4975(3) 0.1016(2) 0.0368(13) Uani 1 1 d . . . H1C1 H 0.2247 0.4428 0.1239 0.044 Uiso 1 1 calc R . . H1C2 H 0.1667 0.4880 0.0507 0.044 Uiso 1 1 calc R . . C2C C 0.0260(4) 0.5018(3) 0.1235(2) 0.0329(12) Uani 1 1 d . . . H2C1 H -0.0262 0.4439 0.1089 0.039 Uiso 1 1 calc R . . H2C2 H 0.0326 0.5058 0.1748 0.039 Uiso 1 1 calc R . . N3C N -0.0530(4) 0.5812(2) 0.09329(18) 0.0301(9) Uani 1 1 d . . . H3C1 H -0.1283 0.5918 0.1188 0.036 Uiso 1 1 calc R . . H3C2 H -0.0916 0.5648 0.0492 0.036 Uiso 1 1 calc R . . Cl1 Cl -0.25558(9) 0.75071(8) -0.00619(5) 0.0262(2) Uani 1 1 d D . . O1 O -0.1282(3) 0.71736(18) -0.03390(14) 0.0321(7) Uani 1 1 d D A . O2 O -0.2102(3) 0.8148(2) 0.04843(16) 0.0525(10) Uani 1 1 d D A . O3 O -0.3487(3) 0.79537(19) -0.05884(15) 0.0375(8) Uani 1 1 d D A . O4 O -0.3253(15) 0.6714(7) 0.0215(8) 0.022(5) Uiso 0.33 1 d PD A 1 O4' O -0.3307(12) 0.6879(7) 0.0349(6) 0.030(4) Uiso 0.33 1 d PD A 2 O4" O -0.3262(14) 0.6629(6) 0.0061(7) 0.038(5) Uiso 0.33 1 d PD A 3 Cl2 Cl 0.75135(13) 0.52639(8) 0.24810(7) 0.0363(3) Uani 1 1 d D . . O5 O 0.8840(3) 0.5656(2) 0.27764(17) 0.0495(9) Uani 1 1 d D B . O6 O 0.7725(4) 0.4328(2) 0.2299(2) 0.0713(12) Uani 1 1 d D B . O7 O 0.6475(4) 0.5311(2) 0.29568(18) 0.0686(12) Uani 1 1 d D B . O8 O 0.7005(11) 0.5796(8) 0.1864(4) 0.018(3) Uiso 0.33 1 d PD B 1 O8' O 0.7092(13) 0.6028(7) 0.2004(5) 0.049(5) Uiso 0.33 1 d PD B 2 O8" O 0.6934(13) 0.5474(8) 0.1769(4) 0.061(5) Uiso 0.33 1 d PD B 3 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 Ba 0.01919(11) 0.02285(12) 0.02056(11) -0.00103(15) 0.00383(8) -0.00278(14) N1 0.025(2) 0.0208(19) 0.025(2) 0.0034(16) 0.0006(17) -0.0012(16) C2 0.025(2) 0.028(2) 0.035(3) -0.002(2) -0.003(2) -0.006(2) C3 0.038(3) 0.025(2) 0.026(3) -0.007(2) -0.003(2) -0.004(2) N4 0.0308(17) 0.0207(16) 0.0185(15) -0.0009(19) 0.0046(14) -0.001(2) C5 0.033(3) 0.023(2) 0.026(3) -0.003(2) -0.005(2) 0.007(2) C6 0.039(3) 0.023(2) 0.028(3) 0.004(2) 0.001(2) 0.007(2) N7 0.021(2) 0.0193(18) 0.031(2) -0.0055(16) 0.0071(17) -0.0019(15) C8 0.024(3) 0.030(3) 0.044(3) -0.009(2) 0.005(2) 0.001(2) C9 0.027(3) 0.038(3) 0.032(3) -0.016(2) 0.015(2) -0.005(2) O10 0.0289(18) 0.0383(18) 0.0228(17) -0.0017(14) 0.0111(14) 0.0017(14) C11 0.040(3) 0.048(3) 0.027(3) -0.013(2) 0.016(2) -0.016(2) C12 0.035(3) 0.055(3) 0.019(2) 0.001(2) 0.000(2) -0.022(2) O13 0.0289(18) 0.0410(19) 0.0295(19) -0.0009(15) 0.0079(15) -0.0103(15) C14 0.035(3) 0.038(3) 0.025(3) 0.007(2) 0.008(2) -0.007(2) C15 0.026(3) 0.028(2) 0.034(3) 0.002(2) 0.009(2) -0.007(2) C1A 0.045(3) 0.019(2) 0.038(3) -0.001(2) 0.000(2) -0.004(2) C2A 0.044(3) 0.030(3) 0.051(3) 0.011(2) 0.014(3) 0.008(2) N3A 0.036(2) 0.032(2) 0.047(3) 0.0044(19) 0.015(2) 0.0061(19) C1B 0.043(2) 0.032(2) 0.025(2) 0.000(3) 0.0030(19) 0.004(3) C2B 0.044(3) 0.036(3) 0.024(3) -0.007(2) 0.013(2) 0.000(2) N3B 0.033(2) 0.034(2) 0.037(2) 0.0005(18) 0.0104(17) 0.0029(18) C1C 0.037(3) 0.022(2) 0.053(3) -0.008(2) 0.010(3) -0.003(2) C2C 0.031(3) 0.023(2) 0.045(3) 0.001(2) 0.005(2) -0.006(2) N3C 0.028(2) 0.028(2) 0.033(2) 0.0002(17) 0.0008(18) -0.0066(17) Cl1 0.0202(4) 0.0299(5) 0.0286(5) 0.0019(6) 0.0028(4) -0.0024(6) O1 0.0226(15) 0.0396(18) 0.0352(18) -0.0024(14) 0.0084(14) 0.0028(13) O2 0.044(2) 0.067(2) 0.044(2) -0.0342(18) -0.0055(18) 0.0079(18) O3 0.0310(18) 0.0445(19) 0.0356(19) 0.0103(15) -0.0019(15) 0.0074(15) Cl2 0.0301(6) 0.0459(8) 0.0337(6) 0.0037(7) 0.0073(5) 0.0029(6) O5 0.047(2) 0.041(2) 0.060(2) 0.0019(18) 0.0018(19) -0.0085(17) O6 0.065(3) 0.058(2) 0.088(3) -0.035(2) -0.004(2) -0.006(2) O7 0.064(3) 0.084(3) 0.065(3) 0.000(2) 0.040(2) -0.007(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 Ba O10 2.846(3) . y Ba N3A 2.889(3) . y Ba N3B 2.889(3) . y Ba N3C 2.902(3) . y Ba O13 2.911(3) . y Ba N1 2.939(3) . y Ba N4 2.949(3) . y Ba O1 2.978(3) . y Ba N7 2.996(3) . y Ba O2 3.015(3) . y Ba Cl1 3.5669(10) . y N1 C1A 1.478(5) . ? N1 C2 1.477(5) . ? N1 C15 1.478(5) . ? C2 C3 1.513(5) . ? C3 N4 1.480(5) . ? N4 C5 1.473(5) . ? N4 C1B 1.488(4) . ? C5 C6 1.512(5) . ? C6 N7 1.483(5) . ? N7 C8 1.471(5) . ? N7 C1C 1.473(5) . ? C8 C9 1.490(6) . ? C9 O10 1.426(5) . ? O10 C11 1.423(5) . ? C11 C12 1.504(6) . ? C12 O13 1.434(5) . ? O13 C14 1.433(5) . ? C14 C15 1.507(6) . ? C1A C2A 1.532(6) . ? C2A N3A 1.440(5) . ? C1B C2B 1.505(5) . ? C2B N3B 1.460(5) . ? C1C C2C 1.507(5) . ? C2C N3C 1.449(5) . ? Cl1 O3 1.420(3) . ? Cl1 O2 1.430(3) . ? Cl1 O4' 1.439(6) . ? Cl1 O1 1.448(3) . ? Cl1 O4 1.448(6) . ? Cl1 O4" 1.457(6) . ? Cl2 O6 1.410(3) . ? Cl2 O7 1.418(3) . ? Cl2 O5 1.428(3) . ? Cl2 O8 1.452(5) . ? Cl2 O8" 1.456(7) . ? Cl2 O8' 1.460(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Ba N3A 132.74(9) . . y O10 Ba N3B 155.00(9) . . y N3A Ba N3B 70.71(10) . . y O10 Ba N3C 87.57(9) . . y N3A Ba N3C 135.92(10) . . y N3B Ba N3C 74.45(10) . . y O10 Ba O13 57.58(8) . . y N3A Ba O13 76.97(9) . . y N3B Ba O13 147.26(9) . . y N3C Ba O13 129.89(9) . . y O10 Ba N1 83.92(8) . . y N3A Ba N1 60.71(9) . . y N3B Ba N1 106.57(9) . . y N3C Ba N1 158.46(9) . . y O13 Ba N1 59.79(9) . . y O10 Ba N4 104.28(8) . . y N3A Ba N4 88.39(10) . . y N3B Ba N4 62.81(8) . . y N3C Ba N4 99.02(9) . . y O13 Ba N4 122.24(8) . . y N1 Ba N4 64.29(9) . . y O10 Ba O1 79.19(8) . . y N3A Ba O1 100.94(9) . . y N3B Ba O1 107.56(8) . . y N3C Ba O1 65.05(9) . . y O13 Ba O1 73.22(8) . . y N1 Ba O1 131.90(8) . . y N4 Ba O1 163.76(8) . . y O10 Ba N7 57.83(8) . . y N3A Ba N7 150.01(10) . . y N3B Ba N7 97.64(9) . . y N3C Ba N7 60.04(9) . . y O13 Ba N7 113.30(8) . . y N1 Ba N7 98.88(9) . . y N4 Ba N7 62.06(9) . . y O1 Ba N7 108.97(8) . . y O10 Ba O2 123.90(8) . . y N3A Ba O2 65.16(9) . . y N3B Ba O2 69.87(9) . . y N3C Ba O2 78.12(9) . . y O13 Ba O2 92.10(9) . . y N1 Ba O2 122.88(9) . . y N4 Ba O2 131.31(8) . . y O1 Ba O2 45.50(7) . . y N7 Ba O2 138.15(9) . . y O10 Ba Cl1 102.58(6) . . ? N3A Ba Cl1 85.95(8) . . ? N3B Ba Cl1 85.71(7) . . ? N3C Ba Cl1 65.13(7) . . ? O13 Ba Cl1 86.95(6) . . ? N1 Ba Cl1 136.12(7) . . ? N4 Ba Cl1 148.05(5) . . ? O1 Ba Cl1 23.42(5) . . ? N7 Ba Cl1 121.54(7) . . ? O2 Ba Cl1 23.21(5) . . ? C1A N1 C2 109.4(3) . . ? C1A N1 C15 111.6(3) . . ? C2 N1 C15 107.2(3) . . ? C1A N1 Ba 115.0(2) . . ? C2 N1 Ba 107.5(2) . . ? C15 N1 Ba 105.8(2) . . ? N1 C2 C3 114.0(3) . . ? N4 C3 C2 113.8(3) . . ? C5 N4 C3 108.7(3) . . ? C5 N4 C1B 107.8(3) . . ? C3 N4 C1B 109.2(3) . . ? C5 N4 Ba 113.4(2) . . ? C3 N4 Ba 107.6(2) . . ? C1B N4 Ba 110.1(2) . . ? N4 C5 C6 113.5(3) . . ? N7 C6 C5 114.7(3) . . ? C8 N7 C1C 109.2(3) . . ? C8 N7 C6 109.7(3) . . ? C1C N7 C6 108.4(3) . . ? C8 N7 Ba 108.5(2) . . ? C1C N7 Ba 111.6(2) . . ? C6 N7 Ba 109.4(2) . . ? N7 C8 C9 114.2(4) . . ? O10 C9 C8 109.9(3) . . ? C11 O10 C9 111.9(3) . . ? C11 O10 Ba 122.6(2) . . ? C9 O10 Ba 125.0(2) . . ? O10 C11 C12 108.8(3) . . ? O13 C12 C11 112.5(4) . . ? C12 O13 C14 114.1(3) . . ? C12 O13 Ba 106.6(2) . . ? C14 O13 Ba 118.7(2) . . ? O13 C14 C15 112.2(3) . . ? N1 C15 C14 113.7(3) . . ? N1 C1A C2A 113.7(3) . . ? N3A C2A C1A 111.2(4) . . ? C2A N3A Ba 111.2(2) . . ? N4 C1B C2B 114.8(3) . . ? N3B C2B C1B 111.5(3) . . ? C2B N3B Ba 110.1(2) . . ? N7 C1C C2C 114.6(3) . . ? N3C C2C C1C 111.5(3) . . ? C2C N3C Ba 118.5(2) . . ? O3 Cl1 O2 110.39(19) . . ? O3 Cl1 O4' 112.2(5) . . ? O2 Cl1 O4' 96.8(5) . . ? O3 Cl1 O1 110.60(16) . . ? O2 Cl1 O1 107.27(17) . . ? O4' Cl1 O1 118.4(5) . . ? O3 Cl1 O4 110.7(6) . . ? O2 Cl1 O4 110.1(6) . . ? O4' Cl1 O4 14.3(9) . . ? O1 Cl1 O4 107.8(6) . . ? O3 Cl1 O4" 104.6(6) . . ? O2 Cl1 O4" 122.7(6) . . ? O4' Cl1 O4" 26.7(7) . . ? O1 Cl1 O4" 100.6(6) . . ? O4 Cl1 O4" 12.7(10) . . ? O3 Cl1 Ba 143.43(13) . . ? O2 Cl1 Ba 56.19(13) . . ? O4' Cl1 Ba 103.5(5) . . ? O1 Cl1 Ba 54.83(11) . . ? O4 Cl1 Ba 105.9(6) . . ? O4" Cl1 Ba 110.8(6) . . ? Cl1 O1 Ba 101.75(13) . . ? Cl1 O2 Ba 100.60(14) . . ? O6 Cl2 O7 109.6(2) . . ? O6 Cl2 O5 109.6(2) . . ? O7 Cl2 O5 110.8(2) . . ? O6 Cl2 O8 109.8(5) . . ? O7 Cl2 O8 108.8(5) . . ? O5 Cl2 O8 108.2(5) . . ? O6 Cl2 O8" 90.5(5) . . ? O7 Cl2 O8" 113.2(5) . . ? O5 Cl2 O8" 120.9(5) . . ? O8 Cl2 O8" 19.8(7) . . ? O6 Cl2 O8' 126.5(5) . . ? O7 Cl2 O8' 102.6(5) . . ? O5 Cl2 O8' 96.8(5) . . ? O8 Cl2 O8' 17.0(7) . . ? O8" Cl2 O8' 36.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Ba N1 C1A 145.1(3) . . . . ? N3A Ba N1 C1A -2.3(3) . . . . ? N3B Ba N1 C1A -58.1(3) . . . . ? N3C Ba N1 C1A -147.6(3) . . . . ? O13 Ba N1 C1A 89.3(3) . . . . ? N4 Ba N1 C1A -105.8(3) . . . . ? O1 Ba N1 C1A 75.5(3) . . . . ? N7 Ba N1 C1A -158.8(3) . . . . ? O2 Ba N1 C1A 18.3(3) . . . . ? Cl1 Ba N1 C1A 43.3(3) . . . . ? O10 Ba N1 C2 -92.8(2) . . . . ? N3A Ba N1 C2 119.8(3) . . . . ? N3B Ba N1 C2 64.0(2) . . . . ? N3C Ba N1 C2 -25.5(4) . . . . ? O13 Ba N1 C2 -148.6(3) . . . . ? N4 Ba N1 C2 16.2(2) . . . . ? O1 Ba N1 C2 -162.4(2) . . . . ? N7 Ba N1 C2 -36.8(3) . . . . ? O2 Ba N1 C2 140.4(2) . . . . ? Cl1 Ba N1 C2 165.3(2) . . . . ? O10 Ba N1 C15 21.5(2) . . . . ? N3A Ba N1 C15 -125.9(3) . . . . ? N3B Ba N1 C15 178.3(2) . . . . ? N3C Ba N1 C15 88.8(3) . . . . ? O13 Ba N1 C15 -34.3(2) . . . . ? N4 Ba N1 C15 130.5(3) . . . . ? O1 Ba N1 C15 -48.1(3) . . . . ? N7 Ba N1 C15 77.5(2) . . . . ? O2 Ba N1 C15 -105.3(2) . . . . ? Cl1 Ba N1 C15 -80.4(2) . . . . ? C1A N1 C2 C3 76.7(4) . . . . ? C15 N1 C2 C3 -162.2(3) . . . . ? Ba N1 C2 C3 -48.8(4) . . . . ? N1 C2 C3 N4 71.0(5) . . . . ? C2 C3 N4 C5 75.9(4) . . . . ? C2 C3 N4 C1B -166.7(3) . . . . ? C2 C3 N4 Ba -47.3(4) . . . . ? O10 Ba N4 C5 -29.4(3) . . . . ? N3A Ba N4 C5 -163.3(2) . . . . ? N3B Ba N4 C5 127.6(3) . . . . ? N3C Ba N4 C5 60.4(2) . . . . ? O13 Ba N4 C5 -89.8(3) . . . . ? N1 Ba N4 C5 -105.3(3) . . . . ? O1 Ba N4 C5 71.1(4) . . . . ? N7 Ba N4 C5 11.4(2) . . . . ? O2 Ba N4 C5 142.5(2) . . . . ? Cl1 Ba N4 C5 117.0(2) . . . . ? O10 Ba N4 C3 90.8(2) . . . . ? N3A Ba N4 C3 -43.1(2) . . . . ? N3B Ba N4 C3 -112.1(3) . . . . ? N3C Ba N4 C3 -179.4(2) . . . . ? O13 Ba N4 C3 30.4(3) . . . . ? N1 Ba N4 C3 15.0(2) . . . . ? O1 Ba N4 C3 -168.7(3) . . . . ? N7 Ba N4 C3 131.7(2) . . . . ? O2 Ba N4 C3 -97.3(2) . . . . ? Cl1 Ba N4 C3 -122.8(2) . . . . ? O10 Ba N4 C1B -150.3(3) . . . . ? N3A Ba N4 C1B 75.8(3) . . . . ? N3B Ba N4 C1B 6.8(3) . . . . ? N3C Ba N4 C1B -60.5(3) . . . . ? O13 Ba N4 C1B 149.3(2) . . . . ? N1 Ba N4 C1B 133.8(3) . . . . ? O1 Ba N4 C1B -49.8(4) . . . . ? N7 Ba N4 C1B -109.4(3) . . . . ? O2 Ba N4 C1B 21.6(3) . . . . ? Cl1 Ba N4 C1B -3.9(3) . . . . ? C3 N4 C5 C6 -160.4(4) . . . . ? C1B N4 C5 C6 81.4(4) . . . . ? Ba N4 C5 C6 -40.8(4) . . . . ? N4 C5 C6 N7 63.1(5) . . . . ? C5 C6 N7 C8 71.1(4) . . . . ? C5 C6 N7 C1C -169.7(3) . . . . ? C5 C6 N7 Ba -47.8(4) . . . . ? O10 Ba N7 C8 29.7(2) . . . . ? N3A Ba N7 C8 -91.3(3) . . . . ? N3B Ba N7 C8 -155.5(2) . . . . ? N3C Ba N7 C8 137.4(3) . . . . ? O13 Ba N7 C8 13.5(3) . . . . ? N1 Ba N7 C8 -47.3(3) . . . . ? N4 Ba N7 C8 -101.9(3) . . . . ? O1 Ba N7 C8 92.9(2) . . . . ? O2 Ba N7 C8 136.2(2) . . . . ? Cl1 Ba N7 C8 114.8(2) . . . . ? O10 Ba N7 C1C -90.7(3) . . . . ? N3A Ba N7 C1C 148.3(3) . . . . ? N3B Ba N7 C1C 84.1(3) . . . . ? N3C Ba N7 C1C 17.0(2) . . . . ? O13 Ba N7 C1C -106.9(3) . . . . ? N1 Ba N7 C1C -167.7(3) . . . . ? N4 Ba N7 C1C 137.7(3) . . . . ? O1 Ba N7 C1C -27.5(3) . . . . ? O2 Ba N7 C1C 15.8(3) . . . . ? Cl1 Ba N7 C1C -5.6(3) . . . . ? O10 Ba N7 C6 149.3(3) . . . . ? N3A Ba N7 C6 28.4(3) . . . . ? N3B Ba N7 C6 -35.9(2) . . . . ? N3C Ba N7 C6 -102.9(3) . . . . ? O13 Ba N7 C6 133.2(2) . . . . ? N1 Ba N7 C6 72.3(2) . . . . ? N4 Ba N7 C6 17.8(2) . . . . ? O1 Ba N7 C6 -147.5(2) . . . . ? O2 Ba N7 C6 -104.1(2) . . . . ? Cl1 Ba N7 C6 -125.5(2) . . . . ? C1C N7 C8 C9 65.8(4) . . . . ? C6 N7 C8 C9 -175.4(3) . . . . ? Ba N7 C8 C9 -56.0(4) . . . . ? N7 C8 C9 O10 51.4(5) . . . . ? C8 C9 O10 C11 152.5(3) . . . . ? C8 C9 O10 Ba -19.1(4) . . . . ? N3A Ba O10 C11 -32.2(3) . . . . ? N3B Ba O10 C11 171.3(3) . . . . ? N3C Ba O10 C11 127.8(3) . . . . ? O13 Ba O10 C11 -14.1(3) . . . . ? N1 Ba O10 C11 -72.0(3) . . . . ? N4 Ba O10 C11 -133.5(3) . . . . ? O1 Ba O10 C11 62.8(3) . . . . ? N7 Ba O10 C11 -176.5(3) . . . . ? O2 Ba O10 C11 53.9(3) . . . . ? Cl1 Ba O10 C11 64.0(3) . . . . ? N3A Ba O10 C9 138.6(3) . . . . ? N3B Ba O10 C9 -18.0(4) . . . . ? N3C Ba O10 C9 -61.4(3) . . . . ? O13 Ba O10 C9 156.7(3) . . . . ? N1 Ba O10 C9 98.8(3) . . . . ? N4 Ba O10 C9 37.3(3) . . . . ? O1 Ba O10 C9 -126.5(3) . . . . ? N7 Ba O10 C9 -5.7(3) . . . . ? O2 Ba O10 C9 -135.3(3) . . . . ? Cl1 Ba O10 C9 -125.2(3) . . . . ? C9 O10 C11 C12 177.0(3) . . . . ? Ba O10 C11 C12 -11.1(4) . . . . ? O10 C11 C12 O13 52.2(4) . . . . ? C11 C12 O13 C14 68.2(4) . . . . ? C11 C12 O13 Ba -64.8(3) . . . . ? O10 Ba O13 C12 37.9(2) . . . . ? N3A Ba O13 C12 -155.7(3) . . . . ? N3B Ba O13 C12 -146.4(2) . . . . ? N3C Ba O13 C12 -15.5(3) . . . . ? N1 Ba O13 C12 140.8(3) . . . . ? N4 Ba O13 C12 124.7(2) . . . . ? O1 Ba O13 C12 -49.8(2) . . . . ? N7 Ba O13 C12 54.1(3) . . . . ? O2 Ba O13 C12 -91.8(2) . . . . ? Cl1 Ba O13 C12 -69.1(2) . . . . ? O10 Ba O13 C14 -92.6(3) . . . . ? N3A Ba O13 C14 73.8(3) . . . . ? N3B Ba O13 C14 83.2(3) . . . . ? N3C Ba O13 C14 -146.0(3) . . . . ? N1 Ba O13 C14 10.3(3) . . . . ? N4 Ba O13 C14 -5.8(3) . . . . ? O1 Ba O13 C14 179.7(3) . . . . ? N7 Ba O13 C14 -76.4(3) . . . . ? O2 Ba O13 C14 137.7(3) . . . . ? Cl1 Ba O13 C14 160.4(3) . . . . ? C12 O13 C14 C15 -111.3(4) . . . . ? Ba O13 C14 C15 15.7(4) . . . . ? C1A N1 C15 C14 -63.8(4) . . . . ? C2 N1 C15 C14 176.4(3) . . . . ? Ba N1 C15 C14 61.9(4) . . . . ? O13 C14 C15 N1 -54.6(5) . . . . ? C2 N1 C1A C2A -146.2(4) . . . . ? C15 N1 C1A C2A 95.4(4) . . . . ? Ba N1 C1A C2A -25.1(4) . . . . ? N1 C1A C2A N3A 57.2(5) . . . . ? C1A C2A N3A Ba -58.4(4) . . . . ? O10 Ba N3A C2A -15.9(4) . . . . ? N3B Ba N3A C2A 153.8(3) . . . . ? N3C Ba N3A C2A -166.5(3) . . . . ? O13 Ba N3A C2A -31.5(3) . . . . ? N1 Ba N3A C2A 31.0(3) . . . . ? N4 Ba N3A C2A 92.2(3) . . . . ? O1 Ba N3A C2A -101.2(3) . . . . ? N7 Ba N3A C2A 82.8(3) . . . . ? O2 Ba N3A C2A -130.0(3) . . . . ? Cl1 Ba N3A C2A -119.3(3) . . . . ? C5 N4 C1B C2B -162.0(3) . . . . ? C3 N4 C1B C2B 80.1(4) . . . . ? Ba N4 C1B C2B -37.8(4) . . . . ? N4 C1B C2B N3B 65.7(5) . . . . ? C1B C2B N3B Ba -54.4(4) . . . . ? O10 Ba N3B C2B 87.4(3) . . . . ? N3A Ba N3B C2B -74.6(3) . . . . ? N3C Ba N3B C2B 132.9(3) . . . . ? O13 Ba N3B C2B -84.2(3) . . . . ? N1 Ba N3B C2B -24.7(3) . . . . ? N4 Ba N3B C2B 23.8(2) . . . . ? O1 Ba N3B C2B -170.3(2) . . . . ? N7 Ba N3B C2B 77.0(3) . . . . ? O2 Ba N3B C2B -144.3(3) . . . . ? Cl1 Ba N3B C2B -161.8(3) . . . . ? C8 N7 C1C C2C -165.4(4) . . . . ? C6 N7 C1C C2C 75.1(4) . . . . ? Ba N7 C1C C2C -45.4(4) . . . . ? N7 C1C C2C N3C 57.7(5) . . . . ? C1C C2C N3C Ba -39.1(4) . . . . ? O10 Ba N3C C2C 65.6(3) . . . . ? N3A Ba N3C C2C -135.6(3) . . . . ? N3B Ba N3C C2C -96.9(3) . . . . ? O13 Ba N3C C2C 108.3(3) . . . . ? N1 Ba N3C C2C -1.1(5) . . . . ? N4 Ba N3C C2C -38.5(3) . . . . ? O1 Ba N3C C2C 144.8(3) . . . . ? N7 Ba N3C C2C 11.8(3) . . . . ? O2 Ba N3C C2C -169.0(3) . . . . ? Cl1 Ba N3C C2C 170.6(3) . . . . ? O10 Ba Cl1 O3 -79.9(2) . . . . ? N3A Ba Cl1 O3 53.1(2) . . . . ? N3B Ba Cl1 O3 124.0(2) . . . . ? N3C Ba Cl1 O3 -161.1(2) . . . . ? O13 Ba Cl1 O3 -24.0(2) . . . . ? N1 Ba Cl1 O3 14.5(2) . . . . ? N4 Ba Cl1 O3 133.5(2) . . . . ? O1 Ba Cl1 O3 -76.9(2) . . . . ? N7 Ba Cl1 O3 -139.6(2) . . . . ? O2 Ba Cl1 O3 78.5(3) . . . . ? O10 Ba Cl1 O2 -158.36(18) . . . . ? N3A Ba Cl1 O2 -25.42(19) . . . . ? N3B Ba Cl1 O2 45.51(18) . . . . ? N3C Ba Cl1 O2 120.34(19) . . . . ? O13 Ba Cl1 O2 -102.56(18) . . . . ? N1 Ba Cl1 O2 -64.0(2) . . . . ? N4 Ba Cl1 O2 55.0(2) . . . . ? O1 Ba Cl1 O2 -155.4(2) . . . . ? N7 Ba Cl1 O2 141.84(19) . . . . ? O10 Ba Cl1 O4' 112.4(5) . . . . ? N3A Ba Cl1 O4' -114.6(5) . . . . ? N3B Ba Cl1 O4' -43.7(5) . . . . ? N3C Ba Cl1 O4' 31.1(5) . . . . ? O13 Ba Cl1 O4' 168.2(5) . . . . ? N1 Ba Cl1 O4' -153.2(5) . . . . ? N4 Ba Cl1 O4' -34.2(5) . . . . ? O1 Ba Cl1 O4' 115.4(5) . . . . ? N7 Ba Cl1 O4' 52.6(5) . . . . ? O2 Ba Cl1 O4' -89.2(5) . . . . ? O10 Ba Cl1 O1 -2.99(14) . . . . ? N3A Ba Cl1 O1 129.96(15) . . . . ? N3B Ba Cl1 O1 -159.12(15) . . . . ? N3C Ba Cl1 O1 -84.28(15) . . . . ? O13 Ba Cl1 O1 52.82(14) . . . . ? N1 Ba Cl1 O1 91.34(16) . . . . ? N4 Ba Cl1 O1 -149.65(18) . . . . ? N7 Ba Cl1 O1 -62.79(15) . . . . ? O2 Ba Cl1 O1 155.4(2) . . . . ? O10 Ba Cl1 O4 97.8(6) . . . . ? N3A Ba Cl1 O4 -129.2(6) . . . . ? N3B Ba Cl1 O4 -58.3(6) . . . . ? N3C Ba Cl1 O4 16.5(6) . . . . ? O13 Ba Cl1 O4 153.6(6) . . . . ? N1 Ba Cl1 O4 -167.9(6) . . . . ? N4 Ba Cl1 O4 -48.8(7) . . . . ? O1 Ba Cl1 O4 100.8(6) . . . . ? N7 Ba Cl1 O4 38.0(6) . . . . ? O2 Ba Cl1 O4 -103.8(6) . . . . ? O10 Ba Cl1 O4" 85.5(6) . . . . ? N3A Ba Cl1 O4" -141.6(6) . . . . ? N3B Ba Cl1 O4" -70.6(6) . . . . ? N3C Ba Cl1 O4" 4.2(6) . . . . ? O13 Ba Cl1 O4" 141.3(6) . . . . ? N1 Ba Cl1 O4" 179.8(6) . . . . ? N4 Ba Cl1 O4" -61.2(6) . . . . ? O1 Ba Cl1 O4" 88.5(6) . . . . ? N7 Ba Cl1 O4" 25.7(6) . . . . ? O2 Ba Cl1 O4" -116.2(6) . . . . ? O3 Cl1 O1 Ba 141.70(15) . . . . ? O2 Cl1 O1 Ba 21.26(19) . . . . ? O4' Cl1 O1 Ba -86.8(6) . . . . ? O4 Cl1 O1 Ba -97.2(6) . . . . ? O4" Cl1 O1 Ba -108.1(6) . . . . ? O10 Ba O1 Cl1 177.03(14) . . . . ? N3A Ba O1 Cl1 -51.15(15) . . . . ? N3B Ba O1 Cl1 21.89(15) . . . . ? N3C Ba O1 Cl1 84.67(14) . . . . ? O13 Ba O1 Cl1 -123.81(14) . . . . ? N1 Ba O1 Cl1 -111.40(14) . . . . ? N4 Ba O1 Cl1 73.0(3) . . . . ? N7 Ba O1 Cl1 126.73(13) . . . . ? O2 Ba O1 Cl1 -13.32(12) . . . . ? O3 Cl1 O2 Ba -141.47(14) . . . . ? O4' Cl1 O2 Ba 101.7(5) . . . . ? O1 Cl1 O2 Ba -20.90(18) . . . . ? O4 Cl1 O2 Ba 96.1(6) . . . . ? O4" Cl1 O2 Ba 94.5(7) . . . . ? O10 Ba O2 Cl1 25.7(2) . . . . ? N3A Ba O2 Cl1 151.9(2) . . . . ? N3B Ba O2 Cl1 -130.74(19) . . . . ? N3C Ba O2 Cl1 -53.14(17) . . . . ? O13 Ba O2 Cl1 77.25(17) . . . . ? N1 Ba O2 Cl1 132.10(16) . . . . ? N4 Ba O2 Cl1 -144.77(14) . . . . ? O1 Ba O2 Cl1 13.43(12) . . . . ? N7 Ba O2 Cl1 -52.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.635 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.113 data_n3o2cu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H38 Cl2 Cu N6 O10' _chemical_formula_weight 608.96 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' 'Cu' 'Cu' 0.3201 1.2651 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2446(13) _cell_length_b 13.129(2) _cell_length_c 20.653(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.116(11) _cell_angle_gamma 90.00 _cell_volume 2459.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16.5 _exptl_crystal_description plate _exptl_crystal_colour 'vibrant blue' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.904 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'linear isotropic decay 5.8' _diffrn_reflns_number 6015 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4313 _reflns_number_gt 3568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 v1.07 (Stoe & Cie, 1996a)' _computing_cell_refinement 'STADI4 v1.07' _computing_data_reduction 'X-RED v1.09 (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v5.03 (Sheldrick,1994)' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.4953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'from difference map' _atom_sites_solution_hydrogens 'CH constrained, NH from difference map' _refine_ls_hydrogen_treatment 'CH riding, NH distance restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4313 _refine_ls_number_parameters 349 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.44757(5) 0.26108(3) 0.16593(2) 0.02061(14) Uani 1 d . . . N1 N 0.5689(3) 0.3348(2) 0.10578(15) 0.0216(7) Uani 1 d . . . C2 C 0.4654(4) 0.4047(3) 0.0614(2) 0.0257(9) Uani 1 d . . . H2A H 0.4413 0.3755 0.0164 0.031 Uiso 1 calc R . . H2B H 0.5133 0.4716 0.0587 0.031 Uiso 1 calc R . . C3 C 0.3258(4) 0.4186(3) 0.0882(2) 0.0243(8) Uani 1 d . . . H3A H 0.3475 0.4573 0.1301 0.029 Uiso 1 calc R . . H3B H 0.2529 0.4576 0.0563 0.029 Uiso 1 calc R . . N4 N 0.2634(3) 0.3159(2) 0.09994(15) 0.0202(7) Uani 1 d . . . C5 C 0.1994(4) 0.2703(3) 0.03366(19) 0.0253(9) Uani 1 d . . . H5A H 0.2702 0.2812 0.0039 0.030 Uiso 1 calc R . . H5B H 0.1080 0.3078 0.0148 0.030 Uiso 1 calc R . . C6 C 0.1636(4) 0.1577(3) 0.0340(2) 0.0264(9) Uani 1 d . . . H6A H 0.1248 0.1419 0.0743 0.032 Uiso 1 calc R . . H6B H 0.0849 0.1422 -0.0045 0.032 Uiso 1 calc R . . N7 N 0.2916(4) 0.0917(2) 0.03188(16) 0.0241(7) Uani 1 d . . . C8 C 0.2913(4) 0.0538(3) -0.0352(2) 0.0281(9) Uani 1 d . . . H8A H 0.1972 0.0177 -0.0511 0.034 Uiso 1 calc R . . H8B H 0.3719 0.0036 -0.0329 0.034 Uiso 1 calc R . . C9 C 0.3096(4) 0.1346(3) -0.08507(19) 0.0271(9) Uani 1 d . . . H9A H 0.3015 0.1032 -0.1292 0.033 Uiso 1 calc R . . H9B H 0.2306 0.1862 -0.0876 0.033 Uiso 1 calc R . . O10 O 0.4492(3) 0.1821(2) -0.06640(13) 0.0276(6) Uani 1 d . . . C11 C 0.4777(5) 0.2560(4) -0.1133(2) 0.0341(10) Uani 1 d . . . H11A H 0.4091 0.3141 -0.1144 0.041 Uiso 1 calc R . . H11B H 0.4617 0.2252 -0.1578 0.041 Uiso 1 calc R . . C12 C 0.6338(5) 0.2926(3) -0.0942(2) 0.0321(10) Uani 1 d . . . H12A H 0.7008 0.2331 -0.0883 0.038 Uiso 1 calc R . . H12B H 0.6580 0.3347 -0.1305 0.038 Uiso 1 calc R . . O13 O 0.6584(3) 0.3511(2) -0.03495(14) 0.0306(7) Uani 1 d . . . C14 C 0.7372(5) 0.3017(4) 0.0225(2) 0.0325(10) Uani 1 d . . . H14A H 0.8074 0.3509 0.0478 0.039 Uiso 1 calc R . . H14B H 0.7955 0.2453 0.0087 0.039 Uiso 1 calc R . . C15 C 0.6405(4) 0.2591(3) 0.06793(19) 0.0249(8) Uani 1 d . . . H15A H 0.5619 0.2174 0.0410 0.030 Uiso 1 calc R . . H15B H 0.7014 0.2128 0.0999 0.030 Uiso 1 calc R . . C1A C 0.6782(5) 0.3964(3) 0.1518(2) 0.0278(9) Uani 1 d . . . H1A1 H 0.6283 0.4551 0.1681 0.033 Uiso 1 calc R . . H1A2 H 0.7540 0.4231 0.1283 0.033 Uiso 1 calc R . . C2A C 0.7509(4) 0.3310(3) 0.20953(19) 0.0266(9) Uani 1 d . . . H2A1 H 0.8135 0.2784 0.1943 0.032 Uiso 1 calc R . . H2A2 H 0.8139 0.3736 0.2432 0.032 Uiso 1 calc R . . N3A N 0.6336(4) 0.2822(3) 0.23803(17) 0.0290(8) Uani 1 d D . . H3A1 H 0.612(5) 0.324(3) 0.2686(18) 0.035 Uiso 1 d D . . H3A2 H 0.664(5) 0.223(2) 0.257(2) 0.035 Uiso 1 d D . . C1B C 0.1415(4) 0.3280(3) 0.13735(19) 0.0226(8) Uani 1 d . . . H1B1 H 0.0791 0.2662 0.1316 0.027 Uiso 1 calc R . . H1B2 H 0.0792 0.3866 0.1194 0.027 Uiso 1 calc R . . C2B C 0.2012(4) 0.3450(3) 0.21029(19) 0.0255(9) Uani 1 d . . . H2B1 H 0.2476 0.4131 0.2174 0.031 Uiso 1 calc R . . H2B2 H 0.1200 0.3415 0.2353 0.031 Uiso 1 calc R . . N3B N 0.3113(4) 0.2648(3) 0.23331(17) 0.0263(7) Uani 1 d D . . H3B1 H 0.268(5) 0.204(2) 0.235(2) 0.032 Uiso 1 d D . . H3B2 H 0.351(5) 0.279(3) 0.2745(12) 0.032 Uiso 1 d D . . C1C C 0.2949(5) 0.0041(3) 0.0762(2) 0.0275(9) Uani 1 d . . . H1C1 H 0.3675 -0.0461 0.0662 0.033 Uiso 1 calc R . . H1C2 H 0.1969 -0.0290 0.0678 0.033 Uiso 1 calc R . . C2C C 0.3347(5) 0.0327(3) 0.1482(2) 0.0306(9) Uani 1 d . . . H2C1 H 0.2520 0.0711 0.1606 0.037 Uiso 1 calc R . . H2C2 H 0.3493 -0.0301 0.1752 0.037 Uiso 1 calc R . . N3C N 0.4697(4) 0.0953(3) 0.16320(18) 0.0278(8) Uani 1 d D . . H3C1 H 0.521(4) 0.075(3) 0.2023(14) 0.033 Uiso 1 d D . . H3C2 H 0.527(4) 0.074(3) 0.1355(18) 0.033 Uiso 1 d D . . Cl1 Cl -0.01590(11) 0.61120(7) 0.13790(5) 0.0292(2) Uani 1 d D . . O2 O 0.0101(4) 0.7168(2) 0.12597(17) 0.0433(8) Uani 1 d D . . O1 O -0.1098(11) 0.5910(9) 0.1856(5) 0.034(3) Uiso 0.33 d PD A 1 O3 O -0.040(2) 0.5468(9) 0.0806(5) 0.013(3) Uiso 0.33 d PD A 1 O4 O 0.1308(9) 0.5761(10) 0.1731(6) 0.033(5) Uiso 0.33 d PD A 1 O1' O -0.1427(11) 0.6082(8) 0.1698(6) 0.020(2) Uiso 0.33 d PD A 2 O3' O -0.0698(15) 0.5518(11) 0.0800(5) 0.034(6) Uiso 0.33 d PD A 2 O4' O 0.1122(12) 0.5729(8) 0.1848(6) 0.013(3) Uiso 0.33 d PD A 2 O1" O -0.1721(9) 0.6179(13) 0.1389(9) 0.084(5) Uiso 0.33 d PD A 3 O3" O 0.0028(14) 0.5647(10) 0.0765(4) 0.046(4) Uiso 0.33 d PD A 3 O4" O 0.0600(16) 0.5616(10) 0.1952(5) 0.064(5) Uiso 0.33 d PD A 3 Cl2 Cl 0.94575(10) 0.06083(7) 0.20275(5) 0.0267(2) Uani 1 d D . . O5 O 0.8017(3) 0.0596(3) 0.21819(18) 0.0471(9) Uani 1 d D . . O6 O 0.9390(4) 0.1117(3) 0.14106(16) 0.0452(8) Uani 1 d D . . O7 O 0.9752(17) -0.0464(6) 0.1908(10) 0.033(5) Uiso 0.33 d PD B 1 O8 O 1.0657(12) 0.1091(12) 0.2475(6) 0.037(4) Uiso 0.33 d PD B 1 O7' O 1.0048(14) -0.0389(6) 0.2128(6) 0.030(3) Uiso 0.33 d PD B 2 O8' O 1.0314(11) 0.1343(7) 0.2479(5) 0.025(3) Uiso 0.33 d PD B 2 O7" O 1.0032(18) -0.0386(6) 0.1877(9) 0.027(4) Uiso 0.33 d PD B 3 O8" O 1.0444(14) 0.0916(11) 0.2625(5) 0.042(3) Uiso 0.33 d PD B 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0210(2) 0.0202(3) 0.0205(2) 0.00320(19) 0.00377(18) 0.00188(19) N1 0.0239(16) 0.0200(16) 0.0203(16) 0.0023(13) 0.0027(13) 0.0007(13) C2 0.028(2) 0.024(2) 0.026(2) 0.0082(17) 0.0059(17) 0.0037(16) C3 0.027(2) 0.0163(19) 0.029(2) 0.0064(16) 0.0049(17) 0.0031(16) N4 0.0228(16) 0.0169(15) 0.0207(16) -0.0007(13) 0.0033(13) 0.0026(13) C5 0.025(2) 0.025(2) 0.025(2) -0.0014(17) 0.0027(16) 0.0037(16) C6 0.025(2) 0.026(2) 0.028(2) -0.0043(17) 0.0034(16) -0.0018(17) N7 0.0279(18) 0.0193(17) 0.0250(17) -0.0010(14) 0.0053(14) -0.0001(13) C8 0.026(2) 0.029(2) 0.028(2) -0.0063(18) 0.0015(17) -0.0016(17) C9 0.025(2) 0.032(2) 0.022(2) -0.0081(17) 0.0002(16) -0.0006(17) O10 0.0268(15) 0.0304(15) 0.0249(15) 0.0005(12) 0.0030(12) -0.0039(12) C11 0.040(2) 0.040(3) 0.022(2) 0.0037(19) 0.0032(18) 0.000(2) C12 0.039(2) 0.035(2) 0.024(2) -0.0001(18) 0.0099(18) -0.006(2) O13 0.0374(16) 0.0259(15) 0.0313(16) 0.0005(13) 0.0135(13) -0.0014(13) C14 0.029(2) 0.043(3) 0.025(2) -0.0023(19) 0.0055(18) 0.0008(19) C15 0.026(2) 0.024(2) 0.024(2) -0.0010(17) 0.0026(16) 0.0039(16) C1A 0.030(2) 0.027(2) 0.026(2) -0.0051(17) 0.0048(17) -0.0051(17) C2A 0.023(2) 0.030(2) 0.025(2) -0.0066(17) 0.0007(16) -0.0047(17) N3A 0.0297(19) 0.031(2) 0.0240(18) 0.0014(15) -0.0010(15) -0.0014(16) C1B 0.0185(18) 0.022(2) 0.027(2) -0.0037(16) 0.0044(16) 0.0031(15) C2B 0.026(2) 0.025(2) 0.026(2) -0.0026(17) 0.0051(16) 0.0025(16) N3B 0.0265(18) 0.0303(19) 0.0223(17) 0.0030(15) 0.0054(14) 0.0020(15) C1C 0.031(2) 0.021(2) 0.032(2) -0.0019(17) 0.0098(18) -0.0033(16) C2C 0.035(2) 0.027(2) 0.030(2) 0.0060(18) 0.0056(18) -0.0032(18) N3C 0.0270(19) 0.0243(18) 0.0303(19) -0.0003(16) 0.0010(15) 0.0050(15) Cl1 0.0327(5) 0.0227(5) 0.0327(5) -0.0038(4) 0.0076(4) 0.0017(4) O2 0.050(2) 0.0243(16) 0.051(2) 0.0063(15) -0.0039(16) -0.0015(14) Cl2 0.0231(5) 0.0286(5) 0.0276(5) 0.0016(4) 0.0028(4) -0.0027(4) O5 0.0311(17) 0.052(2) 0.063(2) 0.0100(18) 0.0204(16) 0.0014(15) O6 0.054(2) 0.046(2) 0.0390(19) 0.0146(16) 0.0163(16) 0.0030(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3B 2.050(3) . Y Cu1 N3A 2.065(3) . Y Cu1 N1 2.068(3) . Y Cu1 N4 2.093(3) . Y Cu1 N3C 2.188(4) . Y N1 C1A 1.486(5) . ? N1 C15 1.496(5) . ? N1 C2 1.503(5) . ? C2 C3 1.510(5) . ? C3 N4 1.505(5) . ? N4 C1B 1.492(5) . ? N4 C5 1.506(5) . ? C5 C6 1.515(5) . ? C6 N7 1.475(5) . ? N7 C1C 1.467(5) . ? N7 C8 1.470(5) . ? C8 C9 1.511(6) . ? C9 O10 1.418(5) . ? O10 C11 1.430(5) . ? C11 C12 1.500(6) . ? C12 O13 1.426(5) . ? O13 C14 1.424(5) . ? C14 C15 1.522(6) . ? C1A C2A 1.517(6) . ? C2A N3A 1.476(5) . ? C1B C2B 1.518(5) . ? C2B N3B 1.478(5) . ? C1C C2C 1.508(6) . ? C2C N3C 1.476(5) . ? Cl1 O4" 1.414(7) . ? Cl1 O3' 1.434(7) . ? Cl1 O3 1.436(6) . ? Cl1 O2 1.436(3) . ? Cl1 O3" 1.448(7) . ? Cl1 O1' 1.452(6) . ? Cl1 O1" 1.451(7) . ? Cl1 O1 1.458(6) . ? Cl1 O4' 1.467(6) . ? Cl1 O4 1.484(6) . ? Cl2 O7' 1.418(6) . ? Cl2 O5 1.428(3) . ? Cl2 O6 1.429(3) . ? Cl2 O8" 1.443(7) . ? Cl2 O8 1.446(7) . ? Cl2 O8' 1.464(6) . ? Cl2 O7 1.463(7) . ? Cl2 O7" 1.465(6) . ? 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 N3B Cu1 N3A 92.43(14) . . Y N3B Cu1 N1 150.70(14) . . Y N3A Cu1 N1 84.12(13) . . Y N3B Cu1 N4 84.52(13) . . Y N3A Cu1 N4 152.04(14) . . Y N1 Cu1 N4 85.14(12) . . Y N3B Cu1 N3C 96.56(14) . . Y N3A Cu1 N3C 94.78(14) . . Y N1 Cu1 N3C 112.71(13) . . Y N4 Cu1 N3C 113.18(13) . . Y C1A N1 C15 112.4(3) . . ? C1A N1 C2 109.4(3) . . ? C15 N1 C2 112.4(3) . . ? C1A N1 Cu1 104.6(2) . . ? C15 N1 Cu1 110.4(2) . . ? C2 N1 Cu1 107.3(2) . . ? N1 C2 C3 109.8(3) . . ? N4 C3 C2 109.4(3) . . ? C1B N4 C3 109.8(3) . . ? C1B N4 C5 108.0(3) . . ? C3 N4 C5 107.7(3) . . ? C1B N4 Cu1 107.5(2) . . ? C3 N4 Cu1 97.1(2) . . ? C5 N4 Cu1 125.7(2) . . ? N4 C5 C6 115.5(3) . . ? N7 C6 C5 113.3(3) . . ? C1C N7 C8 108.6(3) . . ? C1C N7 C6 111.3(3) . . ? C8 N7 C6 111.8(3) . . ? N7 C8 C9 115.2(3) . . ? O10 C9 C8 109.8(3) . . ? C9 O10 C11 113.0(3) . . ? O10 C11 C12 109.5(3) . . ? O13 C12 C11 112.6(3) . . ? C14 O13 C12 116.2(3) . . ? O13 C14 C15 114.5(3) . . ? N1 C15 C14 116.7(3) . . ? N1 C1A C2A 109.8(3) . . ? N3A C2A C1A 108.1(3) . . ? C2A N3A Cu1 110.2(2) . . ? N4 C1B C2B 111.3(3) . . ? N3B C2B C1B 108.1(3) . . ? C2B N3B Cu1 105.9(2) . . ? N7 C1C C2C 113.0(3) . . ? N3C C2C C1C 112.4(3) . . ? C2C N3C Cu1 118.6(3) . . ? O4" Cl1 O3' 119.0(9) . . ? O4" Cl1 O3 113.1(8) . . ? O3' Cl1 O3 11.1(10) . . ? O4" Cl1 O2 121.0(6) . . ? O3' Cl1 O2 115.1(7) . . ? O3 Cl1 O2 115.6(6) . . ? O4" Cl1 O3" 114.6(8) . . ? O3' Cl1 O3" 28.5(8) . . ? O3 Cl1 O3" 19.4(8) . . ? O2 Cl1 O3" 101.8(6) . . ? O4" Cl1 O1' 85.5(8) . . ? O3' Cl1 O1' 100.5(8) . . ? O3 Cl1 O1' 110.2(9) . . ? O2 Cl1 O1' 106.3(5) . . ? O3" Cl1 O1' 129.0(7) . . ? O4" Cl1 O1" 110.5(10) . . ? O3' Cl1 O1" 81.9(9) . . ? O3 Cl1 O1" 92.8(10) . . ? O2 Cl1 O1" 98.3(7) . . ? O3" Cl1 O1" 109.0(9) . . ? O1' Cl1 O1" 26.1(7) . . ? O4" Cl1 O1 67.3(8) . . ? O3' Cl1 O1 107.9(8) . . ? O3 Cl1 O1 115.4(9) . . ? O2 Cl1 O1 115.7(5) . . ? O3" Cl1 O1 134.6(7) . . ? O1' Cl1 O1 18.2(6) . . ? O1" Cl1 O1 43.7(8) . . ? O4" Cl1 O4' 23.3(7) . . ? O3' Cl1 O4' 118.1(8) . . ? O3 Cl1 O4' 108.7(8) . . ? O2 Cl1 O4' 107.7(5) . . ? O3" Cl1 O4' 102.5(7) . . ? O1' Cl1 O4' 108.1(8) . . ? O1" Cl1 O4' 133.7(10) . . ? O1 Cl1 O4' 90.1(8) . . ? O4" Cl1 O4 35.6(8) . . ? O3' Cl1 O4 112.2(8) . . ? O3 Cl1 O4 101.8(8) . . ? O2 Cl1 O4 102.5(5) . . ? O3" Cl1 O4 92.6(7) . . ? O1' Cl1 O4 120.8(8) . . ? O1" Cl1 O4 146.1(9) . . ? O1 Cl1 O4 102.7(7) . . ? O4' Cl1 O4 12.7(7) . . ? O7' Cl2 O5 107.8(6) . . ? O7' Cl2 O6 120.8(5) . . ? O5 Cl2 O6 108.8(2) . . ? O7' Cl2 O8" 88.4(8) . . ? O5 Cl2 O8" 106.0(6) . . ? O6 Cl2 O8" 122.9(6) . . ? O7' Cl2 O8 94.9(9) . . ? O5 Cl2 O8 119.7(6) . . ? O6 Cl2 O8 105.1(7) . . ? O8" Cl2 O8 18.3(7) . . ? O7' Cl2 O8' 111.7(7) . . ? O5 Cl2 O8' 106.2(5) . . ? O6 Cl2 O8' 100.7(5) . . ? O8" Cl2 O8' 25.3(6) . . ? O8 Cl2 O8' 18.2(7) . . ? O7' Cl2 O7 19.6(8) . . ? O5 Cl2 O7 103.8(7) . . ? O6 Cl2 O7 106.1(8) . . ? O8" Cl2 O7 107.8(9) . . ? O8 Cl2 O7 112.6(9) . . ? O8' Cl2 O7 130.2(8) . . ? O7' Cl2 O7" 20.5(7) . . ? O5 Cl2 O7" 115.4(6) . . ? O6 Cl2 O7" 100.6(7) . . ? O8" Cl2 O7" 103.6(10) . . ? O8 Cl2 O7" 105.1(10) . . ? O8' Cl2 O7" 123.3(9) . . ? O7 Cl2 O7" 11.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N4 -52.6(4) . . . . Y C2 C3 N4 C5 -72.6(4) . . . . Y C3 N4 C5 C6 166.2(3) . . . . Y N4 C5 C6 N7 -84.0(4) . . . . Y C5 C6 N7 C8 -99.4(4) . . . . Y C6 N7 C8 C9 65.1(4) . . . . Y N7 C8 C9 O10 63.1(4) . . . . Y C8 C9 O10 C11 176.9(3) . . . . Y C9 O10 C11 C12 -172.9(3) . . . . Y O10 C11 C12 O13 -68.1(5) . . . . Y C11 C12 O13 C14 105.0(4) . . . . Y C12 O13 C14 C15 -99.3(4) . . . . Y O13 C14 C15 N1 -71.4(5) . . . . Y C14 C15 N1 C2 61.8(4) . . . . Y C15 N1 C2 C3 137.2(3) . . . . Y N1 C1A C2A N3A -52.3(4) . . . . Y N4 C1B C2B N3B -50.4(4) . . . . Y N7 C1C C2C N3C -50.7(5) . . . . Y N3B Cu1 N1 C1A 60.2(4) . . . . ? N3A Cu1 N1 C1A -24.3(2) . . . . ? N4 Cu1 N1 C1A 129.9(2) . . . . ? N3C Cu1 N1 C1A -117.0(2) . . . . ? N3B Cu1 N1 C15 -178.7(3) . . . . ? N3A Cu1 N1 C15 96.9(2) . . . . ? N4 Cu1 N1 C15 -109.0(2) . . . . ? N3C Cu1 N1 C15 4.1(3) . . . . ? N3B Cu1 N1 C2 -55.9(4) . . . . ? N3A Cu1 N1 C2 -140.4(3) . . . . ? N4 Cu1 N1 C2 13.8(2) . . . . ? N3C Cu1 N1 C2 126.9(2) . . . . ? C1A N1 C2 C3 -97.2(4) . . . . ? Cu1 N1 C2 C3 15.7(4) . . . . ? C2 C3 N4 C1B 170.0(3) . . . . ? C2 C3 N4 Cu1 58.5(3) . . . . ? N3B Cu1 N4 C1B 0.8(2) . . . . ? N3A Cu1 N4 C1B -84.1(4) . . . . ? N1 Cu1 N4 C1B -151.8(2) . . . . ? N3C Cu1 N4 C1B 95.6(2) . . . . ? N3B Cu1 N4 C3 114.2(2) . . . . ? N3A Cu1 N4 C3 29.3(4) . . . . ? N1 Cu1 N4 C3 -38.4(2) . . . . ? N3C Cu1 N4 C3 -151.0(2) . . . . ? N3B Cu1 N4 C5 -127.9(3) . . . . ? N3A Cu1 N4 C5 147.2(3) . . . . ? N1 Cu1 N4 C5 79.5(3) . . . . ? N3C Cu1 N4 C5 -33.1(3) . . . . ? C1B N4 C5 C6 -75.2(4) . . . . ? Cu1 N4 C5 C6 53.3(4) . . . . ? C5 C6 N7 C1C 139.0(3) . . . . ? C1C N7 C8 C9 -171.7(3) . . . . ? C1A N1 C15 C14 -62.2(4) . . . . ? Cu1 N1 C15 C14 -178.5(3) . . . . ? C15 N1 C1A C2A -72.0(4) . . . . ? C2 N1 C1A C2A 162.4(3) . . . . ? Cu1 N1 C1A C2A 47.7(3) . . . . ? C1A C2A N3A Cu1 29.2(4) . . . . ? N3B Cu1 N3A C2A -153.7(3) . . . . ? N1 Cu1 N3A C2A -2.8(3) . . . . ? N4 Cu1 N3A C2A -70.8(4) . . . . ? N3C Cu1 N3A C2A 109.5(3) . . . . ? C3 N4 C1B C2B -78.6(4) . . . . ? C5 N4 C1B C2B 164.1(3) . . . . ? Cu1 N4 C1B C2B 25.9(4) . . . . ? C1B C2B N3B Cu1 48.2(3) . . . . ? N3A Cu1 N3B C2B 125.0(3) . . . . ? N1 Cu1 N3B C2B 42.7(4) . . . . ? N4 Cu1 N3B C2B -27.2(2) . . . . ? N3C Cu1 N3B C2B -139.9(2) . . . . ? C8 N7 C1C C2C 165.1(3) . . . . ? C6 N7 C1C C2C -71.4(4) . . . . ? C1C C2C N3C Cu1 96.0(4) . . . . ? N3B Cu1 N3C C2C 54.7(3) . . . . ? N3A Cu1 N3C C2C 147.7(3) . . . . ? N1 Cu1 N3C C2C -126.7(3) . . . . ? N4 Cu1 N3C C2C -32.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.746 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.083 data_n3o2zn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H38 Cl2 N6 O10 Zn' _chemical_formula_weight 610.79 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' 'Zn' 'Zn' 0.2839 1.4301 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.273(5) _cell_length_b 13.154(8) _cell_length_c 20.692(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.24(5) _cell_angle_gamma 90.00 _cell_volume 2476(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.969 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +-4.6' _diffrn_reflns_number 4228 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.1081 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3233 _reflns_number_gt 2103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 v1.07 (Stoe & Cie, 1996a)' _computing_cell_refinement 'STADI4 v1.07' _computing_data_reduction 'X-RED v1.09 (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v5.03 (Sheldrick,1994)' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+20.1296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Fourier Difference methods' _atom_sites_solution_hydrogens 'CH constrained, NH from difference map' _refine_ls_hydrogen_treatment 'CH riding, N-H distance restrained' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3233 _refine_ls_number_parameters 331 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.212 _refine_ls_shift/su_max 0.007 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.94873(12) 0.24518(10) 0.16460(6) 0.0179(3) Uani 1 1 d . . . N7 N 0.7896(8) 0.0925(6) 0.0317(4) 0.018(2) Uani 1 1 d . . . C6 C 0.6583(10) 0.1578(8) 0.0316(5) 0.020(2) Uani 1 1 d . . . H6A H 0.6168 0.1417 0.0710 0.024 Uiso 1 1 calc R . . H6B H 0.5826 0.1416 -0.0078 0.024 Uiso 1 1 calc R . . C5 C 0.6919(11) 0.2695(8) 0.0316(5) 0.024(3) Uani 1 1 d . . . H5A H 0.7599 0.2816 0.0010 0.029 Uiso 1 1 calc R . . H5B H 0.5995 0.3065 0.0141 0.029 Uiso 1 1 calc R . . N4 N 0.7589(9) 0.3139(6) 0.0975(4) 0.018(2) Uani 1 1 d . . . C3 C 0.8239(11) 0.4153(7) 0.0866(5) 0.023(3) Uani 1 1 d . . . H3A H 0.8464 0.4535 0.1286 0.028 Uiso 1 1 calc R . . H3B H 0.7529 0.4554 0.0546 0.028 Uiso 1 1 calc R . . C2 C 0.9652(11) 0.3983(8) 0.0599(5) 0.023(3) Uani 1 1 d . . . H2A H 0.9404 0.3657 0.0160 0.028 Uiso 1 1 calc R . . H2B H 1.0117 0.4647 0.0546 0.028 Uiso 1 1 calc R . . N1 N 1.0700(9) 0.3335(7) 0.1045(4) 0.021(2) Uani 1 1 d . . . C15 C 1.1470(10) 0.2586(8) 0.0668(4) 0.018(2) Uani 1 1 d . . . H15A H 1.0714 0.2149 0.0398 0.022 Uiso 1 1 calc R . . H15B H 1.2103 0.2140 0.0991 0.022 Uiso 1 1 calc R . . C14 C 1.2416(12) 0.3055(10) 0.0216(6) 0.039(3) Uani 1 1 d . . . H14A H 1.3082 0.3564 0.0470 0.047 Uiso 1 1 calc R . . H14B H 1.3035 0.2515 0.0077 0.047 Uiso 1 1 calc R . . O13 O 1.1595(8) 0.3531(6) -0.0356(3) 0.0271(18) Uani 1 1 d . . . C12 C 1.1363(11) 0.2928(9) -0.0943(5) 0.031(3) Uani 1 1 d . . . H12A H 1.2034 0.2336 -0.0875 0.037 Uiso 1 1 calc R . . H12B H 1.1603 0.3338 -0.1309 0.037 Uiso 1 1 calc R . . C11 C 0.9799(11) 0.2558(10) -0.1129(5) 0.033(3) Uani 1 1 d . . . H11A H 0.9114 0.3138 -0.1138 0.040 Uiso 1 1 calc R . . H11B H 0.9632 0.2251 -0.1574 0.040 Uiso 1 1 calc R . . O10 O 0.9524(7) 0.1823(5) -0.0662(3) 0.0213(17) Uani 1 1 d . . . C9 C 0.8122(11) 0.1360(8) -0.0853(5) 0.023(3) Uani 1 1 d . . . H9A H 0.8037 0.1050 -0.1295 0.028 Uiso 1 1 calc R . . H9B H 0.7342 0.1881 -0.0877 0.028 Uiso 1 1 calc R . . C8 C 0.7921(12) 0.0546(8) -0.0355(5) 0.025(3) Uani 1 1 d . . . H8A H 0.6988 0.0183 -0.0521 0.031 Uiso 1 1 calc R . . H8B H 0.8730 0.0047 -0.0326 0.031 Uiso 1 1 calc R . . C1C C 0.7908(11) 0.0040(8) 0.0749(5) 0.021(3) Uani 1 1 d . . . H1C1 H 0.8646 -0.0455 0.0657 0.025 Uiso 1 1 calc R . . H1C2 H 0.6932 -0.0294 0.0650 0.025 Uiso 1 1 calc R . . C2C C 0.8263(12) 0.0328(8) 0.1469(5) 0.027(3) Uani 1 1 d . . . H2C1 H 0.7451 0.0746 0.1575 0.032 Uiso 1 1 calc R . . H2C2 H 0.8335 -0.0297 0.1740 0.032 Uiso 1 1 calc R . . N3C N 0.9664(10) 0.0907(7) 0.1643(5) 0.027(2) Uani 1 1 d D . . H3C1 H 1.001(10) 0.062(8) 0.204(3) 0.032 Uiso 1 1 d D . . H3C2 H 1.041(8) 0.065(8) 0.148(5) 0.032 Uiso 1 1 d D . . C1B C 0.6408(10) 0.3253(8) 0.1359(4) 0.017(2) Uani 1 1 d . . . H1B1 H 0.5826 0.2618 0.1326 0.020 Uiso 1 1 calc R . . H1B2 H 0.5741 0.3809 0.1166 0.020 Uiso 1 1 calc R . . C2B C 0.7012(11) 0.3487(8) 0.2084(5) 0.023(3) Uani 1 1 d . . . H2B1 H 0.7508 0.4157 0.2130 0.027 Uiso 1 1 calc R . . H2B2 H 0.6205 0.3500 0.2334 0.027 Uiso 1 1 calc R . . N3B N 0.8085(9) 0.2659(8) 0.2336(4) 0.023(2) Uani 1 1 d D . . H3B1 H 0.739(8) 0.218(6) 0.233(5) 0.027 Uiso 1 1 d D . . H3B2 H 0.861(9) 0.295(7) 0.270(3) 0.027 Uiso 1 1 d D . . C1A C 1.1753(12) 0.3950(8) 0.1513(5) 0.028(3) Uani 1 1 d . . . H1A1 H 1.1218 0.4514 0.1679 0.034 Uiso 1 1 calc R . . H1A2 H 1.2485 0.4251 0.1280 0.034 Uiso 1 1 calc R . . C2A C 1.2536(11) 0.3340(9) 0.2085(5) 0.024(3) Uani 1 1 d . . . H2A1 H 1.3209 0.2849 0.1934 0.029 Uiso 1 1 calc R . . H2A2 H 1.3129 0.3796 0.2414 0.029 Uiso 1 1 calc R . . N3A N 1.1442(10) 0.2786(8) 0.2389(4) 0.030(2) Uani 1 1 d D . . H3A1 H 1.171(11) 0.216(4) 0.255(5) 0.035 Uiso 1 1 d D . . H3A2 H 1.111(11) 0.314(7) 0.270(4) 0.035 Uiso 1 1 d D . . Cl1 Cl 1.0146(3) 0.1109(2) 0.36001(13) 0.0268(7) Uani 1 1 d D . . O2 O 0.9941(9) 0.2168(5) 0.3710(4) 0.042(2) Uani 1 1 d D A . O1 O 1.0533(14) 0.0484(8) 0.4175(4) 0.033(3) Uiso 0.70 1 d PD A 1 O3 O 1.1217(12) 0.0944(9) 0.3190(6) 0.045(3) Uiso 0.70 1 d PD A 1 O4 O 0.8768(10) 0.0772(9) 0.3196(5) 0.037(3) Uiso 0.70 1 d PD A 1 O1' O 0.991(3) 0.0615(17) 0.4194(7) 0.018(6) Uiso 0.30 1 d PD A 2 O3' O 1.1696(11) 0.117(2) 0.3597(14) 0.039(7) Uiso 0.30 1 d PD A 2 O4' O 0.942(3) 0.0649(19) 0.2998(8) 0.034(7) Uiso 0.30 1 d PD A 2 Cl2 Cl 1.4425(3) 0.0601(2) 0.20230(12) 0.0230(6) Uani 1 1 d D . . O5 O 1.2958(6) 0.0604(6) 0.2133(4) 0.039(2) Uani 1 1 d D . . O6 O 1.4432(8) 0.1078(6) 0.1406(3) 0.043(2) Uani 1 1 d D . . O7 O 1.5359(9) 0.1147(8) 0.2522(4) 0.077(4) Uani 1 1 d D . . O8 O 1.4924(8) -0.0408(5) 0.1997(4) 0.057(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0179(6) 0.0178(6) 0.0177(6) 0.0030(6) 0.0027(5) 0.0022(6) N7 0.016(5) 0.020(5) 0.016(5) -0.004(4) -0.001(4) 0.000(4) C6 0.016(6) 0.025(6) 0.017(6) -0.004(5) 0.002(4) -0.005(5) C5 0.024(6) 0.028(7) 0.018(6) 0.000(5) 0.002(5) 0.001(5) N4 0.023(5) 0.023(5) 0.010(5) -0.003(4) 0.006(4) 0.004(4) C3 0.034(7) 0.011(6) 0.026(6) 0.003(5) 0.006(5) 0.004(5) C2 0.033(6) 0.026(7) 0.012(6) 0.011(5) 0.005(5) 0.009(5) N1 0.024(5) 0.024(5) 0.014(5) 0.000(4) 0.004(4) -0.001(4) C15 0.026(6) 0.014(6) 0.011(5) -0.008(5) -0.007(4) 0.004(5) C14 0.026(7) 0.061(9) 0.031(7) -0.008(7) 0.010(6) -0.001(6) O13 0.036(4) 0.028(5) 0.019(4) -0.004(4) 0.010(3) -0.004(4) C12 0.030(7) 0.042(8) 0.022(6) 0.002(6) 0.010(5) -0.003(6) C11 0.038(7) 0.047(8) 0.012(5) 0.006(7) 0.000(5) -0.002(7) O10 0.019(4) 0.024(4) 0.019(4) 0.003(3) 0.000(3) -0.003(3) C9 0.028(6) 0.029(7) 0.010(6) 0.004(5) 0.001(5) -0.001(5) C8 0.034(6) 0.022(6) 0.020(6) -0.015(5) 0.006(5) 0.000(5) C1C 0.020(6) 0.022(6) 0.019(6) -0.006(5) -0.001(5) -0.007(5) C2C 0.039(7) 0.020(7) 0.019(6) 0.012(5) 0.000(5) -0.003(5) N3C 0.025(6) 0.025(5) 0.027(6) 0.007(5) -0.002(4) 0.010(5) C1B 0.023(6) 0.008(5) 0.017(6) -0.007(5) 0.001(5) -0.005(5) C2B 0.030(6) 0.015(6) 0.023(6) -0.001(5) 0.006(5) 0.011(5) N3B 0.019(5) 0.035(6) 0.014(5) -0.002(5) 0.003(4) 0.003(5) C1A 0.029(6) 0.029(7) 0.029(7) -0.005(6) 0.012(5) -0.013(6) C2A 0.018(6) 0.029(7) 0.023(6) -0.010(5) -0.001(5) -0.014(5) N3A 0.030(6) 0.037(7) 0.018(5) 0.008(5) -0.003(4) -0.007(5) Cl1 0.0298(16) 0.0233(16) 0.0284(16) 0.0053(13) 0.0083(13) -0.0008(13) O2 0.052(5) 0.023(5) 0.044(5) -0.007(4) -0.011(4) -0.002(4) Cl2 0.0205(14) 0.0259(16) 0.0221(15) 0.0019(13) 0.0028(11) -0.0010(13) O5 0.020(4) 0.045(5) 0.057(6) -0.006(5) 0.020(4) -0.007(4) O6 0.061(6) 0.033(5) 0.037(5) 0.018(4) 0.018(5) -0.001(4) O7 0.053(6) 0.127(10) 0.046(6) -0.046(7) -0.003(5) -0.027(7) O8 0.037(5) 0.041(6) 0.093(8) 0.016(5) 0.010(5) 0.012(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 Zn N1 2.170(8) . y Zn N4 2.211(8) . y Zn N3A 2.181(9) . y Zn N3B 2.128(8) . y Zn N3C 2.039(9) . y N7 C1C 1.466(13) . ? N7 C8 1.481(12) . ? N7 C6 1.490(12) . ? C6 C5 1.502(15) . ? C5 N4 1.502(12) . ? N4 C1B 1.481(11) . ? N4 C3 1.498(12) . ? C3 C2 1.534(14) . ? C2 N1 1.474(12) . ? N1 C1A 1.476(13) . ? N1 C15 1.518(12) . ? C15 C14 1.533(14) . ? C14 O13 1.421(13) . ? O13 C12 1.431(12) . ? C12 C11 1.507(14) . ? C11 O10 1.425(12) . ? O10 C9 1.420(11) . ? C9 C8 1.523(14) . ? C1C C2C 1.511(13) . ? C2C N3C 1.488(13) . ? C1B C2B 1.526(13) . ? C2B N3B 1.500(13) . ? C1A C2A 1.495(14) . ? C2A N3A 1.485(13) . ? Cl1 O2 1.430(6) . ? Cl1 O4' 1.430(9) . ? Cl1 O1 1.432(7) . ? Cl1 O3' 1.440(9) . ? Cl1 O3 1.442(7) . ? Cl1 O1' 1.444(8) . ? Cl1 O4 1.454(7) . ? Cl2 O8 1.410(6) . ? Cl2 O7 1.409(6) . ? Cl2 O5 1.421(6) . ? Cl2 O6 1.424(6) . ? 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 N3C Zn N3B 100.9(4) . . ? N3C Zn N1 118.7(4) . . ? N3B Zn N1 140.3(4) . . ? N3C Zn N3A 98.4(4) . . ? N3B Zn N3A 91.9(3) . . ? N1 Zn N3A 81.0(3) . . ? N3C Zn N4 117.4(3) . . ? N3B Zn N4 81.6(3) . . ? N1 Zn N4 81.9(3) . . ? N3A Zn N4 144.1(3) . . ? C1C N7 C8 107.8(8) . . ? C1C N7 C6 111.6(8) . . ? C8 N7 C6 110.9(8) . . ? N7 C6 C5 113.3(8) . . ? N4 C5 C6 115.4(8) . . ? C1B N4 C3 110.6(7) . . ? C1B N4 C5 107.9(7) . . ? C3 N4 C5 108.4(8) . . ? C1B N4 Zn 106.6(6) . . ? C3 N4 Zn 99.5(6) . . ? C5 N4 Zn 123.3(6) . . ? N4 C3 C2 108.7(8) . . ? N1 C2 C3 111.4(8) . . ? C2 N1 C1A 111.4(8) . . ? C2 N1 C15 111.9(7) . . ? C1A N1 C15 112.1(8) . . ? C2 N1 Zn 108.4(6) . . ? C1A N1 Zn 105.5(6) . . ? C15 N1 Zn 107.1(6) . . ? N1 C15 C14 115.7(9) . . ? O13 C14 C15 114.1(9) . . ? C14 O13 C12 115.5(9) . . ? O13 C12 C11 112.0(8) . . ? O10 C11 C12 109.7(8) . . ? C9 O10 C11 112.2(7) . . ? O10 C9 C8 109.8(8) . . ? N7 C8 C9 115.2(9) . . ? N7 C1C C2C 112.1(8) . . ? N3C C2C C1C 112.3(8) . . ? C2C N3C Zn 116.3(7) . . ? N4 C1B C2B 112.3(8) . . ? N3B C2B C1B 106.7(8) . . ? C2B N3B Zn 108.1(6) . . ? N1 C1A C2A 112.5(9) . . ? N3A C2A C1A 109.4(8) . . ? C2A N3A Zn 110.1(6) . . ? O2 Cl1 O4' 119.7(11) . . ? O2 Cl1 O1 116.5(6) . . ? O4' Cl1 O1 118.7(12) . . ? O2 Cl1 O3' 96.4(12) . . ? O4' Cl1 O3' 108.7(16) . . ? O1 Cl1 O3' 86.9(12) . . ? O2 Cl1 O3 111.6(6) . . ? O4' Cl1 O3 71.7(12) . . ? O1 Cl1 O3 108.2(7) . . ? O3' Cl1 O3 37.3(10) . . ? O2 Cl1 O1' 104.8(11) . . ? O4' Cl1 O1' 115.4(15) . . ? O1 Cl1 O1' 24.4(10) . . ? O3' Cl1 O1' 110.0(15) . . ? O3 Cl1 O1' 131.9(12) . . ? O2 Cl1 O4 105.0(6) . . ? O4' Cl1 O4 32.6(10) . . ? O1 Cl1 O4 110.6(7) . . ? O3' Cl1 O4 141.3(12) . . ? O3 Cl1 O4 104.1(7) . . ? O1' Cl1 O4 95.3(11) . . ? O8 Cl2 O7 110.4(5) . . ? O8 Cl2 O5 109.9(5) . . ? O7 Cl2 O5 110.7(5) . . ? O8 Cl2 O6 108.7(5) . . ? O7 Cl2 O6 108.8(5) . . ? O5 Cl2 O6 108.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1C N7 C6 C5 140.0(8) . . . . ? C8 N7 C6 C5 -99.8(10) . . . . ? N7 C6 C5 N4 -80.3(10) . . . . ? C6 C5 N4 C1B -76.0(10) . . . . ? C6 C5 N4 C3 164.2(8) . . . . ? C6 C5 N4 Zn 48.9(11) . . . . ? N3C Zn N4 C1B 92.6(6) . . . . ? N3B Zn N4 C1B -5.3(6) . . . . ? N1 Zn N4 C1B -149.1(6) . . . . ? N3A Zn N4 C1B -86.9(8) . . . . ? N3C Zn N4 C3 -152.4(6) . . . . ? N3B Zn N4 C3 109.6(6) . . . . ? N1 Zn N4 C3 -34.1(6) . . . . ? N3A Zn N4 C3 28.1(8) . . . . ? N3C Zn N4 C5 -32.8(8) . . . . ? N3B Zn N4 C5 -130.8(8) . . . . ? N1 Zn N4 C5 85.4(7) . . . . ? N3A Zn N4 C5 147.6(7) . . . . ? C1B N4 C3 C2 168.2(8) . . . . ? C5 N4 C3 C2 -73.6(10) . . . . ? Zn N4 C3 C2 56.3(8) . . . . ? N4 C3 C2 N1 -56.2(11) . . . . ? C3 C2 N1 C1A -93.4(10) . . . . ? C3 C2 N1 C15 140.1(9) . . . . ? C3 C2 N1 Zn 22.2(10) . . . . ? N3C Zn N1 C2 124.1(7) . . . . ? N3B Zn N1 C2 -59.1(8) . . . . ? N3A Zn N1 C2 -141.2(7) . . . . ? N4 Zn N1 C2 7.2(6) . . . . ? N3C Zn N1 C1A -116.5(7) . . . . ? N3B Zn N1 C1A 60.4(8) . . . . ? N3A Zn N1 C1A -21.7(7) . . . . ? N4 Zn N1 C1A 126.6(7) . . . . ? N3C Zn N1 C15 3.1(7) . . . . ? N3B Zn N1 C15 180.0(5) . . . . ? N3A Zn N1 C15 97.9(6) . . . . ? N4 Zn N1 C15 -113.8(6) . . . . ? C2 N1 C15 C14 62.1(11) . . . . ? C1A N1 C15 C14 -63.9(11) . . . . ? Zn N1 C15 C14 -179.2(7) . . . . ? N1 C15 C14 O13 -71.2(12) . . . . ? C15 C14 O13 C12 -97.7(11) . . . . ? C14 O13 C12 C11 106.8(11) . . . . ? O13 C12 C11 O10 -69.3(12) . . . . ? C12 C11 O10 C9 -173.2(9) . . . . ? C11 O10 C9 C8 177.2(8) . . . . ? C1C N7 C8 C9 -172.1(8) . . . . ? C6 N7 C8 C9 65.5(11) . . . . ? O10 C9 C8 N7 64.4(11) . . . . ? C8 N7 C1C C2C 165.7(8) . . . . ? C6 N7 C1C C2C -72.3(10) . . . . ? N7 C1C C2C N3C -54.4(12) . . . . ? C1C C2C N3C Zn 95.7(9) . . . . ? N3B Zn N3C C2C 57.4(8) . . . . ? N1 Zn N3C C2C -124.7(7) . . . . ? N3A Zn N3C C2C 151.0(7) . . . . ? N4 Zn N3C C2C -28.7(8) . . . . ? C3 N4 C1B C2B -73.5(10) . . . . ? C5 N4 C1B C2B 168.0(8) . . . . ? Zn N4 C1B C2B 33.7(9) . . . . ? N4 C1B C2B N3B -55.2(11) . . . . ? C1B C2B N3B Zn 47.1(9) . . . . ? N3C Zn N3B C2B -139.8(6) . . . . ? N1 Zn N3B C2B 43.1(8) . . . . ? N3A Zn N3B C2B 121.3(7) . . . . ? N4 Zn N3B C2B -23.3(6) . . . . ? C2 N1 C1A C2A 163.6(8) . . . . ? C15 N1 C1A C2A -70.1(11) . . . . ? Zn N1 C1A C2A 46.2(9) . . . . ? N1 C1A C2A N3A -52.0(12) . . . . ? C1A C2A N3A Zn 29.4(10) . . . . ? N3C Zn N3A C2A 113.8(8) . . . . ? N3B Zn N3A C2A -144.8(7) . . . . ? N1 Zn N3A C2A -4.1(7) . . . . ? N4 Zn N3A C2A -66.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.725 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.128 data_PBNOAM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H38 N6 O10 Pb . 2ClO~4' _chemical_formula_sum 'C16 H38 Cl2 N6 O10 Pb' _chemical_formula_weight 752.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 10.816(8) _cell_length_b 15.486(9) _cell_length_c 15.844(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.59(6) _cell_angle_gamma 90.00 _cell_volume 2624(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 11 _cell_measurement_theta_max 13 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 6.693 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.606 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'linear isotropic decay 10' _diffrn_reflns_number 6538 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5145 _reflns_number_gt 3729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 v1.07 (Stoe & Cie, 1996a)' _computing_cell_refinement 'STADI4 v1.07' _computing_data_reduction 'X-RED v1.09 (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v5.03 (Sheldrick,1994)' _computing_publication_material 'SHELXL-97' _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^)+(0.0920P)^2^+20.0400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Fourier Difference methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5145 _refine_ls_number_parameters 293 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.73580(4) 0.10582(3) 0.24545(3) 0.05094(19) Uani 1 1 d U . . N1 N 0.6560(10) 0.0493(7) 0.4001(6) 0.062(2) Uani 1 1 d DU A . C2 C 0.6779(14) -0.0448(10) 0.4029(10) 0.076(3) Uani 1 1 d U . . H2A H 0.6041 -0.0737 0.3738 0.091 Uiso 1 1 calc R A . H2B H 0.6904 -0.0636 0.4619 0.091 Uiso 1 1 calc R . . C3 C 0.7892(13) -0.0714(9) 0.3623(9) 0.071(3) Uani 1 1 d U A . H3A H 0.8617 -0.0399 0.3898 0.085 Uiso 1 1 calc R . . H3B H 0.8047 -0.1323 0.3735 0.085 Uiso 1 1 calc R . . N4 N 0.7779(9) -0.0573(7) 0.2703(7) 0.061(2) Uani 1 1 d U A . C5 C 0.9009(14) -0.0719(11) 0.2407(11) 0.084(4) Uani 1 1 d U . . H5A H 0.9227 -0.1324 0.2480 0.101 Uiso 1 1 calc R A . H5B H 0.9643 -0.0388 0.2766 0.101 Uiso 1 1 calc R . . C6 C 0.9029(16) -0.0470(11) 0.1479(10) 0.088(4) Uani 1 1 d U A . H6A H 0.9788 -0.0691 0.1300 0.106 Uiso 1 1 calc R . . H6B H 0.8324 -0.0738 0.1124 0.106 Uiso 1 1 calc R . . N7 N 0.8970(9) 0.0486(8) 0.1342(7) 0.071(3) Uani 1 1 d DU A . C8 C 1.0290(13) 0.0755(15) 0.1575(16) 0.077(7) Uiso 0.70 1 d PDU A 1 H8A H 1.0664 0.0824 0.1059 0.092 Uiso 0.70 1 calc PR A 1 H8B H 1.0747 0.0307 0.1917 0.092 Uiso 0.70 1 calc PR A 1 C9 C 1.040(3) 0.1585(13) 0.2063(11) 0.092(7) Uiso 0.70 1 d PDU A 1 H9A H 1.1230 0.1837 0.2088 0.110 Uiso 0.70 1 calc PR A 1 H9B H 0.9779 0.2002 0.1824 0.110 Uiso 0.70 1 calc PR A 1 O10 O 1.0181(14) 0.1281(11) 0.2892(9) 0.071(4) Uiso 0.70 1 d PDU A 1 C11 C 1.050(2) 0.1924(14) 0.3550(11) 0.074(6) Uiso 0.70 1 d PDU A 1 H11A H 1.0037 0.2452 0.3404 0.089 Uiso 0.70 1 calc PR A 1 H11B H 1.1390 0.2056 0.3613 0.089 Uiso 0.70 1 calc PR A 1 C12 C 1.0181(17) 0.155(2) 0.4353(14) 0.100(10) Uiso 0.70 1 d PDU A 1 H12A H 1.0634 0.1020 0.4488 0.121 Uiso 0.70 1 calc PR A 1 H12B H 1.0410 0.1956 0.4820 0.121 Uiso 0.70 1 calc PR A 1 O13 O 0.8849(14) 0.1394(11) 0.4240(9) 0.072(4) Uiso 0.70 1 d PDU A 1 C14 C 0.8469(18) 0.0950(15) 0.4961(12) 0.080(6) Uiso 0.70 1 d PDU A 1 H14A H 0.8776 0.1244 0.5492 0.096 Uiso 0.70 1 calc PR A 1 H14B H 0.8766 0.0358 0.4994 0.096 Uiso 0.70 1 calc PR A 1 C15 C 0.7076(18) 0.0986(17) 0.4770(12) 0.078(8) Uiso 0.70 1 d PDU A 1 H15A H 0.6728 0.0759 0.5255 0.094 Uiso 0.70 1 calc PR A 1 H15B H 0.6817 0.1584 0.4694 0.094 Uiso 0.70 1 calc PR A 1 C8' C 1.007(3) 0.106(3) 0.137(3) 0.062(12) Uiso 0.30 1 d PDU A 2 H8'1 H 0.9795 0.1633 0.1190 0.075 Uiso 0.30 1 calc PR A 2 H8'2 H 1.0598 0.0844 0.0967 0.075 Uiso 0.30 1 calc PR A 2 C9' C 1.080(4) 0.109(3) 0.224(2) 0.081(14) Uiso 0.30 1 d PDU A 2 H9'1 H 1.0896 0.0514 0.2489 0.098 Uiso 0.30 1 calc PR A 2 H9'2 H 1.1628 0.1328 0.2227 0.098 Uiso 0.30 1 calc PR A 2 O10' O 1.009(3) 0.164(2) 0.2728(18) 0.066(9) Uiso 0.30 1 d PDU A 2 C11' C 1.082(3) 0.155(3) 0.3568(18) 0.060(11) Uiso 0.30 1 d PDU A 2 H11C H 1.1573 0.1895 0.3611 0.072 Uiso 0.30 1 calc PR A 2 H11D H 1.1065 0.0947 0.3672 0.072 Uiso 0.30 1 calc PR A 2 C12' C 1.002(4) 0.184(2) 0.420(3) 0.055(11) Uiso 0.30 1 d PDU A 2 H12C H 1.0506 0.1958 0.4753 0.066 Uiso 0.30 1 calc PR A 2 H12D H 0.9531 0.2345 0.4002 0.066 Uiso 0.30 1 calc PR A 2 O13' O 0.924(3) 0.1078(19) 0.4218(18) 0.056(7) Uiso 0.30 1 d PDU A 2 C14' C 0.829(4) 0.146(3) 0.465(4) 0.092(16) Uiso 0.30 1 d PDU A 2 H14C H 0.7865 0.1922 0.4307 0.111 Uiso 0.30 1 calc PR A 2 H14D H 0.8662 0.1701 0.5195 0.111 Uiso 0.30 1 calc PR A 2 C15' C 0.738(5) 0.077(4) 0.479(2) 0.09(2) Uiso 0.30 1 d PDU A 2 H15C H 0.7838 0.0269 0.5035 0.102 Uiso 0.30 1 calc PR A 2 H15D H 0.6857 0.0972 0.5193 0.102 Uiso 0.30 1 calc PR A 2 C1A C 0.5216(15) 0.0709(11) 0.3921(12) 0.095(5) Uani 1 1 d DU . . H1A1 H 0.5016 0.0769 0.4495 0.114 Uiso 1 1 calc R A 1 H1A2 H 0.4753 0.0213 0.3668 0.114 Uiso 1 1 calc R A 1 C2A C 0.471(3) 0.1485(16) 0.3430(14) 0.073(8) Uiso 0.50 1 d PDU A 1 H2A1 H 0.3808 0.1497 0.3403 0.087 Uiso 0.50 1 calc PR A 1 H2A2 H 0.5045 0.2000 0.3729 0.087 Uiso 0.50 1 calc PR A 1 N3A N 0.502(2) 0.1498(17) 0.2556(13) 0.065(6) Uiso 0.50 1 d PDU A 1 H3A1 H 0.4879 0.2032 0.2340 0.078 Uiso 0.50 1 calc PR A 1 H3A2 H 0.4502 0.1134 0.2230 0.078 Uiso 0.50 1 calc PR A 1 C2A' C 0.509(4) 0.1656(12) 0.3750(19) 0.097(11) Uiso 0.50 1 d PDU A 2 H2A3 H 0.4253 0.1842 0.3812 0.117 Uiso 0.50 1 calc PR A 2 H2A4 H 0.5678 0.1967 0.4164 0.117 Uiso 0.50 1 calc PR A 2 N3A' N 0.534(3) 0.186(2) 0.2881(16) 0.087(8) Uiso 0.50 1 d PDU A 2 H3A3 H 0.5443 0.2436 0.2841 0.105 Uiso 0.50 1 calc PR A 2 H3A4 H 0.4664 0.1714 0.2504 0.105 Uiso 0.50 1 calc PR A 2 C1B C 0.6781(14) -0.1141(8) 0.2240(10) 0.074(4) Uani 1 1 d DU . . H1B1 H 0.7179 -0.1599 0.1961 0.089 Uiso 1 1 calc R A 1 H1B2 H 0.6329 -0.1408 0.2656 0.089 Uiso 1 1 calc R A 1 C2B C 0.586(3) -0.0696(15) 0.1586(16) 0.080(9) Uiso 0.50 1 d PDU A 1 H2B1 H 0.6226 -0.0620 0.1068 0.096 Uiso 0.50 1 calc PR A 1 H2B2 H 0.5123 -0.1055 0.1451 0.096 Uiso 0.50 1 calc PR A 1 N3B N 0.5490(18) 0.0155(12) 0.1886(14) 0.059(5) Uiso 0.50 1 d PDU A 1 H3B1 H 0.5013 0.0078 0.2299 0.070 Uiso 0.50 1 calc PR A 1 H3B2 H 0.5029 0.0435 0.1451 0.070 Uiso 0.50 1 calc PR A 1 C2B' C 0.5580(18) -0.0686(18) 0.195(2) 0.085(10) Uiso 0.50 1 d PDU A 2 H2B3 H 0.4989 -0.1066 0.1606 0.102 Uiso 0.50 1 calc PR A 2 H2B4 H 0.5208 -0.0474 0.2426 0.102 Uiso 0.50 1 calc PR A 2 N3B' N 0.594(2) 0.0034(15) 0.1427(14) 0.065(5) Uiso 0.50 1 d PDU A 2 H3B3 H 0.5261 0.0318 0.1175 0.078 Uiso 0.50 1 calc PR A 2 H3B4 H 0.6364 -0.0165 0.1018 0.078 Uiso 0.50 1 calc PR A 2 C1C C 0.825(4) 0.057(3) 0.0479(13) 0.082(14) Uiso 0.50 1 d PDU A 1 H1C1 H 0.7647 0.0101 0.0394 0.098 Uiso 0.50 1 calc PR A 1 H1C2 H 0.8817 0.0498 0.0066 0.098 Uiso 0.50 1 calc PR A 1 C2C C 0.756(4) 0.140(3) 0.029(2) 0.110(14) Uiso 0.50 1 d PDU A 1 H2C1 H 0.8162 0.1863 0.0298 0.132 Uiso 0.50 1 calc PR A 1 H2C2 H 0.7089 0.1368 -0.0279 0.132 Uiso 0.50 1 calc PR A 1 N3C N 0.669(2) 0.1605(18) 0.0899(16) 0.070(7) Uiso 0.50 1 d PDU A 1 H3C1 H 0.5941 0.1380 0.0699 0.084 Uiso 0.50 1 calc PR A 1 H3C2 H 0.6605 0.2183 0.0914 0.084 Uiso 0.50 1 calc PR A 1 C1C' C 0.848(4) 0.074(2) 0.0457(11) 0.072(12) Uiso 0.50 1 d PDU A 2 H1C3 H 0.7780 0.0375 0.0243 0.087 Uiso 0.50 1 calc PR A 2 H1C4 H 0.9130 0.0647 0.0103 0.087 Uiso 0.50 1 calc PR A 2 C2C' C 0.808(3) 0.1661(19) 0.038(2) 0.079(9) Uiso 0.50 1 d PDU A 2 H2C3 H 0.8794 0.2034 0.0552 0.095 Uiso 0.50 1 calc PR A 2 H2C4 H 0.7754 0.1788 -0.0211 0.095 Uiso 0.50 1 calc PR A 2 N3C' N 0.711(2) 0.1838(17) 0.0918(15) 0.065(7) Uiso 0.50 1 d PDU A 2 H3C3 H 0.6365 0.1682 0.0624 0.078 Uiso 0.50 1 calc PR A 2 H3C4 H 0.7083 0.2412 0.1003 0.078 Uiso 0.50 1 calc PR A 2 Cl1 Cl 0.6691(3) -0.3120(3) 0.4545(2) 0.0770(10) Uani 1 1 d DU . . O1 O 0.5984(17) -0.3822(11) 0.4781(14) 0.098(8) Uiso 0.50 1 d PDU B 1 O2 O 0.7967(11) -0.3202(13) 0.4915(13) 0.094(7) Uiso 0.50 1 d PDU B 1 O3 O 0.621(2) -0.2355(11) 0.4870(17) 0.201(18) Uiso 0.50 1 d PDU B 1 O4 O 0.662(2) -0.3039(16) 0.3654(8) 0.142(11) Uiso 0.50 1 d PDU B 1 O1' O 0.631(2) -0.3986(8) 0.4434(15) 0.102(8) Uiso 0.50 1 d PDU B 2 O2' O 0.769(2) -0.2973(19) 0.407(2) 0.33(4) Uiso 0.50 1 d PDU B 2 O3' O 0.5721(18) -0.2538(13) 0.4242(17) 0.134(10) Uiso 0.50 1 d PDU B 2 O4' O 0.713(3) -0.2940(16) 0.5413(9) 0.173(14) Uiso 0.50 1 d PDU B 2 Cl2 Cl 0.7293(3) 0.3688(3) 0.2381(3) 0.0811(11) Uani 1 1 d DU . . O5 O 0.6166(12) 0.3489(11) 0.1822(11) 0.069(5) Uiso 0.50 1 d PDU C 1 O6 O 0.8326(17) 0.3578(18) 0.1929(14) 0.165(16) Uiso 0.50 1 d PDU C 1 O7 O 0.7419(19) 0.3116(12) 0.3091(11) 0.105(8) Uiso 0.50 1 d PDU C 1 O8 O 0.726(2) 0.4553(9) 0.2671(15) 0.138(11) Uiso 0.50 1 d PDU C 1 O5' O 0.6093(17) 0.3302(19) 0.221(2) 0.26(3) Uiso 0.50 1 d PDU C 2 O6' O 0.8178(19) 0.3183(16) 0.2009(14) 0.106(8) Uiso 0.50 1 d PDU C 2 O7' O 0.769(2) 0.3761(19) 0.3272(9) 0.146(12) Uiso 0.50 1 d PDU C 2 O8' O 0.727(3) 0.4534(11) 0.2019(18) 0.169(14) Uiso 0.50 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.0476(3) 0.0511(3) 0.0545(3) -0.0005(2) 0.00868(18) 0.00043(19) N1 0.066(6) 0.070(6) 0.053(5) -0.001(5) 0.014(4) -0.014(5) C2 0.085(9) 0.069(7) 0.076(8) 0.017(7) 0.013(7) -0.016(6) C3 0.072(8) 0.060(7) 0.076(6) 0.010(6) -0.004(6) -0.003(6) N4 0.052(5) 0.056(5) 0.070(5) -0.011(5) -0.001(4) 0.001(4) C5 0.067(7) 0.077(9) 0.109(9) 0.001(8) 0.017(7) 0.024(7) C6 0.095(11) 0.081(8) 0.093(9) -0.032(8) 0.030(8) 0.012(8) N7 0.062(6) 0.080(7) 0.078(7) -0.023(5) 0.027(5) -0.013(6) C1A 0.079(8) 0.108(12) 0.110(13) -0.004(11) 0.048(9) -0.001(8) C1B 0.088(8) 0.056(7) 0.079(9) -0.024(7) 0.013(7) -0.014(7) Cl1 0.075(2) 0.083(3) 0.066(2) 0.0085(19) -0.0113(17) -0.0084(19) Cl2 0.0585(19) 0.074(2) 0.104(3) -0.002(2) -0.0106(19) -0.0025(16) _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 Pb N1 2.853(10) . y Pb N4 2.587(11) . y Pb N7 2.802(10) . y Pb N3A 2.65(2) . y Pb N3B 2.51(2) . y Pb N3C 2.60(3) . y Pb O10 3.048(15) . y Pb O13 3.083(14) . y Pb N3A' 2.69(3) . y Pb N3B' 2.60(2) . y Pb N3C' 2.69(2) . y Pb O10' 3.05(3) . y N1 C15 1.475(11) . ? N1 C2 1.476(18) . ? N1 C15' 1.477(11) . ? N1 C1A 1.479(18) . ? C2 C3 1.50(2) . ? C3 N4 1.460(17) . ? N4 C5 1.493(16) . ? N4 C1B 1.497(17) . ? C5 C6 1.52(2) . ? C6 N7 1.50(2) . ? N7 C1C' 1.476(11) . ? N7 C1C 1.477(11) . ? N7 C8' 1.477(11) . ? N7 C8 1.480(11) . ? C8 C9 1.496(13) . ? C9 O10 1.449(12) . ? O10 C11 1.447(12) . ? C11 C12 1.484(12) . ? C12 O13 1.447(12) . ? O13 C14 1.445(12) . ? C14 C15 1.493(13) . ? C8' C9' 1.493(13) . ? C9' O10' 1.450(13) . ? O10' C11' 1.451(12) . ? C11' C12' 1.491(13) . ? C12' O13' 1.451(12) . ? O13' C14' 1.450(13) . ? C14' C15' 1.493(13) . ? C1A C2A 1.491(13) . ? C1A C2A' 1.494(13) . ? C2A N3A 1.473(11) . ? C2A' N3A' 1.475(11) . ? C1B C2B' 1.490(13) . ? C1B C2B 1.493(13) . ? C2B N3B 1.475(11) . ? C2B' N3B' 1.473(11) . ? C1C C2C 1.489(13) . ? C2C N3C 1.475(11) . ? C1C' C2C' 1.490(13) . ? C2C' N3C' 1.475(11) . ? Cl1 O1' 1.404(11) . ? Cl1 O4 1.408(11) . ? Cl1 O1 1.412(11) . ? Cl1 O3' 1.412(11) . ? Cl1 O4' 1.414(12) . ? Cl1 O3 1.421(12) . ? Cl1 O2' 1.422(12) . ? Cl1 O2 1.422(11) . ? Cl2 O7' 1.418(12) . ? Cl2 O5' 1.418(12) . ? Cl2 O8 1.420(12) . ? Cl2 O7 1.422(12) . ? Cl2 O6 1.424(12) . ? Cl2 O5 1.428(11) . ? Cl2 O8' 1.429(12) . ? Cl2 O6' 1.429(12) . ? 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 Pb N1 68.8(3) . . y N7 Pb N1 137.7(4) . . y N4 Pb N7 71.0(3) . . y N3A Pb N1 67.2(5) . . y N3B Pb N1 78.9(5) . . y N3C Pb N1 146.8(6) . . y N3A Pb N4 112.9(6) . . y N3B Pb N4 67.9(5) . . y N3C Pb N4 118.7(7) . . y N3A Pb N7 144.0(5) . . y N3B Pb N7 98.1(5) . . y N3C Pb N7 67.5(6) . . y N3B Pb N3A 56.0(7) . . y N3B Pb N3C 75.4(8) . . y N3C Pb N3A 81.0(7) . . y N1 Pb O10 105.1(3) . . y N4 Pb O10 85.9(4) . . y N7 Pb O10 58.8(3) . . y N3A Pb O10 153.0(6) . . y N3B Pb O10 150.4(5) . . y N3C Pb O10 107.7(7) . . y N1 Pb O13 56.5(3) . . y N4 Pb O13 88.2(4) . . y N7 Pb O13 109.9(4) . . y N3A Pb O13 105.9(6) . . y N3B Pb O13 134.9(6) . . y N3C Pb O13 147.8(7) . . y O10 Pb O13 53.4(4) . . y N3A' Pb N1 64.2(6) . . y N3B' Pb N1 97.2(5) . . y N3C' Pb N1 155.6(5) . . y N4 Pb N3A' 123.0(7) . . y N4 Pb N3B' 64.8(5) . . y N4 Pb N3C' 124.5(6) . . y N3A' Pb N7 155.6(6) . . y N3B' Pb N7 77.1(6) . . y N3C' Pb N7 64.0(5) . . y N3B' Pb N3A' 90.9(9) . . y N3B' Pb N3C' 74.8(7) . . y N3A' Pb N3C' 92.5(7) . . y N3A' Pb O10 135.7(7) . . y N3B' Pb O10 133.4(6) . . y N3C' Pb O10 96.7(6) . . y N1 Pb O10' 112.2(6) . . y N4 Pb O10' 97.0(7) . . y N7 Pb O10' 60.2(6) . . y N3A Pb O10' 145.9(9) . . y N3B Pb O10' 157.5(7) . . y N3C Pb O10' 99.4(9) . . y N3A' Pb O10' 129.3(9) . . y N3B' Pb O10' 137.2(8) . . y N3C' Pb O10' 87.8(8) . . y N3A' Pb O13 91.4(7) . . y N3B' Pb O13 148.8(5) . . y N3C' Pb O13 136.2(6) . . y C15 N1 C2 116.5(15) . . ? C2 N1 C15' 101(3) . . ? C15 N1 C1A 101.5(13) . . ? C2 N1 C1A 112.1(11) . . ? C15' N1 C1A 118(3) . . ? C15 N1 Pb 115.2(11) . . ? C2 N1 Pb 105.1(8) . . ? C15' N1 Pb 115(2) . . ? C1A N1 Pb 106.1(8) . . ? N1 C2 C3 113.1(11) . . ? N4 C3 C2 115.6(11) . . ? C3 N4 C5 110.2(11) . . ? C3 N4 C1B 110.4(11) . . ? C5 N4 C1B 111.6(11) . . ? C3 N4 Pb 106.5(8) . . ? C5 N4 Pb 104.1(9) . . ? C1B N4 Pb 113.7(8) . . ? N4 C5 C6 114.1(12) . . ? N7 C6 C5 112.5(12) . . ? C1C' N7 C8' 92(2) . . ? C1C N7 C8' 106(3) . . ? C1C' N7 C8 111(2) . . ? C1C N7 C8 124(2) . . ? C1C' N7 C6 113.8(16) . . ? C1C N7 C6 103.1(18) . . ? C8' N7 C6 125(2) . . ? C8 N7 C6 103.0(14) . . ? C1C' N7 Pb 110.2(16) . . ? C1C N7 Pb 105.1(17) . . ? C8' N7 Pb 112(2) . . ? C8 N7 Pb 115.0(10) . . ? C6 N7 Pb 103.9(8) . . ? N7 C8 C9 111.9(16) . . ? O10 C9 C8 100.2(17) . . ? C11 O10 C9 111.9(16) . . ? C11 O10 Pb 111.6(12) . . ? C9 O10 Pb 97.3(13) . . ? O10 C11 C12 106.9(18) . . ? O13 C12 C11 108.5(17) . . ? C14 O13 C12 112.3(15) . . ? C14 O13 Pb 118.3(11) . . ? C12 O13 Pb 121.2(12) . . ? O13 C14 C15 102.7(17) . . ? N1 C15 C14 113.2(17) . . ? N7 C8' C9' 111(3) . . ? O10' C9' C8' 105(3) . . ? C9' O10' C11' 100(3) . . ? C9' O10' Pb 110(3) . . ? C11' O10' Pb 119(2) . . ? O10' C11' C12' 107(3) . . ? O13' C12' C11' 99(3) . . ? C14' O13' C12' 98(3) . . ? C14' O13' Pb 91(3) . . ? C12' O13' Pb 107(2) . . ? O13' C14' C15' 108(4) . . ? N1 C15' C14' 114(4) . . ? N1 C1A C2A 120.4(16) . . ? N1 C1A C2A' 107.3(19) . . ? N3A C2A C1A 112.6(19) . . ? C2A N3A Pb 114.0(16) . . ? N3A' C2A' C1A 111(2) . . ? C2A' N3A' Pb 114(2) . . ? C2B' C1B N4 114.0(16) . . ? C2B C1B N4 115.2(16) . . ? N3B C2B C1B 111.9(17) . . ? C2B N3B Pb 111.7(17) . . ? N3B' C2B' C1B 103.8(17) . . ? C2B' N3B' Pb 107.1(18) . . ? N7 C1C C2C 116(3) . . ? N3C C2C C1C 114(3) . . ? C2C N3C Pb 116(2) . . ? N7 C1C' C2C' 113(2) . . ? N3C' C2C' C1C' 111(3) . . ? C2C' N3C' Pb 117.1(18) . . ? O4 Cl1 O1 112.7(9) . . ? O4 Cl1 O3 108.8(9) . . ? O1 Cl1 O3 107.7(9) . . ? O4 Cl1 O2 108.9(8) . . ? O1 Cl1 O2 110.7(8) . . ? O3 Cl1 O2 108.0(9) . . ? O1' Cl1 O3' 112.3(9) . . ? O1' Cl1 O4' 111.0(9) . . ? O3' Cl1 O4' 109.3(9) . . ? O1' Cl1 O2' 108.5(9) . . ? O3' Cl1 O2' 107.6(9) . . ? O4' Cl1 O2' 107.9(9) . . ? O8 Cl2 O7 109.6(9) . . ? O8 Cl2 O6 109.6(9) . . ? O7 Cl2 O6 109.5(9) . . ? O8 Cl2 O5 110.1(8) . . ? O7 Cl2 O5 109.1(8) . . ? O6 Cl2 O5 108.9(9) . . ? O7' Cl2 O5' 110.7(9) . . ? O7' Cl2 O8' 108.1(9) . . ? O5' Cl2 O8' 110.3(9) . . ? O7' Cl2 O6' 109.6(9) . . ? O5' Cl2 O6' 110.0(9) . . ? O8' Cl2 O6' 108.1(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3B Pb N1 C15 -163.5(13) . . . . ? N4 Pb N1 C15 126.1(13) . . . . ? N3B' Pb N1 C15 -174.6(13) . . . . ? N3C Pb N1 C15 -123.7(16) . . . . ? N3A Pb N1 C15 -105.9(14) . . . . ? N3A' Pb N1 C15 -87.1(14) . . . . ? N3C' Pb N1 C15 -105.8(19) . . . . ? N7 Pb N1 C15 106.7(13) . . . . ? O10 Pb N1 C15 46.7(13) . . . . ? O10' Pb N1 C15 37.1(15) . . . . ? O13 Pb N1 C15 23.6(12) . . . . ? N3B Pb N1 C2 66.9(9) . . . . ? N4 Pb N1 C2 -3.6(8) . . . . ? N3B' Pb N1 C2 55.7(10) . . . . ? N3C Pb N1 C2 106.7(14) . . . . ? N3A Pb N1 C2 124.5(10) . . . . ? N3A' Pb N1 C2 143.2(11) . . . . ? N3C' Pb N1 C2 124.5(16) . . . . ? N7 Pb N1 C2 -23.0(10) . . . . ? O10 Pb N1 C2 -83.0(8) . . . . ? O10' Pb N1 C2 -92.6(10) . . . . ? O13 Pb N1 C2 -106.1(9) . . . . ? N3B Pb N1 C15' 176(3) . . . . ? N4 Pb N1 C15' 106(3) . . . . ? N3B' Pb N1 C15' 165(3) . . . . ? N3C Pb N1 C15' -144(3) . . . . ? N3A Pb N1 C15' -126(3) . . . . ? N3A' Pb N1 C15' -107(3) . . . . ? N3C' Pb N1 C15' -126(4) . . . . ? N7 Pb N1 C15' 87(3) . . . . ? O10 Pb N1 C15' 27(3) . . . . ? O10' Pb N1 C15' 17(3) . . . . ? O13 Pb N1 C15' 3(3) . . . . ? N3B Pb N1 C1A -52.1(10) . . . . ? N4 Pb N1 C1A -122.6(10) . . . . ? N3B' Pb N1 C1A -63.2(11) . . . . ? N3C Pb N1 C1A -12.3(16) . . . . ? N3A Pb N1 C1A 5.5(11) . . . . ? N3A' Pb N1 C1A 24.3(12) . . . . ? N3C' Pb N1 C1A 5.6(18) . . . . ? N7 Pb N1 C1A -141.9(9) . . . . ? O10 Pb N1 C1A 158.1(9) . . . . ? O10' Pb N1 C1A 148.5(11) . . . . ? O13 Pb N1 C1A 134.9(11) . . . . ? C15 N1 C2 C3 -96.4(16) . . . . ? C15' N1 C2 C3 -87(3) . . . . ? C1A N1 C2 C3 147.3(13) . . . . ? Pb N1 C2 C3 32.4(13) . . . . ? N1 C2 C3 N4 -66.1(16) . . . . ? C2 C3 N4 C5 170.3(13) . . . . ? C2 C3 N4 C1B -65.9(15) . . . . ? C2 C3 N4 Pb 57.9(13) . . . . ? N3B Pb N4 C3 -111.4(10) . . . . ? N3B' Pb N4 C3 -134.6(10) . . . . ? N3C Pb N4 C3 -169.4(9) . . . . ? N3A Pb N4 C3 -77.3(9) . . . . ? N3A' Pb N4 C3 -61.2(11) . . . . ? N3C' Pb N4 C3 178.0(9) . . . . ? N7 Pb N4 C3 141.1(8) . . . . ? N1 Pb N4 C3 -25.2(7) . . . . ? O10 Pb N4 C3 82.7(8) . . . . ? O10' Pb N4 C3 85.9(9) . . . . ? O13 Pb N4 C3 29.3(8) . . . . ? N3B Pb N4 C5 132.0(11) . . . . ? N3B' Pb N4 C5 108.9(10) . . . . ? N3C Pb N4 C5 74.1(11) . . . . ? N3A Pb N4 C5 166.2(9) . . . . ? N3A' Pb N4 C5 -177.8(11) . . . . ? N3C' Pb N4 C5 61.5(11) . . . . ? N7 Pb N4 C5 24.6(8) . . . . ? N1 Pb N4 C5 -141.8(9) . . . . ? O10 Pb N4 C5 -33.8(9) . . . . ? O10' Pb N4 C5 -30.6(10) . . . . ? O13 Pb N4 C5 -87.2(9) . . . . ? N3B Pb N4 C1B 10.4(10) . . . . ? N3B' Pb N4 C1B -12.8(10) . . . . ? N3C Pb N4 C1B -47.6(12) . . . . ? N3A Pb N4 C1B 44.6(11) . . . . ? N3A' Pb N4 C1B 60.6(12) . . . . ? N3C' Pb N4 C1B -60.2(12) . . . . ? N7 Pb N4 C1B -97.1(10) . . . . ? N1 Pb N4 C1B 96.6(10) . . . . ? O10 Pb N4 C1B -155.5(10) . . . . ? O10' Pb N4 C1B -152.2(11) . . . . ? O13 Pb N4 C1B 151.1(10) . . . . ? C3 N4 C5 C6 -172.1(13) . . . . ? C1B N4 C5 C6 64.8(17) . . . . ? Pb N4 C5 C6 -58.2(14) . . . . ? N4 C5 C6 N7 70.5(18) . . . . ? C5 C6 N7 C1C' -157(2) . . . . ? C5 C6 N7 C1C -146(2) . . . . ? C5 C6 N7 C8' 93(2) . . . . ? C5 C6 N7 C8 83.5(16) . . . . ? C5 C6 N7 Pb -36.7(14) . . . . ? N3B Pb N7 C1C' 65.0(18) . . . . ? N4 Pb N7 C1C' 128.2(17) . . . . ? N3B' Pb N7 C1C' 60.8(18) . . . . ? N3C Pb N7 C1C' -5.5(18) . . . . ? N3A Pb N7 C1C' 25(2) . . . . ? N3A' Pb N7 C1C' -1(3) . . . . ? N3C' Pb N7 C1C' -18.4(18) . . . . ? N1 Pb N7 C1C' 147.3(17) . . . . ? O10 Pb N7 C1C' -134.9(18) . . . . ? O10' Pb N7 C1C' -121.6(19) . . . . ? O13 Pb N7 C1C' -151.0(17) . . . . ? N3B Pb N7 C1C 50.7(19) . . . . ? N4 Pb N7 C1C 113.9(19) . . . . ? N3B' Pb N7 C1C 46.5(19) . . . . ? N3C Pb N7 C1C -20(2) . . . . ? N3A Pb N7 C1C 11(2) . . . . ? N3A' Pb N7 C1C -16(3) . . . . ? N3C' Pb N7 C1C -33(2) . . . . ? N1 Pb N7 C1C 133.0(19) . . . . ? O10 Pb N7 C1C -149(2) . . . . ? O10' Pb N7 C1C -136(2) . . . . ? O13 Pb N7 C1C -165.3(19) . . . . ? N3B Pb N7 C8' 166(2) . . . . ? N4 Pb N7 C8' -131(2) . . . . ? N3B' Pb N7 C8' 162(2) . . . . ? N3C Pb N7 C8' 95(2) . . . . ? N3A Pb N7 C8' 126(2) . . . . ? N3A' Pb N7 C8' 99(3) . . . . ? N3C' Pb N7 C8' 82(2) . . . . ? N1 Pb N7 C8' -112(2) . . . . ? O10 Pb N7 C8' -34(2) . . . . ? O10' Pb N7 C8' -21(2) . . . . ? O13 Pb N7 C8' -50(2) . . . . ? N3B Pb N7 C8 -169.1(14) . . . . ? N4 Pb N7 C8 -105.8(14) . . . . ? N3B' Pb N7 C8 -173.3(15) . . . . ? N3C Pb N7 C8 120.4(15) . . . . ? N3A Pb N7 C8 151.0(15) . . . . ? N3A' Pb N7 C8 125(2) . . . . ? N3C' Pb N7 C8 107.6(15) . . . . ? N1 Pb N7 C8 -86.7(14) . . . . ? O10 Pb N7 C8 -9.0(14) . . . . ? O10' Pb N7 C8 4.3(15) . . . . ? O13 Pb N7 C8 -25.0(14) . . . . ? N3B Pb N7 C6 -57.3(10) . . . . ? N4 Pb N7 C6 5.9(8) . . . . ? N3B' Pb N7 C6 -61.5(9) . . . . ? N3C Pb N7 C6 -127.8(11) . . . . ? N3A Pb N7 C6 -97.3(13) . . . . ? N3A' Pb N7 C6 -123.7(18) . . . . ? N3C' Pb N7 C6 -140.7(11) . . . . ? N1 Pb N7 C6 25.0(10) . . . . ? O10 Pb N7 C6 102.8(9) . . . . ? O10' Pb N7 C6 116.0(12) . . . . ? O13 Pb N7 C6 86.7(9) . . . . ? C1C' N7 C8 C9 98(2) . . . . ? C1C N7 C8 C9 104(3) . . . . ? C8' N7 C8 C9 59(5) . . . . ? C6 N7 C8 C9 -140.1(18) . . . . ? Pb N7 C8 C9 -28(2) . . . . ? N7 C8 C9 O10 76(2) . . . . ? C8 C9 O10 C11 167.4(18) . . . . ? C8 C9 O10 Pb -75.8(16) . . . . ? N3B Pb O10 C11 -155.3(14) . . . . ? N4 Pb O10 C11 -128.0(13) . . . . ? N3B' Pb O10 C11 -177.0(12) . . . . ? N3C Pb O10 C11 113.2(14) . . . . ? N3A Pb O10 C11 8(2) . . . . ? N3A' Pb O10 C11 7.1(17) . . . . ? N3C' Pb O10 C11 107.7(14) . . . . ? N7 Pb O10 C11 161.7(14) . . . . ? N1 Pb O10 C11 -61.2(13) . . . . ? O10' Pb O10 C11 68(3) . . . . ? O13 Pb O10 C11 -37.2(12) . . . . ? N3B Pb O10 C9 87.6(16) . . . . ? N4 Pb O10 C9 114.9(11) . . . . ? N3B' Pb O10 C9 65.9(14) . . . . ? N3C Pb O10 C9 -3.9(13) . . . . ? N3A Pb O10 C9 -109.1(15) . . . . ? N3A' Pb O10 C9 -110.0(13) . . . . ? N3C' Pb O10 C9 -9.5(13) . . . . ? N7 Pb O10 C9 44.6(11) . . . . ? N1 Pb O10 C9 -178.4(11) . . . . ? O10' Pb O10 C9 -49(3) . . . . ? O13 Pb O10 C9 -154.3(13) . . . . ? C9 O10 C11 C12 177(2) . . . . ? Pb O10 C11 C12 70(2) . . . . ? O10 C11 C12 O13 -62(3) . . . . ? C11 C12 O13 C14 174(2) . . . . ? C11 C12 O13 Pb 26(3) . . . . ? N3B Pb O13 C14 1.0(19) . . . . ? N4 Pb O13 C14 -54.9(15) . . . . ? N3B' Pb O13 C14 -26(2) . . . . ? N3C Pb O13 C14 156.9(16) . . . . ? N3A Pb O13 C14 58.5(17) . . . . ? N3A' Pb O13 C14 68.1(16) . . . . ? N3C' Pb O13 C14 163.3(14) . . . . ? N7 Pb O13 C14 -123.9(15) . . . . ? N1 Pb O13 C14 10.7(14) . . . . ? O10 Pb O13 C14 -141.1(17) . . . . ? O10' Pb O13 C14 -154.3(18) . . . . ? N3B Pb O13 C12 146.9(18) . . . . ? N4 Pb O13 C12 91.1(19) . . . . ? N3B' Pb O13 C12 120(2) . . . . ? N3C Pb O13 C12 -57(2) . . . . ? N3A Pb O13 C12 -155.5(19) . . . . ? N3A' Pb O13 C12 -146(2) . . . . ? N3C' Pb O13 C12 -51(2) . . . . ? N7 Pb O13 C12 22(2) . . . . ? N1 Pb O13 C12 157(2) . . . . ? O10 Pb O13 C12 4.9(18) . . . . ? O10' Pb O13 C12 -8(2) . . . . ? C12 O13 C14 C15 171(2) . . . . ? Pb O13 C14 C15 -40(2) . . . . ? C2 N1 C15 C14 63(2) . . . . ? C15' N1 C15 C14 32(7) . . . . ? C1A N1 C15 C14 -174.7(19) . . . . ? Pb N1 C15 C14 -61(2) . . . . ? O13 C14 C15 N1 65(3) . . . . ? C1C' N7 C8' C9' 173(4) . . . . ? C1C N7 C8' C9' 174(3) . . . . ? C8 N7 C8' C9' -43(3) . . . . ? C6 N7 C8' C9' -66(4) . . . . ? Pb N7 C8' C9' 60(4) . . . . ? N7 C8' C9' O10' -76(5) . . . . ? C8' C9' O10' C11' 175(4) . . . . ? C8' C9' O10' Pb 49(4) . . . . ? N3B Pb O10' C9' 2(4) . . . . ? N4 Pb O10' C9' 48(3) . . . . ? N3B' Pb O10' C9' -12(3) . . . . ? N3C Pb O10' C9' -73(3) . . . . ? N3A Pb O10' C9' -161(2) . . . . ? N3A' Pb O10' C9' -168(3) . . . . ? N3C' Pb O10' C9' -77(3) . . . . ? N7 Pb O10' C9' -16(3) . . . . ? N1 Pb O10' C9' 118(3) . . . . ? O10 Pb O10' C9' 64(4) . . . . ? O13 Pb O10' C9' 131(3) . . . . ? N3B Pb O10' C11' -112(3) . . . . ? N4 Pb O10' C11' -66(3) . . . . ? N3B' Pb O10' C11' -126(3) . . . . ? N3C Pb O10' C11' 174(3) . . . . ? N3A Pb O10' C11' 86(3) . . . . ? N3A' Pb O10' C11' 78(3) . . . . ? N3C' Pb O10' C11' 170(3) . . . . ? N7 Pb O10' C11' -129(3) . . . . ? N1 Pb O10' C11' 4(3) . . . . ? O10 Pb O10' C11' -50(3) . . . . ? O13 Pb O10' C11' 18(3) . . . . ? C9' O10' C11' C12' -163(4) . . . . ? Pb O10' C11' C12' -44(4) . . . . ? O10' C11' C12' O13' 78(5) . . . . ? C11' C12' O13' C14' -166(4) . . . . ? C11' C12' O13' Pb -73(3) . . . . ? N3B Pb O13' C14' -74(3) . . . . ? N4 Pb O13' C14' -117(2) . . . . ? N3B' Pb O13' C14' -103(3) . . . . ? N3C Pb O13' C14' 113(3) . . . . ? N3A Pb O13' C14' -7(3) . . . . ? N3A' Pb O13' C14' 4(3) . . . . ? N3C' Pb O13' C14' 113(2) . . . . ? N7 Pb O13' C14' 175(2) . . . . ? N1 Pb O13' C14' -45(2) . . . . ? O10 Pb O13' C14' 147(3) . . . . ? O10' Pb O13' C14' 135(3) . . . . ? O13 Pb O13' C14' 27(3) . . . . ? N3B Pb O13' C12' -171.9(19) . . . . ? N4 Pb O13' C12' 144(2) . . . . ? N3B' Pb O13' C12' 158.4(19) . . . . ? N3C Pb O13' C12' 15(3) . . . . ? N3A Pb O13' C12' -105(2) . . . . ? N3A' Pb O13' C12' -94(2) . . . . ? N3C' Pb O13' C12' 14(3) . . . . ? N7 Pb O13' C12' 76(2) . . . . ? N1 Pb O13' C12' -144(2) . . . . ? O10 Pb O13' C12' 49(2) . . . . ? O10' Pb O13' C12' 37(2) . . . . ? O13 Pb O13' C12' -71(3) . . . . ? C12' O13' C14' C15' -177(4) . . . . ? Pb O13' C14' C15' 76(4) . . . . ? C15 N1 C15' C14' -82(8) . . . . ? C2 N1 C15' C14' 126(5) . . . . ? C1A N1 C15' C14' -111(5) . . . . ? Pb N1 C15' C14' 14(6) . . . . ? O13' C14' C15' N1 -72(7) . . . . ? C15 N1 C1A C2A 89(2) . . . . ? C2 N1 C1A C2A -146.4(19) . . . . ? C15' N1 C1A C2A 98(3) . . . . ? Pb N1 C1A C2A -32(2) . . . . ? C15 N1 C1A C2A' 64(2) . . . . ? C2 N1 C1A C2A' -170.5(16) . . . . ? C15' N1 C1A C2A' 73(3) . . . . ? Pb N1 C1A C2A' -56.3(17) . . . . ? N1 C1A C2A N3A 54(3) . . . . ? C2A' C1A C2A N3A 119(5) . . . . ? C1A C2A N3A Pb -43(3) . . . . ? N3B Pb N3A C2A 111(2) . . . . ? N4 Pb N3A C2A 72.3(19) . . . . ? N3B' Pb N3A C2A 125(2) . . . . ? N3C Pb N3A C2A -170(2) . . . . ? N3A' Pb N3A C2A -57(3) . . . . ? N3C' Pb N3A C2A -160.5(19) . . . . ? N7 Pb N3A C2A 161.3(14) . . . . ? N1 Pb N3A C2A 19.4(17) . . . . ? O10 Pb N3A C2A -59(3) . . . . ? O10' Pb N3A C2A -77(2) . . . . ? O13 Pb N3A C2A -23(2) . . . . ? N1 C1A C2A' N3A' 71(3) . . . . ? C2A C1A C2A' N3A' -54(3) . . . . ? C1A C2A' N3A' Pb -45(3) . . . . ? N3B Pb N3A' C2A' 95(2) . . . . ? N4 Pb N3A' C2A' 47(2) . . . . ? N3B' Pb N3A' C2A' 107(2) . . . . ? N3C Pb N3A' C2A' 171(2) . . . . ? N3A Pb N3A' C2A' 106(4) . . . . ? N3C' Pb N3A' C2A' -178(2) . . . . ? N7 Pb N3A' C2A' 167.0(15) . . . . ? N1 Pb N3A' C2A' 10(2) . . . . ? O10 Pb N3A' C2A' -76(2) . . . . ? O10' Pb N3A' C2A' -89(2) . . . . ? O13 Pb N3A' C2A' -41(2) . . . . ? C3 N4 C1B C2B' 102.1(18) . . . . ? C5 N4 C1B C2B' -134.9(17) . . . . ? Pb N4 C1B C2B' -18(2) . . . . ? C3 N4 C1B C2B 131.3(19) . . . . ? C5 N4 C1B C2B -105.7(19) . . . . ? Pb N4 C1B C2B 12(2) . . . . ? C2B' C1B C2B N3B 52(3) . . . . ? N4 C1B C2B N3B -41(3) . . . . ? C1B C2B N3B Pb 51(3) . . . . ? N4 Pb N3B C2B -31.6(16) . . . . ? N3B' Pb N3B C2B 45.3(17) . . . . ? N3C Pb N3B C2B 98.2(18) . . . . ? N3A Pb N3B C2B -173(2) . . . . ? N3A' Pb N3B C2B -169.3(19) . . . . ? N3C' Pb N3B C2B 97.4(18) . . . . ? N7 Pb N3B C2B 34.1(18) . . . . ? N1 Pb N3B C2B -103.1(18) . . . . ? O10 Pb N3B C2B -2(3) . . . . ? O10' Pb N3B C2B 19(3) . . . . ? O13 Pb N3B C2B -94.8(18) . . . . ? C2B C1B C2B' N3B' -43(3) . . . . ? N4 C1B C2B' N3B' 56(3) . . . . ? C1B C2B' N3B' Pb -66(3) . . . . ? N3B Pb N3B' C2B' -51.8(16) . . . . ? N4 Pb N3B' C2B' 41.9(15) . . . . ? N3C Pb N3B' C2B' -172.1(19) . . . . ? N3A Pb N3B' C2B' -84.2(16) . . . . ? N3A' Pb N3B' C2B' -84.7(16) . . . . ? N3C' Pb N3B' C2B' -177.0(18) . . . . ? N7 Pb N3B' C2B' 116.8(16) . . . . ? N1 Pb N3B' C2B' -20.6(16) . . . . ? O10 Pb N3B' C2B' 98.2(16) . . . . ? O10' Pb N3B' C2B' 113.7(17) . . . . ? O13 Pb N3B' C2B' 10(2) . . . . ? C1C' N7 C1C C2C -66(9) . . . . ? C8' N7 C1C C2C -73(4) . . . . ? C8 N7 C1C C2C -89(4) . . . . ? C6 N7 C1C C2C 155(3) . . . . ? Pb N7 C1C C2C 46(4) . . . . ? N7 C1C C2C N3C -56(5) . . . . ? C1C C2C N3C Pb 31(4) . . . . ? N3B Pb N3C C2C -111(3) . . . . ? N4 Pb N3C C2C -56(3) . . . . ? N3B' Pb N3C C2C -92(3) . . . . ? N3A Pb N3C C2C -168(3) . . . . ? N3A' Pb N3C C2C 176(3) . . . . ? N3C' Pb N3C C2C 65(4) . . . . ? N7 Pb N3C C2C -5(2) . . . . ? N1 Pb N3C C2C -151(2) . . . . ? O10 Pb N3C C2C 39(3) . . . . ? O10' Pb N3C C2C 47(3) . . . . ? O13 Pb N3C C2C 87(3) . . . . ? C1C N7 C1C' C2C' 119(11) . . . . ? C8' N7 C1C' C2C' -67(4) . . . . ? C8 N7 C1C' C2C' -81(3) . . . . ? C6 N7 C1C' C2C' 163(2) . . . . ? Pb N7 C1C' C2C' 47(3) . . . . ? N7 C1C' C2C' N3C' -58(4) . . . . ? C1C' C2C' N3C' Pb 38(3) . . . . ? N3B Pb N3C' C2C' -111(2) . . . . ? N4 Pb N3C' C2C' -50(2) . . . . ? N3B' Pb N3C' C2C' -93(2) . . . . ? N3C Pb N3C' C2C' -114(5) . . . . ? N3A Pb N3C' C2C' -167(2) . . . . ? N3A' Pb N3C' C2C' 177(2) . . . . ? N7 Pb N3C' C2C' -10.4(19) . . . . ? N1 Pb N3C' C2C' -166.6(16) . . . . ? O10 Pb N3C' C2C' 40(2) . . . . ? O10' Pb N3C' C2C' 47(2) . . . . ? O13 Pb N3C' C2C' 82(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.104 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.184