# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/159 data_p4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H72 Cl8 Gd6 O73' _chemical_formula_weight 2467.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/mnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 14.2740(8) _cell_length_b 14.2140(6) _cell_length_c 15.1040(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3064.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 6.895 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.246 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1404 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1404 _reflns_number_gt 1370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+33.8989P] 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 1404 _refine_ls_number_parameters 128 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1726 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.033 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.83535(7) 0.06665(7) 0.0000 0.0529(4) Uani 1 2 d SU . . Gd2 Gd 1.0000 0.0000 0.16849(8) 0.0546(4) Uani 1 4 d SU . . Cl1 Cl 0.7505(13) 0.0166(10) 0.5000 0.209(7) Uani 1 2 d SDU . . Cl2 Cl 0.8217(5) 0.3217(5) 0.2500 0.114(3) Uani 1 2 d SDU . . O1 O 1.0000 0.0000 0.0000 0.052(4) Uani 1 8 d SU . . O2 O 0.8622(6) -0.0582(6) -0.1004(6) 0.057(2) Uani 1 1 d U . . O3 O 0.6844(11) -0.0227(13) 0.0000 0.085(4) Uani 1 2 d SU . . O4 O 0.7378(9) 0.1065(10) 0.1322(8) 0.087(3) Uani 1 1 d U . . O5 O 0.7885(11) 0.2389(10) 0.0000 0.075(4) Uani 1 2 d SU . . O6 O 0.8714(10) 0.0489(10) 0.2717(8) 0.104(5) Uani 1 1 d U . . O7 O 0.558(3) 0.093(5) 0.187(5) 0.24(3) Uani 0.50 1 d PU . . O7' O 0.555(2) 0.040(4) 0.122(4) 0.170(18) Uani 0.50 1 d PU . . O8 O 0.832(3) -0.045(3) 0.5000 0.38(3) Uani 1 2 d SDU . . O9 O 0.663(3) -0.034(4) 0.5000 0.38(4) Uani 1 2 d SDU . . O10 O 0.755(3) 0.0856(16) 0.570(2) 0.25(2) Uani 0.50 1 d PDU . . O10' O 0.678(6) 0.029(5) 0.570(5) 0.27(2) Uani 0.50 1 d PU . . O11 O 0.813(2) 0.2422(13) 0.3138(16) 0.236(14) Uani 1 1 d DU . . O12 O 0.8117(17) 0.4070(11) 0.2963(15) 0.186(10) Uani 1 1 d DU . . 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 Gd1 0.0526(6) 0.0539(6) 0.0522(6) 0.000 0.000 0.0016(4) Gd2 0.0609(6) 0.0609(6) 0.0421(7) 0.000 0.000 0.000 Cl1 0.247(18) 0.119(9) 0.259(19) 0.000 0.000 -0.020(10) Cl2 0.114(3) 0.114(3) 0.112(5) -0.035(3) 0.035(3) 0.020(5) O1 0.051(5) 0.051(5) 0.052(7) 0.000 0.000 0.000 O2 0.050(5) 0.060(5) 0.060(5) -0.009(4) -0.013(4) 0.001(4) O3 0.059(6) 0.086(9) 0.110(11) 0.000 0.000 -0.013(7) O4 0.090(8) 0.093(8) 0.078(6) -0.009(5) 0.028(6) 0.007(7) O5 0.076(9) 0.059(6) 0.090(9) 0.000 0.000 0.015(6) O6 0.113(10) 0.117(11) 0.082(8) -0.011(7) 0.036(7) 0.013(9) O7 0.11(3) 0.27(7) 0.33(8) -0.11(5) 0.04(4) 0.04(4) O7' 0.055(17) 0.22(5) 0.23(5) -0.02(4) 0.02(3) 0.00(2) O8 0.45(5) 0.12(3) 0.56(8) 0.000 0.000 0.11(3) O9 0.41(4) 0.28(7) 0.46(12) 0.000 0.000 -0.21(4) O10 0.39(6) 0.037(15) 0.31(4) 0.008(19) 0.05(4) -0.05(2) O10' 0.31(5) 0.24(6) 0.25(6) 0.10(4) 0.05(5) -0.07(3) O11 0.31(4) 0.181(15) 0.22(2) 0.036(15) 0.12(2) 0.06(2) O12 0.20(2) 0.151(12) 0.21(2) -0.091(14) 0.083(18) -0.005(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.365(9) . ? Gd1 O2 2.365(9) 10 ? Gd1 O2 2.373(9) 11_665 ? Gd1 O2 2.373(9) 4_665 ? Gd1 O4 2.500(11) 10 ? Gd1 O4 2.500(11) . ? Gd1 O3 2.501(16) . ? Gd1 O1 2.5340(10) . ? Gd1 O5 2.538(14) . ? Gd1 Gd1 3.5729(15) 3_645 ? Gd1 Gd1 3.5834(15) 11_665 ? Gd1 Gd2 3.5913(11) 9_755 ? Gd2 O2 2.362(10) 11_665 ? Gd2 O2 2.362(10) 12_645 ? Gd2 O2 2.368(10) 10 ? Gd2 O2 2.368(10) 9_755 ? Gd2 O6 2.501(12) 4_665 ? Gd2 O6 2.501(12) 3_645 ? Gd2 O6 2.506(12) . ? Gd2 O6 2.506(12) 2_755 ? Gd2 O1 2.5449(12) . ? Gd2 Gd1 3.5859(11) 3_645 ? Gd2 Gd1 3.5859(11) 11_665 ? Gd2 Gd1 3.5913(11) 9_755 ? Cl1 O10 1.447(17) . ? Cl1 O10 1.447(17) 10_556 ? Cl1 O9 1.447(17) . ? Cl1 O8 1.454(17) . ? Cl1 O10' 1.49(8) 10_556 ? Cl1 O10' 1.49(8) . ? Cl2 O12 1.407(13) . ? Cl2 O12 1.412(13) 7_545 ? Cl2 O11 1.489(15) . ? Cl2 O11 1.492(15) 7_545 ? O1 Gd1 2.5263(10) 11_665 ? O1 Gd1 2.5263(10) 3_645 ? O1 Gd1 2.5340(10) 9_755 ? O1 Gd2 2.5449(12) 9_755 ? O2 Gd2 2.368(10) 9_755 ? O2 Gd1 2.371(9) 3_645 ? O7 O7' 1.23(6) . ? O9 O10' 1.41(9) . ? O9 O10' 1.41(9) 10_556 ? O10 O10' 1.36(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O2 79.8(5) . 10 ? O2 Gd1 O2 128.7(4) . 11_665 ? O2 Gd1 O2 78.8(5) 10 11_665 ? O2 Gd1 O2 78.8(5) . 4_665 ? O2 Gd1 O2 128.7(4) 10 4_665 ? O2 Gd1 O2 79.4(5) 11_665 4_665 ? O2 Gd1 O4 75.4(4) . 10 ? O2 Gd1 O4 140.6(4) 10 10 ? O2 Gd1 O4 140.4(4) 11_665 10 ? O2 Gd1 O4 75.5(4) 4_665 10 ? O2 Gd1 O4 140.6(4) . . ? O2 Gd1 O4 75.4(4) 10 . ? O2 Gd1 O4 75.5(4) 11_665 . ? O2 Gd1 O4 140.4(4) 4_665 . ? O4 Gd1 O4 106.0(6) 10 . ? O2 Gd1 O3 76.1(4) . . ? O2 Gd1 O3 76.1(4) 10 . ? O2 Gd1 O3 140.2(2) 11_665 . ? O2 Gd1 O3 140.2(2) 4_665 . ? O4 Gd1 O3 68.6(4) 10 . ? O4 Gd1 O3 68.6(4) . . ? O2 Gd1 O1 64.5(2) . . ? O2 Gd1 O1 64.5(2) 10 . ? O2 Gd1 O1 64.2(2) 11_665 . ? O2 Gd1 O1 64.2(2) 4_665 . ? O4 Gd1 O1 127.0(3) 10 . ? O4 Gd1 O1 127.0(3) . . ? O3 Gd1 O1 127.5(4) . . ? O2 Gd1 O5 140.0(2) . . ? O2 Gd1 O5 140.0(2) 10 . ? O2 Gd1 O5 76.0(4) 11_665 . ? O2 Gd1 O5 76.0(4) 4_665 . ? O4 Gd1 O5 68.6(4) 10 . ? O4 Gd1 O5 68.6(4) . . ? O3 Gd1 O5 105.2(6) . . ? O1 Gd1 O5 127.2(4) . . ? O2 Gd1 Gd1 41.1(2) . 3_645 ? O2 Gd1 Gd1 41.1(2) 10 3_645 ? O2 Gd1 Gd1 98.1(2) 11_665 3_645 ? O2 Gd1 Gd1 98.1(2) 4_665 3_645 ? O4 Gd1 Gd1 115.3(3) 10 3_645 ? O4 Gd1 Gd1 115.3(3) . 3_645 ? O3 Gd1 Gd1 82.5(4) . 3_645 ? O1 Gd1 Gd1 45.0 . 3_645 ? O5 Gd1 Gd1 172.2(4) . 3_645 ? O2 Gd1 Gd1 98.2(2) . 11_665 ? O2 Gd1 Gd1 98.2(2) 10 11_665 ? O2 Gd1 Gd1 40.9(2) 11_665 11_665 ? O2 Gd1 Gd1 40.9(2) 4_665 11_665 ? O4 Gd1 Gd1 115.2(3) 10 11_665 ? O4 Gd1 Gd1 115.2(3) . 11_665 ? O3 Gd1 Gd1 172.4(4) . 11_665 ? O1 Gd1 Gd1 44.830(1) . 11_665 ? O5 Gd1 Gd1 82.4(4) . 11_665 ? Gd1 Gd1 Gd1 89.827(1) 3_645 11_665 ? O2 Gd1 Gd2 40.7(2) . 9_755 ? O2 Gd1 Gd2 98.6(2) 10 9_755 ? O2 Gd1 Gd2 98.4(2) 11_665 9_755 ? O2 Gd1 Gd2 40.6(2) 4_665 9_755 ? O4 Gd1 Gd2 81.9(3) 10 9_755 ? O4 Gd1 Gd2 172.1(3) . 9_755 ? O3 Gd1 Gd2 115.5(3) . 9_755 ? O1 Gd1 Gd2 45.124(18) . 9_755 ? O5 Gd1 Gd2 115.3(2) . 9_755 ? Gd1 Gd1 Gd2 60.070(10) 3_645 9_755 ? Gd1 Gd1 Gd2 59.973(10) 11_665 9_755 ? O2 Gd2 O2 128.4(4) 11_665 12_645 ? O2 Gd2 O2 78.96(18) 11_665 10 ? O2 Gd2 O2 79.25(18) 12_645 10 ? O2 Gd2 O2 79.25(18) 11_665 9_755 ? O2 Gd2 O2 78.96(18) 12_645 9_755 ? O2 Gd2 O2 128.5(4) 10 9_755 ? O2 Gd2 O6 76.3(4) 11_665 4_665 ? O2 Gd2 O6 141.1(4) 12_645 4_665 ? O2 Gd2 O6 139.2(4) 10 4_665 ? O2 Gd2 O6 77.5(4) 9_755 4_665 ? O2 Gd2 O6 141.1(4) 11_665 3_645 ? O2 Gd2 O6 76.3(4) 12_645 3_645 ? O2 Gd2 O6 77.5(4) 10 3_645 ? O2 Gd2 O6 139.2(4) 9_755 3_645 ? O6 Gd2 O6 102.9(7) 4_665 3_645 ? O2 Gd2 O6 77.5(4) 11_665 . ? O2 Gd2 O6 139.3(4) 12_645 . ? O2 Gd2 O6 76.0(4) 10 . ? O2 Gd2 O6 141.4(4) 9_755 . ? O6 Gd2 O6 67.3(4) 4_665 . ? O6 Gd2 O6 67.1(4) 3_645 . ? O2 Gd2 O6 139.3(4) 11_665 2_755 ? O2 Gd2 O6 77.5(4) 12_645 2_755 ? O2 Gd2 O6 141.4(4) 10 2_755 ? O2 Gd2 O6 76.0(4) 9_755 2_755 ? O6 Gd2 O6 67.1(4) 4_665 2_755 ? O6 Gd2 O6 67.3(4) 3_645 2_755 ? O6 Gd2 O6 103.1(7) . 2_755 ? O2 Gd2 O1 64.2(2) 11_665 . ? O2 Gd2 O1 64.2(2) 12_645 . ? O2 Gd2 O1 64.3(2) 10 . ? O2 Gd2 O1 64.3(2) 9_755 . ? O6 Gd2 O1 128.6(3) 4_665 . ? O6 Gd2 O1 128.6(3) 3_645 . ? O6 Gd2 O1 128.5(3) . . ? O6 Gd2 O1 128.5(3) 2_755 . ? O2 Gd2 Gd1 98.0(2) 11_665 3_645 ? O2 Gd2 Gd1 40.8(2) 12_645 3_645 ? O2 Gd2 Gd1 40.9(2) 10 3_645 ? O2 Gd2 Gd1 98.0(2) 9_755 3_645 ? O6 Gd2 Gd1 173.3(3) 4_665 3_645 ? O6 Gd2 Gd1 83.8(3) 3_645 3_645 ? O6 Gd2 Gd1 115.4(3) . 3_645 ? O6 Gd2 Gd1 117.0(3) 2_755 3_645 ? O1 Gd2 Gd1 44.790(18) . 3_645 ? O2 Gd2 Gd1 40.8(2) 11_665 11_665 ? O2 Gd2 Gd1 98.0(2) 12_645 11_665 ? O2 Gd2 Gd1 98.0(2) 10 11_665 ? O2 Gd2 Gd1 40.9(2) 9_755 11_665 ? O6 Gd2 Gd1 83.8(3) 4_665 11_665 ? O6 Gd2 Gd1 173.3(3) 3_645 11_665 ? O6 Gd2 Gd1 117.0(3) . 11_665 ? O6 Gd2 Gd1 115.4(3) 2_755 11_665 ? O1 Gd2 Gd1 44.790(18) . 11_665 ? Gd1 Gd2 Gd1 89.58(4) 3_645 11_665 ? O2 Gd2 Gd1 98.1(2) 11_665 9_755 ? O2 Gd2 Gd1 40.8(2) 12_645 9_755 ? O2 Gd2 Gd1 98.3(2) 10 9_755 ? O2 Gd2 Gd1 40.6(2) 9_755 9_755 ? O6 Gd2 Gd1 116.9(3) 4_665 9_755 ? O6 Gd2 Gd1 115.6(3) 3_645 9_755 ? O6 Gd2 Gd1 173.3(3) . 9_755 ? O6 Gd2 Gd1 83.6(3) 2_755 9_755 ? O1 Gd2 Gd1 44.876(18) . 9_755 ? Gd1 Gd2 Gd1 59.90(2) 3_645 9_755 ? Gd1 Gd2 Gd1 59.71(2) 11_665 9_755 ? O10 Cl1 O10 94(3) . 10_556 ? O10 Cl1 O9 112.1(15) . . ? O10 Cl1 O9 112.1(15) 10_556 . ? O10 Cl1 O8 112.2(15) . . ? O10 Cl1 O8 112.2(15) 10_556 . ? O9 Cl1 O8 112.6(15) . . ? O10 Cl1 O10' 118(4) . 10_556 ? O10 Cl1 O10' 55(3) 10_556 10_556 ? O9 Cl1 O10' 57(3) . 10_556 ? O8 Cl1 O10' 128(3) . 10_556 ? O10 Cl1 O10' 55(3) . . ? O10 Cl1 O10' 118(4) 10_556 . ? O9 Cl1 O10' 57(3) . . ? O8 Cl1 O10' 128(3) . . ? O10' Cl1 O10' 91(7) 10_556 . ? O12 Cl2 O12 114.8(19) . 7_545 ? O12 Cl2 O11 108.9(11) . . ? O12 Cl2 O11 108.3(16) 7_545 . ? O12 Cl2 O11 108.2(16) . 7_545 ? O12 Cl2 O11 109.2(11) 7_545 7_545 ? O11 Cl2 O11 107(3) . 7_545 ? Gd1 O1 Gd1 180.000(17) 11_665 3_645 ? Gd1 O1 Gd1 90.168(1) 11_665 . ? Gd1 O1 Gd1 89.832(1) 3_645 . ? Gd1 O1 Gd1 89.8 11_665 9_755 ? Gd1 O1 Gd1 90.2 3_645 9_755 ? Gd1 O1 Gd1 180.00(4) . 9_755 ? Gd1 O1 Gd2 90.0 11_665 . ? Gd1 O1 Gd2 90.0 3_645 . ? Gd1 O1 Gd2 90.0 . . ? Gd1 O1 Gd2 90.0 9_755 . ? Gd1 O1 Gd2 90.0 11_665 9_755 ? Gd1 O1 Gd2 90.0 3_645 9_755 ? Gd1 O1 Gd2 90.0 . 9_755 ? Gd1 O1 Gd2 90.0 9_755 9_755 ? Gd2 O1 Gd2 180.0 . 9_755 ? Gd1 O2 Gd2 98.7(3) . 9_755 ? Gd1 O2 Gd1 97.9(3) . 3_645 ? Gd2 O2 Gd1 98.3(3) 9_755 3_645 ? O10' O9 O10' 98(6) . 10_556 ? O10' O9 Cl1 63(3) . . ? O10' O9 Cl1 63(3) 10_556 . ? O10' O10 Cl1 64(4) . . ? O10 O10' O9 120(6) . . ? O10 O10' Cl1 61(3) . . ? O9 O10' Cl1 60(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.219 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.319 data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H72 Cl8 Nd6 O73' _chemical_formula_weight 2389.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' '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 Tetragonal _symmetry_space_group_name_H-M P4/mnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 14.5147(7) _cell_length_b 14.5079(7) _cell_length_c 15.2546(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3212.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 5.233 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8323 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11881 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.05 _reflns_number_total 2021 _reflns_number_gt 1641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2021 _refine_ls_number_parameters 147 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.83218(2) 0.06725(2) 0.0000 0.03707(13) Uani 1 2 d S . . Nd2 Nd 1.0000 0.0000 0.17196(3) 0.03962(16) Uani 1 4 d S . . Cl1 Cl 0.7469(5) 0.0156(4) 0.5000 0.188(2) Uani 1 2 d SD . . Cl2 Cl 0.82176(16) 0.32176(16) 0.2500 0.0931(9) Uani 1 2 d SD . . O1 O 1.0000 0.0000 0.0000 0.0313(17) Uani 1 8 d S . . O2 O 0.8618(2) -0.0592(2) -0.1009(2) 0.0399(7) Uani 1 1 d . . . O3 O 0.6805(4) -0.0233(5) 0.0000 0.0769(18) Uani 1 2 d S . . O4 O 0.7343(3) 0.1063(3) 0.1345(3) 0.0777(13) Uani 1 1 d . . . O5 O 0.7846(4) 0.2399(4) 0.0000 0.0679(16) Uani 1 2 d S . . O6 O 0.8684(4) 0.0491(4) 0.2738(4) 0.1008(18) Uani 1 1 d . . . O7 O 0.5505(18) 0.0478(18) 0.130(2) 0.212(12) Uani 0.50 1 d PU . . O7' O 0.556(2) 0.098(3) 0.187(3) 0.34(3) Uani 0.50 1 d PU . . O8 O 0.7450(16) 0.0823(15) 0.4277(19) 0.31(3) Uani 0.50 1 d PDU . . O8' O 0.7456(18) 0.0801(16) 0.4266(16) 0.38(3) Uani 0.50 1 d PDU . . O11 O 0.7981(15) 0.4010(12) 0.292(2) 0.115(9) Uani 0.50 1 d PDU . . O11' O 0.8317(19) 0.3985(14) 0.304(2) 0.158(13) Uani 0.50 1 d PDU . . O12 O 0.856(3) 0.2505(19) 0.311(3) 0.45(4) Uani 0.50 1 d PDU . . O12' O 0.7990(12) 0.2412(8) 0.3036(10) 0.128(6) Uani 0.50 1 d PDU . . O10 O 0.6633(14) -0.0355(15) 0.5000 0.322(15) Uani 1 2 d SDU . . O9 O 0.8294(16) -0.0384(14) 0.5000 0.66(4) Uani 1 2 d SDU . . 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 0.0337(2) 0.0363(2) 0.0412(2) 0.000 0.000 0.00150(14) Nd2 0.0448(2) 0.0448(2) 0.0293(2) 0.000 0.000 0.000 Cl1 0.241(7) 0.094(3) 0.227(7) 0.000 0.000 -0.021(4) Cl2 0.0915(12) 0.0915(12) 0.0965(18) -0.0320(10) 0.0320(10) 0.0184(15) O1 0.033(3) 0.033(3) 0.028(4) 0.000 0.000 0.000 O2 0.0439(17) 0.0405(17) 0.0352(16) -0.0011(12) -0.0061(14) -0.0023(13) O3 0.052(3) 0.080(4) 0.099(5) 0.000 0.000 -0.016(3) O4 0.065(3) 0.081(3) 0.087(3) -0.010(3) 0.030(2) 0.005(2) O5 0.067(4) 0.049(3) 0.088(4) 0.000 0.000 0.018(3) O6 0.112(4) 0.111(4) 0.080(4) -0.008(3) 0.046(3) 0.015(3) O7 0.139(17) 0.19(2) 0.31(3) 0.01(2) 0.10(2) 0.024(16) O7' 0.112(17) 0.40(5) 0.50(7) -0.20(4) 0.08(3) 0.03(2) O8 0.40(5) 0.15(2) 0.37(5) 0.07(2) 0.15(4) -0.12(3) O8' 0.63(6) 0.39(5) 0.119(18) 0.05(2) 0.06(3) 0.38(5) O11 0.075(11) 0.104(11) 0.165(19) -0.079(12) 0.064(12) -0.019(8) O11' 0.14(3) 0.149(18) 0.18(2) -0.088(16) 0.032(19) 0.039(15) O12 0.51(7) 0.50(7) 0.35(5) 0.07(5) -0.16(5) -0.21(6) O12' 0.161(13) 0.070(7) 0.153(12) -0.006(8) 0.095(10) 0.003(8) O10 0.31(3) 0.28(2) 0.38(3) 0.000 0.000 -0.19(2) O9 0.98(7) 0.112(14) 0.88(7) 0.000 0.000 0.21(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 O2 2.431(3) 11_665 y Nd1 O2 2.431(3) 4_665 y Nd1 O2 2.433(3) . y Nd1 O2 2.433(3) 10 y Nd1 O4 2.559(4) 10 y Nd1 O4 2.559(4) . y Nd1 O3 2.564(6) . y Nd1 O5 2.598(6) . y Nd1 O1 2.6239(4) . y Nd2 O2 2.436(3) 11_665 y Nd2 O2 2.436(3) 12_645 y Nd2 O2 2.437(3) 10 y Nd2 O2 2.437(3) 9_755 y Nd2 O6 2.562(5) 4_665 y Nd2 O6 2.562(5) 3_645 y Nd2 O6 2.563(5) . y Nd2 O6 2.563(5) 2_755 y Nd2 O1 2.6232(5) . y Cl1 O10 1.422(13) . ? Cl1 O9 1.431(14) . ? Cl1 O8' 1.460(13) 10_556 ? Cl1 O8' 1.460(13) . ? Cl1 O8 1.468(14) . ? Cl1 O8 1.468(14) 10_556 ? Cl2 O11 1.363(13) . ? Cl2 O11 1.364(13) 7_545 ? Cl2 O11' 1.393(17) . ? Cl2 O11' 1.393(17) 7_545 ? Cl2 O12' 1.464(11) . ? Cl2 O12' 1.464(11) 7_545 ? Cl2 O12 1.475(19) . ? Cl2 O12 1.476(19) 7_545 ? O1 Nd1 2.6231(4) 11_665 ? O1 Nd1 2.6231(4) 3_645 ? O1 Nd2 2.6232(5) 9_755 ? O1 Nd1 2.6239(3) 9_755 ? O2 Nd1 2.431(3) 3_645 ? O2 Nd2 2.437(3) 9_755 ? 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 Nd1 O2 78.54(15) 11_665 4_665 y O2 Nd1 O2 127.24(14) 11_665 . y O2 Nd1 O2 78.73(15) 4_665 . y O2 Nd1 O2 78.73(15) 11_665 10 y O2 Nd1 O2 127.24(14) 4_665 10 y O2 Nd1 O2 78.47(14) . 10 y O2 Nd1 O4 140.67(13) 11_665 10 y O2 Nd1 O4 76.03(14) 4_665 10 y O2 Nd1 O4 75.99(14) . 10 y O2 Nd1 O4 140.54(14) 10 10 y O2 Nd1 O4 76.03(14) 11_665 . y O2 Nd1 O4 140.67(13) 4_665 . y O2 Nd1 O4 140.54(14) . . y O2 Nd1 O4 75.99(14) 10 . y O4 Nd1 O4 106.6(2) 10 . y O2 Nd1 O3 140.67(7) 11_665 . y O2 Nd1 O3 140.67(7) 4_665 . y O2 Nd1 O3 76.41(14) . . y O2 Nd1 O3 76.41(14) 10 . y O4 Nd1 O3 68.71(14) 10 . y O4 Nd1 O3 68.71(14) . . y O2 Nd1 O5 76.35(13) 11_665 . y O2 Nd1 O5 76.35(13) 4_665 . y O2 Nd1 O5 140.71(7) . . y O2 Nd1 O5 140.71(7) 10 . y O4 Nd1 O5 68.84(13) 10 . y O4 Nd1 O5 68.84(13) . . y O3 Nd1 O5 105.4(2) . . y O2 Nd1 O1 63.63(8) 11_665 . y O2 Nd1 O1 63.63(8) 4_665 . y O2 Nd1 O1 63.62(8) . . y O2 Nd1 O1 63.62(8) 10 . y O4 Nd1 O1 126.70(12) 10 . y O4 Nd1 O1 126.70(12) . . y O3 Nd1 O1 127.33(16) . . y O5 Nd1 O1 127.24(14) . . y O2 Nd2 O2 127.15(15) 11_665 12_645 y O2 Nd2 O2 78.57(6) 11_665 10 y O2 Nd2 O2 78.60(6) 12_645 10 y O2 Nd2 O2 78.60(6) 11_665 9_755 y O2 Nd2 O2 78.57(6) 12_645 9_755 y O2 Nd2 O2 127.17(15) 10 9_755 y O2 Nd2 O6 75.82(16) 11_665 4_665 y O2 Nd2 O6 141.69(14) 12_645 4_665 y O2 Nd2 O6 139.60(14) 10 4_665 y O2 Nd2 O6 77.17(16) 9_755 4_665 y O2 Nd2 O6 141.69(14) 11_665 3_645 y O2 Nd2 O6 75.82(16) 12_645 3_645 y O2 Nd2 O6 77.17(16) 10 3_645 y O2 Nd2 O6 139.60(14) 9_755 3_645 y O6 Nd2 O6 105.3(3) 4_665 3_645 y O2 Nd2 O6 77.17(16) 11_665 . y O2 Nd2 O6 139.61(14) 12_645 . y O2 Nd2 O6 75.78(16) 10 . y O2 Nd2 O6 141.72(14) 9_755 . y O6 Nd2 O6 68.45(16) 4_665 . y O6 Nd2 O6 68.42(16) 3_645 . y O2 Nd2 O6 139.61(14) 11_665 2_755 y O2 Nd2 O6 77.17(16) 12_645 2_755 y O2 Nd2 O6 141.72(14) 10 2_755 y O2 Nd2 O6 75.78(16) 9_755 2_755 y O6 Nd2 O6 68.42(16) 4_665 2_755 y O6 Nd2 O6 68.45(16) 3_645 2_755 y O6 Nd2 O6 105.4(3) . 2_755 y O2 Nd2 O1 63.58(7) 11_665 . y O2 Nd2 O1 63.58(7) 12_645 . y O2 Nd2 O1 63.58(7) 10 . y O2 Nd2 O1 63.58(7) 9_755 . y O6 Nd2 O1 127.33(15) 4_665 . y O6 Nd2 O1 127.33(15) 3_645 . y O6 Nd2 O1 127.32(15) . . y O6 Nd2 O1 127.32(15) 2_755 . y O6 Nd2 Nd1 114.55(13) 3_645 9_755 ? O6 Nd2 Nd1 172.26(15) . 9_755 ? O6 Nd2 Nd1 82.32(15) 2_755 9_755 ? O1 Nd2 Nd1 45.009(6) . 9_755 ? Nd1 Nd2 Nd1 60.015(7) 3_645 9_755 y Nd1 Nd2 Nd1 59.993(7) 11_665 9_755 y O10 Cl1 O9 115.4(10) . . ? O10 Cl1 O8' 108.9(13) . 10_556 ? O9 Cl1 O8' 111.2(10) . 10_556 ? O10 Cl1 O8' 108.9(13) . . ? O9 Cl1 O8' 111.2(11) . . ? O8' Cl1 O8' 100(2) 10_556 . ? O10 Cl1 O8 109.2(11) . . ? O9 Cl1 O8 112.1(12) . . ? O8' Cl1 O8 98.8(12) 10_556 . ? O8' Cl1 O8 1(2) . . ? O10 Cl1 O8 109.2(11) . 10_556 ? O9 Cl1 O8 112.1(12) . 10_556 ? O8' Cl1 O8 1(2) 10_556 10_556 ? O8' Cl1 O8 98.8(12) . 10_556 ? O8 Cl1 O8 97(3) . 10_556 ? O11 Cl2 O11 130.6(17) . 7_545 ? O11 Cl2 O11' 22(2) . . ? O11 Cl2 O11' 113.2(10) 7_545 . ? O11 Cl2 O11' 113.3(10) . 7_545 ? O11 Cl2 O11' 22(2) 7_545 7_545 ? O11' Cl2 O11' 101(2) . 7_545 ? O11 Cl2 O12' 110.5(14) . . ? O11 Cl2 O12' 104.7(13) 7_545 . ? O11' Cl2 O12' 109.3(15) . . ? O11' Cl2 O12' 126.4(14) 7_545 . ? O11 Cl2 O12' 104.7(13) . 7_545 ? O11 Cl2 O12' 110.6(14) 7_545 7_545 ? O11' Cl2 O12' 126.4(14) . 7_545 ? O11' Cl2 O12' 109.4(15) 7_545 7_545 ? O12' Cl2 O12' 87.3(16) . 7_545 ? O11 Cl2 O12 112.2(17) . . ? O11 Cl2 O12 81(2) 7_545 . ? O11' Cl2 O12 99(3) . . ? O11' Cl2 O12 100(3) 7_545 . ? O12' Cl2 O12 33.5(19) . . ? O12' Cl2 O12 117.6(15) 7_545 . ? O11 Cl2 O12 81(2) . 7_545 ? O11 Cl2 O12 112.2(17) 7_545 7_545 ? O11' Cl2 O12 100(3) . 7_545 ? O11' Cl2 O12 99(3) 7_545 7_545 ? O12' Cl2 O12 117.6(16) . 7_545 ? O12' Cl2 O12 33.5(19) 7_545 7_545 ? O12 Cl2 O12 150(3) . 7_545 ? Nd1 O1 Nd1 180.0 11_665 3_645 ? Nd1 O1 Nd2 90.0 11_665 9_755 ? Nd1 O1 Nd2 90.0 3_645 9_755 ? Nd1 O1 Nd2 90.0 11_665 . ? Nd1 O1 Nd2 90.0 3_645 . ? Nd2 O1 Nd2 180.0 9_755 . ? Nd1 O1 Nd1 90.0 11_665 . ? Nd1 O1 Nd1 90.0 3_645 . ? Nd2 O1 Nd1 90.0 9_755 . ? Nd2 O1 Nd1 90.0 . . ? Nd1 O1 Nd1 90.0 11_665 9_755 ? Nd1 O1 Nd1 90.0 3_645 9_755 ? Nd2 O1 Nd1 90.0 9_755 9_755 ? Nd2 O1 Nd1 90.0 . 9_755 ? Nd1 O1 Nd1 180.000(14) . 9_755 ? Nd1 O2 Nd1 99.39(11) 3_645 . ? Nd1 O2 Nd2 99.29(12) 3_645 9_755 ? Nd1 O2 Nd2 99.25(11) . 9_755 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.085 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.146