# 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: 440/228 data_wt0131w-Winnie025 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 24 18:20:06 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.993(1) _cell_length_b 10.993(1) _cell_length_c 21.554(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2255.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3 c 1 ' _symmetry_Int_Tables_number 158 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -y, +x-y, +z' ' -x+y, -x, +z' ' -y, -x,1/2+z' ' +x, +x-y,1/2+z' ' -x+y, +y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_meas ? _chemical_formula_weight 1010.02 _chemical_formula_analytical ? _chemical_formula_sum 'C35 H45 N8 Nd O18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1030.00 _exptl_absorpt_coefficient_mu 1.229 _exptl_absorpt_correction_type 'smart ccd abs' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'ccd' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 6553 _reflns_number_total 1965 _reflns_number_observed 1158 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 5.61 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nd 0 2 -0.194 3.018 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 36 0.011 0.006 'International Tables' C 0 70 0.003 0.002 'International Tables' H 0 90 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Nd(1) 0.6667 0.3333 0.4429 0.04498(10) Uij ? ? O(1) 0.826(1) 0.516(1) 0.5108(4) 0.055(3) Uij ? ? O(2) 0.6848(8) 0.7481(9) 0.5653(4) 0.069(3) Uij ? ? O(3) 0.599(1) 0.759(1) 0.6817(5) 0.110(4) Uij ? ? O(4) 0.6504(9) 0.5533(8) 0.4204(4) 0.072(3) Uij ? ? O(5) 0.531(1) 0.374(1) 0.3591(4) 0.075(4) Uij ? ? O(6) 0.527(2) 0.572(2) 0.3490(7) 0.141(6) Uij ? ? N(1) 0.942(1) 0.754(1) 0.5124(5) 0.055(3) Uij ? ? N(2) 1.0000 1.0000 0.4298(6) 0.044(2) Uij ? ? N(3) 0.571(1) 0.501(2) 0.3739(6) 0.073(5) Uij ? ? N(4) 1.0000 1.0000 0.6061(7) 0.065(3) Uij ? ? C(1) 0.856(1) 0.627(1) 0.5373(6) 0.045(4) Uij ? ? C(2) 0.800(1) 0.6243(10) 0.6008(4) 0.046(3) Uij ? ? C(3) 0.720(1) 0.686(1) 0.6134(5) 0.052(3) Uij ? ? C(4) 0.673(1) 0.688(1) 0.6735(6) 0.065(4) Uij ? ? C(5) 0.709(2) 0.627(1) 0.7204(6) 0.083(5) Uij ? ? C(6) 0.788(2) 0.564(1) 0.7083(5) 0.075(4) Uij ? ? C(7) 0.832(1) 0.564(1) 0.6490(5) 0.064(4) Uij ? ? C(8) 0.541(2) 0.676(2) 0.5476(7) 0.097(6) Uij ? ? C(9) 0.574(2) 0.792(2) 0.7410(8) 0.116(6) Uij ? ? C(10) 1.002(1) 0.779(1) 0.4501(5) 0.054(3) Uij ? ? C(11) 0.9513(10) 0.854(1) 0.4091(4) 0.047(3) Uij ? ? C(12) 1.0000 1.0000 0.7268(9) 0.077(3) Uij ? ? C(13) 1.0000 1.0000 0.6567(9) 0.055(3) Uij ? ? H(1) 0.6788 0.6287 0.7616 0.0997 Uij ? ? H(2) 0.8120 0.5209 0.7407 0.0901 Uij ? ? H(3) 0.8858 0.5201 0.6409 0.0773 Uij ? ? H(4) 0.4845 0.6670 0.5824 0.1166 Uij ? ? H(5) 0.5164 0.5851 0.5326 0.1166 Uij ? ? H(6) 0.5264 0.7270 0.5158 0.1166 Uij ? ? H(7) 0.5206 0.8379 0.7380 0.1391 Uij ? ? H(8) 0.6615 0.8531 0.7607 0.1391 Uij ? ? H(9) 0.5243 0.7087 0.7647 0.1391 Uij ? ? H(10) 0.9555 0.8306 0.5259 0.0766 Uij ? ? H(11) 1.1015 0.8336 0.4533 0.0650 Uij ? ? H(12) 0.9772 0.6906 0.4317 0.0650 Uij ? ? H(13) 0.8515 0.8035 0.4090 0.0561 Uij ? ? H(14) 0.9848 0.8569 0.3682 0.0561 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nd(1) 0.0507(3) 0.0507 0.0336(3) 0.0253 0.0000 0.0000 O(1) 0.075(7) 0.045(6) 0.041(5) 0.027(5) 0.001(4) -0.001(4) O(2) 0.060(5) 0.089(6) 0.073(5) 0.049(5) 0.013(4) 0.023(5) O(3) 0.133(10) 0.108(8) 0.109(8) 0.074(7) 0.066(8) 0.015(7) O(4) 0.057(5) 0.054(5) 0.094(8) 0.021(5) -0.004(6) 0.012(5) O(5) 0.095(8) 0.079(8) 0.052(6) 0.046(6) -0.022(5) -0.006(5) O(6) 0.19(1) 0.12(1) 0.14(1) 0.11(1) -0.05(1) 0.02(1) N(1) 0.059(6) 0.042(6) 0.057(6) 0.020(5) 0.004(5) -0.004(5) N(2) 0.044(4) 0.0442 0.043(6) 0.0221 0.0000 0.0000 N(3) 0.083(10) 0.086(10) 0.054(8) 0.045(9) 0.007(7) 0.032(7) N(4) 0.071(7) 0.0709 0.053(9) 0.0355 0.0000 0.0000 C(1) 0.049(7) 0.057(8) 0.043(7) 0.036(6) -0.006(5) 0.000(6) C(2) 0.056(8) 0.040(5) 0.043(4) 0.024(6) 0.003(6) -0.001(4) C(3) 0.057(7) 0.044(6) 0.051(6) 0.023(6) 0.006(5) -0.002(5) C(4) 0.068(8) 0.054(7) 0.068(8) 0.027(7) 0.023(8) 0.004(7) C(5) 0.10(1) 0.069(10) 0.057(7) 0.022(9) 0.017(8) -0.007(7) C(6) 0.10(1) 0.090(9) 0.045(5) 0.050(10) -0.006(9) 0.006(6) C(7) 0.079(8) 0.078(9) 0.051(6) 0.051(7) -0.004(6) 0.003(6) C(8) 0.10(1) 0.13(2) 0.09(1) 0.08(1) 0.012(9) 0.01(1) C(9) 0.11(1) 0.08(1) 0.13(1) 0.03(1) 0.05(1) -0.01(1) C(10) 0.055(7) 0.048(6) 0.056(6) 0.023(5) 0.015(6) -0.004(5) C(11) 0.042(7) 0.057(6) 0.041(5) 0.025(5) 0.004(4) -0.004(4) C(12) 0.089(9) 0.0888 0.05(1) 0.0444 0.0000 0.0000 C(13) 0.044(6) 0.0444 0.07(1) 0.0222 0.0000 0.0000 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1158 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0422 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0435 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.242 _refine_ls_shift/esd_max 0.0440 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.47 _refine_diff_density_max 0.89 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd(1) O(1) 2.40(1) ? ? yes Nd(1) O(1) 2.40(1) ? ? yes Nd(1) O(1) 2.40(1) ? ? yes Nd(1) O(4) 2.559(8) ? ? yes Nd(1) O(4) 2.559(8) ? ? yes Nd(1) O(4) 2.559(8) ? ? yes Nd(1) O(5) 2.52(1) ? ? yes Nd(1) O(5) 2.52(1) ? ? yes Nd(1) O(5) 2.52(1) ? ? yes O(1) C(1) 1.23(2) ? ? yes O(2) C(3) 1.40(1) ? ? yes O(2) C(8) 1.42(2) ? ? yes O(3) C(4) 1.38(2) ? ? yes O(3) C(9) 1.40(2) ? ? yes O(4) N(3) 1.26(1) ? ? yes O(5) N(3) 1.27(2) ? ? yes O(6) N(3) 1.22(2) ? ? yes N(1) C(1) 1.34(1) ? ? yes N(1) C(10) 1.46(1) ? ? yes N(2) C(11) 1.48(1) ? ? yes N(2) C(11) 1.48(1) ? ? yes N(2) C(11) 1.48(1) ? ? yes N(4) C(13) 1.09(2) ? ? yes C(1) C(2) 1.50(1) ? ? yes C(2) C(3) 1.38(1) ? ? yes C(2) C(7) 1.37(1) ? ? yes C(3) C(4) 1.40(1) ? ? yes C(4) C(5) 1.38(2) ? ? yes C(5) C(6) 1.39(2) ? ? yes C(6) C(7) 1.36(2) ? ? yes C(10) C(11) 1.50(2) ? ? yes C(12) C(13) 1.51(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Nd(1) O(1) 86.5(3) ? ? ? yes O(1) Nd(1) O(1) 86.5(3) ? ? ? yes O(1) Nd(1) O(4) 71.9(3) ? ? ? yes O(1) Nd(1) O(4) 153.1(3) ? ? ? yes O(1) Nd(1) O(4) 76.5(3) ? ? ? yes O(1) Nd(1) O(5) 122.5(3) ? ? ? yes O(1) Nd(1) O(5) 149.1(3) ? ? ? yes O(1) Nd(1) O(5) 85.2(3) ? ? ? yes O(1) Nd(1) O(1) 86.5(3) ? ? ? yes O(1) Nd(1) O(4) 76.5(3) ? ? ? yes O(1) Nd(1) O(4) 71.9(3) ? ? ? yes O(1) Nd(1) O(4) 153.1(3) ? ? ? yes O(1) Nd(1) O(5) 85.2(3) ? ? ? yes O(1) Nd(1) O(5) 122.5(3) ? ? ? yes O(1) Nd(1) O(5) 149.1(3) ? ? ? yes O(1) Nd(1) O(4) 153.1(3) ? ? ? yes O(1) Nd(1) O(4) 76.5(3) ? ? ? yes O(1) Nd(1) O(4) 71.9(3) ? ? ? yes O(1) Nd(1) O(5) 149.1(3) ? ? ? yes O(1) Nd(1) O(5) 85.2(3) ? ? ? yes O(1) Nd(1) O(5) 122.5(3) ? ? ? yes O(4) Nd(1) O(4) 116.5(1) ? ? ? yes O(4) Nd(1) O(4) 116.5(1) ? ? ? yes O(4) Nd(1) O(5) 50.8(3) ? ? ? yes O(4) Nd(1) O(5) 121.5(4) ? ? ? yes O(4) Nd(1) O(5) 72.7(4) ? ? ? yes O(4) Nd(1) O(4) 116.5(1) ? ? ? yes O(4) Nd(1) O(5) 72.7(4) ? ? ? yes O(4) Nd(1) O(5) 50.8(3) ? ? ? yes O(4) Nd(1) O(5) 121.5(4) ? ? ? yes O(4) Nd(1) O(5) 121.5(4) ? ? ? yes O(4) Nd(1) O(5) 72.7(4) ? ? ? yes O(4) Nd(1) O(5) 50.8(3) ? ? ? yes O(5) Nd(1) O(5) 74.4(4) ? ? ? yes O(5) Nd(1) O(5) 74.4(4) ? ? ? yes O(5) Nd(1) O(5) 74.4(4) ? ? ? yes Nd(1) O(1) C(1) 146.5(9) ? ? ? yes C(3) O(2) C(8) 115.2(10) ? ? ? yes C(4) O(3) C(9) 120(1) ? ? ? yes Nd(1) O(4) N(3) 94.4(8) ? ? ? yes Nd(1) O(5) N(3) 95.9(9) ? ? ? yes C(1) N(1) C(10) 125(1) ? ? ? yes C(11) N(2) C(11) 111.3(5) ? ? ? yes C(11) N(2) C(11) 111.3(5) ? ? ? yes C(11) N(2) C(11) 111.3(5) ? ? ? yes O(4) N(3) O(5) 118(1) ? ? ? yes O(4) N(3) O(6) 117(1) ? ? ? yes O(5) N(3) O(6) 123(1) ? ? ? yes O(1) C(1) N(1) 122(1) ? ? ? yes O(1) C(1) C(2) 119(1) ? ? ? yes N(1) C(1) C(2) 117(1) ? ? ? yes C(1) C(2) C(3) 121.9(9) ? ? ? yes C(1) C(2) C(7) 120(1) ? ? ? yes C(3) C(2) C(7) 118.0(10) ? ? ? yes O(2) C(3) C(2) 119.4(9) ? ? ? yes O(2) C(3) C(4) 118(1) ? ? ? yes C(2) C(3) C(4) 121(1) ? ? ? yes O(3) C(4) C(3) 117(1) ? ? ? yes O(3) C(4) C(5) 124(1) ? ? ? yes C(3) C(4) C(5) 118(1) ? ? ? yes C(4) C(5) C(6) 120(1) ? ? ? yes C(5) C(6) C(7) 118(1) ? ? ? yes C(2) C(7) C(6) 122(1) ? ? ? yes N(1) C(10) C(11) 112.8(9) ? ? ? yes N(2) C(11) C(10) 112.8(8) ? ? ? yes N(4) C(13) C(12) 180.0000(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;