# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email czlu@ms.fjirsm.ac.cn _publ_contact_author_name 'Can-Zhong Lu' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Chuan-De Wu' 'Can-Zhong Lu' 'Xiang Lin' 'Ding-Ming Wu' 'Shao-Fang Lu' ; Hong-Hui Zhuang ; 'Jin-Shun Huang' data_B301542D _database_code_CSD 203714 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Gd Mo2 N O26' _chemical_formula_weight 903.44 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' Mo Mo -1.6832 0.6857 '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 Hexagonal _symmetry_space_group_name_H-M P6522 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' 'y, x, -z+2/3' 'x-y, -y, -z' '-x, -x+y, -z+1/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' _cell_length_a 15.2980(2) _cell_length_b 15.2980(2) _cell_length_c 18.6613(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3782.2(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7371 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 25.09 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2634 _exptl_absorpt_coefficient_mu 3.692 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8555 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11499 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.09 _reflns_number_total 2253 _reflns_number_gt 2038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+3.8408P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(1) _refine_ls_number_reflns 2253 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0333 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 Gd Gd 0.272424(15) -0.45515(3) 0.2500 0.02538(13) Uani 1 2 d S . . Mo Mo 0.12684(4) -0.72043(4) -0.02144(2) 0.02985(16) Uani 1 1 d . . . O1 O 0.1708(3) -0.6062(4) 0.0655(2) 0.0360(11) Uani 1 1 d . . . O2 O 0.2967(3) -0.5036(3) 0.1360(2) 0.0358(11) Uani 1 1 d . . . O3 O 0.2707(3) -0.6675(3) -0.00734(18) 0.0310(9) Uani 1 1 d . . . O4 O 0.2979(3) -0.7123(3) 0.13849(19) 0.0339(10) Uani 1 1 d . . . O5 O 0.5035(3) -0.6212(4) 0.0174(2) 0.0429(12) Uani 1 1 d . . . O6 O 0.4194(3) -0.7599(3) 0.0827(2) 0.0366(10) Uani 1 1 d . . . O7 O 0.0709(4) -0.8157(4) 0.0393(2) 0.0463(13) Uani 1 1 d . . . O8 O 0.1242(4) -0.7803(4) -0.0985(2) 0.0502(13) Uani 1 1 d . . . O9 O 0.4453(4) -0.3955(5) 0.2752(3) 0.0697(18) Uani 1 1 d . . . H9A H 0.4805 -0.3455 0.2507 0.084 Uiso 1 1 calc R . . H9B H 0.4627 -0.4275 0.3078 0.084 Uiso 1 1 d R . . O10 O 0.2916(6) -0.5982(5) 0.2675(3) 0.087(2) Uani 1 1 d . . . H10A H 0.3372 -0.5936 0.2418 0.105 Uiso 1 1 calc R . . H10B H 0.2513 -0.6467 0.2986 0.105 Uiso 1 1 d R . . O11 O 0.3655(5) -0.3086(4) 0.1735(3) 0.079(2) Uani 1 1 d . . . H11A H 0.4085 -0.3142 0.1510 0.095 Uiso 1 1 calc R . . H11B H 0.3491 -0.2597 0.1733 0.095 Uiso 1 1 d R . . O101 O 0.5625(7) -0.5028(7) -0.0998(4) 0.114(3) Uani 1 1 d . . . O102 O 0.716(2) -0.1422(10) 0.4167 0.147(11) Uani 0.50 2 d SP . . O103 O 0.6280(13) -0.2984(14) 0.3773(7) 0.113(6) Uani 0.50 1 d P . . O104 O 0.0329(11) -0.9836(6) -0.0833 0.25(2) Uani 0.50 2 d SP . . N1 N 0.2197(5) -0.7803(5) 0.3333 0.051(2) Uani 1 2 d S . . C1 C 0.2599(5) -0.5661(4) 0.0850(3) 0.0291(14) Uani 1 1 d . . . C2 C 0.3272(5) -0.5945(5) 0.0452(3) 0.0260(13) Uani 1 1 d . . . H2A H 0.3810 -0.5344 0.0216 0.031 Uiso 1 1 calc R . . C3 C 0.3745(5) -0.6353(5) 0.0979(3) 0.0280(14) Uani 1 1 d . . . H3A H 0.4184 -0.5805 0.1305 0.034 Uiso 1 1 calc R . . C4 C 0.4381(5) -0.6748(6) 0.0618(3) 0.0353(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.02667(19) 0.0239(2) 0.0246(2) 0.000 0.00405(16) 0.01196(12) Mo 0.0308(3) 0.0330(3) 0.0249(3) -0.0006(2) -0.0031(2) 0.0153(3) O1 0.036(3) 0.049(3) 0.029(2) -0.009(2) -0.003(2) 0.026(2) O2 0.045(3) 0.032(3) 0.031(2) -0.005(2) 0.000(2) 0.020(2) O3 0.032(2) 0.046(3) 0.0221(18) -0.0097(19) -0.0086(19) 0.025(2) O4 0.041(3) 0.041(3) 0.027(2) 0.014(2) 0.0081(19) 0.026(2) O5 0.035(3) 0.060(3) 0.040(3) 0.014(2) 0.012(2) 0.028(3) O6 0.045(3) 0.041(3) 0.038(2) 0.012(2) 0.008(2) 0.032(2) O7 0.050(3) 0.042(3) 0.044(3) 0.016(2) 0.003(2) 0.020(3) O8 0.049(3) 0.057(3) 0.037(3) -0.016(2) -0.008(2) 0.021(3) O9 0.039(3) 0.102(5) 0.057(3) 0.012(3) 0.000(3) 0.027(3) O10 0.140(6) 0.096(5) 0.077(4) 0.053(4) 0.070(4) 0.098(5) O11 0.115(5) 0.043(3) 0.094(4) 0.031(3) 0.077(4) 0.050(4) O101 0.172(9) 0.135(7) 0.080(5) 0.010(5) 0.009(5) 0.109(7) O102 0.15(2) 0.24(2) 0.019(7) 0.027(12) 0.000 0.077(11) O103 0.135(15) 0.139(15) 0.062(8) 0.055(9) 0.002(8) 0.066(12) O104 0.025(9) 0.010(6) 0.71(7) 0.039(18) 0.000 0.012(5) N1 0.043(4) 0.043(4) 0.059(5) -0.014(2) 0.014(2) 0.016(4) C1 0.039(4) 0.031(4) 0.022(3) 0.002(3) -0.002(3) 0.022(3) C2 0.029(3) 0.028(3) 0.024(3) 0.004(3) 0.001(3) 0.017(3) C3 0.031(4) 0.034(4) 0.022(3) 0.001(2) -0.004(2) 0.019(3) C4 0.032(4) 0.051(5) 0.029(3) 0.004(3) -0.006(3) 0.026(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 Gd O2 2.343(4) . ? Gd O2 2.343(4) 11_655 ? Gd O10 2.372(5) . ? Gd O10 2.372(5) 11_655 ? Gd O9 2.374(5) . ? Gd O9 2.374(5) 11_655 ? Gd O11 2.430(5) 11_655 ? Gd O11 2.430(5) . ? Mo O8 1.695(4) . ? Mo O7 1.701(4) . ? Mo O4 1.944(4) 6_444 ? Mo O3 1.946(4) . ? Mo O6 2.205(4) 6_444 ? Mo O1 2.227(4) . ? O1 C1 1.238(7) . ? O2 C1 1.264(7) . ? O3 C2 1.410(7) . ? O4 C3 1.397(7) . ? O4 Mo 1.944(4) 5_655 ? O5 C4 1.241(7) . ? O6 C4 1.247(8) . ? O6 Mo 2.205(4) 5_655 ? C1 C2 1.499(8) . ? C2 C3 1.527(8) . ? C3 C4 1.535(9) . ? 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 Gd O2 148.2(2) . 11_655 ? O2 Gd O10 73.80(17) . . ? O2 Gd O10 80.88(17) 11_655 . ? O2 Gd O10 80.88(17) . 11_655 ? O2 Gd O10 73.80(17) 11_655 11_655 ? O10 Gd O10 73.9(4) . 11_655 ? O2 Gd O9 88.82(17) . . ? O2 Gd O9 101.70(16) 11_655 . ? O10 Gd O9 72.5(3) . . ? O10 Gd O9 146.4(2) 11_655 . ? O2 Gd O9 101.70(16) . 11_655 ? O2 Gd O9 88.82(17) 11_655 11_655 ? O10 Gd O9 146.4(2) . 11_655 ? O10 Gd O9 72.5(3) 11_655 11_655 ? O9 Gd O9 141.1(3) . 11_655 ? O2 Gd O11 142.39(16) . 11_655 ? O2 Gd O11 69.25(16) 11_655 11_655 ? O10 Gd O11 129.1(2) . 11_655 ? O10 Gd O11 130.30(19) 11_655 11_655 ? O9 Gd O11 74.5(2) . 11_655 ? O9 Gd O11 74.7(2) 11_655 11_655 ? O2 Gd O11 69.25(16) . . ? O2 Gd O11 142.39(16) 11_655 . ? O10 Gd O11 130.30(19) . . ? O10 Gd O11 129.1(2) 11_655 . ? O9 Gd O11 74.7(2) . . ? O9 Gd O11 74.5(2) 11_655 . ? O11 Gd O11 73.9(3) 11_655 . ? O8 Mo O7 103.7(2) . . ? O8 Mo O4 104.3(2) . 6_444 ? O7 Mo O4 93.5(2) . 6_444 ? O8 Mo O3 93.2(2) . . ? O7 Mo O3 104.3(2) . . ? O4 Mo O3 151.31(18) 6_444 . ? O8 Mo O6 88.5(2) . 6_444 ? O7 Mo O6 165.2(2) . 6_444 ? O4 Mo O6 74.96(16) 6_444 6_444 ? O3 Mo O6 83.14(16) . 6_444 ? O8 Mo O1 163.4(2) . . ? O7 Mo O1 90.7(2) . . ? O4 Mo O1 82.68(16) 6_444 . ? O3 Mo O1 74.93(15) . . ? O6 Mo O1 78.69(16) 6_444 . ? C1 O1 Mo 115.4(4) . . ? C1 O2 Gd 147.3(4) . . ? C2 O3 Mo 122.8(3) . . ? C3 O4 Mo 123.1(4) . 5_655 ? C4 O6 Mo 116.4(4) . 5_655 ? O1 C1 O2 124.0(6) . . ? O1 C1 C2 117.2(5) . . ? O2 C1 C2 118.8(6) . . ? O3 C2 C1 109.6(5) . . ? O3 C2 C3 110.7(5) . . ? C1 C2 C3 109.5(5) . . ? O4 C3 C2 109.0(5) . . ? O4 C3 C4 109.6(5) . . ? C2 C3 C4 113.6(5) . . ? O5 C4 O6 126.0(6) . . ? O5 C4 C3 119.5(6) . . ? O6 C4 C3 114.4(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.513 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.089