# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1758

#
# Article submitted to J. Chem. Soc., Dalton Trans.
#
# 'Crystal structure of
# p-chloro-N-benzyl-hexahomotriazacalix[3]arene 
# and of the complex of its zwitterionic form with neodymium(III) nitrate.'
#
# P. ThuZry et al.
#
data_global

_publ_contact_author
;
      Pierre Thu\'ery
      CEA Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_phone        '16(1)69 08 63 29'
_publ_contact_author_fax          '16(1)69 08 66 40'
_publ_contact_author_email        thuery@drecam.cea.fr
_publ_requested_journal            'J. Chem. Soc., Dalton Trans.'
_publ_requested_coeditor_name     ?
_publ_contact_letter                        ?

data_1
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic         ?
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C45 H42 Cl3 N3 O3' 
_chemical_formula_weight          779.17 
 
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' 
 
_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                    11.9409(10) 
_cell_length_b                    30.824(3) 
_cell_length_c                    10.4671(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  94.297(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      3842(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     123(2) 
_cell_measurement_reflns_used     24486
_cell_measurement_theta_min       2.83 
_cell_measurement_theta_max       25.68
 
_exptl_crystal_description        platelet 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.347 
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1632 
_exptl_absorpt_coefficient_mu     0.285 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ?  
_exptl_special_details 
; 
/f scans with 2/% steps
; 
 
_diffrn_ambient_temperature       123(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   'Nonius Kappa-CCD' 
_diffrn_measurement_method        '\f scans' 
_diffrn_detector_area_resol_mean  18 
_diffrn_standards_decay_%         none 
_diffrn_reflns_number             12342 
_diffrn_reflns_av_R_equivalents   0.107 
_diffrn_reflns_av_sigmaI/netI     0.137 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -35 
_diffrn_reflns_limit_k_max        35 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        0 
_diffrn_reflns_theta_min          2.83 
_diffrn_reflns_theta_max          25.68 
_reflns_number_total              6409 
_reflns_number_gt                 4269 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Kappa-CCD software (Nonius, 1997)' 
_computing_cell_refinement        'HKL package (Otwinowski & Minor, 1997)' 
_computing_data_reduction         'HKL package (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1999)' 
_computing_publication_material   'SHELXTL (Sheldrick, 1999)'  
 
_refine_special_details 
; 
 Structure solved by direct methods. All non-hydrogen atoms refined
 anisotropically. Hydroxyl protons found on the Fourier-difference map
 and introduced as riding atoms with a displacement factor equal to 
 1.2 times that of the attached oxygen atom. All other hydrogen atoms 
 introduced at calculated positions as riding atoms, with a displacement
 factor equal to 1.2 times that of the attached carbon atom.
 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^)+(0.0719P)^2^+1.5679P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6409 
_refine_ls_number_parameters      496 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1069 
_refine_ls_R_factor_gt            0.0670 
_refine_ls_wR_factor_ref          0.1672 
_refine_ls_wR_factor_gt           0.1444 
_refine_ls_goodness_of_fit_ref    0.990 
_refine_ls_restrained_S_all       0.990 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
_diffrn_measured_fraction_theta_max    0.877 
_diffrn_reflns_theta_full              25.68 
_diffrn_measured_fraction_theta_full   0.877 
_refine_diff_density_max    0.477 
_refine_diff_density_min   -0.456 
_refine_diff_density_rms    0.071 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O 0.0988(2) 0.06142(8) 0.9326(2) 0.0306(6) Uani 1 1 d . . . 
H1O H 0.131(3) 0.0539(15) 0.996(4) 0.037 Uiso 1 1 d . . . 
O2 O 0.1044(2) 0.15533(8) 0.9623(2) 0.0301(6) Uani 1 1 d . . . 
H2O H 0.089(3) 0.1344(15) 0.897(4) 0.036 Uiso 1 1 d . . . 
O3 O 0.1685(2) 0.09540(9) 1.1690(2) 0.0308(6) Uani 1 1 d . . . 
H3O H 0.162(3) 0.1261(16) 1.167(3) 0.037 Uiso 1 1 d . . . 
Cl1 Cl 0.19775(9) -0.07163(3) 0.55631(9) 0.0461(3) Uani 1 1 d . . . 
Cl2 Cl 0.51772(8) 0.24408(3) 0.84015(10) 0.0451(3) Uani 1 1 d . . . 
Cl3 Cl 0.46428(9) 0.06004(4) 1.63004(9) 0.0471(3) Uani 1 1 d . . . 
N1 N 0.0826(2) 0.12203(10) 0.7281(3) 0.0284(7) Uani 1 1 d . . . 
N2 N 0.1884(2) 0.17979(10) 1.2252(3) 0.0286(7) Uani 1 1 d . . . 
N3 N 0.2299(2) 0.00780(10) 1.1054(2) 0.0272(6) Uani 1 1 d . . . 
C1 C 0.1210(3) 0.02992(11) 0.8463(3) 0.0263(7) Uani 1 1 d . . . 
C2 C 0.1041(3) 0.03982(12) 0.7159(3) 0.0272(8) Uani 1 1 d . . . 
C3 C 0.1274(3) 0.00781(13) 0.6274(3) 0.0317(8) Uani 1 1 d . . . 
H3 H 0.1178 0.0138 0.5401 0.038 Uiso 1 1 calc R . . 
C4 C 0.1649(3) -0.03284(13) 0.6686(3) 0.0333(8) Uani 1 1 d . . . 
C5 C 0.1774(3) -0.04262(12) 0.7975(3) 0.0335(8) Uani 1 1 d . . . 
H5 H 0.2013 -0.0701 0.8240 0.040 Uiso 1 1 calc R . . 
C6 C 0.1544(3) -0.01156(12) 0.8874(3) 0.0275(8) Uani 1 1 d . . . 
C7 C 0.0502(3) 0.08127(12) 0.6628(3) 0.0326(8) Uani 1 1 d . . . 
H7A H 0.0670 0.0839 0.5740 0.039 Uiso 1 1 calc R . . 
H7B H -0.0306 0.0781 0.6637 0.039 Uiso 1 1 calc R . . 
C8 C 0.0156(3) 0.15819(13) 0.6689(3) 0.0328(8) Uani 1 1 d . . . 
H8A H 0.0282 0.1595 0.5785 0.039 Uiso 1 1 calc R . . 
H8B H 0.0422 0.1852 0.7077 0.039 Uiso 1 1 calc R . . 
C9 C -0.1083(3) 0.15434(12) 0.6825(3) 0.0305(8) Uani 1 1 d . . . 
C10 C -0.1834(3) 0.16814(13) 0.5834(4) 0.0363(9) Uani 1 1 d . . . 
H10 H -0.1564 0.1787 0.5084 0.044 Uiso 1 1 calc R . . 
C11 C -0.2983(4) 0.16634(15) 0.5949(4) 0.0455(10) Uani 1 1 d . . . 
H11 H -0.3477 0.1759 0.5279 0.055 Uiso 1 1 calc R . . 
C12\ C -0.3393(4) 0.15063(15) 0.7040(4) 0.0463(10) Uani 1 1 d . . . 
H12\ H -0.4164 0.1498 0.7115 0.056 Uiso 1 1 calc R . . 
C13 C -0.2664(4) 0.13603(15) 0.8029(4) 0.0448(10) Uani 1 1 d . . . 
H13 H -0.2943 0.1246 0.8763 0.054 Uiso 1 1 calc R . . 
C14 C -0.1517(3) 0.13845(14) 0.7930(4) 0.0399(9) Uani 1 1 d . . . 
H14 H -0.1030 0.1293 0.8612 0.048 Uiso 1 1 calc R . . 
C15 C 0.2035(3) 0.13022(12) 0.7241(3) 0.0318(8) Uani 1 1 d . . . 
H15A H 0.2186 0.1381 0.6373 0.038 Uiso 1 1 calc R . . 
H15B H 0.2440 0.1036 0.7457 0.038 Uiso 1 1 calc R . . 
C16 C 0.2480(3) 0.16594(12) 0.8146(3) 0.0300(8) Uani 1 1 d . . . 
C17 C 0.1992(3) 0.17509(12) 0.9295(3) 0.0281(8) Uani 1 1 d . . . 
C18 C 0.2472(3) 0.20624(11) 1.0158(3) 0.0284(8) Uani 1 1 d . . . 
C19 C 0.3463(3) 0.22651(12) 0.9877(3) 0.0324(8) Uani 1 1 d . . . 
H19 H 0.3808 0.2461 1.0456 0.039 Uiso 1 1 calc R . . 
C20 C 0.3939(3) 0.21782(12) 0.8746(3) 0.0337(8) Uani 1 1 d . . . 
C21 C 0.3443(3) 0.18803(12) 0.7872(3) 0.0312(8) Uani 1 1 d . . . 
H21 H 0.3762 0.1830 0.7102 0.037 Uiso 1 1 calc R . . 
C22 C 0.1907(3) 0.21680(12) 1.1360(3) 0.0303(8) Uani 1 1 d . . . 
H22A H 0.2299 0.2408 1.1793 0.036 Uiso 1 1 calc R . . 
H22B H 0.1143 0.2260 1.1126 0.036 Uiso 1 1 calc R . . 
C23 C 0.1195(3) 0.18961(13) 1.3329(3) 0.0363(9) Uani 1 1 d . . . 
H23A H 0.1498 0.2151 1.3776 0.044 Uiso 1 1 calc R . . 
H23B H 0.1244 0.1655 1.3927 0.044 Uiso 1 1 calc R . . 
C24 C -0.0024(3) 0.19763(12) 1.2905(3) 0.0343(9) Uani 1 1 d . . . 
C25 C -0.0574(4) 0.23518(12) 1.3271(4) 0.0391(9) Uani 1 1 d . . . 
H25 H -0.0178 0.2559 1.3768 0.047 Uiso 1 1 calc R . . 
C26 C -0.1692(4) 0.24198(14) 1.2908(4) 0.0453(10) Uani 1 1 d . . . 
H26 H -0.2047 0.2669 1.3175 0.054 Uiso 1 1 calc R . . 
C27 C -0.2291(4) 0.21193(16) 1.2147(5) 0.0518(11) Uani 1 1 d . . . 
H27 H -0.3042 0.2167 1.1885 0.062 Uiso 1 1 calc R . . 
C28 C -0.1744(4) 0.17410(17) 1.1778(5) 0.0557(12) Uani 1 1 d . . . 
H28 H -0.2136 0.1536 1.1269 0.067 Uiso 1 1 calc R . . 
C29 C -0.0641(4) 0.16722(15) 1.2163(4) 0.0469(10) Uani 1 1 d . . . 
H29 H -0.0295 0.1417 1.1926 0.056 Uiso 1 1 calc R . . 
C30 C 0.3019(3) 0.16669(12) 1.2753(3) 0.0311(8) Uani 1 1 d . . . 
H30A H 0.3302 0.1875 1.3394 0.037 Uiso 1 1 calc R . . 
H30B H 0.3516 0.1671 1.2061 0.037 Uiso 1 1 calc R . . 
C31 C 0.3036(3) 0.12215(12) 1.3340(3) 0.0293(8) Uani 1 1 d . . . 
C32 C 0.2413(3) 0.08801(12) 1.2737(3) 0.0281(8) Uani 1 1 d . . . 
C33 C 0.2550(3) 0.04522(12) 1.3150(3) 0.0292(8) Uani 1 1 d . . . 
C34 C 0.3248(3) 0.03680(12) 1.4252(3) 0.0315(8) Uani 1 1 d . . . 
H34 H 0.3332 0.0086 1.4560 0.038 Uiso 1 1 calc R . . 
C35 C 0.3816(3) 0.07055(13) 1.4884(3) 0.0320(8) Uani 1 1 d . . . 
C36 C 0.3730(3) 0.11259(13) 1.4435(3) 0.0330(8) Uani 1 1 d . . . 
H36 H 0.4135 0.1346 1.4863 0.040 Uiso 1 1 calc R . . 
C37 C 0.1973(3) 0.00889(12) 1.2391(3) 0.0304(8) Uani 1 1 d . . . 
H37A H 0.2167 -0.0186 1.2803 0.036 Uiso 1 1 calc R . . 
H37B H 0.1166 0.0126 1.2387 0.036 Uiso 1 1 calc R . . 
C38 C 0.3512(3) -0.00082(13) 1.0974(3) 0.0311(8) Uani 1 1 d . . . 
H38A H 0.3611 -0.0178 1.0210 0.037 Uiso 1 1 calc R . . 
H38B H 0.3783 -0.0181 1.1709 0.037 Uiso 1 1 calc R . . 
C39 C 0.4211(3) 0.03986(12) 1.0935(3) 0.0292(8) Uani 1 1 d . . . 
C40 C 0.4057(3) 0.06754(15) 0.9898(4) 0.0425(10) Uani 1 1 d . . . 
H40 H 0.3539 0.0604 0.9222 0.051 Uiso 1 1 calc R . . 
C41 C 0.4659(3) 0.10537(16) 0.9855(5) 0.0531(12) Uani 1 1 d . . . 
H41 H 0.4568 0.1231 0.9135 0.064 Uiso 1 1 calc R . . 
C42 C 0.5397(3) 0.11735(15) 1.0870(5) 0.0510(11) Uani 1 1 d . . . 
H42 H 0.5773 0.1437 1.0853 0.061 Uiso 1 1 calc R . . 
C43 C 0.5574(3) 0.09027(15) 1.1903(4) 0.0441(10) Uani 1 1 d . . . 
H43 H 0.6078 0.0980 1.2586 0.053 Uiso 1 1 calc R . . 
C44 C 0.4999(3) 0.05123(14) 1.1927(3) 0.0358(9) Uani 1 1 d . . . 
H44 H 0.5141 0.0324 1.2614 0.043 Uiso 1 1 calc R . . 
C45 C 0.1595(3) -0.02287(12) 1.0289(3) 0.0300(8) Uani 1 1 d . . . 
H45A H 0.0842 -0.0226 1.0578 0.036 Uiso 1 1 calc R . . 
H45B H 0.1895 -0.0519 1.0415 0.036 Uiso 1 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
O1 0.0416(16) 0.0239(14) 0.0263(13) -0.0013(10) 0.0014(10) 0.0035(11) 
O2 0.0336(15) 0.0249(14) 0.0325(13) -0.0015(10) 0.0063(10) -0.0051(11) 
O3 0.0400(16) 0.0220(14) 0.0294(13) 0.0023(9) -0.0031(10) 0.0015(11) 
Cl1 0.0665(7) 0.0334(6) 0.0369(5) -0.0099(4) -0.0050(4) 0.0112(5) 
Cl2 0.0362(6) 0.0362(6) 0.0642(6) 0.0002(4) 0.0135(4) -0.0070(4) 
Cl3 0.0596(7) 0.0398(6) 0.0391(5) 0.0032(4) -0.0154(4) 0.0028(5) 
N1 0.0308(17) 0.0234(17) 0.0310(15) 0.0023(11) 0.0028(11) 0.0034(12) 
N2 0.0297(17) 0.0264(17) 0.0297(15) 0.0013(11) 0.0036(11) 0.0036(13) 
N3 0.0301(17) 0.0219(17) 0.0292(15) -0.0004(11) -0.0006(11) -0.0016(12) 
C1 0.0226(19) 0.0205(19) 0.0361(19) -0.0022(13) 0.0030(13) -0.0034(14) 
C2 0.0256(19) 0.026(2) 0.0292(19) 0.0003(13) -0.0003(13) -0.0008(15) 
C3 0.032(2) 0.037(2) 0.0264(17) -0.0027(14) 0.0009(13) 0.0001(16) 
C4 0.037(2) 0.029(2) 0.034(2) -0.0067(14) -0.0020(15) -0.0023(16) 
C5 0.038(2) 0.020(2) 0.041(2) -0.0013(14) -0.0037(15) 0.0020(15) 
C6 0.0273(19) 0.024(2) 0.0313(18) 0.0002(13) 0.0015(13) -0.0052(14) 
C7 0.038(2) 0.028(2) 0.0309(19) -0.0014(14) -0.0010(14) 0.0033(16) 
C8 0.044(2) 0.028(2) 0.0274(18) 0.0055(13) 0.0049(14) 0.0030(16) 
C9 0.031(2) 0.022(2) 0.038(2) -0.0028(14) 0.0010(15) 0.0035(15) 
C10 0.040(2) 0.029(2) 0.039(2) 0.0003(15) -0.0007(15) 0.0056(17) 
C11 0.042(3) 0.044(3) 0.049(2) -0.0013(18) -0.0071(18) 0.0012(19) 
C12\ 0.029(2) 0.039(3) 0.070(3) -0.007(2) 0.0025(19) 0.0025(18) 
C13 0.040(3) 0.039(3) 0.056(2) 0.0056(18) 0.0107(18) 0.0018(19) 
C14 0.034(2) 0.043(3) 0.042(2) 0.0108(17) 0.0044(16) 0.0049(18) 
C15 0.031(2) 0.029(2) 0.0352(19) -0.0034(14) 0.0049(14) 0.0055(16) 
C16 0.030(2) 0.029(2) 0.0307(18) 0.0041(14) 0.0015(14) 0.0044(15) 
C17 0.027(2) 0.027(2) 0.0306(18) 0.0052(14) 0.0013(13) 0.0015(15) 
C18 0.032(2) 0.022(2) 0.0309(18) 0.0035(13) 0.0021(14) 0.0024(15) 
C19 0.031(2) 0.024(2) 0.041(2) 0.0031(14) -0.0018(15) -0.0022(15) 
C20 0.035(2) 0.024(2) 0.042(2) 0.0085(15) 0.0034(15) -0.0001(16) 
C21 0.032(2) 0.029(2) 0.0330(19) 0.0060(14) 0.0043(14) 0.0050(16) 
C22 0.037(2) 0.021(2) 0.0333(18) 0.0010(13) 0.0030(14) 0.0014(15) 
C23 0.046(2) 0.032(2) 0.0318(19) -0.0010(15) 0.0083(15) 0.0053(17) 
C24 0.044(2) 0.026(2) 0.034(2) 0.0025(14) 0.0108(15) 0.0042(16) 
C25 0.058(3) 0.020(2) 0.041(2) 0.0010(14) 0.0125(17) 0.0032(18) 
C26 0.046(3) 0.032(2) 0.060(3) 0.0053(18) 0.0139(19) 0.0101(19) 
C27 0.035(2) 0.046(3) 0.074(3) 0.004(2) 0.004(2) 0.005(2) 
C28 0.040(3) 0.047(3) 0.080(3) -0.013(2) 0.007(2) 0.000(2) 
C29 0.038(2) 0.033(3) 0.071(3) -0.012(2) 0.0101(19) 0.0014(18) 
C30 0.032(2) 0.031(2) 0.0310(18) -0.0012(14) 0.0045(14) -0.0009(16) 
C31 0.033(2) 0.026(2) 0.0298(18) -0.0006(13) 0.0082(14) 0.0033(15) 
C32 0.032(2) 0.028(2) 0.0241(18) 0.0017(13) 0.0043(13) 0.0016(15) 
C33 0.033(2) 0.029(2) 0.0272(18) 0.0019(13) 0.0075(14) 0.0004(15) 
C34 0.037(2) 0.029(2) 0.0285(19) 0.0036(14) 0.0051(14) 0.0017(16) 
C35 0.033(2) 0.037(2) 0.0252(18) 0.0023(14) 0.0019(14) 0.0030(17) 
C36 0.037(2) 0.032(2) 0.0293(19) -0.0051(14) 0.0016(14) 0.0002(16) 
C37 0.034(2) 0.023(2) 0.0341(19) 0.0020(14) 0.0033(14) -0.0015(15) 
C38 0.032(2) 0.028(2) 0.0331(19) -0.0020(14) 0.0029(14) 0.0004(15) 
C39 0.0243(19) 0.029(2) 0.0343(19) 0.0010(14) 0.0027(13) 0.0016(15) 
C40 0.032(2) 0.047(3) 0.047(2) 0.0174(18) -0.0021(16) 0.0008(18) 
C41 0.029(2) 0.051(3) 0.078(3) 0.032(2) -0.004(2) -0.001(2) 
C42 0.027(2) 0.031(2) 0.096(3) 0.002(2) 0.010(2) -0.0018(18) 
C43 0.033(2) 0.049(3) 0.051(2) -0.0143(19) 0.0072(17) -0.0068(19) 
C44 0.030(2) 0.044(3) 0.034(2) 0.0035(15) 0.0051(15) -0.0017(17) 
C45 0.036(2) 0.022(2) 0.0318(19) 0.0008(13) 0.0021(14) -0.0011(15) 
 
_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 
O1 C1 1.366(4) . ? 
O2 C17 1.352(4) . ? 
O3 C32 1.366(4) . ? 
Cl1 C4 1.742(4) . ? 
Cl2 C20 1.747(4) . ? 
Cl3 C35 1.749(3) . ? 
N1 C7 1.468(5) . ? 
N1 C15 1.469(5) . ? 
N1 C8 1.481(5) . ? 
N2 C30 1.472(5) . ? 
N2 C23 1.476(4) . ? 
N2 C22 1.476(4) . ? 
N3 C45 1.463(4) . ? 
N3 C37 1.480(4) . ? 
N3 C38 1.481(5) . ? 
C1 C2 1.399(5) . ? 
C1 C6 1.398(5) . ? 
C2 C3 1.396(5) . ? 
C2 C7 1.517(5) . ? 
C3 C4 1.388(6) . ? 
C4 C5 1.380(5) . ? 
C5 C6 1.384(5) . ? 
C6 C45 1.518(5) . ? 
C8 C9 1.502(5) . ? 
C9 C10 1.386(5) . ? 
C9 C14 1.392(5) . ? 
C10 C11 1.388(6) . ? 
C11 C12\ 1.364(6) . ? 
C12\ C13 1.378(6) . ? 
C13 C14 1.383(6) . ? 
C15 C16 1.522(5) . ? 
C16 C21 1.385(5) . ? 
C16 C17 1.403(5) . ? 
C17 C18 1.411(5) . ? 
C18 C19 1.389(5) . ? 
C18 C22 1.506(5) . ? 
C19 C20 1.377(5) . ? 
C20 C21 1.396(5) . ? 
C23 C24 1.510(5) . ? 
C24 C29 1.393(6) . ? 
C24 C25 1.398(5) . ? 
C25 C26 1.376(6) . ? 
C26 C27 1.385(6) . ? 
C27 C28 1.405(7) . ? 
C28 C29 1.364(6) . ? 
C30 C31 1.503(5) . ? 
C31 C36 1.394(5) . ? 
C31 C32 1.410(5) . ? 
C32 C33 1.394(5) . ? 
C33 C34 1.396(5) . ? 
C33 C37 1.509(5) . ? 
C34 C35 1.383(5) . ? 
C35 C36 1.380(5) . ? 
C38 C39 1.509(5) . ? 
C39 C40 1.382(5) . ? 
C39 C44 1.392(5) . ? 
C40 C41 1.372(6) . ? 
C41 C42 1.379(6) . ? 
C42 C43 1.370(6) . ? 
C43 C44 1.387(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 
C7 N1 C15 111.1(3) . . ? 
C7 N1 C8 109.5(3) . . ? 
C15 N1 C8 111.1(3) . . ? 
C30 N2 C23 109.6(3) . . ? 
C30 N2 C22 112.2(3) . . ? 
C23 N2 C22 111.3(3) . . ? 
C45 N3 C37 110.6(3) . . ? 
C45 N3 C38 112.2(3) . . ? 
C37 N3 C38 112.6(3) . . ? 
O1 C1 C2 118.0(3) . . ? 
O1 C1 C6 120.8(3) . . ? 
C2 C1 C6 121.1(3) . . ? 
C3 C2 C1 118.2(3) . . ? 
C3 C2 C7 116.9(3) . . ? 
C1 C2 C7 124.5(3) . . ? 
C4 C3 C2 120.5(3) . . ? 
C5 C4 C3 120.6(3) . . ? 
C5 C4 Cl1 119.8(3) . . ? 
C3 C4 Cl1 119.6(3) . . ? 
C4 C5 C6 120.1(3) . . ? 
C5 C6 C1 119.3(3) . . ? 
C5 C6 C45 120.6(3) . . ? 
C1 C6 C45 120.0(3) . . ? 
N1 C7 C2 117.4(3) . . ? 
N1 C8 C9 113.9(3) . . ? 
C10 C9 C14 118.0(3) . . ? 
C10 C9 C8 119.4(3) . . ? 
C14 C9 C8 122.5(3) . . ? 
C9 C10 C11 120.7(4) . . ? 
C12\ C11 C10 120.4(4) . . ? 
C11 C12\ C13 119.9(4) . . ? 
C12\ C13 C14 120.0(4) . . ? 
C13 C14 C9 120.9(4) . . ? 
N1 C15 C16 113.9(3) . . ? 
C21 C16 C17 118.9(3) . . ? 
C21 C16 C15 118.9(3) . . ? 
C17 C16 C15 122.0(3) . . ? 
O2 C17 C16 122.4(3) . . ? 
O2 C17 C18 116.9(3) . . ? 
C16 C17 C18 120.7(3) . . ? 
C19 C18 C17 118.8(3) . . ? 
C19 C18 C22 121.5(3) . . ? 
C17 C18 C22 119.7(3) . . ? 
C20 C19 C18 120.5(3) . . ? 
C19 C20 C21 120.6(3) . . ? 
C19 C20 Cl2 119.8(3) . . ? 
C21 C20 Cl2 119.6(3) . . ? 
C16 C21 C20 120.4(3) . . ? 
N2 C22 C18 113.1(3) . . ? 
N2 C23 C24 113.0(3) . . ? 
C29 C24 C25 118.0(4) . . ? 
C29 C24 C23 120.8(3) . . ? 
C25 C24 C23 121.2(4) . . ? 
C26 C25 C24 121.1(4) . . ? 
C25 C26 C27 120.4(4) . . ? 
C26 C27 C28 118.8(4) . . ? 
C29 C28 C27 120.4(4) . . ? 
C28 C29 C24 121.3(4) . . ? 
N2 C30 C31 112.3(3) . . ? 
C36 C31 C32 118.1(3) . . ? 
C36 C31 C30 121.2(3) . . ? 
C32 C31 C30 120.5(3) . . ? 
O3 C32 C33 117.3(3) . . ? 
O3 C32 C31 121.2(3) . . ? 
C33 C32 C31 121.4(3) . . ? 
C32 C33 C34 118.8(3) . . ? 
C32 C33 C37 120.0(3) . . ? 
C34 C33 C37 121.2(3) . . ? 
C35 C34 C33 119.8(4) . . ? 
C36 C35 C34 121.5(3) . . ? 
C36 C35 Cl3 119.1(3) . . ? 
C34 C35 Cl3 119.4(3) . . ? 
C35 C36 C31 120.2(3) . . ? 
N3 C37 C33 111.9(3) . . ? 
N3 C38 C39 113.5(3) . . ? 
C40 C39 C44 118.2(4) . . ? 
C40 C39 C38 119.5(3) . . ? 
C44 C39 C38 122.2(3) . . ? 
C41 C40 C39 120.7(4) . . ? 
C40 C41 C42 120.6(4) . . ? 
C43 C42 C41 119.8(4) . . ? 
C42 C43 C44 119.7(4) . . ? 
C43 C44 C39 120.9(3) . . ? 
N3 C45 C6 111.4(3) . . ? 

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 
O1 C1 C2 C3 179.6(3) . . . . ? 
C6 C1 C2 C3 -3.4(5) . . . . ? 
O1 C1 C2 C7 -7.4(5) . . . . ? 
C6 C1 C2 C7 169.6(3) . . . . ? 
C1 C2 C3 C4 0.8(5) . . . . ? 
C7 C2 C3 C4 -172.7(3) . . . . ? 
C2 C3 C4 C5 1.4(6) . . . . ? 
C2 C3 C4 Cl1 -177.9(3) . . . . ? 
C3 C4 C5 C6 -1.2(6) . . . . ? 
Cl1 C4 C5 C6 178.2(3) . . . . ? 
C4 C5 C6 C1 -1.4(5) . . . . ? 
C4 C5 C6 C45 175.4(3) . . . . ? 
O1 C1 C6 C5 -179.4(3) . . . . ? 
C2 C1 C6 C5 3.7(5) . . . . ? 
O1 C1 C6 C45 3.8(5) . . . . ? 
C2 C1 C6 C45 -173.1(3) . . . . ? 
C15 N1 C7 C2 61.0(4) . . . . ? 
C8 N1 C7 C2 -175.9(3) . . . . ? 
C3 C2 C7 N1 -144.8(3) . . . . ? 
C1 C2 C7 N1 42.1(5) . . . . ? 
C7 N1 C8 C9 63.4(4) . . . . ? 
C15 N1 C8 C9 -173.6(3) . . . . ? 
N1 C8 C9 C10 -144.0(3) . . . . ? 
N1 C8 C9 C14 37.9(5) . . . . ? 
C14 C9 C10 C11 0.4(6) . . . . ? 
C8 C9 C10 C11 -177.8(4) . . . . ? 
C9 C10 C11 C12\ -0.5(6) . . . . ? 
C10 C11 C12\ C13 -0.6(7) . . . . ? 
C11 C12\ C13 C14 1.8(7) . . . . ? 
C12\ C13 C14 C9 -1.9(6) . . . . ? 
C10 C9 C14 C13 0.8(6) . . . . ? 
C8 C9 C14 C13 178.9(4) . . . . ? 
C7 N1 C15 C16 -166.8(3) . . . . ? 
C8 N1 C15 C16 71.1(4) . . . . ? 
N1 C15 C16 C21 -155.4(3) . . . . ? 
N1 C15 C16 C17 29.2(5) . . . . ? 
C21 C16 C17 O2 179.1(3) . . . . ? 
C15 C16 C17 O2 -5.5(5) . . . . ? 
C21 C16 C17 C18 0.0(5) . . . . ? 
C15 C16 C17 C18 175.4(3) . . . . ? 
O2 C17 C18 C19 178.3(3) . . . . ? 
C16 C17 C18 C19 -2.5(5) . . . . ? 
O2 C17 C18 C22 -1.6(5) . . . . ? 
C16 C17 C18 C22 177.5(3) . . . . ? 
C17 C18 C19 C20 3.0(5) . . . . ? 
C22 C18 C19 C20 -177.1(3) . . . . ? 
C18 C19 C20 C21 -1.0(6) . . . . ? 
C18 C19 C20 Cl2 179.3(3) . . . . ? 
C17 C16 C21 C20 2.1(5) . . . . ? 
C15 C16 C21 C20 -173.4(3) . . . . ? 
C19 C20 C21 C16 -1.7(5) . . . . ? 
Cl2 C20 C21 C16 178.1(3) . . . . ? 
C30 N2 C22 C18 64.4(4) . . . . ? 
C23 N2 C22 C18 -172.4(3) . . . . ? 
C19 C18 C22 N2 -115.2(4) . . . . ? 
C17 C18 C22 N2 64.8(4) . . . . ? 
C30 N2 C23 C24 -172.5(3) . . . . ? 
C22 N2 C23 C24 62.9(4) . . . . ? 
N2 C23 C24 C29 54.3(5) . . . . ? 
N2 C23 C24 C25 -127.3(4) . . . . ? 
C29 C24 C25 C26 -0.1(6) . . . . ? 
C23 C24 C25 C26 -178.5(3) . . . . ? 
C24 C25 C26 C27 -1.3(6) . . . . ? 
C25 C26 C27 C28 1.4(7) . . . . ? 
C26 C27 C28 C29 -0.1(7) . . . . ? 
C27 C28 C29 C24 -1.3(8) . . . . ? 
C25 C24 C29 C28 1.4(7) . . . . ? 
C23 C24 C29 C28 179.8(4) . . . . ? 
C23 N2 C30 C31 72.6(4) . . . . ? 
C22 N2 C30 C31 -163.3(3) . . . . ? 
N2 C30 C31 C36 -142.5(3) . . . . ? 
N2 C30 C31 C32 42.4(4) . . . . ? 
C36 C31 C32 O3 177.4(3) . . . . ? 
C30 C31 C32 O3 -7.4(5) . . . . ? 
C36 C31 C32 C33 -5.3(5) . . . . ? 
C30 C31 C32 C33 169.9(3) . . . . ? 
O3 C32 C33 C34 -177.1(3) . . . . ? 
C31 C32 C33 C34 5.5(5) . . . . ? 
O3 C32 C33 C37 4.6(5) . . . . ? 
C31 C32 C33 C37 -172.8(3) . . . . ? 
C32 C33 C34 C35 -2.1(5) . . . . ? 
C37 C33 C34 C35 176.3(3) . . . . ? 
C33 C34 C35 C36 -1.5(5) . . . . ? 
C33 C34 C35 Cl3 177.4(3) . . . . ? 
C34 C35 C36 C31 1.7(5) . . . . ? 
Cl3 C35 C36 C31 -177.1(3) . . . . ? 
C32 C31 C36 C35 1.6(5) . . . . ? 
C30 C31 C36 C35 -173.6(3) . . . . ? 
C45 N3 C37 C33 -170.7(3) . . . . ? 
C38 N3 C37 C33 62.9(4) . . . . ? 
C32 C33 C37 N3 58.0(4) . . . . ? 
C34 C33 C37 N3 -120.3(3) . . . . ? 
C45 N3 C38 C39 141.9(3) . . . . ? 
C37 N3 C38 C39 -92.6(3) . . . . ? 
N3 C38 C39 C40 -65.1(4) . . . . ? 
N3 C38 C39 C44 113.5(4) . . . . ? 
C44 C39 C40 C41 -0.5(6) . . . . ? 
C38 C39 C40 C41 178.1(4) . . . . ? 
C39 C40 C41 C42 -2.6(7) . . . . ? 
C40 C41 C42 C43 3.3(7) . . . . ? 
C41 C42 C43 C44 -0.8(6) . . . . ? 
C42 C43 C44 C39 -2.4(6) . . . . ? 
C40 C39 C44 C43 3.0(5) . . . . ? 
C38 C39 C44 C43 -175.6(3) . . . . ? 
C37 N3 C45 C6 155.7(3) . . . . ? 
C38 N3 C45 C6 -77.7(4) . . . . ? 
C5 C6 C45 N3 128.5(3) . . . . ? 
C1 C6 C45 N3 -54.7(4) . . . . ? 

#####################################
# END

data_2

_audit_creation_method            SHELXL-97 
_chemical_name_systematic         ?
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C50 H47 Cl3 N7 Nd O12' 
_chemical_formula_weight          1188.54 
 
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    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                    12.8151(6) 
_cell_length_b                    14.1674(9) 
_cell_length_c                    27.8909(18) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.938(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5002(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     34280 
_cell_measurement_theta_min       5.14 
_cell_measurement_theta_max       25.68

_exptl_crystal_description        platelet 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.35
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.578 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2412 
_exptl_absorpt_coefficient_mu     1.269 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.650 
_exptl_absorpt_correction_T_max   0.737 
_exptl_absorpt_process_details    'MULABS (Spek, 1997)'  
_exptl_special_details 
;
/f scans with 2/% steps
;
_diffrn_ambient_temperature       100(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   'Nonius Kappa-CCD' 
_diffrn_measurement_method        '\f scans' 
_diffrn_detector_area_resol_mean  18 
_diffrn_standards_decay_%         none 
_diffrn_reflns_number             29856 
_diffrn_reflns_av_R_equivalents   0.0940 
_diffrn_reflns_av_sigmaI/netI     0.0808 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -33 
_diffrn_reflns_limit_l_max        33 
_diffrn_reflns_theta_min          5.14 
_diffrn_reflns_theta_max          25.68 
_reflns_number_total              9210 
_reflns_number_gt                 6995 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Kappa-CCD software (Nonius, 1997)' 
_computing_cell_refinement        'HKL package (Otwinowski & Minor, 1997)' 
_computing_data_reduction         'HKL package (Otwinowski & Minor, 1997)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1999)' 
_computing_publication_material   'SHELXTL (Sheldrick, 1999)'  

_refine_special_details 
;
 Structure solved by direct methods. All non-hydrogen atoms refined 
 anisotropically. Protons bonded to nitrogen atoms of the calixarene
 found on the Fourier difference map and introduced as riding atoms 
 with a displacement factor equal to 1.2 times that of the parent atom.
 Other hydrogen atoms introduced at calculated positions
 as riding atoms with a displacement
 factor equal to 1.2 times that of the attached carbon atom. Higher 
 electronic residual density located near the neodymium atom as a
 result of imperfect absorption correction. Other peaks lower than 
 0.8 e A-3. 
 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^)+(0.0358P)^2^+28.5311P] 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        0.0027(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          9210 
_refine_ls_number_parameters      659 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0852 
_refine_ls_R_factor_gt            0.0593 
_refine_ls_wR_factor_ref          0.1338 
_refine_ls_wR_factor_gt           0.1234 
_refine_ls_goodness_of_fit_ref    1.048 
_refine_ls_restrained_S_all       1.048 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000  
_diffrn_measured_fraction_theta_max    0.969 
_diffrn_reflns_theta_full              25.68 
_diffrn_measured_fraction_theta_full   0.969 
_refine_diff_density_max    2.624 
_refine_diff_density_min   -1.271 
_refine_diff_density_rms    0.127 

loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Nd Nd 0.46717(2) 0.24175(2) 0.229533(12) 0.01742(13) Uani 1 1 d . . . 
O1 O 0.4934(3) 0.3842(3) 0.27166(16) 0.0208(9) Uani 1 1 d . . . 
O2 O 0.3536(3) 0.2125(3) 0.28397(16) 0.0218(9) Uani 1 1 d . . . 
O3 O 0.5878(3) 0.2061(3) 0.30194(16) 0.0196(9) Uani 1 1 d . . . 
O4 O 0.6390(3) 0.2923(3) 0.20060(16) 0.0236(10) Uani 1 1 d . . . 
O5 O 0.5105(3) 0.2548(3) 0.14397(16) 0.0272(10) Uani 1 1 d . . . 
O6 O 0.6663(4) 0.2860(3) 0.12532(18) 0.0330(11) Uani 1 1 d . . . 
O7 O 0.3269(3) 0.3509(3) 0.18183(17) 0.0281(11) Uani 1 1 d . . . 
O8 O 0.2993(3) 0.2021(3) 0.16814(17) 0.0274(10) Uani 1 1 d . . . 
O9 O 0.1870(4) 0.3052(4) 0.1327(2) 0.0459(14) Uani 1 1 d . . . 
O10 O 0.4258(3) 0.0653(3) 0.21792(17) 0.0256(10) Uani 1 1 d . . . 
O11 O 0.5839(3) 0.1007(3) 0.20723(17) 0.0265(10) Uani 1 1 d . . . 
O12 O 0.5252(4) -0.0424(3) 0.19171(19) 0.0324(12) Uani 1 1 d . . . 
N1 N 0.2981(4) 0.4221(4) 0.30703(19) 0.0219(11) Uani 1 1 d . . . 
H1N H 0.3493 0.3827 0.3035 0.026 Uiso 1 1 d R . . 
N2 N 0.4931(4) 0.0771(3) 0.35304(18) 0.0182(11) Uani 1 1 d . . . 
H2N H 0.5011 0.1355 0.3381 0.022 Uiso 1 1 d R . . 
N3 N 0.7064(4) 0.3689(3) 0.31400(19) 0.0187(11) Uani 1 1 d . . . 
H3N H 0.6431 0.3370 0.3064 0.022 Uiso 1 1 d R . . 
N4 N 0.6078(4) 0.2781(3) 0.1560(2) 0.0232(12) Uani 1 1 d . . . 
N5 N 0.2683(4) 0.2860(4) 0.1601(2) 0.0278(13) Uani 1 1 d . . . 
N6 N 0.5126(4) 0.0387(4) 0.20503(19) 0.0231(12) Uani 1 1 d . . . 
Cl1 Cl 0.54552(14) 0.79414(11) 0.29483(8) 0.0352(4) Uani 1 1 d . . . 
Cl2 Cl 0.08736(14) 0.16693(13) 0.43499(7) 0.0340(4) Uani 1 1 d . . . 
Cl3 Cl 0.97952(12) -0.01180(11) 0.35183(7) 0.0295(4) Uani 1 1 d . . . 
C1 C 0.5061(5) 0.4776(4) 0.2774(2) 0.0187(13) Uani 1 1 d . . . 
C2 C 0.4174(5) 0.5370(4) 0.2764(2) 0.0191(13) Uani 1 1 d . . . 
C3 C 0.4306(5) 0.6338(4) 0.2820(2) 0.0221(14) Uani 1 1 d . . . 
H3 H 0.3719 0.6729 0.2810 0.027 Uiso 1 1 calc R . . 
C4 C 0.5308(5) 0.6722(4) 0.2892(2) 0.0207(13) Uani 1 1 d . . . 
C5 C 0.6194(5) 0.6156(4) 0.2920(2) 0.0224(14) Uani 1 1 d . . . 
H5 H 0.6864 0.6424 0.2982 0.027 Uiso 1 1 calc R . . 
C6 C 0.6083(5) 0.5176(4) 0.2856(2) 0.0179(12) Uani 1 1 d . . . 
C7 C 0.3106(5) 0.4937(4) 0.2679(2) 0.0204(13) Uani 1 1 d . . . 
H7A H 0.2995 0.4628 0.2364 0.025 Uiso 1 1 calc R . . 
H7B H 0.2576 0.5426 0.2675 0.025 Uiso 1 1 calc R . . 
C8 C 0.2904(5) 0.4683(5) 0.3554(2) 0.0270(15) Uani 1 1 d . . . 
H8A H 0.2640 0.5321 0.3495 0.032 Uiso 1 1 calc R . . 
H8B H 0.2394 0.4338 0.3708 0.032 Uiso 1 1 calc R . . 
C9 C 0.3924(5) 0.4723(5) 0.3894(2) 0.0280(15) Uani 1 1 d . . . 
C10 C 0.4366(6) 0.3895(5) 0.4111(3) 0.0335(16) Uani 1 1 d . . . 
H10 H 0.4035 0.3318 0.4035 0.040 Uiso 1 1 calc R . . 
C11 C 0.5297(6) 0.3932(6) 0.4440(3) 0.0401(19) Uani 1 1 d . . . 
H11 H 0.5584 0.3380 0.4586 0.048 Uiso 1 1 calc R . . 
C12 C 0.5796(6) 0.4782(7) 0.4551(3) 0.042(2) Uani 1 1 d . . . 
H12 H 0.6419 0.4801 0.4772 0.050 Uiso 1 1 calc R . . 
C13 C 0.5380(6) 0.5602(6) 0.4338(3) 0.043(2) Uani 1 1 d . . . 
H13 H 0.5729 0.6172 0.4410 0.051 Uiso 1 1 calc R . . 
C14 C 0.4438(6) 0.5580(5) 0.4016(3) 0.0345(17) Uani 1 1 d . . . 
H14 H 0.4148 0.6138 0.3880 0.041 Uiso 1 1 calc R . . 
C15 C 0.2055(5) 0.3546(4) 0.2914(2) 0.0215(13) Uani 1 1 d . . . 
H15A H 0.1394 0.3867 0.2934 0.026 Uiso 1 1 calc R . . 
H15B H 0.2051 0.3356 0.2580 0.026 Uiso 1 1 calc R . . 
C16 C 0.2149(5) 0.2694(4) 0.3233(2) 0.0240(14) Uani 1 1 d . . . 
C17 C 0.2918(5) 0.2008(4) 0.3170(2) 0.0207(13) Uani 1 1 d . . . 
C18 C 0.3009(5) 0.1193(4) 0.3468(2) 0.0218(14) Uani 1 1 d . . . 
C19 C 0.2372(5) 0.1094(5) 0.3823(2) 0.0273(15) Uani 1 1 d . . . 
H19 H 0.2434 0.0559 0.4018 0.033 Uiso 1 1 calc R . . 
C20 C 0.1642(5) 0.1787(5) 0.3890(2) 0.0264(15) Uani 1 1 d . . . 
C21 C 0.1525(5) 0.2583(5) 0.3593(2) 0.0243(13) Uani 1 1 d . . . 
H21 H 0.1028 0.3041 0.3636 0.029 Uiso 1 1 calc R . . 
C22 C 0.3794(5) 0.0448(4) 0.3375(2) 0.0214(13) Uani 1 1 d . . . 
H22A H 0.3688 0.0296 0.3031 0.026 Uiso 1 1 calc R . . 
H22B H 0.3671 -0.0122 0.3551 0.026 Uiso 1 1 calc R . . 
C23 C 0.5231(5) 0.0861(4) 0.4070(2) 0.0250(14) Uani 1 1 d . . . 
H23A H 0.4676 0.1198 0.4198 0.030 Uiso 1 1 calc R . . 
H23B H 0.5871 0.1234 0.4139 0.030 Uiso 1 1 calc R . . 
C24 C 0.5411(6) -0.0079(5) 0.4330(2) 0.0292(15) Uani 1 1 d . . . 
C25 C 0.6424(6) -0.0434(5) 0.4444(3) 0.0375(18) Uani 1 1 d . . . 
H25 H 0.6988 -0.0094 0.4359 0.045 Uiso 1 1 calc R . . 
C26 C 0.6613(7) -0.1303(6) 0.4688(3) 0.047(2) Uani 1 1 d . . . 
H26 H 0.7296 -0.1541 0.4758 0.056 Uiso 1 1 calc R . . 
C27 C 0.5788(7) -0.1794(6) 0.4823(3) 0.044(2) Uani 1 1 d . . . 
H27 H 0.5914 -0.2363 0.4988 0.053 Uiso 1 1 calc R . . 
C28 C 0.4781(7) -0.1459(6) 0.4716(3) 0.044(2) Uani 1 1 d . . . 
H28 H 0.4223 -0.1800 0.4807 0.053 Uiso 1 1 calc R . . 
C29 C 0.4590(6) -0.0602(5) 0.4469(3) 0.0339(17) Uani 1 1 d . . . 
H29 H 0.3901 -0.0377 0.4396 0.041 Uiso 1 1 calc R . . 
C30 C 0.5683(5) 0.0165(4) 0.3300(2) 0.0213(13) Uani 1 1 d . . . 
H30A H 0.5379 0.0034 0.2966 0.026 Uiso 1 1 calc R . . 
H30B H 0.5781 -0.0433 0.3471 0.026 Uiso 1 1 calc R . . 
C31 C 0.6745(5) 0.0636(4) 0.3311(2) 0.0186(13) Uani 1 1 d . . . 
C32 C 0.6776(5) 0.1584(4) 0.3161(2) 0.0203(13) Uani 1 1 d . . . 
C33 C 0.7778(5) 0.2021(4) 0.3177(2) 0.0209(13) Uani 1 1 d . . . 
C34 C 0.8695(5) 0.1495(4) 0.3294(2) 0.0213(13) Uani 1 1 d . . . 
H34 H 0.9349 0.1777 0.3292 0.026 Uiso 1 1 calc R . . 
C35 C 0.8635(5) 0.0547(4) 0.3414(2) 0.0221(14) Uani 1 1 d . . . 
C36 C 0.7669(5) 0.0118(4) 0.3431(2) 0.0225(14) Uani 1 1 d . . . 
H36 H 0.7639 -0.0512 0.3521 0.027 Uiso 1 1 calc R . . 
C37 C 0.7873(5) 0.3014(4) 0.2998(2) 0.0202(13) Uani 1 1 d . . . 
H37A H 0.7806 0.3002 0.2647 0.024 Uiso 1 1 calc R . . 
H37B H 0.8572 0.3251 0.3123 0.024 Uiso 1 1 calc R . . 
C38 C 0.7132(5) 0.3861(4) 0.3675(2) 0.0214(13) Uani 1 1 d . . . 
H38A H 0.7047 0.3264 0.3835 0.026 Uiso 1 1 calc R . . 
H38B H 0.6550 0.4266 0.3729 0.026 Uiso 1 1 calc R . . 
C39 C 0.8158(5) 0.4311(4) 0.3909(2) 0.0215(13) Uani 1 1 d . . . 
C40 C 0.9011(5) 0.3763(5) 0.4103(2) 0.0267(15) Uani 1 1 d . . . 
H40 H 0.8963 0.3109 0.4079 0.032 Uiso 1 1 calc R . . 
C41 C 0.9946(5) 0.4176(5) 0.4336(3) 0.0321(16) Uani 1 1 d . . . 
H41 H 1.0522 0.3803 0.4459 0.039 Uiso 1 1 calc R . . 
C42 C 1.0002(6) 0.5153(5) 0.4382(3) 0.0358(17) Uani 1 1 d . . . 
H42 H 1.0619 0.5436 0.4536 0.043 Uiso 1 1 calc R . . 
C43 C 0.9145(6) 0.5702(5) 0.4198(3) 0.0338(17) Uani 1 1 d . . . 
H43 H 0.9187 0.6355 0.4229 0.041 Uiso 1 1 calc R . . 
C44 C 0.8226(5) 0.5292(5) 0.3970(2) 0.0278(15) Uani 1 1 d . . . 
H44 H 0.7647 0.5668 0.3856 0.033 Uiso 1 1 calc R . . 
C45 C 0.7048(5) 0.4580(4) 0.2831(2) 0.0206(13) Uani 1 1 d . . . 
N7 N 0.7540(5) 0.7338(5) 0.0320(2) 0.0421(16) Uani 1 1 d . . . 
C46 C 0.6944(6) 0.6611(6) 0.0403(3) 0.0393(18) Uani 1 1 d . . . 
H46 H 0.7070 0.6325 0.0706 0.047 Uiso 1 1 calc R . . 
C47 C 0.6140(6) 0.6255(6) 0.0060(3) 0.044(2) Uani 1 1 d . . . 
H47 H 0.5757 0.5728 0.0129 0.053 Uiso 1 1 calc R . . 
C48 C 0.5923(7) 0.6692(7) -0.0379(3) 0.049(2) Uani 1 1 d . . . 
H48 H 0.5382 0.6474 -0.0614 0.058 Uiso 1 1 calc R . . 
C49 C 0.6517(6) 0.7459(6) -0.0468(3) 0.0412(18) Uani 1 1 d . . . 
H49 H 0.6383 0.7776 -0.0763 0.049 Uiso 1 1 calc R . . 
C50 C 0.7318(6) 0.7748(6) -0.0111(3) 0.0412(19) Uani 1 1 d . . . 
H50 H 0.7727 0.8261 -0.0176 0.049 Uiso 1 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Nd 0.01562(18) 0.01294(18) 0.02333(19) -0.00041(14) 0.00189(11) -0.00018(14) 
O1 0.019(2) 0.013(2) 0.030(3) -0.0046(17) 0.0024(18) -0.0008(17) 
O2 0.017(2) 0.023(2) 0.027(2) 0.0027(18) 0.0073(17) -0.0012(17) 
O3 0.013(2) 0.014(2) 0.031(3) 0.0043(17) 0.0003(17) 0.0050(16) 
O4 0.025(2) 0.025(2) 0.021(2) -0.0031(18) 0.0028(18) -0.0079(19) 
O5 0.021(2) 0.028(2) 0.032(2) 0.002(2) 0.0002(17) 0.000(2) 
O6 0.031(3) 0.036(3) 0.036(3) -0.006(2) 0.017(2) -0.008(2) 
O7 0.024(2) 0.022(2) 0.036(3) -0.007(2) -0.003(2) -0.0022(19) 
O8 0.020(2) 0.025(2) 0.036(3) 0.000(2) -0.0004(19) -0.0006(19) 
O9 0.028(3) 0.054(4) 0.049(4) 0.000(3) -0.016(2) 0.012(3) 
O10 0.013(2) 0.021(2) 0.044(3) -0.006(2) 0.0096(19) 0.0010(18) 
O11 0.020(2) 0.017(2) 0.044(3) -0.002(2) 0.010(2) -0.0024(19) 
O12 0.030(3) 0.016(2) 0.054(3) -0.011(2) 0.014(2) -0.0030(19) 
N1 0.015(3) 0.020(3) 0.029(3) -0.002(2) 0.002(2) 0.000(2) 
N2 0.016(3) 0.015(2) 0.025(3) 0.000(2) 0.007(2) 0.003(2) 
N3 0.013(3) 0.014(2) 0.029(3) 0.001(2) 0.002(2) 0.000(2) 
N4 0.026(3) 0.014(3) 0.031(3) 0.000(2) 0.007(2) -0.002(2) 
N5 0.023(3) 0.025(3) 0.035(3) 0.005(2) 0.004(2) 0.001(2) 
N6 0.024(3) 0.020(3) 0.024(3) 0.000(2) 0.001(2) 0.002(2) 
Cl1 0.0302(9) 0.0135(8) 0.0633(13) -0.0034(7) 0.0116(8) -0.0010(6) 
Cl2 0.0306(9) 0.0389(10) 0.0357(10) 0.0034(8) 0.0150(7) 0.0030(8) 
Cl3 0.0188(8) 0.0226(8) 0.0460(11) 0.0009(7) 0.0019(7) 0.0064(6) 
C1 0.022(3) 0.017(3) 0.017(3) -0.002(2) 0.004(2) -0.003(2) 
C2 0.015(3) 0.017(3) 0.026(3) 0.002(2) 0.001(2) -0.001(2) 
C3 0.022(3) 0.016(3) 0.027(4) -0.001(2) 0.002(3) 0.005(3) 
C4 0.030(4) 0.007(3) 0.026(3) 0.004(2) 0.007(3) 0.001(2) 
C5 0.016(3) 0.020(3) 0.031(4) 0.000(3) 0.002(3) -0.004(3) 
C6 0.014(3) 0.022(3) 0.017(3) 0.003(2) 0.002(2) 0.002(2) 
C7 0.021(3) 0.013(3) 0.027(4) 0.000(2) 0.002(3) 0.000(2) 
C8 0.024(3) 0.030(4) 0.029(4) 0.001(3) 0.009(3) 0.003(3) 
C9 0.028(4) 0.033(4) 0.024(4) -0.004(3) 0.006(3) -0.003(3) 
C10 0.028(4) 0.037(4) 0.036(4) 0.005(3) 0.007(3) 0.002(3) 
C11 0.028(4) 0.056(5) 0.036(5) 0.007(4) 0.004(3) 0.009(4) 
C12 0.023(4) 0.074(6) 0.028(4) -0.008(4) 0.003(3) 0.000(4) 
C13 0.039(5) 0.054(5) 0.036(5) -0.015(4) 0.008(3) -0.017(4) 
C14 0.037(4) 0.034(4) 0.032(4) -0.003(3) 0.005(3) -0.005(3) 
C15 0.014(3) 0.021(3) 0.030(4) -0.002(3) 0.002(2) -0.007(2) 
C16 0.014(3) 0.020(3) 0.038(4) -0.002(3) 0.004(3) 0.000(2) 
C17 0.018(3) 0.019(3) 0.024(3) -0.002(3) 0.001(2) -0.001(2) 
C18 0.017(3) 0.019(3) 0.029(4) -0.003(3) 0.000(3) -0.004(2) 
C19 0.029(4) 0.025(3) 0.028(4) 0.009(3) 0.004(3) 0.001(3) 
C20 0.020(3) 0.028(4) 0.032(4) 0.001(3) 0.007(3) -0.001(3) 
C21 0.012(3) 0.027(3) 0.035(4) -0.006(3) 0.008(2) -0.004(3) 
C22 0.016(3) 0.015(3) 0.033(4) 0.002(3) 0.001(3) -0.002(2) 
C23 0.024(3) 0.021(3) 0.029(4) -0.003(3) 0.001(3) -0.003(3) 
C24 0.036(4) 0.024(4) 0.026(4) 0.000(3) 0.001(3) -0.004(3) 
C25 0.035(4) 0.036(4) 0.042(5) 0.004(3) 0.008(3) -0.005(3) 
C26 0.054(5) 0.048(5) 0.038(5) 0.014(4) 0.004(4) 0.015(4) 
C27 0.063(6) 0.030(4) 0.036(5) 0.006(3) 0.002(4) 0.000(4) 
C28 0.049(5) 0.046(5) 0.037(5) 0.002(4) 0.006(4) -0.019(4) 
C29 0.029(4) 0.038(4) 0.033(4) 0.008(3) -0.001(3) -0.003(3) 
C30 0.019(3) 0.017(3) 0.029(4) -0.001(3) 0.005(3) 0.003(2) 
C31 0.018(3) 0.017(3) 0.021(3) -0.003(2) 0.002(2) 0.001(2) 
C32 0.013(3) 0.021(3) 0.027(4) -0.001(3) 0.003(2) 0.004(2) 
C33 0.020(3) 0.022(3) 0.021(3) 0.002(3) -0.001(2) -0.001(3) 
C34 0.016(3) 0.019(3) 0.028(4) 0.000(3) 0.002(3) 0.000(2) 
C35 0.015(3) 0.021(3) 0.030(4) -0.002(3) 0.002(3) 0.004(2) 
C36 0.024(3) 0.019(3) 0.025(4) 0.001(3) 0.003(3) 0.000(3) 
C37 0.017(3) 0.016(3) 0.027(4) -0.001(3) 0.001(2) 0.002(2) 
C38 0.022(3) 0.016(3) 0.026(4) 0.004(2) 0.004(3) 0.004(2) 
C39 0.020(3) 0.024(3) 0.021(3) 0.000(3) 0.003(2) -0.005(3) 
C40 0.029(4) 0.024(4) 0.026(4) 0.001(3) 0.003(3) -0.001(3) 
C41 0.022(4) 0.040(4) 0.033(4) 0.004(3) 0.000(3) 0.002(3) 
C42 0.036(4) 0.033(4) 0.036(4) -0.005(3) -0.003(3) -0.015(3) 
C43 0.044(4) 0.025(4) 0.031(4) -0.004(3) -0.001(3) -0.011(3) 
C44 0.031(4) 0.024(3) 0.029(4) 0.006(3) 0.004(3) 0.003(3) 
C45 0.016(3) 0.015(3) 0.030(4) 0.005(3) 0.003(3) 0.003(2) 
N7 0.036(3) 0.054(4) 0.033(4) -0.006(3) -0.005(3) 0.005(3) 
C46 0.039(4) 0.048(5) 0.031(4) -0.001(4) 0.005(3) 0.010(4) 
C47 0.040(5) 0.042(5) 0.052(5) 0.000(4) 0.011(4) -0.001(4) 
C48 0.047(5) 0.060(6) 0.034(5) -0.010(4) -0.006(4) -0.004(4) 
C49 0.042(4) 0.053(5) 0.026(4) 0.000(4) -0.001(3) -0.003(4) 
C50 0.038(4) 0.045(5) 0.037(5) -0.001(3) -0.004(3) 0.003(4) 

_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 
Nd O2 2.298(4) . ? 
Nd O1 2.334(4) . ? 
Nd O3 2.399(4) . ? 
Nd O5 2.540(4) . ? 
Nd O4 2.562(4) . ? 
Nd O10 2.566(4) . ? 
Nd O7 2.578(4) . ? 
Nd O8 2.595(4) . ? 
Nd O11 2.628(4) . ? 
Nd N4 2.979(5) . ? 
O1 C1 1.339(7) . ? 
O2 C17 1.315(7) . ? 
O3 C32 1.340(7) . ? 
O4 N4 1.263(7) . ? 
O5 N4 1.284(7) . ? 
O6 N4 1.226(7) . ? 
O7 N5 1.279(7) . ? 
O8 N5 1.262(7) . ? 
O9 N5 1.223(7) . ? 
O10 N6 1.277(7) . ? 
O11 N6 1.262(7) . ? 
O12 N6 1.227(7) . ? 
N1 C7 1.517(8) . ? 
N1 C8 1.515(8) . ? 
N1 C15 1.534(7) . ? 
N2 C23 1.500(8) . ? 
N2 C30 1.508(7) . ? 
N2 C22 1.524(7) . ? 
N3 C38 1.502(8) . ? 
N3 C37 1.508(8) . ? 
N3 C45 1.526(8) . ? 
Cl1 C4 1.742(6) . ? 
Cl2 C20 1.741(7) . ? 
Cl3 C35 1.746(6) . ? 
C1 C2 1.411(9) . ? 
C1 C6 1.413(8) . ? 
C2 C3 1.388(8) . ? 
C2 C7 1.485(8) . ? 
C3 C4 1.380(9) . ? 
C4 C5 1.382(9) . ? 
C5 C6 1.404(9) . ? 
C6 C45 1.507(8) . ? 
C8 C9 1.492(9) . ? 
C9 C14 1.398(10) . ? 
C9 C10 1.399(10) . ? 
C10 C11 1.387(10) . ? 
C11 C12 1.376(12) . ? 
C12 C13 1.374(12) . ? 
C13 C14 1.389(10) . ? 
C15 C16 1.494(9) . ? 
C16 C21 1.385(9) . ? 
C16 C17 1.414(9) . ? 
C17 C18 1.417(9) . ? 
C18 C19 1.385(9) . ? 
C18 C22 1.509(8) . ? 
C19 C20 1.389(9) . ? 
C20 C21 1.395(9) . ? 
C23 C24 1.517(9) . ? 
C24 C25 1.383(10) . ? 
C24 C29 1.389(10) . ? 
C25 C26 1.410(11) . ? 
C26 C27 1.366(12) . ? 
C27 C28 1.363(12) . ? 
C28 C29 1.400(11) . ? 
C30 C31 1.512(8) . ? 
C31 C36 1.389(9) . ? 
C31 C32 1.408(9) . ? 
C32 C33 1.420(9) . ? 
C33 C34 1.386(9) . ? 
C33 C37 1.505(8) . ? 
C34 C35 1.389(9) . ? 
C35 C36 1.387(9) . ? 
C38 C39 1.516(9) . ? 
C39 C40 1.381(9) . ? 
C39 C44 1.400(9) . ? 
C40 C41 1.400(9) . ? 
C41 C42 1.390(10) . ? 
C42 C43 1.378(11) . ? 
C43 C44 1.377(10) . ? 
N7 C46 1.324(10) . ? 
N7 C50 1.325(10) . ? 
C46 C47 1.386(11) . ? 
C47 C48 1.362(12) . ? 
C48 C49 1.373(12) . ? 
C49 C50 1.376(10) . ? 

loop_
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O2 Nd O1 83.09(15) . . ? 
O2 Nd O3 78.30(15) . . ? 
O1 Nd O3 74.62(14) . . ? 
O2 Nd O5 152.54(14) . . ? 
O1 Nd O5 112.02(15) . . ? 
O3 Nd O5 126.87(14) . . ? 
O2 Nd O4 157.21(14) . . ? 
O1 Nd O4 81.57(14) . . ? 
O3 Nd O4 81.44(14) . . ? 
O5 Nd O4 50.18(13) . . ? 
O2 Nd O10 76.60(14) . . ? 
O1 Nd O10 156.52(15) . . ? 
O3 Nd O10 89.68(14) . . ? 
O5 Nd O10 91.33(15) . . ? 
O4 Nd O10 113.78(13) . . ? 
O2 Nd O7 89.25(15) . . ? 
O1 Nd O7 77.02(14) . . ? 
O3 Nd O7 150.13(14) . . ? 
O5 Nd O7 73.03(14) . . ? 
O4 Nd O7 103.54(14) . . ? 
O10 Nd O7 113.92(14) . . ? 
O2 Nd O8 81.47(15) . . ? 
O1 Nd O8 124.01(14) . . ? 
O3 Nd O8 150.45(14) . . ? 
O5 Nd O8 71.07(14) . . ? 
O4 Nd O8 121.18(14) . . ? 
O10 Nd O8 64.65(14) . . ? 
O7 Nd O8 49.40(14) . . ? 
O2 Nd O11 117.48(14) . . ? 
O1 Nd O11 137.24(14) . . ? 
O3 Nd O11 73.92(14) . . ? 
O5 Nd O11 67.49(15) . . ? 
O4 Nd O11 65.75(13) . . ? 
O10 Nd O11 48.94(13) . . ? 
O7 Nd O11 135.28(15) . . ? 
O8 Nd O11 97.08(14) . . ? 
O2 Nd N4 177.86(15) . . ? 
O1 Nd N4 98.16(14) . . ? 
O3 Nd N4 103.68(14) . . ? 
O5 Nd N4 25.33(14) . . ? 
O4 Nd N4 24.92(14) . . ? 
O10 Nd N4 102.53(14) . . ? 
O7 Nd N4 89.35(15) . . ? 
O8 Nd N4 96.39(15) . . ? 
O11 Nd N4 62.68(14) . . ? 
C1 O1 Nd 156.9(4) . . ? 
C17 O2 Nd 175.9(4) . . ? 
C32 O3 Nd 140.0(4) . . ? 
N4 O4 Nd 96.4(3) . . ? 
N4 O5 Nd 96.9(3) . . ? 
N5 O7 Nd 97.2(3) . . ? 
N5 O8 Nd 96.8(3) . . ? 
N6 O10 Nd 98.7(3) . . ? 
N6 O11 Nd 96.1(3) . . ? 
C7 N1 C8 112.4(5) . . ? 
C7 N1 C15 112.1(5) . . ? 
C8 N1 C15 111.6(5) . . ? 
C23 N2 C30 113.2(5) . . ? 
C23 N2 C22 113.3(5) . . ? 
C30 N2 C22 110.7(5) . . ? 
C38 N3 C37 115.4(5) . . ? 
C38 N3 C45 114.9(5) . . ? 
C37 N3 C45 109.0(5) . . ? 
O6 N4 O4 122.6(5) . . ? 
O6 N4 O5 121.1(5) . . ? 
O4 N4 O5 116.3(5) . . ? 
O6 N4 Nd 175.2(4) . . ? 
O4 N4 Nd 58.7(3) . . ? 
O5 N4 Nd 57.8(3) . . ? 
O9 N5 O8 122.3(6) . . ? 
O9 N5 O7 121.2(6) . . ? 
O8 N5 O7 116.6(5) . . ? 
O12 N6 O11 122.6(5) . . ? 
O12 N6 O10 121.5(5) . . ? 
O11 N6 O10 115.9(5) . . ? 
O1 C1 C2 120.3(5) . . ? 
O1 C1 C6 120.5(5) . . ? 
C2 C1 C6 119.2(6) . . ? 
C3 C2 C1 120.2(6) . . ? 
C3 C2 C7 121.3(6) . . ? 
C1 C2 C7 118.4(5) . . ? 
C4 C3 C2 120.0(6) . . ? 
C3 C4 C5 121.1(6) . . ? 
C3 C4 Cl1 119.3(5) . . ? 
C5 C4 Cl1 119.6(5) . . ? 
C4 C5 C6 120.1(6) . . ? 
C5 C6 C1 119.3(5) . . ? 
C5 C6 C45 119.5(5) . . ? 
C1 C6 C45 120.9(5) . . ? 
C2 C7 N1 111.0(5) . . ? 
C9 C8 N1 114.3(5) . . ? 
C14 C9 C10 118.6(6) . . ? 
C14 C9 C8 121.4(6) . . ? 
C10 C9 C8 120.0(6) . . ? 
C11 C10 C9 120.3(7) . . ? 
C12 C11 C10 120.2(8) . . ? 
C13 C12 C11 120.5(7) . . ? 
C12 C13 C14 120.0(7) . . ? 
C13 C14 C9 120.4(7) . . ? 
C16 C15 N1 110.3(5) . . ? 
C21 C16 C17 120.3(6) . . ? 
C21 C16 C15 121.4(6) . . ? 
C17 C16 C15 118.3(6) . . ? 
O2 C17 C16 120.6(6) . . ? 
O2 C17 C18 120.6(6) . . ? 
C16 C17 C18 118.8(6) . . ? 
C19 C18 C17 119.9(6) . . ? 
C19 C18 C22 122.3(6) . . ? 
C17 C18 C22 117.8(6) . . ? 
C18 C19 C20 120.6(6) . . ? 
C19 C20 C21 120.2(6) . . ? 
C19 C20 Cl2 120.1(5) . . ? 
C21 C20 Cl2 119.7(5) . . ? 
C16 C21 C20 120.1(6) . . ? 
C18 C22 N2 111.9(5) . . ? 
N2 C23 C24 113.6(5) . . ? 
C25 C24 C29 117.8(7) . . ? 
C25 C24 C23 119.8(6) . . ? 
C29 C24 C23 122.4(6) . . ? 
C24 C25 C26 120.9(7) . . ? 
C27 C26 C25 119.7(8) . . ? 
C28 C27 C26 120.7(8) . . ? 
C27 C28 C29 119.8(8) . . ? 
C24 C29 C28 121.2(7) . . ? 
N2 C30 C31 111.9(5) . . ? 
C36 C31 C32 120.9(6) . . ? 
C36 C31 C30 120.1(5) . . ? 
C32 C31 C30 118.8(5) . . ? 
O3 C32 C31 120.4(5) . . ? 
O3 C32 C33 121.4(5) . . ? 
C31 C32 C33 118.2(5) . . ? 
C34 C33 C32 120.2(6) . . ? 
C34 C33 C37 118.1(6) . . ? 
C32 C33 C37 121.1(6) . . ? 
C33 C34 C35 120.0(6) . . ? 
C36 C35 C34 121.0(6) . . ? 
C36 C35 Cl3 120.0(5) . . ? 
C34 C35 Cl3 119.0(5) . . ? 
C35 C36 C31 119.5(6) . . ? 
C33 C37 N3 114.3(5) . . ? 
N3 C38 C39 114.1(5) . . ? 
C40 C39 C44 118.7(6) . . ? 
C40 C39 C38 120.9(6) . . ? 
C44 C39 C38 120.2(6) . . ? 
C39 C40 C41 121.0(6) . . ? 
C42 C41 C40 119.2(7) . . ? 
C43 C42 C41 120.0(7) . . ? 
C44 C43 C42 120.6(7) . . ? 
C43 C44 C39 120.5(6) . . ? 
C6 C45 N3 112.1(5) . . ? 
C46 N7 C50 116.8(7) . . ? 
N7 C46 C47 123.4(7) . . ? 
C48 C47 C46 118.7(8) . . ? 
C47 C48 C49 118.8(7) . . ? 
C48 C49 C50 118.4(8) . . ? 
N7 C50 C49 123.9(8) . . ? 

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 
O2 Nd O1 C1 -137.6(10) . . . . ? 
O3 Nd O1 C1 142.7(10) . . . . ? 
O5 Nd O1 C1 18.7(10) . . . . ? 
O4 Nd O1 C1 59.3(10) . . . . ? 
O10 Nd O1 C1 -167.7(9) . . . . ? 
O7 Nd O1 C1 -46.7(10) . . . . ? 
O8 Nd O1 C1 -62.8(10) . . . . ? 
O11 Nd O1 C1 98.8(10) . . . . ? 
N4 Nd O1 C1 40.7(10) . . . . ? 
O1 Nd O2 C17 -15(6) . . . . ? 
O3 Nd O2 C17 61(6) . . . . ? 
O5 Nd O2 C17 -141(6) . . . . ? 
O4 Nd O2 C17 33(6) . . . . ? 
O10 Nd O2 C17 153(6) . . . . ? 
O7 Nd O2 C17 -92(6) . . . . ? 
O8 Nd O2 C17 -141(6) . . . . ? 
O11 Nd O2 C17 126(6) . . . . ? 
N4 Nd O2 C17 -141(5) . . . . ? 
O2 Nd O3 C32 138.7(6) . . . . ? 
O1 Nd O3 C32 -135.4(6) . . . . ? 
O5 Nd O3 C32 -29.1(6) . . . . ? 
O4 Nd O3 C32 -51.8(6) . . . . ? 
O10 Nd O3 C32 62.3(6) . . . . ? 
O7 Nd O3 C32 -154.1(5) . . . . ? 
O8 Nd O3 C32 90.9(6) . . . . ? 
O11 Nd O3 C32 15.3(6) . . . . ? 
N4 Nd O3 C32 -40.5(6) . . . . ? 
O2 Nd O4 N4 -179.4(4) . . . . ? 
O1 Nd O4 N4 -131.3(3) . . . . ? 
O3 Nd O4 N4 153.1(3) . . . . ? 
O5 Nd O4 N4 -3.2(3) . . . . ? 
O10 Nd O4 N4 67.3(3) . . . . ? 
O7 Nd O4 N4 -56.9(3) . . . . ? 
O8 Nd O4 N4 -6.4(4) . . . . ? 
O11 Nd O4 N4 77.0(3) . . . . ? 
O2 Nd O5 N4 180.0(3) . . . . ? 
O1 Nd O5 N4 60.2(3) . . . . ? 
O3 Nd O5 N4 -26.7(4) . . . . ? 
O4 Nd O5 N4 3.1(3) . . . . ? 
O10 Nd O5 N4 -117.3(3) . . . . ? 
O7 Nd O5 N4 128.1(3) . . . . ? 
O8 Nd O5 N4 -179.8(4) . . . . ? 
O11 Nd O5 N4 -73.4(3) . . . . ? 
O2 Nd O7 N5 -78.3(4) . . . . ? 
O1 Nd O7 N5 -161.4(4) . . . . ? 
O3 Nd O7 N5 -142.9(3) . . . . ? 
O5 Nd O7 N5 80.4(4) . . . . ? 
O4 Nd O7 N5 120.7(4) . . . . ? 
O10 Nd O7 N5 -3.4(4) . . . . ? 
O8 Nd O7 N5 1.0(3) . . . . ? 
O11 Nd O7 N5 51.6(4) . . . . ? 
N4 Nd O7 N5 100.0(4) . . . . ? 
O2 Nd O8 N5 95.3(4) . . . . ? 
O1 Nd O8 N5 19.7(4) . . . . ? 
O3 Nd O8 N5 142.5(4) . . . . ? 
O5 Nd O8 N5 -84.6(4) . . . . ? 
O4 Nd O8 N5 -82.0(4) . . . . ? 
O10 Nd O8 N5 174.5(4) . . . . ? 
O7 Nd O8 N5 -1.1(3) . . . . ? 
O11 Nd O8 N5 -147.8(4) . . . . ? 
N4 Nd O8 N5 -84.7(4) . . . . ? 
O2 Nd O10 N6 -150.4(4) . . . . ? 
O1 Nd O10 N6 -119.6(4) . . . . ? 
O3 Nd O10 N6 -72.3(3) . . . . ? 
O5 Nd O10 N6 54.5(3) . . . . ? 
O4 Nd O10 N6 8.1(4) . . . . ? 
O7 Nd O10 N6 126.5(3) . . . . ? 
O8 Nd O10 N6 122.8(4) . . . . ? 
O11 Nd O10 N6 -3.6(3) . . . . ? 
N4 Nd O10 N6 31.6(4) . . . . ? 
O2 Nd O11 N6 40.5(4) . . . . ? 
O1 Nd O11 N6 151.8(3) . . . . ? 
O3 Nd O11 N6 107.7(4) . . . . ? 
O5 Nd O11 N6 -109.6(4) . . . . ? 
O4 Nd O11 N6 -164.6(4) . . . . ? 
O10 Nd O11 N6 3.6(3) . . . . ? 
O7 Nd O11 N6 -79.7(4) . . . . ? 
O8 Nd O11 N6 -43.5(4) . . . . ? 
N4 Nd O11 N6 -137.1(4) . . . . ? 
Nd O4 N4 O6 -174.6(5) . . . . ? 
Nd O4 N4 O5 5.4(5) . . . . ? 
Nd O5 N4 O6 174.5(5) . . . . ? 
Nd O5 N4 O4 -5.4(5) . . . . ? 
O2 Nd N4 O6 -78(7) . . . . ? 
O1 Nd N4 O6 157(5) . . . . ? 
O3 Nd N4 O6 80(5) . . . . ? 
O5 Nd N4 O6 -78(5) . . . . ? 
O4 Nd N4 O6 108(5) . . . . ? 
O10 Nd N4 O6 -12(5) . . . . ? 
O7 Nd N4 O6 -127(5) . . . . ? 
O8 Nd N4 O6 -78(5) . . . . ? 
O11 Nd N4 O6 17(5) . . . . ? 
O2 Nd N4 O4 174(4) . . . . ? 
O1 Nd N4 O4 48.7(3) . . . . ? 
O3 Nd N4 O4 -27.4(3) . . . . ? 
O5 Nd N4 O4 174.3(5) . . . . ? 
O10 Nd N4 O4 -120.1(3) . . . . ? 
O7 Nd N4 O4 125.5(3) . . . . ? 
O8 Nd N4 O4 174.5(3) . . . . ? 
O11 Nd N4 O4 -90.8(3) . . . . ? 
O2 Nd N4 O5 0(4) . . . . ? 
O1 Nd N4 O5 -125.6(3) . . . . ? 
O3 Nd N4 O5 158.3(3) . . . . ? 
O4 Nd N4 O5 -174.3(5) . . . . ? 
O10 Nd N4 O5 65.5(3) . . . . ? 
O7 Nd N4 O5 -48.8(3) . . . . ? 
O8 Nd N4 O5 0.2(3) . . . . ? 
O11 Nd N4 O5 94.8(3) . . . . ? 
Nd O8 N5 O9 -178.7(6) . . . . ? 
Nd O8 N5 O7 1.8(6) . . . . ? 
Nd O7 N5 O9 178.7(6) . . . . ? 
Nd O7 N5 O8 -1.8(6) . . . . ? 
Nd O11 N6 O12 174.4(5) . . . . ? 
Nd O11 N6 O10 -6.1(5) . . . . ? 
Nd O10 N6 O12 -174.2(5) . . . . ? 
Nd O10 N6 O11 6.3(5) . . . . ? 
Nd O1 C1 C2 88.2(11) . . . . ? 
Nd O1 C1 C6 -93.1(11) . . . . ? 
O1 C1 C2 C3 -179.6(6) . . . . ? 
C6 C1 C2 C3 1.7(9) . . . . ? 
O1 C1 C2 C7 -1.1(9) . . . . ? 
C6 C1 C2 C7 -179.9(5) . . . . ? 
C1 C2 C3 C4 -0.7(10) . . . . ? 
C7 C2 C3 C4 -179.0(6) . . . . ? 
C2 C3 C4 C5 -1.6(10) . . . . ? 
C2 C3 C4 Cl1 178.6(5) . . . . ? 
C3 C4 C5 C6 2.7(10) . . . . ? 
Cl1 C4 C5 C6 -177.5(5) . . . . ? 
C4 C5 C6 C1 -1.6(9) . . . . ? 
C4 C5 C6 C45 173.1(6) . . . . ? 
O1 C1 C6 C5 -179.3(6) . . . . ? 
C2 C1 C6 C5 -0.6(9) . . . . ? 
O1 C1 C6 C45 6.1(9) . . . . ? 
C2 C1 C6 C45 -175.2(6) . . . . ? 
C3 C2 C7 N1 -121.5(6) . . . . ? 
C1 C2 C7 N1 60.1(7) . . . . ? 
C8 N1 C7 C2 71.6(6) . . . . ? 
C15 N1 C7 C2 -161.8(5) . . . . ? 
C7 N1 C8 C9 -96.5(6) . . . . ? 
C15 N1 C8 C9 136.6(6) . . . . ? 
N1 C8 C9 C14 111.4(7) . . . . ? 
N1 C8 C9 C10 -70.8(8) . . . . ? 
C14 C9 C10 C11 -0.1(10) . . . . ? 
C8 C9 C10 C11 -177.9(6) . . . . ? 
C9 C10 C11 C12 -0.6(11) . . . . ? 
C10 C11 C12 C13 0.0(11) . . . . ? 
C11 C12 C13 C14 1.3(12) . . . . ? 
C12 C13 C14 C9 -1.9(11) . . . . ? 
C10 C9 C14 C13 1.3(11) . . . . ? 
C8 C9 C14 C13 179.2(6) . . . . ? 
C7 N1 C15 C16 163.0(5) . . . . ? 
C8 N1 C15 C16 -70.0(6) . . . . ? 
N1 C15 C16 C21 103.9(7) . . . . ? 
N1 C15 C16 C17 -74.3(7) . . . . ? 
Nd O2 C17 C16 68(6) . . . . ? 
Nd O2 C17 C18 -112(6) . . . . ? 
C21 C16 C17 O2 -177.7(6) . . . . ? 
C15 C16 C17 O2 0.4(9) . . . . ? 
C21 C16 C17 C18 2.3(9) . . . . ? 
C15 C16 C17 C18 -179.5(5) . . . . ? 
O2 C17 C18 C19 178.2(6) . . . . ? 
C16 C17 C18 C19 -1.9(9) . . . . ? 
O2 C17 C18 C22 -3.2(9) . . . . ? 
C16 C17 C18 C22 176.7(5) . . . . ? 
C17 C18 C19 C20 0.0(10) . . . . ? 
C22 C18 C19 C20 -178.5(6) . . . . ? 
C18 C19 C20 C21 1.4(10) . . . . ? 
C18 C19 C20 Cl2 -178.1(5) . . . . ? 
C17 C16 C21 C20 -0.9(9) . . . . ? 
C15 C16 C21 C20 -179.0(6) . . . . ? 
C19 C20 C21 C16 -0.9(10) . . . . ? 
Cl2 C20 C21 C16 178.5(5) . . . . ? 
C19 C18 C22 N2 -110.2(7) . . . . ? 
C17 C18 C22 N2 71.3(7) . . . . ? 
C23 N2 C22 C18 68.9(6) . . . . ? 
C30 N2 C22 C18 -162.6(5) . . . . ? 
C30 N2 C23 C24 -52.3(7) . . . . ? 
C22 N2 C23 C24 74.9(6) . . . . ? 
N2 C23 C24 C25 96.3(7) . . . . ? 
N2 C23 C24 C29 -85.0(8) . . . . ? 
C29 C24 C25 C26 0.8(11) . . . . ? 
C23 C24 C25 C26 179.6(7) . . . . ? 
C24 C25 C26 C27 -1.3(12) . . . . ? 
C25 C26 C27 C28 1.1(13) . . . . ? 
C26 C27 C28 C29 -0.3(13) . . . . ? 
C25 C24 C29 C28 -0.1(11) . . . . ? 
C23 C24 C29 C28 -178.8(7) . . . . ? 
C27 C28 C29 C24 -0.2(12) . . . . ? 
C23 N2 C30 C31 -69.8(6) . . . . ? 
C22 N2 C30 C31 161.7(5) . . . . ? 
N2 C30 C31 C36 137.2(6) . . . . ? 
N2 C30 C31 C32 -47.7(8) . . . . ? 
Nd O3 C32 C31 -91.9(7) . . . . ? 
Nd O3 C32 C33 89.7(7) . . . . ? 
C36 C31 C32 O3 176.1(6) . . . . ? 
C30 C31 C32 O3 1.0(9) . . . . ? 
C36 C31 C32 C33 -5.5(9) . . . . ? 
C30 C31 C32 C33 179.5(6) . . . . ? 
O3 C32 C33 C34 -175.7(6) . . . . ? 
C31 C32 C33 C34 5.9(9) . . . . ? 
O3 C32 C33 C37 -4.9(9) . . . . ? 
C31 C32 C33 C37 176.7(6) . . . . ? 
C32 C33 C34 C35 -2.5(10) . . . . ? 
C37 C33 C34 C35 -173.6(6) . . . . ? 
C33 C34 C35 C36 -1.5(10) . . . . ? 
C33 C34 C35 Cl3 175.6(5) . . . . ? 
C34 C35 C36 C31 2.0(10) . . . . ? 
Cl3 C35 C36 C31 -175.1(5) . . . . ? 
C32 C31 C36 C35 1.6(9) . . . . ? 
C30 C31 C36 C35 176.6(6) . . . . ? 
C34 C33 C37 N3 -147.4(6) . . . . ? 
C32 C33 C37 N3 41.6(8) . . . . ? 
C38 N3 C37 C33 64.1(7) . . . . ? 
C45 N3 C37 C33 -164.9(5) . . . . ? 
C37 N3 C38 C39 62.5(7) . . . . ? 
C45 N3 C38 C39 -65.6(6) . . . . ? 
N3 C38 C39 C40 -90.7(7) . . . . ? 
N3 C38 C39 C44 95.0(7) . . . . ? 
C44 C39 C40 C41 -3.1(10) . . . . ? 
C38 C39 C40 C41 -177.5(6) . . . . ? 
C39 C40 C41 C42 1.6(11) . . . . ? 
C40 C41 C42 C43 -0.1(11) . . . . ? 
C41 C42 C43 C44 0.2(12) . . . . ? 
C42 C43 C44 C39 -1.7(11) . . . . ? 
C40 C39 C44 C43 3.2(10) . . . . ? 
C38 C39 C44 C43 177.6(6) . . . . ? 
C5 C6 C45 N3 134.8(6) . . . . ? 
C1 C6 C45 N3 -50.7(8) . . . . ? 
C38 N3 C45 C6 -63.6(6) . . . . ? 
C37 N3 C45 C6 165.2(5) . . . . ? 
C50 N7 C46 C47 2.0(11) . . . . ? 
N7 C46 C47 C48 -2.4(12) . . . . ? 
C46 C47 C48 C49 0.9(13) . . . . ? 
C47 C48 C49 C50 0.8(13) . . . . ? 
C46 N7 C50 C49 -0.2(12) . . . . ? 
C48 C49 C50 N7 -1.2(13) . . . . ?