# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhmiao119@sina.com _publ_contact_author_name 'Ai-hua Yuan' loop_ _publ_author_name 'Hu Zhou' 'Guowang Diao' 'Suyan Qian' 'Xiaozhen Yang' 'Aihua Yuan' 'You Song' 'Yizhi Li' # Attachment '4-Nd.cif' data_yah146 _database_code_depnum_ccdc_archive 'CCDC 846239' #TrackingRef '4-Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 N9 Nd O4 W' _chemical_formula_weight 648.36 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2 ' 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' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 16.462(2) _cell_length_b 14.6853(16) _cell_length_c 14.8818(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3597.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6228 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 9.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1809 _exptl_absorpt_correction_T_max 0.2347 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 10879 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1594 _reflns_number_gt 1131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0193P)^2^+2.0131P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1594 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _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 C1 C 0.6492(4) 0.8893(4) 0.2643(4) 0.0335(14) Uani 1 1 d . . . C2 C 0.6717(4) 1.0905(4) 0.1923(4) 0.0342(14) Uani 1 1 d . . . C3 C 0.8254(3) 1.0503(4) 0.1444(4) 0.0317(14) Uani 1 1 d . . . C4 C 0.7828(4) 0.9245(3) 0.3745(4) 0.0308(13) Uani 1 1 d . . . C5 C 0.5000 0.5786(6) 0.5467(7) 0.043(2) Uani 1 2 d S . . H5A H 0.5000 0.6319 0.5805 0.051 Uiso 1 2 calc SR . . C6 C 0.5000 0.4932(5) 0.5909(6) 0.0338(19) Uani 1 2 d S . . H6A H 0.5000 0.4908 0.6534 0.041 Uiso 1 2 calc SR . . N1 N 0.5967(3) 0.8441(3) 0.2850(4) 0.0381(13) Uani 1 1 d . . . N2 N 0.6211(3) 1.1395(3) 0.1594(3) 0.0337(12) Uani 1 1 d . . . N3 N 0.8677(3) 1.0812(3) 0.0937(3) 0.0333(12) Uani 1 1 d . . . N4 N 0.7998(3) 0.8853(3) 0.4399(4) 0.0398(13) Uani 1 1 d . . . N5 N 0.5000 0.5838(5) 0.4565(5) 0.0335(17) Uani 1 2 d S . . Nd1 Nd 0.5000 0.74311(3) 0.37078(3) 0.03351(13) Uani 1 2 d S . . O1 O 0.5000 0.6868(4) 0.2100(4) 0.0430(16) Uani 1 2 d S . . H1X H 0.4465 0.6663 0.1943 0.052 Uiso 0.50 1 d PR . . H1Y H 0.5376 0.6371 0.2045 0.052 Uiso 0.50 1 d PR . . O2 O 0.5000 0.9025(4) 0.4391(4) 0.0368(15) Uani 1 2 d S . . H2X H 0.4656 0.9415 0.4039 0.044 Uiso 0.50 1 d PR . . H2Y H 0.4800 0.8999 0.4996 0.044 Uiso 0.50 1 d PR . . O3 O 0.5974(2) 0.7561(3) 0.4932(3) 0.0404(10) Uani 1 1 d . . . H3X H 0.6269 0.8121 0.4870 0.048 Uiso 1 1 d R . . H3Y H 0.6345 0.7057 0.4909 0.048 Uiso 1 1 d R . . W1 W 0.7500 0.98891(2) 0.2500 0.03396(11) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.032(3) 0.039(4) 0.010(3) 0.012(3) 0.014(2) C2 0.027(3) 0.030(3) 0.046(4) 0.007(3) 0.012(3) 0.011(3) C3 0.022(3) 0.041(3) 0.033(4) 0.007(3) -0.002(3) -0.006(3) C4 0.034(3) 0.024(3) 0.034(3) -0.003(2) 0.001(3) 0.015(2) C5 0.033(5) 0.045(5) 0.050(6) -0.005(5) 0.000 0.000 C6 0.031(4) 0.040(5) 0.030(5) -0.007(4) 0.000 0.000 N1 0.040(3) 0.036(3) 0.039(3) 0.008(2) 0.006(3) -0.006(2) N2 0.033(3) 0.036(3) 0.032(3) -0.006(2) -0.011(2) 0.009(2) N3 0.039(3) 0.030(2) 0.030(3) 0.004(2) 0.002(2) -0.017(2) N4 0.032(3) 0.034(3) 0.054(4) 0.021(3) 0.003(3) -0.002(2) N5 0.038(5) 0.038(4) 0.024(4) 0.002(3) 0.000 0.000 Nd1 0.0311(2) 0.0366(3) 0.0328(3) 0.00004(19) 0.000 0.000 O1 0.042(4) 0.041(3) 0.046(4) -0.010(3) 0.000 0.000 O2 0.030(4) 0.048(4) 0.032(4) -0.017(3) 0.000 0.000 O3 0.043(2) 0.038(2) 0.040(2) -0.0061(16) -0.013(2) 0.002(2) W1 0.03023(16) 0.0385(2) 0.0331(2) 0.000 0.0015(2) 0.000 _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 C1 N1 1.133(7) . ? C1 W1 2.222(6) . ? C2 N2 1.205(7) . ? C2 W1 2.150(6) . ? C3 N3 1.122(7) . ? C3 W1 2.197(6) . ? C4 N4 1.165(7) . ? C4 W1 2.149(6) . ? C5 N5 1.345(12) . ? C5 C6 1.417(12) . ? C5 H5A 0.9300 . ? C6 N5 1.332(10) 9_666 ? C6 H6A 0.9300 . ? N1 Nd1 2.523(5) . ? N2 Nd1 2.547(5) 10_566 ? N5 C6 1.332(10) 9_666 ? N5 Nd1 2.664(7) . ? Nd1 O3 2.434(4) . ? Nd1 O3 2.434(4) 11_655 ? Nd1 N1 2.523(5) 11_655 ? Nd1 O1 2.531(6) . ? Nd1 N2 2.547(5) 4_645 ? Nd1 N2 2.547(5) 10_556 ? Nd1 O2 2.552(5) . ? O1 H1X 0.9600 . ? O1 H1Y 0.9599 . ? O2 H2X 0.9599 . ? O2 H2Y 0.9600 . ? O3 H3X 0.9601 . ? O3 H3Y 0.9600 . ? W1 C4 2.149(6) 8_645 ? W1 C2 2.150(6) 8_645 ? W1 C3 2.197(6) 8_645 ? W1 C1 2.222(6) 8_645 ? 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 N1 C1 W1 169.0(5) . . ? N2 C2 W1 172.4(5) . . ? N3 C3 W1 175.9(5) . . ? N4 C4 W1 176.5(5) . . ? N5 C5 C6 120.9(8) . . ? N5 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? N5 C6 C5 120.3(8) 9_666 . ? N5 C6 H6A 119.8 9_666 . ? C5 C6 H6A 119.8 . . ? C1 N1 Nd1 164.5(5) . . ? C2 N2 Nd1 165.8(5) . 10_566 ? C6 N5 C5 118.7(7) 9_666 . ? C6 N5 Nd1 119.4(6) 9_666 . ? C5 N5 Nd1 121.8(5) . . ? O3 Nd1 O3 82.4(2) . 11_655 ? O3 Nd1 N1 85.27(16) . . ? O3 Nd1 N1 138.45(16) 11_655 . ? O3 Nd1 N1 138.45(16) . 11_655 ? O3 Nd1 N1 85.27(16) 11_655 11_655 ? N1 Nd1 N1 78.2(2) . 11_655 ? O3 Nd1 O1 137.14(11) . . ? O3 Nd1 O1 137.14(11) 11_655 . ? N1 Nd1 O1 73.37(16) . . ? N1 Nd1 O1 73.37(16) 11_655 . ? O3 Nd1 N2 133.95(15) . 4_645 ? O3 Nd1 N2 70.35(15) 11_655 4_645 ? N1 Nd1 N2 139.07(17) . 4_645 ? N1 Nd1 N2 76.59(16) 11_655 4_645 ? O1 Nd1 N2 68.78(14) . 4_645 ? O3 Nd1 N2 70.35(15) . 10_556 ? O3 Nd1 N2 133.95(15) 11_655 10_556 ? N1 Nd1 N2 76.59(16) . 10_556 ? N1 Nd1 N2 139.07(17) 11_655 10_556 ? O1 Nd1 N2 68.78(14) . 10_556 ? N2 Nd1 N2 103.0(2) 4_645 10_556 ? O3 Nd1 O2 68.29(15) . . ? O3 Nd1 O2 68.29(15) 11_655 . ? N1 Nd1 O2 70.26(15) . . ? N1 Nd1 O2 70.26(15) 11_655 . ? O1 Nd1 O2 132.54(19) . . ? N2 Nd1 O2 128.18(12) 4_645 . ? N2 Nd1 O2 128.18(12) 10_556 . ? O3 Nd1 N5 73.17(15) . . ? O3 Nd1 N5 73.17(15) 11_655 . ? N1 Nd1 N5 139.33(12) . . ? N1 Nd1 N5 139.33(12) 11_655 . ? O1 Nd1 N5 99.5(2) . . ? N2 Nd1 N5 63.90(13) 4_645 . ? N2 Nd1 N5 63.90(13) 10_556 . ? O2 Nd1 N5 127.9(2) . . ? Nd1 O1 H1X 109.4 . . ? Nd1 O1 H1Y 109.2 . . ? H1X O1 H1Y 109.5 . . ? Nd1 O2 H2X 109.3 . . ? Nd1 O2 H2Y 109.7 . . ? H2X O2 H2Y 109.5 . . ? Nd1 O3 H3X 109.2 . . ? Nd1 O3 H3Y 109.3 . . ? H3X O3 H3Y 109.5 . . ? C4 W1 C4 127.8(3) . 8_645 ? C4 W1 C2 79.1(2) . 8_645 ? C4 W1 C2 143.1(2) 8_645 8_645 ? C4 W1 C2 143.1(2) . . ? C4 W1 C2 79.1(2) 8_645 . ? C2 W1 C2 92.2(3) 8_645 . ? C4 W1 C3 72.9(2) . 8_645 ? C4 W1 C3 131.0(2) 8_645 8_645 ? C2 W1 C3 76.6(2) 8_645 8_645 ? C2 W1 C3 70.2(2) . 8_645 ? C4 W1 C3 131.0(2) . . ? C4 W1 C3 72.9(2) 8_645 . ? C2 W1 C3 70.2(2) 8_645 . ? C2 W1 C3 76.6(2) . . ? C3 W1 C3 131.5(3) 8_645 . ? C4 W1 C1 79.4(2) . . ? C4 W1 C1 66.7(2) 8_645 . ? C2 W1 C1 150.0(2) 8_645 . ? C2 W1 C1 92.7(2) . . ? C3 W1 C1 77.3(2) 8_645 . ? C3 W1 C1 139.5(2) . . ? C4 W1 C1 66.7(2) . 8_645 ? C4 W1 C1 79.4(2) 8_645 8_645 ? C2 W1 C1 92.7(2) 8_645 8_645 ? C2 W1 C1 150.0(2) . 8_645 ? C3 W1 C1 139.5(2) 8_645 8_645 ? C3 W1 C1 77.3(2) . 8_645 ? C1 W1 C1 97.6(3) . 8_645 ? 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 N5 C5 C6 N5 0.000(4) . . . 9_666 ? W1 C1 N1 Nd1 -39(4) . . . . ? W1 C2 N2 Nd1 78(5) . . . 10_566 ? C6 C5 N5 C6 0.000(4) . . . 9_666 ? C6 C5 N5 Nd1 180.000(2) . . . . ? C1 N1 Nd1 O3 -3.0(18) . . . . ? C1 N1 Nd1 O3 69.9(18) . . . 11_655 ? C1 N1 Nd1 N1 138.7(17) . . . 11_655 ? C1 N1 Nd1 O1 -145.4(18) . . . . ? C1 N1 Nd1 N2 -168.3(17) . . . 4_645 ? C1 N1 Nd1 N2 -73.9(18) . . . 10_556 ? C1 N1 Nd1 O2 65.6(18) . . . . ? C1 N1 Nd1 N5 -60.2(19) . . . . ? C6 N5 Nd1 O3 -136.54(11) 9_666 . . . ? C5 N5 Nd1 O3 43.46(11) . . . . ? C6 N5 Nd1 O3 136.54(11) 9_666 . . 11_655 ? C5 N5 Nd1 O3 -43.46(11) . . . 11_655 ? C6 N5 Nd1 N1 -75.5(3) 9_666 . . . ? C5 N5 Nd1 N1 104.5(3) . . . . ? C6 N5 Nd1 N1 75.5(3) 9_666 . . 11_655 ? C5 N5 Nd1 N1 -104.5(3) . . . 11_655 ? C6 N5 Nd1 O1 0.000(2) 9_666 . . . ? C5 N5 Nd1 O1 180.000(2) . . . . ? C6 N5 Nd1 N2 60.60(15) 9_666 . . 4_645 ? C5 N5 Nd1 N2 -119.40(15) . . . 4_645 ? C6 N5 Nd1 N2 -60.60(15) 9_666 . . 10_556 ? C5 N5 Nd1 N2 119.40(15) . . . 10_556 ? C6 N5 Nd1 O2 180.000(2) 9_666 . . . ? C5 N5 Nd1 O2 0.000(2) . . . . ? N4 C4 W1 C4 -3(9) . . . 8_645 ? N4 C4 W1 C2 -155(9) . . . 8_645 ? N4 C4 W1 C2 126(9) . . . . ? N4 C4 W1 C3 126(9) . . . 8_645 ? N4 C4 W1 C3 -103(9) . . . . ? N4 C4 W1 C1 46(9) . . . . ? N4 C4 W1 C1 -57(9) . . . 8_645 ? N2 C2 W1 C4 -86(4) . . . . ? N2 C2 W1 C4 56(4) . . . 8_645 ? N2 C2 W1 C2 -160(4) . . . 8_645 ? N2 C2 W1 C3 -85(4) . . . 8_645 ? N2 C2 W1 C3 131(4) . . . . ? N2 C2 W1 C1 -10(4) . . . . ? N2 C2 W1 C1 101(4) . . . 8_645 ? N3 C3 W1 C4 -10(7) . . . . ? N3 C3 W1 C4 -135(7) . . . 8_645 ? N3 C3 W1 C2 45(7) . . . 8_645 ? N3 C3 W1 C2 142(7) . . . . ? N3 C3 W1 C3 95(7) . . . 8_645 ? N3 C3 W1 C1 -140(7) . . . . ? N3 C3 W1 C1 -53(7) . . . 8_645 ? N1 C1 W1 C4 51(3) . . . . ? N1 C1 W1 C4 -170(3) . . . 8_645 ? N1 C1 W1 C2 6(3) . . . 8_645 ? N1 C1 W1 C2 -93(3) . . . . ? N1 C1 W1 C3 -24(3) . . . 8_645 ? N1 C1 W1 C3 -166(2) . . . . ? N1 C1 W1 C1 115(3) . . . 8_645 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.484 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.137 # Attachment '6-Eu.cif' data_yah127 _database_code_depnum_ccdc_archive 'CCDC 846240' #TrackingRef '6-Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Eu N9 O4 W' _chemical_formula_sum 'C10 H10 Eu N9 O4 W' _chemical_formula_weight 656.08 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x+1/2, y, -z+1/2' '-x+1/2, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x+1, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, z' 'x-1/2, -y, z-1/2' 'x-1/2, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' 'x, y+1/2, -z-1/2' _cell_length_a 16.4652(15) _cell_length_b 14.4351(14) _cell_length_c 14.8544(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3530.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3648 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 10.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1649 _exptl_absorpt_correction_T_max 0.2155 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 12939 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1806 _reflns_number_gt 1326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.06P)^2^+1.99P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1806 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1716(4) 0.5892(6) 0.1935(6) 0.038(2) Uani 1 1 d . . . C2 C 0.2842(6) 0.4224(6) 0.3743(5) 0.0401(19) Uani 1 1 d . . . C3 C 0.1516(6) 0.3900(6) 0.2642(6) 0.043(2) Uani 1 1 d . . . C4 C 0.3238(4) 0.5505(5) 0.1432(5) 0.0293(16) Uani 1 1 d . . . C5 C 0.0000 0.5047(8) 0.0935(7) 0.039(3) Uani 1 2 d S . . H5 H 0.0000 0.5055 0.1575 0.046 Uiso 1 2 calc SR . . C6 C 0.0000 0.5795(8) -0.0461(7) 0.033(2) Uani 1 2 d S . . H6 H 0.0000 0.6357 -0.0794 0.040 Uiso 1 2 calc SR . . N1 N 0.1257(5) 0.6361(5) 0.1571(4) 0.0380(16) Uani 1 1 d . . . N2 N 0.2988(4) 0.3806(4) 0.4395(4) 0.0353(15) Uani 1 1 d . . . N3 N 0.1026(5) 0.3460(5) 0.2783(5) 0.0480(18) Uani 1 1 d . . . N4 N 0.3707(5) 0.5793(5) 0.0932(4) 0.0406(16) Uani 1 1 d . . . N5 N 0.0000 0.5844(6) 0.0458(5) 0.033(2) Uani 1 2 d S . . O1 O 0.0000 0.7006(5) 0.2769(4) 0.0304(17) Uani 1 2 d S . . H1X H 0.0553 0.6846 0.2952 0.036 Uiso 0.50 1 d PR . . H1Y H -0.0353 0.6465 0.2844 0.036 Uiso 0.50 1 d PR . . O2 O 0.0985(5) 0.7602(3) 0.0117(4) 0.0397(15) Uani 1 1 d . . . H2X H 0.1494 0.7307 0.0297 0.048 Uiso 1 1 d R . . H2Y H 0.0741 0.7941 -0.0386 0.048 Uiso 1 1 d R . . O3 O 0.0000 0.9079(5) 0.0684(5) 0.0322(16) Uani 1 2 d S . . H3X H 0.0242 0.9496 0.1130 0.039 Uiso 0.50 1 d PR . . H3Y H -0.0558 0.9273 0.0561 0.039 Uiso 0.50 1 d PR . . Eu1 Eu 0.0000 0.74371(4) 0.13062(3) 0.0332(2) Uani 1 2 d S . . W1 W 0.2500 0.48789(3) 0.2500 0.03102(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.032(5) 0.068(6) -0.005(4) -0.009(4) 0.000(3) C2 0.047(5) 0.034(5) 0.039(4) -0.006(4) -0.010(4) -0.006(4) C3 0.044(6) 0.014(4) 0.072(6) 0.006(4) 0.007(4) -0.002(4) C4 0.031(4) 0.031(4) 0.026(3) -0.005(3) -0.003(3) 0.016(3) C5 0.060(8) 0.018(6) 0.038(6) -0.005(4) 0.000 0.000 C6 0.026(5) 0.031(6) 0.043(6) -0.010(5) 0.000 0.000 N1 0.048(4) 0.034(4) 0.033(3) 0.001(3) 0.017(3) -0.003(3) N2 0.052(4) 0.034(4) 0.019(3) 0.002(2) 0.009(3) 0.006(3) N3 0.059(5) 0.031(4) 0.054(4) -0.011(3) 0.005(4) 0.000(4) N4 0.059(4) 0.037(4) 0.026(3) -0.015(3) 0.000(3) -0.005(3) N5 0.038(5) 0.027(5) 0.034(4) 0.002(4) 0.000 0.000 O1 0.014(3) 0.042(5) 0.034(3) -0.014(3) 0.000 0.000 O2 0.050(4) 0.025(3) 0.044(3) 0.011(2) 0.014(3) 0.006(2) O3 0.028(4) 0.030(4) 0.039(4) 0.002(3) 0.000 0.000 Eu1 0.0377(4) 0.0335(4) 0.0283(3) -0.0008(2) 0.000 0.000 W1 0.0364(3) 0.0276(3) 0.0291(3) 0.000 -0.00129(17) 0.000 _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 C1 N1 1.150(10) . ? C1 W1 2.123(8) . ? C2 N2 1.166(9) . ? C2 W1 2.149(8) . ? C3 N3 1.048(11) . ? C3 W1 2.160(10) . ? C4 N4 1.150(10) . ? C4 W1 2.193(8) . ? C5 N5 1.351(14) . ? C5 C6 1.404(15) 9_565 ? C5 H5 0.9500 . ? C6 N5 1.367(13) . ? C6 C5 1.404(15) 9_565 ? C6 H6 0.9500 . ? N1 Eu1 2.617(8) . ? N3 Eu1 2.620(8) 7_445 ? N5 Eu1 2.622(9) . ? O1 Eu1 2.260(7) . ? O1 H1X 0.9780 . ? O1 H1Y 0.9792 . ? O2 Eu1 2.410(6) . ? O2 H2X 0.9784 . ? O2 H2Y 0.9793 . ? O3 Eu1 2.545(7) . ? O3 H3X 0.9794 . ? O3 H3Y 0.9780 . ? Eu1 O2 2.410(6) 10 ? Eu1 N3 2.620(9) 16_556 ? Eu1 N3 2.620(9) 7_455 ? Eu1 N1 2.617(8) 10 ? Eu1 H1X 2.7452 . ? Eu1 H1Y 2.7428 . ? W1 C1 2.123(8) 3 ? W1 C2 2.149(8) 3 ? W1 C3 2.160(10) 3 ? W1 C4 2.193(8) 3 ? 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 N1 C1 W1 172.3(7) . . ? N2 C2 W1 174.3(7) . . ? N3 C3 W1 173.5(9) . . ? N4 C4 W1 171.3(6) . . ? N5 C5 C6 118.3(10) . 9_565 ? N5 C5 H5 120.9 . . ? C6 C5 H5 120.9 9_565 . ? N5 C6 C5 123.1(11) . 9_565 ? N5 C6 H6 118.5 . . ? C5 C6 H6 118.5 9_565 . ? C1 N1 Eu1 160.1(6) . . ? C3 N3 Eu1 160.2(8) . 7_445 ? C6 N5 C5 118.7(10) . . ? C6 N5 Eu1 121.7(7) . . ? C5 N5 Eu1 119.7(7) . . ? Eu1 O1 H1X 109.4 . . ? Eu1 O1 H1Y 109.2 . . ? H1X O1 H1Y 109.4 . . ? Eu1 O2 H2X 109.5 . . ? Eu1 O2 H2Y 109.4 . . ? H2X O2 H2Y 141.1 . . ? Eu1 O3 H3X 109.1 . . ? Eu1 O3 H3Y 109.5 . . ? H3X O3 H3Y 109.4 . . ? O1 Eu1 O2 137.06(17) . . ? O1 Eu1 O2 137.06(17) . 10 ? O2 Eu1 O2 84.6(4) . 10 ? O1 Eu1 O3 127.3(3) . . ? O2 Eu1 O3 69.00(16) . . ? O2 Eu1 O3 69.00(16) 10 . ? O1 Eu1 N3 70.0(2) . 16_556 ? O2 Eu1 N3 83.6(2) . 16_556 ? O2 Eu1 N3 139.19(18) 10 16_556 ? O3 Eu1 N3 70.3(2) . 16_556 ? O1 Eu1 N3 70.0(2) . 7_455 ? O2 Eu1 N3 139.19(18) . 7_455 ? O2 Eu1 N3 83.6(2) 10 7_455 ? O3 Eu1 N3 70.3(2) . 7_455 ? N3 Eu1 N3 80.3(4) 16_556 7_455 ? O1 Eu1 N1 72.07(17) . 10 ? O2 Eu1 N1 134.5(2) . 10 ? O2 Eu1 N1 68.7(2) 10 10 ? O3 Eu1 N1 127.40(14) . 10 ? N3 Eu1 N1 140.1(2) 16_556 10 ? N3 Eu1 N1 75.3(2) 7_455 10 ? O1 Eu1 N1 72.07(17) . . ? O2 Eu1 N1 68.7(2) . . ? O2 Eu1 N1 134.5(2) 10 . ? O3 Eu1 N1 127.40(14) . . ? N3 Eu1 N1 75.3(2) 16_556 . ? N3 Eu1 N1 140.1(2) 7_455 . ? N1 Eu1 N1 104.5(3) 10 . ? O1 Eu1 N5 102.7(3) . . ? O2 Eu1 N5 74.60(18) . . ? O2 Eu1 N5 74.60(18) 10 . ? O3 Eu1 N5 130.0(3) . . ? N3 Eu1 N5 137.91(18) 16_556 . ? N3 Eu1 N5 137.91(18) 7_455 . ? N1 Eu1 N5 63.38(18) 10 . ? N1 Eu1 N5 63.38(18) . . ? O1 Eu1 H1X 19.6 . . ? O2 Eu1 H1X 117.4 . . ? O2 Eu1 H1X 155.1 10 . ? O3 Eu1 H1X 127.8 . . ? N3 Eu1 H1X 60.1 16_556 . ? N3 Eu1 H1X 85.9 7_455 . ? N1 Eu1 H1X 86.8 10 . ? N1 Eu1 H1X 54.5 . . ? N5 Eu1 H1X 98.9 . . ? O1 Eu1 H1Y 19.7 . . ? O2 Eu1 H1Y 143.5 . . ? O2 Eu1 H1Y 121.2 10 . ? O3 Eu1 H1Y 141.2 . . ? N3 Eu1 H1Y 89.7 16_556 . ? N3 Eu1 H1Y 73.8 7_455 . ? N1 Eu1 H1Y 53.4 10 . ? N1 Eu1 H1Y 74.9 . . ? N5 Eu1 H1Y 87.2 . . ? H1X Eu1 H1Y 33.8 . . ? C1 W1 C1 92.9(4) 3 . ? C1 W1 C2 78.7(3) 3 . ? C1 W1 C2 143.3(3) . . ? C1 W1 C2 143.3(3) 3 3 ? C1 W1 C2 78.7(3) . 3 ? C2 W1 C2 127.8(4) . 3 ? C1 W1 C3 150.2(3) 3 . ? C1 W1 C3 91.9(3) . . ? C2 W1 C3 79.9(3) . . ? C2 W1 C3 66.4(3) 3 . ? C1 W1 C3 91.9(3) 3 3 ? C1 W1 C3 150.2(3) . 3 ? C2 W1 C3 66.4(3) . 3 ? C2 W1 C3 79.9(3) 3 3 ? C3 W1 C3 98.3(5) . 3 ? C1 W1 C4 76.5(3) 3 3 ? C1 W1 C4 70.5(3) . 3 ? C2 W1 C4 72.8(3) . 3 ? C2 W1 C4 131.1(3) 3 3 ? C3 W1 C4 77.5(3) . 3 ? C3 W1 C4 139.1(3) 3 3 ? C1 W1 C4 70.5(3) 3 . ? C1 W1 C4 76.5(3) . . ? C2 W1 C4 131.1(3) . . ? C2 W1 C4 72.8(3) 3 . ? C3 W1 C4 139.1(3) . . ? C3 W1 C4 77.5(3) 3 . ? C4 W1 C4 131.3(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 C5 C6 N5 C5 0.000(2) 9_565 . . . ? C5 C6 N5 Eu1 180.000(1) 9_565 . . . ? C6 C5 N5 C6 0.000(2) 9_565 . . . ? C6 C5 N5 Eu1 180.000(1) 9_565 . . . ? C1 N1 Eu1 O1 -0.4(19) . . . . ? C1 N1 Eu1 O2 162(2) . . . . ? C1 N1 Eu1 O2 -140.0(19) . . . 10 ? C1 N1 Eu1 O3 123.2(19) . . . . ? C1 N1 Eu1 N3 72.9(19) . . . 16_556 ? C1 N1 Eu1 N3 19(2) . . . 7_455 ? C1 N1 Eu1 N1 -66(2) . . . 10 ? C1 N1 Eu1 N5 -115(2) . . . . ? C6 N5 Eu1 O1 180.000(1) . . . . ? C5 N5 Eu1 O1 0.000(2) . . . . ? C6 N5 Eu1 O2 -44.25(18) . . . . ? C5 N5 Eu1 O2 135.75(18) . . . . ? C6 N5 Eu1 O2 44.25(18) . . . 10 ? C5 N5 Eu1 O2 -135.75(18) . . . 10 ? C6 N5 Eu1 O3 0.000(2) . . . . ? C5 N5 Eu1 O3 180.000(2) . . . . ? C6 N5 Eu1 N3 -105.8(3) . . . 16_556 ? C5 N5 Eu1 N3 74.2(3) . . . 16_556 ? C6 N5 Eu1 N3 105.8(3) . . . 7_455 ? C5 N5 Eu1 N3 -74.2(3) . . . 7_455 ? C6 N5 Eu1 N1 117.80(17) . . . 10 ? C5 N5 Eu1 N1 -62.20(17) . . . 10 ? C6 N5 Eu1 N1 -117.80(17) . . . . ? C5 N5 Eu1 N1 62.20(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.393 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.152 # Attachment '7-Gd.cif' data_yah128 _database_code_depnum_ccdc_archive 'CCDC 846241' #TrackingRef '7-Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Gd N9 O4 W' _chemical_formula_sum 'C10 H10 Gd N9 O4 W' _chemical_formula_weight 661.37 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.4265(18) _cell_length_b 14.3441(16) _cell_length_c 14.8343(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3495.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2021 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 26.91 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 10.375 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.1734 _exptl_absorpt_correction_T_max 0.2308 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 13169 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1792 _reflns_number_gt 1396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.07P)^2^+1.99P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1792 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _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 C1 C 0.1705(5) 0.5923(5) 0.1897(6) 0.0372(18) Uani 1 1 d . . . C2 C 0.2814(5) 0.4211(5) 0.3742(5) 0.0341(17) Uani 1 1 d . . . C3 C 0.1536(5) 0.3898(6) 0.2670(5) 0.0359(19) Uani 1 1 d . . . C4 C 0.3227(5) 0.5489(5) 0.1420(5) 0.0336(17) Uani 1 1 d . . . C5 C 0.0000 0.5008(7) 0.0923(6) 0.036(3) Uani 1 2 d S . . H5 H 0.0000 0.5009 0.1563 0.043 Uiso 1 2 calc SR . . C6 C 0.0000 0.5831(8) -0.0442(6) 0.032(2) Uani 1 2 d S . . H6 H 0.0000 0.6402 -0.0765 0.039 Uiso 1 2 calc SR . . Gd1 Gd 0.0000 0.74302(4) 0.13057(4) 0.0374(2) Uani 1 2 d S . . N1 N 0.1248(4) 0.6372(4) 0.1588(4) 0.0328(15) Uani 1 1 d . . . N2 N 0.2998(4) 0.3792(4) 0.4397(4) 0.0365(15) Uani 1 1 d . . . N3 N 0.1016(5) 0.3463(5) 0.2775(5) 0.0379(16) Uani 1 1 d . . . N4 N 0.3677(4) 0.5828(5) 0.0905(4) 0.0391(16) Uani 1 1 d . . . N5 N 0.0000 0.5850(6) 0.0436(6) 0.034(2) Uani 1 2 d S . . O1 O 0.0000 0.6972(6) 0.2768(5) 0.0373(18) Uani 1 2 d S . . H1X H 0.0553 0.6812 0.2951 0.045 Uiso 0.50 1 d PR . . H1Y H -0.0353 0.6431 0.2843 0.045 Uiso 0.50 1 d PR . . O2 O 0.0981(4) 0.7617(3) 0.0129(4) 0.0369(13) Uani 1 1 d . . . H2X H 0.1244 0.7017 0.0007 0.044 Uiso 1 1 d R . . H2Y H 0.1393 0.8072 0.0317 0.044 Uiso 1 1 d R . . O3 O 0.0000 0.9059(5) 0.0682(5) 0.0362(17) Uani 1 2 d S . . H3X H 0.0487 0.9389 0.0890 0.043 Uiso 0.50 1 d PR . . H3Y H -0.0487 0.9389 0.0890 0.043 Uiso 0.50 1 d PR . . W1 W 0.2500 0.48745(3) 0.2500 0.03064(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(4) 0.036(4) 0.049(5) 0.004(4) -0.002(4) 0.000(4) C2 0.043(5) 0.025(4) 0.034(4) -0.005(3) -0.005(3) 0.009(3) C3 0.038(5) 0.038(4) 0.032(4) -0.016(3) -0.007(3) -0.003(4) C4 0.034(4) 0.036(4) 0.031(4) 0.002(3) -0.002(3) 0.006(3) C5 0.061(8) 0.024(5) 0.024(5) 0.000(4) 0.000 0.000 C6 0.040(7) 0.035(5) 0.022(5) -0.003(4) 0.000 0.000 Gd1 0.0376(4) 0.0380(4) 0.0365(4) -0.0013(2) 0.000 0.000 N1 0.033(4) 0.037(4) 0.028(3) 0.002(3) -0.004(3) 0.010(3) N2 0.042(4) 0.036(3) 0.031(3) -0.001(3) -0.007(3) 0.005(3) N3 0.039(4) 0.031(4) 0.043(4) -0.004(3) -0.009(3) -0.010(3) N4 0.050(4) 0.031(3) 0.036(4) -0.003(3) 0.010(3) 0.007(3) N5 0.025(5) 0.034(5) 0.042(6) -0.006(4) 0.000 0.000 O1 0.028(4) 0.046(5) 0.039(4) -0.011(4) 0.000 0.000 O2 0.036(4) 0.032(3) 0.042(3) -0.003(2) 0.009(3) 0.001(2) O3 0.033(4) 0.040(4) 0.036(4) 0.009(3) 0.000 0.000 W1 0.0301(3) 0.0319(3) 0.0300(3) 0.000 -0.00167(18) 0.000 _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 C1 N1 1.090(10) . ? C1 W1 2.184(8) . ? C2 N2 1.183(9) . ? C2 W1 2.137(7) . ? C3 N3 1.070(11) . ? C3 W1 2.129(9) . ? C4 N4 1.169(10) . ? C4 W1 2.184(8) . ? C5 C6 1.398(14) 9_565 ? C5 N5 1.408(14) . ? C5 H5 0.9500 . ? C6 N5 1.303(12) . ? C6 C5 1.398(14) 9_565 ? C6 H6 0.9500 . ? Gd1 O1 2.266(8) . ? Gd1 O2 2.390(6) 12 ? Gd1 O2 2.390(6) . ? Gd1 O3 2.512(7) . ? Gd1 N1 2.584(6) 12 ? Gd1 N1 2.584(6) . ? Gd1 N5 2.608(9) . ? Gd1 N3 2.615(7) 10_566 ? Gd1 N3 2.615(7) 3 ? N3 Gd1 2.615(7) 10_556 ? O1 H1X 0.9755 . ? O1 H1Y 0.9745 . ? O2 H2X 0.9800 . ? O2 H2Y 0.9800 . ? O3 H3X 0.9800 . ? O3 H3Y 0.9800 . ? W1 C3 2.129(9) 7_545 ? W1 C2 2.137(7) 7_545 ? W1 C1 2.184(8) 7_545 ? W1 C4 2.184(8) 7_545 ? 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 N1 C1 W1 172.3(7) . . ? N2 C2 W1 175.6(7) . . ? N3 C3 W1 174.5(8) . . ? N4 C4 W1 173.2(7) . . ? C6 C5 N5 118.4(8) 9_565 . ? C6 C5 H5 120.8 9_565 . ? N5 C5 H5 120.8 . . ? N5 C6 C5 121.9(10) . 9_565 ? N5 C6 H6 119.0 . . ? C5 C6 H6 119.0 9_565 . ? O1 Gd1 O2 136.99(16) . 12 ? O1 Gd1 O2 136.99(16) . . ? O2 Gd1 O2 84.8(3) 12 . ? O1 Gd1 O3 128.5(3) . . ? O2 Gd1 O3 68.08(17) 12 . ? O2 Gd1 O3 68.08(17) . . ? O1 Gd1 N1 70.99(18) . 12 ? O2 Gd1 N1 69.5(2) 12 12 ? O2 Gd1 N1 135.97(19) . 12 ? O3 Gd1 N1 127.29(15) . 12 ? O1 Gd1 N1 70.99(18) . . ? O2 Gd1 N1 135.97(19) 12 . ? O2 Gd1 N1 69.5(2) . . ? O3 Gd1 N1 127.29(15) . . ? N1 Gd1 N1 104.9(3) 12 . ? O1 Gd1 N5 102.8(3) . . ? O2 Gd1 N5 74.71(19) 12 . ? O2 Gd1 N5 74.71(19) . . ? O3 Gd1 N5 128.7(3) . . ? N1 Gd1 N5 64.53(17) 12 . ? N1 Gd1 N5 64.53(17) . . ? O1 Gd1 N3 70.4(2) . 10_566 ? O2 Gd1 N3 138.37(19) 12 10_566 ? O2 Gd1 N3 83.5(2) . 10_566 ? O3 Gd1 N3 70.5(2) . 10_566 ? N1 Gd1 N3 138.9(2) 12 10_566 ? N1 Gd1 N3 75.0(2) . 10_566 ? N5 Gd1 N3 138.61(17) . 10_566 ? O1 Gd1 N3 70.4(2) . 3 ? O2 Gd1 N3 83.5(2) 12 3 ? O2 Gd1 N3 138.37(19) . 3 ? O3 Gd1 N3 70.5(2) . 3 ? N1 Gd1 N3 75.0(2) 12 3 ? N1 Gd1 N3 138.9(2) . 3 ? N5 Gd1 N3 138.61(17) . 3 ? N3 Gd1 N3 79.3(3) 10_566 3 ? C1 N1 Gd1 164.0(7) . . ? C3 N3 Gd1 156.3(7) . 10_556 ? C6 N5 C5 119.6(9) . . ? C6 N5 Gd1 120.9(7) . . ? C5 N5 Gd1 119.5(6) . . ? Gd1 O1 H1X 109.6 . . ? Gd1 O1 H1Y 109.9 . . ? H1X O1 H1Y 109.5 . . ? Gd1 O2 H2X 109.5 . . ? Gd1 O2 H2Y 109.5 . . ? H2X O2 H2Y 109.5 . . ? Gd1 O3 H3X 109.5 . . ? Gd1 O3 H3Y 109.5 . . ? H3X O3 H3Y 109.5 . . ? C3 W1 C3 97.7(4) 7_545 . ? C3 W1 C2 68.3(3) 7_545 . ? C3 W1 C2 77.6(3) . . ? C3 W1 C2 77.6(3) 7_545 7_545 ? C3 W1 C2 68.3(3) . 7_545 ? C2 W1 C2 127.1(4) . 7_545 ? C3 W1 C1 93.3(3) 7_545 7_545 ? C3 W1 C1 148.2(3) . 7_545 ? C2 W1 C1 79.0(3) . 7_545 ? C2 W1 C1 143.6(3) 7_545 7_545 ? C3 W1 C1 148.2(3) 7_545 . ? C3 W1 C1 93.3(3) . . ? C2 W1 C1 143.6(3) . . ? C2 W1 C1 79.0(3) 7_545 . ? C1 W1 C1 92.9(4) 7_545 . ? C3 W1 C4 139.4(3) 7_545 7_545 ? C3 W1 C4 76.8(3) . 7_545 ? C2 W1 C4 71.3(3) . 7_545 ? C2 W1 C4 132.8(3) 7_545 7_545 ? C1 W1 C4 75.4(3) 7_545 7_545 ? C1 W1 C4 72.3(3) . 7_545 ? C3 W1 C4 76.8(3) 7_545 . ? C3 W1 C4 139.4(3) . . ? C2 W1 C4 132.8(3) . . ? C2 W1 C4 71.3(3) 7_545 . ? C1 W1 C4 72.3(3) 7_545 . ? C1 W1 C4 75.4(3) . . ? C4 W1 C4 132.4(4) 7_545 . ? 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 Gd1 N1 C1 -1(2) . . . . ? O2 Gd1 N1 C1 -140(2) 12 . . . ? O2 Gd1 N1 C1 162(2) . . . . ? O3 Gd1 N1 C1 124(2) . . . . ? N1 Gd1 N1 C1 -64(2) 12 . . . ? N5 Gd1 N1 C1 -116(2) . . . . ? N3 Gd1 N1 C1 73(2) 10_566 . . . ? N3 Gd1 N1 C1 20(3) 3 . . . ? C5 C6 N5 C5 0.000(2) 9_565 . . . ? C5 C6 N5 Gd1 180.0 9_565 . . . ? C6 C5 N5 C6 0.000(2) 9_565 . . . ? C6 C5 N5 Gd1 180.000(1) 9_565 . . . ? O1 Gd1 N5 C6 180.000(1) . . . . ? O2 Gd1 N5 C6 44.34(16) 12 . . . ? O2 Gd1 N5 C6 -44.34(16) . . . . ? O3 Gd1 N5 C6 0.000(2) . . . . ? N1 Gd1 N5 C6 118.57(18) 12 . . . ? N1 Gd1 N5 C6 -118.56(18) . . . . ? N3 Gd1 N5 C6 -105.2(3) 10_566 . . . ? N3 Gd1 N5 C6 105.2(3) 3 . . . ? O1 Gd1 N5 C5 0.000(1) . . . . ? O2 Gd1 N5 C5 -135.66(16) 12 . . . ? O2 Gd1 N5 C5 135.66(16) . . . . ? O3 Gd1 N5 C5 180.000(1) . . . . ? N1 Gd1 N5 C5 -61.43(18) 12 . . . ? N1 Gd1 N5 C5 61.44(18) . . . . ? N3 Gd1 N5 C5 74.8(3) 10_566 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.035 _refine_diff_density_min -1.526 _refine_diff_density_rms 0.167 data_x _database_code_depnum_ccdc_archive 'CCDC 866861' #TrackingRef '2a-Ce.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 Ce N8 O5 W' _chemical_formula_sum 'C8 H10 Ce N8 O5 W' _chemical_formula_weight 622.21 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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/ncc _symmetry_space_group_name_Hall '-P 4a 2ac ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 11.1891(6) _cell_length_b 11.1891(6) _cell_length_c 14.0286(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1756.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6509 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 9.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2499 _exptl_absorpt_correction_T_max 0.3227 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD ' _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 12155 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.98 _reflns_number_total 871 _reflns_number_gt 575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.05P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 871 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 W1 W 0.2500 0.7500 0.5000 0.02736(17) Uani 1 4 d S . . Ce1 Ce 0.2500 0.2500 0.37033(3) 0.02838(18) Uani 1 4 d S . . O1 O 0.2500 0.2500 0.5514(4) 0.0350(15) Uani 1 4 d S A . H1B H 0.2225 0.1739 0.5742 0.053 Uiso 0.25 1 d PR . . H1C H 0.1978 0.3118 0.5742 0.053 Uiso 0.25 1 d PR . . N2 N 0.2958(4) 0.9406(4) 0.6757(3) 0.0408(10) Uani 1 1 d . . . C2 C 0.2783(5) 0.8650(5) 0.6212(3) 0.0436(13) Uani 1 1 d . . . C1 C 0.2239(5) 0.5663(6) 0.4519(4) 0.0487(14) Uani 1 1 d . . . N1 N 0.2181(4) 0.4695(4) 0.4315(3) 0.0442(10) Uani 1 1 d . A . O2A O 0.3766(12) 0.089(2) 0.2846(15) 0.038(4) Uani 0.34(3) 1 d P A 1 H2A4 H 0.3267 0.0505 0.2381 0.046 Uiso 0.34(3) 1 d PR A 1 H2A6 H 0.4431 0.1261 0.2531 0.046 Uiso 0.34(3) 1 d PR A 1 O2B O 0.3754(6) 0.1427(16) 0.2490(10) 0.050(4) Uani 0.66(3) 1 d P A 2 H2B1 H 0.4498 0.1848 0.2431 0.060 Uiso 0.66(3) 1 d PR A 2 H2B2 H 0.3344 0.1437 0.1889 0.060 Uiso 0.66(3) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02724(19) 0.02724(19) 0.0276(2) 0.000 0.000 0.000 Ce1 0.0284(2) 0.0284(2) 0.0283(3) 0.000 0.000 0.000 O1 0.036(2) 0.036(2) 0.033(3) 0.000 0.000 0.000 N2 0.041(2) 0.041(3) 0.040(2) 0.0035(19) 0.0018(19) -0.005(2) C2 0.052(4) 0.033(3) 0.046(3) -0.004(2) 0.001(2) -0.002(2) C1 0.062(3) 0.041(3) 0.043(3) -0.013(2) 0.001(2) -0.001(2) N1 0.050(3) 0.041(3) 0.042(2) -0.0073(19) 0.0039(17) -0.003(2) O2A 0.046(6) 0.029(9) 0.039(7) 0.013(7) 0.015(5) -0.004(5) O2B 0.041(4) 0.059(8) 0.049(6) -0.013(5) 0.000(2) 0.012(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 W1 C1 2.183(6) 12_666 ? W1 C1 2.183(6) . ? W1 C1 2.183(6) 3_565 ? W1 C1 2.183(6) 10_566 ? W1 C2 2.156(5) . ? W1 C2 2.156(5) 3_565 ? W1 C2 2.156(5) 12_666 ? W1 C2 2.156(5) 10_566 ? Ce1 O2B 2.511(6) 4 ? Ce1 O2B 2.511(6) . ? Ce1 O2B 2.511(6) 2 ? Ce1 O2B 2.511(6) 3 ? Ce1 O1 2.540(6) . ? Ce1 O2A 2.588(15) 4 ? Ce1 O2A 2.588(15) 2 ? Ce1 O2A 2.588(15) . ? Ce1 O2A 2.588(15) 3 ? Ce1 N1 2.626(5) 4 ? Ce1 N1 2.626(5) . ? Ce1 N1 2.626(5) 3 ? O1 H1B 0.9600 . ? O1 H1C 0.9600 . ? N2 C2 1.157(6) . ? C1 N1 1.123(7) . ? O2A H2A4 0.9600 . ? O2A H2A6 0.9600 . ? O2B H2A4 1.1769 . ? O2B H2A6 0.7822 . ? O2B H2B1 0.9600 . ? O2B H2B2 0.9600 . ? 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 C1 W1 C1 95.48(9) 12_666 . ? C1 W1 C1 95.48(9) 12_666 3_565 ? C1 W1 C1 144.0(3) . 3_565 ? C1 W1 C1 144.0(3) 12_666 10_566 ? C1 W1 C1 95.48(9) . 10_566 ? C1 W1 C1 95.48(9) 3_565 10_566 ? C1 W1 C2 72.4(2) 12_666 . ? C1 W1 C2 145.6(2) . . ? C1 W1 C2 70.3(2) 3_565 . ? C1 W1 C2 79.3(2) 10_566 . ? C1 W1 C2 79.3(2) 12_666 3_565 ? C1 W1 C2 70.3(2) . 3_565 ? C1 W1 C2 145.6(2) 3_565 3_565 ? C1 W1 C2 72.4(2) 10_566 3_565 ? C2 W1 C2 75.9(3) . 3_565 ? C1 W1 C2 145.6(2) 12_666 12_666 ? C1 W1 C2 79.3(2) . 12_666 ? C1 W1 C2 72.4(2) 3_565 12_666 ? C1 W1 C2 70.3(2) 10_566 12_666 ? C2 W1 C2 128.48(17) . 12_666 ? C2 W1 C2 128.48(18) 3_565 12_666 ? C1 W1 C2 70.3(2) 12_666 10_566 ? C1 W1 C2 72.4(2) . 10_566 ? C1 W1 C2 79.3(2) 3_565 10_566 ? C1 W1 C2 145.6(2) 10_566 10_566 ? C2 W1 C2 128.48(18) . 10_566 ? C2 W1 C2 128.48(17) 3_565 10_566 ? C2 W1 C2 75.9(3) 12_666 10_566 ? O2B Ce1 O2B 62.7(4) 4 . ? O2B Ce1 O2B 94.7(8) 4 2 ? O2B Ce1 O2B 62.7(4) . 2 ? O2B Ce1 O2B 62.7(4) 4 3 ? O2B Ce1 O2B 94.7(8) . 3 ? O2B Ce1 O2B 62.7(4) 2 3 ? O2B Ce1 O1 132.7(4) 4 . ? O2B Ce1 O1 132.7(4) . . ? O2B Ce1 O1 132.7(4) 2 . ? O2B Ce1 O1 132.7(4) 3 . ? O2B Ce1 O2A 17.5(2) 4 4 ? O2B Ce1 O2A 79.2(4) . 4 ? O2B Ce1 O2A 108.9(10) 2 4 ? O2B Ce1 O2A 63.7(7) 3 4 ? O1 Ce1 O2A 117.7(6) . 4 ? O2B Ce1 O2A 108.9(10) 4 2 ? O2B Ce1 O2A 63.7(7) . 2 ? O2B Ce1 O2A 17.5(2) 2 2 ? O2B Ce1 O2A 79.2(4) 3 2 ? O1 Ce1 O2A 117.7(6) . 2 ? O2A Ce1 O2A 124.6(12) 4 2 ? O2B Ce1 O2A 63.7(7) 4 . ? O2B Ce1 O2A 17.5(2) . . ? O2B Ce1 O2A 79.2(4) 2 . ? O2B Ce1 O2A 108.9(10) 3 . ? O1 Ce1 O2A 117.7(6) . . ? O2A Ce1 O2A 77.5(5) 4 . ? O2A Ce1 O2A 77.5(5) 2 . ? O2B Ce1 O2A 79.2(4) 4 3 ? O2B Ce1 O2A 108.9(10) . 3 ? O2B Ce1 O2A 63.7(7) 2 3 ? O2B Ce1 O2A 17.5(2) 3 3 ? O1 Ce1 O2A 117.7(6) . 3 ? O2A Ce1 O2A 77.5(5) 4 3 ? O2A Ce1 O2A 77.5(5) 2 3 ? O2A Ce1 O2A 124.6(12) . 3 ? O2B Ce1 N1 138.1(5) 4 4 ? O2B Ce1 N1 76.34(18) . 4 ? O2B Ce1 N1 72.5(5) 2 4 ? O2B Ce1 N1 132.8(3) 3 4 ? O1 Ce1 N1 70.92(9) . 4 ? O2A Ce1 N1 151.3(3) 4 4 ? O2A Ce1 N1 55.0(6) 2 4 ? O2A Ce1 N1 74.6(3) . 4 ? O2A Ce1 N1 124.7(3) 3 4 ? O2B Ce1 N1 132.8(3) 4 . ? O2B Ce1 N1 138.1(5) . . ? O2B Ce1 N1 76.34(18) 2 . ? O2B Ce1 N1 72.5(5) 3 . ? O1 Ce1 N1 70.92(9) . . ? O2A Ce1 N1 124.7(3) 4 . ? O2A Ce1 N1 74.6(3) 2 . ? O2A Ce1 N1 151.3(3) . . ? O2A Ce1 N1 55.0(6) 3 . ? N1 Ce1 N1 83.87(6) 4 . ? O2B Ce1 N1 76.34(18) 4 3 ? O2B Ce1 N1 72.5(5) . 3 ? O2B Ce1 N1 132.8(3) 2 3 ? O2B Ce1 N1 138.1(5) 3 3 ? O1 Ce1 N1 70.92(9) . 3 ? O2A Ce1 N1 74.6(3) 4 3 ? O2A Ce1 N1 124.7(3) 2 3 ? O2A Ce1 N1 55.0(6) . 3 ? O2A Ce1 N1 151.3(3) 3 3 ? N1 Ce1 N1 83.87(6) 4 3 ? N1 Ce1 N1 141.85(19) . 3 ? Ce1 O1 H1B 109.5 . . ? Ce1 O1 H1C 109.5 . . ? H1B O1 H1C 109.5 . . ? N2 C2 W1 169.2(4) . . ? N1 C1 W1 174.5(5) . . ? C1 N1 Ce1 168.1(4) . . ? Ce1 O2A H2A4 108.0 . . ? Ce1 O2A H2A6 109.7 . . ? H2A4 O2A H2A6 109.5 . . ? Ce1 O2B H2A4 104.4 . . ? Ce1 O2B H2A6 127.2 . . ? H2A4 O2B H2A6 104.5 . . ? Ce1 O2B H2B1 107.9 . . ? H2A4 O2B H2B1 145.2 . . ? Ce1 O2B H2B2 108.8 . . ? H2A4 O2B H2B2 71.0 . . ? H2A6 O2B H2B2 122.0 . . ? H2B1 O2B H2B2 109.5 . . ? 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 C1 W1 C2 N2 100(3) 12_666 . . . ? C1 W1 C2 N2 174(3) . . . . ? C1 W1 C2 N2 -2(3) 3_565 . . . ? C1 W1 C2 N2 -102(3) 10_566 . . . ? C2 W1 C2 N2 -177(3) 3_565 . . . ? C2 W1 C2 N2 -48(3) 12_666 . . . ? C2 W1 C2 N2 55(3) 10_566 . . . ? O2B Ce1 N1 C1 -120(2) 4 . . . ? O2B Ce1 N1 C1 -24(2) . . . . ? O2B Ce1 N1 C1 -36(2) 2 . . . ? O2B Ce1 N1 C1 -101(2) 3 . . . ? O1 Ce1 N1 C1 109(2) . . . . ? O2A Ce1 N1 C1 -140(2) 4 . . . ? O2A Ce1 N1 C1 -18(2) 2 . . . ? O2A Ce1 N1 C1 -4(3) . . . . ? O2A Ce1 N1 C1 -103(2) 3 . . . ? N1 Ce1 N1 C1 37(2) 4 . . . ? N1 Ce1 N1 C1 109(2) 3 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.551 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.091 # Attachment '5-Sm.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 866862' #TrackingRef '5-Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 N9 O4 Sm W' _chemical_formula_sum 'C10 H10 N9 O4 Sm W' _chemical_formula_weight 654.47 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2 ' 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' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 16.5021(15) _cell_length_b 14.435(2) _cell_length_c 14.8641(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3540.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4048 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 9.812 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.1698 _exptl_absorpt_correction_T_max 0.2214 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 12759 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1751 _reflns_number_gt 1425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.05P)^2^+1.55P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1751 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _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 C1 C 0.1718(4) 0.5895(4) 0.1939(5) 0.0325(14) Uani 1 1 d . . . C2 C 0.2848(5) 0.4223(5) 0.3738(4) 0.0360(16) Uani 1 1 d . . . C3 C 0.1493(5) 0.3885(5) 0.2651(5) 0.0371(17) Uani 1 1 d . . . C4 C 0.3236(4) 0.5503(4) 0.1420(4) 0.0294(15) Uani 1 1 d . . . C5 C 0.0000 0.5044(6) 0.0927(6) 0.035(2) Uani 1 2 d S . . H5 H 0.0000 0.5052 0.1566 0.042 Uiso 1 2 calc SR . . C6 C 0.0000 0.5799(7) -0.0447(6) 0.036(2) Uani 1 2 d S . . H6 H 0.0000 0.6362 -0.0778 0.043 Uiso 1 2 calc SR . . N1 N 0.1252(4) 0.6364(4) 0.1583(4) 0.0335(13) Uani 1 1 d . . . N2 N 0.2981(4) 0.3799(3) 0.4392(4) 0.0358(14) Uani 1 1 d . . . N3 N 0.1006(4) 0.3451(4) 0.2776(4) 0.0406(15) Uani 1 1 d . . . N4 N 0.3700(4) 0.5785(4) 0.0928(4) 0.0372(14) Uani 1 1 d . . . N5 N 0.0000 0.5845(5) 0.0445(5) 0.0325(18) Uani 1 2 d S . . O1 O 0.0000 0.6992(4) 0.2769(4) 0.0305(14) Uani 1 2 d S . . H1X H 0.0553 0.6832 0.2952 0.037 Uiso 0.50 1 d PR . . H1Y H -0.0353 0.6452 0.2844 0.037 Uiso 0.50 1 d PR . . O2 O 0.0984(3) 0.7606(3) 0.0118(3) 0.0381(11) Uani 1 1 d . . . H2X H 0.1494 0.7311 0.0298 0.046 Uiso 1 1 d R . . H2Y H 0.0740 0.7945 -0.0385 0.046 Uiso 1 1 d R . . O3 O 0.0000 0.9073(4) 0.0684(4) 0.0308(14) Uani 1 2 d S . . H3X H 0.0242 0.9490 0.1130 0.037 Uiso 0.50 1 d PR . . H3Y H -0.0558 0.9267 0.0561 0.037 Uiso 0.50 1 d PR . . Sm1 Sm 0.0000 0.74337(3) 0.13061(3) 0.03284(16) Uani 1 2 d S . . W1 W 0.2500 0.48770(3) 0.2500 0.03166(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(4) 0.027(3) 0.049(4) -0.001(3) 0.002(3) -0.005(3) C2 0.034(5) 0.037(4) 0.037(4) 0.000(3) -0.007(3) -0.001(3) C3 0.042(5) 0.025(3) 0.044(4) 0.007(3) 0.003(3) 0.002(3) C4 0.028(4) 0.034(3) 0.026(3) -0.006(3) -0.001(3) 0.014(3) C5 0.043(7) 0.029(4) 0.032(5) 0.001(3) 0.000 0.000 C6 0.034(6) 0.037(5) 0.037(5) -0.001(4) 0.000 0.000 N1 0.041(4) 0.033(3) 0.027(3) 0.005(2) 0.014(3) 0.004(3) N2 0.046(4) 0.028(3) 0.033(3) 0.003(2) 0.011(3) 0.005(3) N3 0.042(4) 0.037(3) 0.043(3) -0.007(3) 0.001(3) -0.007(3) N4 0.042(4) 0.041(3) 0.028(3) -0.012(2) 0.007(3) -0.003(3) N5 0.040(5) 0.028(4) 0.029(4) -0.004(3) 0.000 0.000 O1 0.027(4) 0.037(3) 0.028(3) -0.013(3) 0.000 0.000 O2 0.043(3) 0.031(2) 0.040(3) 0.0074(18) 0.010(2) 0.001(2) O3 0.025(4) 0.035(3) 0.032(3) 0.011(3) 0.000 0.000 Sm1 0.0364(3) 0.0340(3) 0.0281(3) -0.00039(18) 0.000 0.000 W1 0.0379(3) 0.0267(2) 0.0303(2) 0.000 -0.00120(18) 0.000 _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 C1 N1 1.152(9) . ? C1 W1 2.127(7) . ? C2 N2 1.170(8) . ? C2 W1 2.146(7) . ? C3 N3 1.036(9) . ? C3 W1 2.205(8) . ? C4 N4 1.134(9) . ? C4 W1 2.207(7) . ? C5 N5 1.359(11) . ? C5 C6 1.412(12) 9_565 ? C5 H5 0.9500 . ? C6 N5 1.327(11) . ? C6 C5 1.412(12) 9_565 ? C6 H6 0.9500 . ? N1 Sm1 2.613(6) . ? N3 Sm1 2.603(7) 10_556 ? N5 Sm1 2.627(7) . ? O1 Sm1 2.265(6) . ? O1 H1X 0.9800 . ? O1 H1Y 0.9800 . ? O2 Sm1 2.412(5) . ? O2 H2X 0.9801 . ? O2 H2Y 0.9800 . ? O3 Sm1 2.541(6) . ? O3 H3X 0.9800 . ? O3 H3Y 0.9799 . ? Sm1 O2 2.412(5) 11 ? Sm1 N3 2.603(7) 10_566 ? Sm1 N3 2.603(7) 4 ? Sm1 N1 2.613(6) 11 ? W1 C1 2.127(7) 8_545 ? W1 C2 2.146(7) 8_545 ? W1 C3 2.205(8) 8_545 ? W1 C4 2.207(7) 8_545 ? 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 N1 C1 W1 172.1(6) . . ? N2 C2 W1 173.2(6) . . ? N3 C3 W1 174.7(7) . . ? N4 C4 W1 171.0(6) . . ? N5 C5 C6 117.8(8) . 9_565 ? N5 C5 H5 121.1 . . ? C6 C5 H5 121.1 9_565 . ? N5 C6 C5 123.2(8) . 9_565 ? N5 C6 H6 118.4 . . ? C5 C6 H6 118.4 9_565 . ? C1 N1 Sm1 161.3(5) . . ? C3 N3 Sm1 158.4(6) . 10_556 ? C6 N5 C5 119.0(8) . . ? C6 N5 Sm1 122.0(6) . . ? C5 N5 Sm1 119.0(6) . . ? Sm1 O1 H1X 109.5 . . ? Sm1 O1 H1Y 109.5 . . ? H1X O1 H1Y 109.5 . . ? Sm1 O2 H2X 109.5 . . ? Sm1 O2 H2Y 109.5 . . ? H2X O2 H2Y 141.1 . . ? Sm1 O3 H3X 109.0 . . ? Sm1 O3 H3Y 109.5 . . ? H3X O3 H3Y 109.5 . . ? O1 Sm1 O2 137.01(14) . . ? O1 Sm1 O2 137.01(14) . 11 ? O2 Sm1 O2 84.7(3) . 11 ? O1 Sm1 O3 127.7(2) . . ? O2 Sm1 O3 68.77(14) . . ? O2 Sm1 O3 68.76(14) 11 . ? O1 Sm1 N3 69.85(17) . 10_566 ? O2 Sm1 N3 84.06(19) . 10_566 ? O2 Sm1 N3 139.05(17) 11 10_566 ? O3 Sm1 N3 70.44(17) . 10_566 ? O1 Sm1 N3 69.85(17) . 4 ? O2 Sm1 N3 139.05(17) . 4 ? O2 Sm1 N3 84.06(19) 11 4 ? O3 Sm1 N3 70.44(17) . 4 ? N3 Sm1 N3 79.2(3) 10_566 4 ? O1 Sm1 N1 71.48(14) . . ? O2 Sm1 N1 69.12(17) . . ? O2 Sm1 N1 135.14(17) 11 . ? O3 Sm1 N1 127.44(12) . . ? N3 Sm1 N1 75.3(2) 10_566 . ? N3 Sm1 N1 139.05(17) 4 . ? O1 Sm1 N1 71.48(14) . 11 ? O2 Sm1 N1 135.14(17) . 11 ? O2 Sm1 N1 69.12(17) 11 11 ? O3 Sm1 N1 127.44(12) . 11 ? N3 Sm1 N1 139.05(17) 10_566 11 ? N3 Sm1 N1 75.3(2) 4 11 ? N1 Sm1 N1 104.6(3) . 11 ? O1 Sm1 N5 102.8(2) . . ? O2 Sm1 N5 74.52(15) . . ? O2 Sm1 N5 74.52(15) 11 . ? O3 Sm1 N5 129.5(2) . . ? N3 Sm1 N5 138.44(16) 10_566 . ? N3 Sm1 N5 138.44(16) 4 . ? N1 Sm1 N5 63.94(15) . . ? N1 Sm1 N5 63.94(15) 11 . ? C1 W1 C1 92.5(3) . 8_545 ? C1 W1 C2 78.8(3) . 8_545 ? C1 W1 C2 143.4(3) 8_545 8_545 ? C1 W1 C2 143.4(3) . . ? C1 W1 C2 78.8(3) 8_545 . ? C2 W1 C2 127.8(4) 8_545 . ? C1 W1 C3 150.0(3) . 8_545 ? C1 W1 C3 91.8(3) 8_545 8_545 ? C2 W1 C3 80.2(3) 8_545 8_545 ? C2 W1 C3 66.4(3) . 8_545 ? C1 W1 C3 91.8(3) . . ? C1 W1 C3 150.0(3) 8_545 . ? C2 W1 C3 66.4(3) 8_545 . ? C2 W1 C3 80.2(3) . . ? C3 W1 C3 99.0(4) 8_545 . ? C1 W1 C4 70.6(2) . 8_545 ? C1 W1 C4 76.4(2) 8_545 8_545 ? C2 W1 C4 131.0(3) 8_545 8_545 ? C2 W1 C4 72.8(3) . 8_545 ? C3 W1 C4 139.0(3) 8_545 8_545 ? C3 W1 C4 77.1(2) . 8_545 ? C1 W1 C4 76.4(2) . . ? C1 W1 C4 70.6(2) 8_545 . ? C2 W1 C4 72.8(3) 8_545 . ? C2 W1 C4 131.0(3) . . ? C3 W1 C4 77.1(2) 8_545 . ? C3 W1 C4 139.0(3) . . ? C4 W1 C4 131.6(3) 8_545 . ? 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 C5 C6 N5 C5 0.000(2) 9_565 . . . ? C5 C6 N5 Sm1 180.0 9_565 . . . ? C6 C5 N5 C6 0.000(2) 9_565 . . . ? C6 C5 N5 Sm1 180.0 9_565 . . . ? C1 N1 Sm1 O1 -1.0(17) . . . . ? C1 N1 Sm1 O2 161.4(17) . . . . ? C1 N1 Sm1 O2 -140.2(16) . . . 11 ? C1 N1 Sm1 O3 122.7(17) . . . . ? C1 N1 Sm1 N3 72.3(17) . . . 10_566 ? C1 N1 Sm1 N3 18.9(18) . . . 4 ? C1 N1 Sm1 N1 -65.3(18) . . . 11 ? C1 N1 Sm1 N5 -116.1(17) . . . . ? C6 N5 Sm1 O1 180.000(1) . . . . ? C5 N5 Sm1 O1 0.000(1) . . . . ? C6 N5 Sm1 O2 -44.32(14) . . . . ? C5 N5 Sm1 O2 135.68(14) . . . . ? C6 N5 Sm1 O2 44.32(14) . . . 11 ? C5 N5 Sm1 O2 -135.68(14) . . . 11 ? C6 N5 Sm1 O3 0.000(1) . . . . ? C5 N5 Sm1 O3 180.000(1) . . . . ? C6 N5 Sm1 N3 -106.0(3) . . . 10_566 ? C5 N5 Sm1 N3 74.0(3) . . . 10_566 ? C6 N5 Sm1 N3 106.0(3) . . . 4 ? C5 N5 Sm1 N3 -74.0(3) . . . 4 ? C6 N5 Sm1 N1 -118.29(15) . . . . ? C5 N5 Sm1 N1 61.71(15) . . . . ? C6 N5 Sm1 N1 118.29(15) . . . 11 ? C5 N5 Sm1 N1 -61.71(15) . . . 11 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.770 _refine_diff_density_min -1.464 _refine_diff_density_rms 0.146