# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1946 data_r32 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C78 H70 Cl3 N20 Nd O14' _chemical_formula_weight 1762.13 _chemical_melting_point ? _chemical_compound_source ? 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 16.403(2) _cell_length_b 16.403(2) _cell_length_c 27.497(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6407.1(16) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Pale purple' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method ? _exptl_crystal_F_000 2703 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Bruker AXS Smart CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7875 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2064 _reflns_number_observed 2029 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(13) _refine_ls_number_reflns 2048 _refine_ls_number_parameters 174 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1466 _refine_ls_wR_factor_obs 0.1230 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_goodness_of_fit_obs 1.060 _refine_ls_restrained_S_all 1.276 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 1.3333 0.6667 0.6667 0.05483(6) Uani 1 d S . N1 N 1.3333 0.6667 0.56570(9) 0.0613(7) Uani 1 d S . N2 N 1.2365(2) 0.4138(2) 0.56085(9) 0.0858(9) Uani 1 d . . H2A H 1.2421(2) 0.3971(2) 0.53039(9) 0.080 Uiso 1 d R . N3 N 1.2595(2) 0.50536(12) 0.62433(6) 0.0661(6) Uani 1 d . . C1 C 1.3398(2) 0.5857(2) 0.54812(9) 0.0713(8) Uani 1 d . . H1B H 1.3199(2) 0.5737(2) 0.51478(9) 0.080 Uiso 1 d R . H1C H 1.4035(2) 0.5982(2) 0.54988(9) 0.080 Uiso 1 d R . C2 C 1.2767(2) 0.5008(2) 0.57785(9) 0.0689(9) Uani 1 d . . C3 C 1.1859(3) 0.3525(2) 0.59875(9) 0.0901(11) Uani 1 d . . C4 C 1.1249(5) 0.2567(2) 0.60169(14) 0.131(2) Uani 1 d . . H4A H 1.1054(5) 0.2176(2) 0.57321(14) 0.080 Uiso 1 d R . C5 C 1.0928(4) 0.2198(3) 0.6451(2) 0.144(3) Uani 1 d . . H5A H 1.0577(4) 0.1527(3) 0.6491(2) 0.080 Uiso 1 d R . C6 C 1.1046(4) 0.2760(3) 0.6854(2) 0.144(3) Uani 1 d . . H6A H 1.0768(4) 0.2481(3) 0.7161(2) 0.080 Uiso 1 d R . C7 C 1.1601(2) 0.3732(2) 0.68272(12) 0.0906(13) Uani 1 d . . H7A H 1.1682(2) 0.4129(2) 0.71009(12) 0.080 Uiso 1 d R . C8 C 1.2007(3) 0.4114(2) 0.63863(8) 0.0766(8) Uani 1 d . . N4 N 1.0314(2) 0.5596(3) 0.87193(10) 0.1085(11) Uani 1 d . . C9 C 0.9924(3) 0.4693(2) 0.94638(12) 0.123(2) Uani 1 d . . H9A H 0.9773(3) 0.4109(2) 0.96183(12) 0.080 Uiso 1 d R . C10 C 1.0053(4) 0.4798(3) 0.89456(12) 0.137(2) Uani 1 d . . H10A H 0.9918(4) 0.4257(3) 0.87526(12) 0.080 Uiso 1 d R . C11 C 1.0414(3) 0.6275(3) 0.89834(14) 0.118(2) Uani 1 d . . H11A H 1.0604(3) 0.6866(3) 0.88267(14) 0.080 Uiso 1 d R . C12 C 1.0331(4) 0.6252(3) 0.94857(14) 0.115(2) Uani 1 d . . H12A H 1.0419(4) 0.6793(3) 0.96650(14) 0.080 Uiso 1 d R . C13 C 1.0074(2) 0.5435(2) 0.97376(10) 0.0834(9) Uani 1 d . . Cl1 Cl 1.22901(10) 0.89567(10) 0.8333 0.1418(6) Uani 1 d SD . O11 O 1.3050(2) 0.9200(3) 0.80161(11) 0.1051(13) Uiso 0.60 d PD . O12 O 1.1743(4) 0.7989(2) 0.8404(2) 0.219(5) Uiso 0.40 d PD . O13 O 1.1710(2) 0.9256(2) 0.8090(2) 0.253(6) Uiso 0.60 d PD . O14 O 1.2582(4) 0.9455(3) 0.87720(10) 0.138(3) Uiso 0.40 d PD . O1W O 1.3333 0.6667 0.9278(5) 0.310(6) Uiso 1 d S . 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 Nd1 0.07186(8) 0.07186(8) 0.02079(10) 0.000 0.000 0.03593(4) N1 0.0790(10) 0.0790(10) 0.0260(12) 0.000 0.000 0.0395(5) N2 0.122(2) 0.0855(11) 0.0501(12) -0.0200(10) -0.0131(11) 0.0518(9) N3 0.0906(10) 0.0762(8) 0.0322(8) -0.0047(7) -0.0076(14) 0.0422(9) C1 0.0926(12) 0.0980(13) 0.0294(12) -0.0069(11) -0.0005(11) 0.0521(10) C2 0.096(2) 0.0824(11) 0.0362(12) -0.0113(9) -0.0121(9) 0.0505(9) C3 0.119(2) 0.0817(13) 0.0551(12) -0.0070(11) -0.024(2) 0.039(2) C4 0.187(3) 0.083(2) 0.095(2) -0.017(2) -0.012(7) 0.046(3) C5 0.167(5) 0.074(2) 0.133(3) 0.004(2) -0.008(4) 0.016(3) C6 0.203(6) 0.089(2) 0.094(2) 0.030(2) 0.003(3) 0.038(2) C7 0.114(2) 0.0818(14) 0.067(2) 0.0073(13) 0.0004(15) 0.0426(13) C8 0.1101(12) 0.0822(11) 0.0499(12) -0.0049(10) -0.007(2) 0.0575(11) N4 0.134(2) 0.152(2) 0.0509(14) 0.0222(13) 0.0317(13) 0.0800(13) C9 0.223(3) 0.101(2) 0.058(2) 0.0125(12) 0.044(2) 0.091(2) C10 0.228(3) 0.145(3) 0.060(2) 0.000(2) 0.033(2) 0.109(2) C11 0.166(3) 0.128(2) 0.069(2) 0.043(2) 0.041(2) 0.080(2) C12 0.180(3) 0.093(2) 0.069(2) 0.021(2) 0.043(2) 0.066(2) C13 0.1183(15) 0.1068(13) 0.0430(14) 0.0128(12) 0.0255(13) 0.0696(11) Cl1 0.1643(5) 0.1643(5) 0.0954(8) -0.0357(4) 0.0357(4) 0.0811(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N3 2.573(2) 3_775 ? Nd1 N3 2.573(2) 11_566 ? Nd1 N3 2.573(2) 10_546 ? Nd1 N3 2.573(2) 12_766 ? Nd1 N3 2.573(2) 2_755 ? Nd1 N3 2.573(2) . ? Nd1 N1 2.776(3) 10_546 ? Nd1 N1 2.776(3) . ? N1 C1 1.466(4) 3_775 ? N1 C1 1.466(4) 2_755 ? N1 C1 1.466(4) . ? N2 C2 1.322(4) . ? N2 C3 1.397(4) . ? N3 C2 1.319(3) . ? N3 C8 1.405(3) . ? C1 C2 1.495(3) . ? C3 C4 1.380(4) . ? C3 C8 1.400(4) . ? C4 C5 1.322(6) . ? C5 C6 1.393(7) . ? C6 C7 1.388(5) . ? C7 C8 1.374(4) . ? N4 C11 1.269(6) . ? N4 C10 1.312(6) . ? C9 C13 1.346(5) . ? C9 C10 1.438(5) . ? C11 C12 1.386(6) . ? C12 C13 1.374(5) . ? C13 C13 1.458(6) 6_767 ? Cl1 O12 1.392(3) 16_546 ? Cl1 O12 1.392(3) . ? Cl1 O14 1.400(3) 16_546 ? Cl1 O14 1.400(3) . ? Cl1 O11 1.406(3) 16_546 ? Cl1 O11 1.406(3) . ? Cl1 O13 1.436(3) . ? Cl1 O13 1.436(3) 16_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Nd1 N3 82.87(15) 3_775 11_566 ? N3 Nd1 N3 75.05(15) 3_775 10_546 ? N3 Nd1 N3 101.12(5) 11_566 10_546 ? N3 Nd1 N3 175.0(2) 3_775 12_766 ? N3 Nd1 N3 101.12(5) 11_566 12_766 ? N3 Nd1 N3 101.12(5) 10_546 12_766 ? N3 Nd1 N3 101.12(5) 3_775 2_755 ? N3 Nd1 N3 75.1(2) 11_566 2_755 ? N3 Nd1 N3 175.0(2) 10_546 2_755 ? N3 Nd1 N3 82.87(15) 12_766 2_755 ? N3 Nd1 N3 101.12(5) 3_775 . ? N3 Nd1 N3 175.0(2) 11_566 . ? N3 Nd1 N3 82.87(15) 10_546 . ? N3 Nd1 N3 75.06(15) 12_766 . ? N3 Nd1 N3 101.12(5) 2_755 . ? N3 Nd1 N1 116.90(4) 3_775 10_546 ? N3 Nd1 N1 63.10(4) 11_566 10_546 ? N3 Nd1 N1 63.09(4) 10_546 10_546 ? N3 Nd1 N1 63.10(4) 12_766 10_546 ? N3 Nd1 N1 116.90(4) 2_755 10_546 ? N3 Nd1 N1 116.90(4) . 10_546 ? N3 Nd1 N1 63.10(4) 3_775 . ? N3 Nd1 N1 116.90(4) 11_566 . ? N3 Nd1 N1 116.90(4) 10_546 . ? N3 Nd1 N1 116.91(4) 12_766 . ? N3 Nd1 N1 63.10(4) 2_755 . ? N3 Nd1 N1 63.10(4) . . ? N1 Nd1 N1 180.0 10_546 . ? C1 N1 C1 109.69(14) 3_775 2_755 ? C1 N1 C1 109.69(14) 3_775 . ? C1 N1 C1 109.69(14) 2_755 . ? C1 N1 Nd1 109.25(14) 3_775 . ? C1 N1 Nd1 109.25(14) 2_755 . ? C1 N1 Nd1 109.25(14) . . ? C2 N2 C3 108.1(2) . . ? C2 N3 C8 104.9(2) . . ? C2 N3 Nd1 119.51(15) . . ? C8 N3 Nd1 135.55(15) . . ? N1 C1 C2 109.5(2) . . ? N3 C2 N2 113.5(2) . . ? N3 C2 C1 123.0(2) . . ? N2 C2 C1 123.4(2) . . ? C4 C3 N2 134.1(3) . . ? C4 C3 C8 121.1(3) . . ? N2 C3 C8 104.6(2) . . ? C5 C4 C3 118.0(3) . . ? C4 C5 C6 121.6(4) . . ? C7 C6 C5 120.8(4) . . ? C8 C7 C6 117.4(3) . . ? C7 C8 C3 120.0(2) . . ? C7 C8 N3 131.0(2) . . ? C3 C8 N3 109.0(2) . . ? C11 N4 C10 115.9(3) . . ? C13 C9 C10 119.7(3) . . ? N4 C10 C9 123.1(4) . . ? N4 C11 C12 125.4(4) . . ? C13 C12 C11 120.4(4) . . ? C9 C13 C12 115.4(3) . . ? C9 C13 C13 122.1(2) . 6_767 ? C12 C13 C13 122.5(2) . 6_767 ? O12 Cl1 O14 112.5(3) 16_546 16_546 ? O12 Cl1 O14 112.5(3) . . ? O12 Cl1 O11 112.6(3) 16_546 16_546 ? O14 Cl1 O11 111.9(3) 16_546 16_546 ? O12 Cl1 O11 112.6(3) . . ? O14 Cl1 O11 111.9(3) . . ? O12 Cl1 O13 107.2(3) . . ? O14 Cl1 O13 107.1(3) . . ? O11 Cl1 O13 105.0(2) . . ? O12 Cl1 O13 107.1(3) 16_546 16_546 ? O14 Cl1 O13 107.1(3) 16_546 16_546 ? O11 Cl1 O13 105.0(2) 16_546 16_546 ? O12 O12 O13 126.4(3) 16_546 16_546 ? _refine_diff_density_max 0.731 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.083 data_scy9842 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H74 Cl3 N20 Nd O13' _chemical_formula_weight 1822.22 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.147(4) _cell_length_b 16.082(3) _cell_length_c 26.748(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.66(3) _cell_angle_gamma 90.00 _cell_volume 8726(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour 'Pale purple' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3732 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 1.139 _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 IP _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13150 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.63 _reflns_number_total 7554 _reflns_number_gt 6895 _reflns_threshold_expression >2sigma(I) _computing_data_collection BIOTEX _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1471P)^2^+7.9441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7554 _refine_ls_number_parameters 537 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2404 _refine_ls_wR_factor_gt 0.2338 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.005 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 Nd1 Nd 0.5000 0.317471(19) 0.2500 0.07920(10) Uani 1 d S . . N1 N 0.63634(16) 0.3197(2) 0.29121(16) 0.0862(10) Uani 1 d . . . N11 N 0.55096(16) 0.3226(2) 0.18007(16) 0.0881(11) Uani 1 d . . . N12 N 0.63643(16) 0.3325(3) 0.15667(17) 0.0973(12) Uani 1 d . . . C11 C 0.65707(17) 0.3645(3) 0.25403(19) 0.0915(13) Uani 1 d . . . C12 C 0.61523(18) 0.3381(3) 0.19696(18) 0.0868(12) Uani 1 d . . . C13 C 0.5820(2) 0.3116(3) 0.1088(2) 0.0984(15) Uani 1 d . . . C14 C 0.5761(3) 0.2944(5) 0.0567(2) 0.124(2) Uani 1 d . . . C15 C 0.5142(3) 0.2808(6) 0.0192(2) 0.142(2) Uani 1 d . . . C16 C 0.4593(3) 0.2766(5) 0.0322(2) 0.1201(19) Uani 1 d . . . C17 C 0.4668(2) 0.2880(4) 0.0854(2) 0.1037(15) Uani 1 d . . . C18 C 0.5290(2) 0.3068(3) 0.12471(19) 0.0896(13) Uani 1 d . . . N21 N 0.55605(15) 0.4390(2) 0.31152(15) 0.0896(10) Uani 1 d . . . N22 N 0.64048(17) 0.5009(3) 0.37825(15) 0.0994(12) Uani 1 d . . . C21 C 0.66135(19) 0.3628(3) 0.34561(19) 0.0951(14) Uani 1 d . . . C22 C 0.62011(18) 0.4338(3) 0.34433(17) 0.0874(12) Uani 1 d . . . C23 C 0.5881(2) 0.5531(3) 0.36764(19) 0.1024(14) Uani 1 d . . . C24 C 0.5802(3) 0.6300(4) 0.3888(2) 0.1175(18) Uani 1 d . . . C25 C 0.5202(3) 0.6656(4) 0.3676(3) 0.1246(19) Uani 1 d . . . C26 C 0.4676(3) 0.6285(4) 0.3255(2) 0.1154(17) Uani 1 d . . . C27 C 0.4737(2) 0.5535(4) 0.3044(2) 0.1040(15) Uani 1 d . . . C28 C 0.5340(2) 0.5149(3) 0.32535(18) 0.0949(13) Uani 1 d . . . N31 N 0.55845(17) 0.1916(2) 0.30684(16) 0.0884(11) Uani 1 d . . . N32 N 0.64375(16) 0.1070(3) 0.34422(17) 0.0982(12) Uani 1 d . . . C31 C 0.66182(17) 0.2341(3) 0.29875(19) 0.0911(13) Uani 1 d . . . C32 C 0.6217(2) 0.1797(3) 0.3176(2) 0.0893(13) Uani 1 d . . . C33 C 0.5915(2) 0.0696(3) 0.3512(2) 0.0952(13) Uani 1 d . . . C34 C 0.5868(3) -0.0059(4) 0.3759(3) 0.124(2) Uani 1 d . . . C35 C 0.5250(3) -0.0255(4) 0.3745(3) 0.130(2) Uani 1 d . . . C36 C 0.4718(2) 0.0290(4) 0.3517(2) 0.1155(18) Uani 1 d . . . C37 C 0.4776(2) 0.1018(3) 0.3281(2) 0.0989(14) Uani 1 d . . . C38 C 0.53877(19) 0.1239(3) 0.32842(18) 0.0904(13) Uani 1 d . . . N2 N 0.26966(18) -0.1578(4) 0.1781(2) 0.1171(15) Uani 1 d . . . C40 C 0.3029(3) -0.2258(5) 0.1763(3) 0.137(2) Uani 1 d . . . C41 C 0.3701(3) -0.2275(5) 0.1979(3) 0.147(2) Uani 1 d . . . C42 C 0.40611(19) -0.1591(4) 0.2223(3) 0.124(2) Uani 1 d D . . C43 C 0.3718(3) -0.0913(4) 0.2245(3) 0.127(2) Uani 1 d . . . C44 C 0.3033(3) -0.0958(4) 0.2027(3) 0.1205(19) Uani 1 d . . . C45 C 0.4778(3) -0.1331(7) 0.2461(5) 0.117(3) Uiso 0.50 d PD . . C46 C 0.4753(3) -0.1913(6) 0.2428(5) 0.105(3) Uiso 0.50 d PD . . N3 N 0.7298(3) -0.0157(5) 0.5529(3) 0.167(3) Uani 1 d . . . C50 C 0.6961(5) 0.0468(9) 0.5306(5) 0.243(5) Uani 1 d U . . C51 C 0.6323(4) 0.0529(9) 0.5132(5) 0.225(6) Uani 1 d . . . C52 C 0.5914(5) 0.0031(10) 0.5183(4) 0.220(5) Uani 1 d U . . C53 C 0.6248(4) -0.0684(8) 0.5469(5) 0.215(5) Uani 1 d . . . C54 C 0.6927(6) -0.0734(8) 0.5645(5) 0.221(6) Uani 1 d . . . C55 C 0.5092(10) 0.0373(10) 0.4947(8) 0.300(8) Uiso 1 d . . . N4 N 0.77766(19) -0.0567(3) 0.8943(2) 0.1196(16) Uani 1 d . . . C60 C 0.7922(3) -0.0278(7) 0.9431(3) 0.166(3) Uani 1 d U . . C61 C 0.8561(3) -0.0115(7) 0.9789(3) 0.183(4) Uani 1 d U . . C62 C 0.9067(2) -0.0199(4) 0.9639(2) 0.1108(17) Uani 1 d . . . C63 C 0.8925(2) -0.0428(5) 0.9142(3) 0.135(2) Uani 1 d . . . C64 C 0.8264(3) -0.0613(5) 0.8783(3) 0.148(3) Uani 1 d . . . C65 C 0.9744(2) -0.0008(5) 1.0044(3) 0.131(2) Uani 1 d . . . Cl1 Cl 0.73010(8) 0.07317(12) 0.20304(8) 0.1465(6) Uani 1 d D . . O14 O 0.7021(3) -0.0075(3) 0.1823(3) 0.209(3) Uani 1 d D . . O13 O 0.6988(5) 0.1273(5) 0.1583(3) 0.231(5) Uiso 0.60 d PD A 1 O12 O 0.7982(2) 0.0725(5) 0.2219(3) 0.160(3) Uiso 0.60 d PD A 1 O11 O 0.7119(4) 0.0863(8) 0.2478(3) 0.239(6) Uiso 0.60 d PD A 1 O13' O 0.7853(3) 0.0750(7) 0.1880(4) 0.156(4) Uiso 0.40 d PD A 2 O12' O 0.7552(9) 0.0727(11) 0.2608(3) 0.38(2) Uiso 0.40 d PD A 2 O11' O 0.6883(4) 0.1416(4) 0.1812(4) 0.118(3) Uiso 0.40 d PD A 2 Cl2 Cl 0.7500 0.2500 0.5000 0.255(2) Uani 1 d SD . . O24 O 0.8009(5) 0.2774(7) 0.5472(3) 0.210(5) Uiso 0.50 d PD . . O23 O 0.6979(4) 0.3043(5) 0.4733(4) 0.174(4) Uiso 0.50 d PD . . O22 O 0.7254(6) 0.1710(5) 0.5091(6) 0.315(13) Uiso 0.50 d PD . . O21 O 0.7753(4) 0.2302(10) 0.4588(3) 0.256(8) Uiso 0.50 d PD . . O1W O 0.6457(10) -0.1922(10) 0.1409(8) 0.233(8) Uiso 0.50 d P . . H12A H 0.6780 0.3396 0.1599 0.080 Uiso 1 d . . . H11A H 0.7025 0.3531 0.2620 0.080 Uiso 1 d . . . H11B H 0.6521 0.4231 0.2577 0.080 Uiso 1 d . . . H14A H 0.6141 0.2980 0.0475 0.080 Uiso 1 d . . . H15A H 0.5080 0.2685 -0.0182 0.080 Uiso 1 d . . . H16A H 0.4165 0.2649 0.0045 0.080 Uiso 1 d . . . H17A H 0.4300 0.2833 0.0955 0.080 Uiso 1 d . . . H22A H 0.6819 0.5091 0.4036 0.080 Uiso 1 d . . . H21A H 0.7056 0.3819 0.3542 0.080 Uiso 1 d . . . H21B H 0.6624 0.3246 0.3732 0.080 Uiso 1 d . . . H24A H 0.6160 0.6569 0.4171 0.080 Uiso 1 d . . . H25A H 0.5129 0.7171 0.3818 0.080 Uiso 1 d . . . H26A H 0.4264 0.6578 0.3111 0.080 Uiso 1 d . . . H27A H 0.4369 0.5279 0.2754 0.080 Uiso 1 d . . . H32A H 0.6852 0.0870 0.3556 0.080 Uiso 1 d . . . H31A H 0.7071 0.2338 0.3251 0.080 Uiso 1 d . . . H31B H 0.6612 0.2142 0.2648 0.080 Uiso 1 d . . . H34A H 0.6240 -0.0426 0.3925 0.080 Uiso 1 d . . . H35A H 0.5196 -0.0769 0.3903 0.080 Uiso 1 d . . . H36A H 0.4300 0.0148 0.3520 0.080 Uiso 1 d . . . H37A H 0.4406 0.1385 0.3124 0.080 Uiso 1 d . . . H60A H 0.7580 -0.0176 0.9547 0.080 Uiso 1 d . . . H61A H 0.8654 0.0043 1.0155 0.080 Uiso 1 d . . . H63A H 0.9265 -0.0496 0.9007 0.080 Uiso 1 d . . . H64A H 0.8158 -0.0771 0.8413 0.080 Uiso 1 d . . . H40A H 0.2791 -0.2758 0.1587 0.080 Uiso 1 d . . . H41A H 0.3915 -0.2784 0.1969 0.080 Uiso 1 d . . . H43A H 0.3948 -0.0417 0.2415 0.080 Uiso 1 d . . . H44A H 0.2794 -0.0478 0.2054 0.080 Uiso 1 d . . . H50A H 0.7231 0.0890 0.5208 0.080 Uiso 1 d . . . H51A H 0.6130 0.1112 0.4966 0.080 Uiso 1 d . . . H53A H 0.5973 -0.1093 0.5526 0.080 Uiso 1 d . . . H54A H 0.7134 -0.1215 0.5860 0.080 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.04117(12) 0.0985(2) 0.09257(17) 0.000 0.02118(11) 0.000 N1 0.0514(15) 0.107(2) 0.095(2) -0.0007(16) 0.0236(14) -0.0007(14) N11 0.0484(13) 0.115(3) 0.100(2) 0.0014(17) 0.0287(13) -0.0050(14) N12 0.0501(14) 0.134(3) 0.109(2) 0.0029(19) 0.0328(14) -0.0093(16) C11 0.0480(15) 0.105(3) 0.113(3) 0.003(2) 0.0236(16) -0.0055(18) C12 0.0511(16) 0.106(3) 0.102(2) 0.002(2) 0.0305(16) -0.0036(17) C13 0.071(2) 0.125(4) 0.100(3) 0.008(2) 0.0358(19) -0.006(2) C14 0.090(3) 0.185(5) 0.105(3) -0.002(3) 0.047(2) -0.011(3) C15 0.126(4) 0.208(6) 0.102(3) -0.015(4) 0.056(3) -0.045(4) C16 0.080(3) 0.166(5) 0.102(3) 0.000(3) 0.023(2) -0.013(3) C17 0.068(2) 0.131(3) 0.110(3) 0.000(3) 0.033(2) -0.015(2) C18 0.0537(18) 0.112(3) 0.097(2) 0.004(2) 0.0245(17) -0.0060(18) N21 0.0580(14) 0.104(2) 0.103(2) -0.0031(18) 0.0286(13) -0.0006(16) N22 0.0649(17) 0.125(3) 0.096(2) -0.008(2) 0.0199(15) -0.0091(19) C21 0.0564(18) 0.118(3) 0.099(2) -0.004(2) 0.0180(17) -0.008(2) C22 0.0595(17) 0.104(3) 0.094(2) -0.007(2) 0.0258(16) -0.0087(18) C23 0.094(2) 0.114(3) 0.103(3) -0.012(2) 0.044(2) -0.016(2) C24 0.114(3) 0.121(4) 0.116(3) -0.021(3) 0.045(3) -0.018(3) C25 0.138(4) 0.112(4) 0.140(4) -0.009(3) 0.073(3) 0.010(3) C26 0.101(3) 0.125(4) 0.130(3) 0.004(3) 0.057(2) 0.018(3) C27 0.076(2) 0.127(4) 0.112(3) -0.005(3) 0.0407(19) 0.009(2) C28 0.078(2) 0.114(3) 0.099(2) -0.003(2) 0.0427(17) -0.006(2) N31 0.0499(14) 0.105(2) 0.101(2) 0.0059(17) 0.0207(14) 0.0094(14) N32 0.0535(14) 0.112(3) 0.118(2) 0.013(2) 0.0227(15) 0.0124(17) C31 0.0508(15) 0.111(3) 0.108(3) 0.004(2) 0.0276(16) 0.0056(19) C32 0.0490(18) 0.107(3) 0.099(3) -0.002(2) 0.0163(17) 0.0058(17) C33 0.070(2) 0.097(3) 0.111(3) 0.008(2) 0.0288(19) 0.004(2) C34 0.099(3) 0.123(4) 0.141(4) 0.021(3) 0.038(3) 0.017(3) C35 0.116(3) 0.137(4) 0.144(4) 0.025(3) 0.061(3) -0.004(3) C36 0.076(2) 0.143(4) 0.123(3) 0.011(3) 0.036(2) -0.005(3) C37 0.0662(19) 0.104(3) 0.120(3) 0.004(2) 0.031(2) 0.000(2) C38 0.0605(18) 0.109(3) 0.094(2) 0.000(2) 0.0224(17) 0.005(2) N2 0.0572(16) 0.153(3) 0.144(3) 0.000(3) 0.0426(18) -0.005(2) C40 0.109(3) 0.135(5) 0.175(5) -0.012(4) 0.066(3) -0.016(4) C41 0.102(3) 0.179(6) 0.161(5) -0.002(5) 0.054(3) 0.045(4) C42 0.065(2) 0.180(5) 0.131(4) 0.014(4) 0.045(2) 0.005(3) C43 0.077(3) 0.140(4) 0.153(4) -0.005(4) 0.034(3) -0.020(3) C44 0.077(2) 0.126(4) 0.154(4) -0.001(3) 0.042(3) 0.012(3) N3 0.094(3) 0.228(7) 0.158(4) -0.041(5) 0.030(3) -0.020(4) C50 0.153(6) 0.306(13) 0.287(11) -0.059(10) 0.106(7) -0.102(7) C51 0.106(5) 0.265(12) 0.258(11) 0.033(10) 0.026(7) -0.016(7) C52 0.118(5) 0.340(14) 0.154(6) -0.046(8) 0.006(5) 0.048(8) C53 0.135(5) 0.290(11) 0.218(8) -0.001(8) 0.068(5) -0.085(6) C54 0.171(9) 0.217(10) 0.225(10) 0.019(9) 0.027(8) -0.014(8) N4 0.0626(18) 0.146(4) 0.133(3) -0.011(3) 0.022(2) -0.020(2) C60 0.072(2) 0.295(10) 0.133(4) -0.038(5) 0.043(3) -0.038(4) C61 0.083(3) 0.346(11) 0.118(4) -0.065(5) 0.038(3) -0.057(5) C62 0.067(2) 0.134(4) 0.117(3) -0.015(3) 0.021(2) -0.016(2) C63 0.065(2) 0.183(5) 0.147(4) -0.044(4) 0.033(2) -0.001(3) C64 0.078(3) 0.210(6) 0.134(4) -0.057(4) 0.021(3) 0.014(4) C65 0.073(2) 0.157(5) 0.150(4) -0.015(4) 0.032(3) -0.011(3) Cl1 0.1127(9) 0.1479(12) 0.1728(13) 0.0300(11) 0.0509(9) 0.0233(9) O14 0.152(4) 0.143(4) 0.300(7) -0.024(5) 0.059(5) -0.031(4) Cl2 0.199(4) 0.239(4) 0.224(4) -0.035(3) -0.023(3) 0.051(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N21 2.536(4) . ? Nd1 N21 2.536(4) 2_655 ? Nd1 N11 2.544(4) 2_655 ? Nd1 N11 2.544(4) . ? Nd1 N31 2.550(4) 2_655 ? Nd1 N31 2.550(4) . ? Nd1 N1 2.768(3) 2_655 ? Nd1 N1 2.768(3) . ? N1 C11 1.444(6) . ? N1 C31 1.470(6) . ? N1 C21 1.503(6) . ? N11 C12 1.333(5) . ? N11 C18 1.384(6) . ? N12 C12 1.340(6) . ? N12 C13 1.402(6) . ? C11 C12 1.494(6) . ? C13 C14 1.374(8) . ? C13 C18 1.402(7) . ? C14 C15 1.354(8) . ? C15 C16 1.395(9) . ? C16 C17 1.377(8) . ? C17 C18 1.389(6) . ? N21 C22 1.338(5) . ? N21 C28 1.417(6) . ? N22 C23 1.366(7) . ? N22 C22 1.366(6) . ? C21 C22 1.453(7) . ? C23 C24 1.400(8) . ? C23 C28 1.416(6) . ? C24 C25 1.346(9) . ? C25 C26 1.388(8) . ? C26 C27 1.360(8) . ? C27 C28 1.372(6) . ? N31 C32 1.326(6) . ? N31 C38 1.382(6) . ? N32 C32 1.355(6) . ? N32 C33 1.380(6) . ? C31 C32 1.472(7) . ? C33 C38 1.389(6) . ? C33 C34 1.407(8) . ? C34 C35 1.391(9) . ? C35 C36 1.398(8) . ? C36 C37 1.361(8) . ? C37 C38 1.396(6) . ? N2 C44 1.261(8) . ? N2 C40 1.329(9) . ? C40 C41 1.364(8) . ? C41 C42 1.362(10) . ? C42 C43 1.344(9) . ? C42 C46 1.498(7) . ? C42 C45 1.514(7) . ? C43 C44 1.392(7) . ? C45 C45 0.919(14) 2_655 ? C45 C46 0.939(13) . ? C45 C46 1.339(12) 2_655 ? C46 C46 1.003(14) 2_655 ? C46 C45 1.339(12) 2_655 ? N3 C50 1.253(15) . ? N3 C54 1.356(15) . ? C50 C51 1.301(13) . ? C51 C52 1.256(17) . ? C52 C53 1.413(17) . ? C52 C55 1.76(2) . ? C53 C54 1.387(15) . ? C55 C55 1.33(3) 5_656 ? N4 C60 1.298(9) . ? N4 C64 1.312(8) . ? C60 C61 1.378(8) . ? C61 C62 1.340(9) . ? C62 C63 1.292(8) . ? C62 C65 1.487(7) . ? C63 C64 1.424(7) . ? C65 C65 1.247(12) 5_757 ? Cl1 O12 1.385(5) . ? Cl1 O11' 1.406(6) . ? Cl1 O12' 1.417(6) . ? Cl1 O13 1.417(6) . ? Cl1 O11 1.424(7) . ? Cl1 O13' 1.432(7) . ? Cl1 O14 1.450(4) . ? Cl2 O24 1.384(7) . ? Cl2 O24 1.384(7) 7_656 ? Cl2 O23 1.394(6) 7_656 ? Cl2 O23 1.394(6) . ? Cl2 O22 1.443(7) . ? Cl2 O22 1.443(7) 7_656 ? Cl2 O21 1.458(7) . ? Cl2 O21 1.458(7) 7_656 ? O24 O23 1.428(14) 7_656 ? O24 O22 1.611(15) 7_656 ? O24 O21 1.633(13) 7_656 ? O23 O24 1.428(14) 7_656 ? O23 O22 1.622(14) 7_656 ? O23 O21 1.760(14) 7_656 ? O22 O24 1.611(15) 7_656 ? O22 O23 1.622(14) 7_656 ? O22 O21 1.810(17) 7_656 ? O21 O24 1.633(13) 7_656 ? O21 O23 1.760(14) 7_656 ? O21 O22 1.810(17) 7_656 ? 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 N21 Nd1 N21 79.13(16) . 2_655 ? N21 Nd1 N11 75.16(12) . 2_655 ? N21 Nd1 N11 101.88(12) 2_655 2_655 ? N21 Nd1 N11 101.88(12) . . ? N21 Nd1 N11 75.16(12) 2_655 . ? N11 Nd1 N11 176.27(17) 2_655 . ? N21 Nd1 N31 176.21(13) . 2_655 ? N21 Nd1 N31 103.04(12) 2_655 2_655 ? N11 Nd1 N31 101.27(13) 2_655 2_655 ? N11 Nd1 N31 81.74(13) . 2_655 ? N21 Nd1 N31 103.04(12) . . ? N21 Nd1 N31 176.21(13) 2_655 . ? N11 Nd1 N31 81.74(13) 2_655 . ? N11 Nd1 N31 101.27(13) . . ? N31 Nd1 N31 74.96(16) 2_655 . ? N21 Nd1 N1 114.84(11) . 2_655 ? N21 Nd1 N1 63.89(11) 2_655 2_655 ? N11 Nd1 N1 63.74(11) 2_655 2_655 ? N11 Nd1 N1 116.20(11) . 2_655 ? N31 Nd1 N1 63.98(11) 2_655 2_655 ? N31 Nd1 N1 117.34(11) . 2_655 ? N21 Nd1 N1 63.89(11) . . ? N21 Nd1 N1 114.84(11) 2_655 . ? N11 Nd1 N1 116.20(11) 2_655 . ? N11 Nd1 N1 63.74(11) . . ? N31 Nd1 N1 117.34(11) 2_655 . ? N31 Nd1 N1 63.98(11) . . ? N1 Nd1 N1 178.52(15) 2_655 . ? C11 N1 C31 110.5(4) . . ? C11 N1 C21 109.9(3) . . ? C31 N1 C21 109.1(3) . . ? C11 N1 Nd1 109.2(2) . . ? C31 N1 Nd1 109.9(2) . . ? C21 N1 Nd1 108.1(3) . . ? C12 N11 C18 105.4(4) . . ? C12 N11 Nd1 119.0(3) . . ? C18 N11 Nd1 135.4(3) . . ? C12 N12 C13 107.5(4) . . ? N1 C11 C12 108.9(3) . . ? N11 C12 N12 112.7(4) . . ? N11 C12 C11 122.6(4) . . ? N12 C12 C11 124.5(4) . . ? C14 C13 N12 132.2(5) . . ? C14 C13 C18 123.0(5) . . ? N12 C13 C18 104.7(4) . . ? C15 C14 C13 116.2(6) . . ? C14 C15 C16 123.2(6) . . ? C17 C16 C15 119.7(5) . . ? C16 C17 C18 118.9(5) . . ? N11 C18 C17 131.7(5) . . ? N11 C18 C13 109.7(4) . . ? C17 C18 C13 118.7(5) . . ? C22 N21 C28 105.6(3) . . ? C22 N21 Nd1 119.4(3) . . ? C28 N21 Nd1 134.7(2) . . ? C23 N22 C22 108.8(3) . . ? C22 C21 N1 110.8(3) . . ? N21 C22 N22 111.5(4) . . ? N21 C22 C21 123.8(4) . . ? N22 C22 C21 124.6(3) . . ? N22 C23 C24 133.8(4) . . ? N22 C23 C28 105.9(4) . . ? C24 C23 C28 120.2(5) . . ? C25 C24 C23 118.0(5) . . ? C24 C25 C26 121.5(6) . . ? C27 C26 C25 121.8(5) . . ? C26 C27 C28 118.3(4) . . ? C27 C28 N21 131.6(4) . . ? C27 C28 C23 120.1(5) . . ? N21 C28 C23 108.2(4) . . ? C32 N31 C38 106.2(4) . . ? C32 N31 Nd1 118.9(3) . . ? C38 N31 Nd1 134.8(3) . . ? C32 N32 C33 107.6(4) . . ? N1 C31 C32 110.6(4) . . ? N31 C32 N32 111.4(4) . . ? N31 C32 C31 124.8(4) . . ? N32 C32 C31 123.6(4) . . ? N32 C33 C38 105.7(4) . . ? N32 C33 C34 131.6(4) . . ? C38 C33 C34 122.7(5) . . ? C35 C34 C33 116.2(5) . . ? C34 C35 C36 121.2(6) . . ? C37 C36 C35 121.5(5) . . ? C36 C37 C38 119.3(4) . . ? C33 C38 N31 109.1(4) . . ? C33 C38 C37 119.1(5) . . ? N31 C38 C37 131.7(4) . . ? C44 N2 C40 116.8(5) . . ? N2 C40 C41 121.8(7) . . ? C42 C41 C40 121.1(7) . . ? C43 C42 C41 116.3(5) . . ? C43 C42 C46 141.1(6) . . ? C41 C42 C46 102.3(6) . . ? C43 C42 C45 105.9(6) . . ? C41 C42 C45 137.6(7) . . ? C46 C42 C45 36.3(5) . . ? C42 C43 C44 118.8(6) . . ? N2 C44 C43 125.1(6) . . ? C45 C45 C46 92.2(7) 2_655 . ? C45 C45 C46 44.5(5) 2_655 2_655 ? C46 C45 C46 48.5(8) . 2_655 ? C45 C45 C42 160.2(13) 2_655 . ? C46 C45 C42 70.9(6) . . ? C46 C45 C42 119.3(8) 2_655 . ? C45 C46 C46 87.1(6) . 2_655 ? C45 C46 C45 43.3(8) . 2_655 ? C46 C46 C45 44.4(5) 2_655 2_655 ? C45 C46 C42 72.8(6) . . ? C46 C46 C42 159.8(5) 2_655 . ? C45 C46 C42 115.4(7) 2_655 . ? C50 N3 C54 111.0(9) . . ? N3 C50 C51 125.8(12) . . ? C52 C51 C50 129.8(13) . . ? C51 C52 C53 109.5(9) . . ? C51 C52 C55 116.7(12) . . ? C53 C52 C55 133.6(12) . . ? C54 C53 C52 119.5(11) . . ? N3 C54 C53 123.8(11) . . ? C55 C55 C52 90.2(18) 5_656 . ? C60 N4 C64 116.2(5) . . ? N4 C60 C61 122.7(6) . . ? C62 C61 C60 121.4(7) . . ? C63 C62 C61 116.7(5) . . ? C63 C62 C65 124.4(6) . . ? C61 C62 C65 118.8(6) . . ? C62 C63 C64 120.8(6) . . ? N4 C64 C63 121.8(6) . . ? C65 C65 C62 126.5(9) 5_757 . ? O12 Cl1 O11' 126.6(5) . . ? O12 Cl1 O12' 73.2(9) . . ? O11' Cl1 O12' 111.2(8) . . ? O12 Cl1 O13 113.8(6) . . ? O11' Cl1 O13 31.8(6) . . ? O12' Cl1 O13 140.3(9) . . ? O12 Cl1 O11 109.3(5) . . ? O11' Cl1 O11 82.6(6) . . ? O12' Cl1 O11 37.2(9) . . ? O13 Cl1 O11 114.3(6) . . ? O12 Cl1 O13' 34.4(5) . . ? O11' Cl1 O13' 111.2(6) . . ? O12' Cl1 O13' 107.5(8) . . ? O13 Cl1 O13' 86.2(6) . . ? O11 Cl1 O13' 142.6(5) . . ? O12 Cl1 O14 111.7(4) . . ? O11' Cl1 O14 115.7(4) . . ? O12' Cl1 O14 109.4(8) . . ? O13 Cl1 O14 103.8(5) . . ? O11 Cl1 O14 103.4(6) . . ? O13' Cl1 O14 101.2(5) . . ? O24 Cl2 O24 180.000(3) . 7_656 ? O24 Cl2 O23 61.8(6) . 7_656 ? O24 Cl2 O23 118.2(6) 7_656 7_656 ? O24 Cl2 O23 118.2(6) . . ? O24 Cl2 O23 61.8(6) 7_656 . ? O23 Cl2 O23 180.000(3) 7_656 . ? O24 Cl2 O22 110.5(7) . . ? O24 Cl2 O22 69.5(7) 7_656 . ? O23 Cl2 O22 69.7(6) 7_656 . ? O23 Cl2 O22 110.3(6) . . ? O24 Cl2 O22 69.5(7) . 7_656 ? O24 Cl2 O22 110.5(7) 7_656 7_656 ? O23 Cl2 O22 110.3(6) 7_656 7_656 ? O23 Cl2 O22 69.7(6) . 7_656 ? O22 Cl2 O22 180.000(2) . 7_656 ? O24 Cl2 O21 109.9(6) . . ? O24 Cl2 O21 70.1(6) 7_656 . ? O23 Cl2 O21 76.1(6) 7_656 . ? O23 Cl2 O21 103.9(6) . . ? O22 Cl2 O21 102.8(8) . . ? O22 Cl2 O21 77.2(8) 7_656 . ? O24 Cl2 O21 70.1(6) . 7_656 ? O24 Cl2 O21 109.9(6) 7_656 7_656 ? O23 Cl2 O21 103.9(6) 7_656 7_656 ? O23 Cl2 O21 76.1(6) . 7_656 ? O22 Cl2 O21 77.2(8) . 7_656 ? O22 Cl2 O21 102.8(8) 7_656 7_656 ? O21 Cl2 O21 180.000(4) . 7_656 ? Cl2 O24 O23 59.4(5) . 7_656 ? Cl2 O24 O22 57.0(4) . 7_656 ? O23 O24 O22 99.9(8) 7_656 7_656 ? Cl2 O24 O21 57.1(4) . 7_656 ? O23 O24 O21 94.2(8) 7_656 7_656 ? O22 O24 O21 88.7(7) 7_656 7_656 ? Cl2 O23 O24 58.7(4) . 7_656 ? Cl2 O23 O22 56.5(4) . 7_656 ? O24 O23 O22 99.0(8) 7_656 7_656 ? Cl2 O23 O21 53.6(4) . 7_656 ? O24 O23 O21 93.2(7) 7_656 7_656 ? O22 O23 O21 84.1(6) 7_656 7_656 ? Cl2 O22 O24 53.6(5) . 7_656 ? Cl2 O22 O23 53.7(4) . 7_656 ? O24 O22 O23 95.0(8) 7_656 7_656 ? Cl2 O22 O21 51.8(4) . 7_656 ? O24 O22 O21 85.5(6) 7_656 7_656 ? O23 O22 O21 81.6(6) 7_656 7_656 ? Cl2 O21 O24 52.8(4) . 7_656 ? Cl2 O21 O23 50.3(4) . 7_656 ? O24 O21 O23 89.2(6) 7_656 7_656 ? Cl2 O21 O22 51.0(5) . 7_656 ? O24 O21 O22 84.7(7) 7_656 7_656 ? O23 O21 O22 81.4(6) 7_656 7_656 ? _diffrn_measured_fraction_theta_max 0.441 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.441 _refine_diff_density_max 0.832 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.108