Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Can-Zhong Lu' _publ_contact_author_address ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_email czlu@ms.fjirsm.ac.cn _publ_contact_author_phone +86-591-3792865 _publ_contact_author_fax +86-591-3714946 _publ_contact_letter ; Please consider this CIF submission for publication as a Full Paper ; _publ_section_title ; Synthesis, Structures and Properties of a Series Novel Left-handed and Right-handed Metal Coordination Double Helicates With Chiral Channels ; loop_ _publ_author_name _publ_author_address 'Chuan-De Wu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Can-Zhong Lu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Shao-Fang Lu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Hong-Hui Zhuang' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; ; Jin-Shun Huang ; ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; data_MoSm _database_code_CSD 175443 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Mo2 N O26 Sm' _chemical_formula_weight 896.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.339(1) _cell_length_b 15.339(1) _cell_length_c 18.668(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3803.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 25.06 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2622 _exptl_absorpt_coefficient_mu 3.371 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5136 _exptl_absorpt_correction_T_max 0.7070 _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 14903 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2253 _reflns_number_gt 2024 _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^)+(0.0305P)^2^+2.7593P] 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 0.00030(12) _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 -0.003(17) _refine_ls_number_reflns 2253 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0384 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Sm Sm 0.727917(17) 0.272083(17) 0.0833 0.02670(15) Uani 1 2 d S . . Mo Mo 0.87384(4) 0.15195(4) 0.35597(3) 0.02946(17) Uani 1 1 d . . . O1 O 0.8312(4) 0.2226(3) 0.2686(2) 0.0355(12) Uani 1 1 d . . . O2 O 0.7038(4) 0.1993(3) 0.1987(2) 0.0350(11) Uani 1 1 d . . . O3 O 0.7305(4) 0.0616(3) 0.3416(2) 0.0314(10) Uani 1 1 d . . . O4 O 0.7035(3) -0.0098(3) 0.1957(2) 0.0324(11) Uani 1 1 d . . . O5 O 0.4969(4) -0.1249(4) 0.3170(3) 0.0444(13) Uani 1 1 d . . . O6 O 0.5822(4) -0.1787(3) 0.2519(3) 0.0384(11) Uani 1 1 d . . . O7 O 0.9304(4) 0.1134(4) 0.2949(2) 0.0425(13) Uani 1 1 d . . . O8 O 0.8760(4) 0.0951(4) 0.4337(2) 0.0486(14) Uani 1 1 d . . . O9 O 0.5524(4) 0.1576(5) 0.0573(3) 0.0715(19) Uani 1 1 d . . . O10 O 0.7077(6) 0.1056(5) 0.0667(3) 0.083(2) Uani 1 1 d . . . O11 O 0.6344(5) 0.3272(5) 0.1615(3) 0.084(2) Uani 1 1 d . . . O101 O 0.9347(7) 0.4941(8) 0.6002(4) 0.139(4) Uani 1 1 d . . . O102 O 0.8589(9) 0.1411(9) 0.5833 0.121(9) Uani 0.50 2 d SP . . O103 O 0.9644(13) -0.0178(6) 0.4167 0.160(13) Uani 0.50 2 d SP . . O104 O 0.6166(18) -0.0762(17) 0.4612(7) 0.138(8) Uani 0.50 1 d P . . N1 N 1.0000 0.2176(6) 0.1667 0.047(2) Uani 1 2 d S . . C1 C 0.7407(5) 0.1736(5) 0.2492(3) 0.0284(15) Uani 1 1 d . . . C2 C 0.6742(5) 0.0784(5) 0.2898(3) 0.0249(14) Uani 1 1 d . . . H2A H 0.6206 0.0846 0.3135 0.030 Uiso 1 1 calc R . . C3 C 0.6268(5) -0.0094(5) 0.2362(3) 0.0276(15) Uani 1 1 d . . . H3A H 0.5833 0.0018 0.2037 0.033 Uiso 1 1 calc R . . C4 C 0.5633(5) -0.1110(5) 0.2728(3) 0.0334(17) 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 Sm 0.0280(2) 0.0280(2) 0.0258(2) 0.00385(19) 0.00385(19) 0.0154(2) Mo 0.0302(3) 0.0340(4) 0.0217(3) -0.0021(2) -0.0019(2) 0.0141(3) O1 0.032(3) 0.037(3) 0.028(2) 0.003(2) -0.003(2) 0.011(2) O2 0.049(3) 0.038(3) 0.026(2) 0.0061(19) 0.000(2) 0.027(2) O3 0.033(3) 0.029(3) 0.0222(19) 0.0030(19) -0.007(2) 0.008(2) O4 0.037(3) 0.032(2) 0.025(2) -0.0040(18) 0.011(2) 0.014(2) O5 0.034(3) 0.035(3) 0.045(3) -0.004(2) 0.009(2) 0.003(2) O6 0.046(3) 0.024(2) 0.038(2) -0.001(2) 0.007(3) 0.012(2) O7 0.047(3) 0.044(3) 0.038(3) -0.008(2) 0.006(2) 0.024(3) O8 0.049(3) 0.068(4) 0.032(3) 0.011(3) -0.005(2) 0.032(3) O9 0.042(3) 0.085(5) 0.056(3) 0.000(3) 0.000(3) 0.008(3) O10 0.138(7) 0.046(4) 0.067(4) 0.012(3) 0.048(4) 0.048(4) O11 0.118(6) 0.069(4) 0.099(4) 0.048(4) 0.080(4) 0.074(5) O101 0.115(7) 0.156(9) 0.088(6) -0.019(6) 0.005(5) 0.023(7) O102 0.19(2) 0.19(2) 0.029(8) 0.013(12) 0.013(12) 0.14(2) O103 0.041(11) 0.028(7) 0.42(4) -0.027(16) 0.000 0.021(5) O104 0.24(2) 0.19(2) 0.065(9) 0.084(11) 0.061(11) 0.168(19) N1 0.059(6) 0.043(4) 0.044(5) 0.012(2) 0.025(5) 0.030(3) C1 0.039(4) 0.027(3) 0.018(3) -0.002(3) 0.002(3) 0.016(3) C2 0.028(4) 0.024(3) 0.023(3) -0.003(3) -0.001(3) 0.014(3) C3 0.029(4) 0.033(4) 0.021(3) -0.005(3) -0.004(3) 0.015(3) C4 0.028(4) 0.037(4) 0.025(3) -0.006(3) -0.002(3) 0.009(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 Sm O2 2.367(4) 10_665 ? Sm O2 2.367(4) . ? Sm O9 2.417(6) . ? Sm O9 2.417(6) 10_665 ? Sm O10 2.433(6) 10_665 ? Sm O10 2.433(6) . ? Sm O11 2.473(5) 10_665 ? Sm O11 2.473(5) . ? Mo O8 1.701(4) . ? Mo O7 1.708(4) . ? Mo O3 1.944(5) . ? Mo O4 1.946(5) 5_665 ? Mo O6 2.209(5) 5_665 ? Mo O1 2.229(4) . ? O1 C1 1.256(8) . ? O2 C1 1.261(8) . ? O3 C2 1.403(7) . ? O3 O104 2.969(16) . ? O4 C3 1.400(7) . ? O4 Mo 1.946(5) 6_544 ? O5 C4 1.243(8) . ? O6 C4 1.272(8) . ? O6 Mo 2.209(5) 6_544 ? O7 N1 2.777(6) . ? O8 O103 2.700(9) . ? O8 O102 2.925(8) . ? O9 O6 2.934(9) 9_665 ? O11 O5 2.713(7) 6_554 ? O101 O9 2.739(10) 2_655 ? O101 O104 2.83(2) 5_665 ? O101 O1 2.973(12) 12 ? O103 O7 2.893(12) 5_665 ? O104 O9 2.874(19) 4_655 ? N1 O10 2.711(9) 5_665 ? C1 C2 1.502(9) . ? C2 C3 1.537(8) . ? C3 C4 1.524(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 Sm O2 148.3(2) 10_665 . ? O2 Sm O9 101.37(17) 10_665 . ? O2 Sm O9 89.21(18) . . ? O2 Sm O9 89.21(18) 10_665 10_665 ? O2 Sm O9 101.37(17) . 10_665 ? O9 Sm O9 140.8(4) . 10_665 ? O2 Sm O10 73.33(18) 10_665 10_665 ? O2 Sm O10 81.41(18) . 10_665 ? O9 Sm O10 146.6(3) . 10_665 ? O9 Sm O10 72.6(3) 10_665 10_665 ? O2 Sm O10 81.41(18) 10_665 . ? O2 Sm O10 73.33(18) . . ? O9 Sm O10 72.6(3) . . ? O9 Sm O10 146.6(3) 10_665 . ? O10 Sm O10 74.0(4) 10_665 . ? O2 Sm O11 69.15(18) 10_665 10_665 ? O2 Sm O11 142.38(18) . 10_665 ? O9 Sm O11 73.9(2) . 10_665 ? O9 Sm O11 75.0(2) 10_665 10_665 ? O10 Sm O11 130.0(2) 10_665 10_665 ? O10 Sm O11 129.2(3) . 10_665 ? O2 Sm O11 142.38(18) 10_665 . ? O2 Sm O11 69.15(18) . . ? O9 Sm O11 75.0(2) . . ? O9 Sm O11 73.9(2) 10_665 . ? O10 Sm O11 129.2(3) 10_665 . ? O10 Sm O11 130.0(2) . . ? O11 Sm O11 74.0(3) 10_665 . ? O8 Mo O7 104.4(2) . . ? O8 Mo O3 93.3(2) . . ? O7 Mo O3 104.5(2) . . ? O8 Mo O4 104.5(2) . 5_665 ? O7 Mo O4 93.1(2) . 5_665 ? O3 Mo O4 151.11(18) . 5_665 ? O8 Mo O6 88.0(2) . 5_665 ? O7 Mo O6 164.8(2) . 5_665 ? O3 Mo O6 83.06(17) . 5_665 ? O4 Mo O6 75.11(16) 5_665 5_665 ? O8 Mo O1 163.4(2) . . ? O7 Mo O1 90.2(2) . . ? O3 Mo O1 75.10(16) . . ? O4 Mo O1 82.24(17) 5_665 . ? O6 Mo O1 78.97(17) 5_665 . ? C1 O1 Mo 115.1(4) . . ? C1 O2 Sm 147.1(4) . . ? C2 O3 Mo 123.0(4) . . ? C2 O3 O104 116.9(5) . . ? Mo O3 O104 117.2(5) . . ? C3 O4 Mo 123.0(4) . 6_544 ? C4 O6 Mo 116.1(4) . 6_544 ? Mo O7 N1 119.5(3) . . ? Mo O8 O103 111.9(2) . . ? Mo O8 O102 131.6(5) . . ? O103 O8 O102 113.7(5) . . ? Sm O9 O6 115.2(3) . 9_665 ? Sm O11 O5 127.9(2) . 6_554 ? O9 O101 O104 62.0(3) 2_655 5_665 ? O9 O101 O1 103.7(3) 2_655 12 ? O104 O101 O1 149.2(6) 5_665 12 ? O8 O103 O7 70.49(18) . 5_665 ? O9 O104 O3 149.4(7) 4_655 . ? O10 N1 O7 93.02(18) 5_665 . ? O1 C1 O2 124.2(6) . . ? O1 C1 C2 116.5(6) . . ? O2 C1 C2 119.2(6) . . ? O3 C2 C1 110.1(5) . . ? O3 C2 C3 110.6(5) . . ? C1 C2 C3 108.5(5) . . ? O4 C3 C4 110.3(5) . . ? O4 C3 C2 108.9(5) . . ? C4 C3 C2 112.6(5) . . ? O5 C4 O6 124.4(7) . . ? O5 C4 C3 121.5(7) . . ? O6 C4 C3 114.0(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.467 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.100 data_D-MoSm _database_code_CSD 175444 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Mo2 N O26 Sm' _chemical_formula_weight 896.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(1)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' 'y, x, -z+1/3' 'x-y, -y, -z' '-x, -x+y, -z+2/3' '-y, -x, -z+5/6' '-x+y, y, -z+1/2' 'x, x-y, -z+1/6' _cell_length_a 15.3286(1) _cell_length_b 15.3286(1) _cell_length_c 18.7066(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3806.5(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7725 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 25.01 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2622 _exptl_absorpt_coefficient_mu 3.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5305 _exptl_absorpt_correction_T_max 0.9048 _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 19376 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2240 _reflns_number_gt 2156 _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^)+(0.0318P)^2^+10.9748P] 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 0.00025(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 -0.015(16) _refine_ls_number_reflns 2240 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0287 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Sm Sm 0.54429(3) 0.272146(15) 0.0833 0.03060(13) Uani 1 2 d S . . Mo Mo 0.27681(4) 0.15150(4) 0.35565(2) 0.03344(15) Uani 1 1 d . . . O1 O 0.6061(6) 0.1588(5) 0.0576(3) 0.0777(19) Uani 1 1 d . . . O2 O 0.6931(4) 0.3278(5) 0.1616(3) 0.091(2) Uani 1 1 d . . . O3 O 0.3981(5) 0.1062(4) 0.0664(3) 0.084(2) Uani 1 1 d . . . O4 O 0.1805(4) 0.1117(4) 0.2946(2) 0.0484(12) Uani 1 1 d . . . O5 O 0.3908(3) 0.2227(3) 0.2686(2) 0.0398(10) Uani 1 1 d . . . O6 O 0.2170(4) 0.0937(4) 0.4331(2) 0.0543(13) Uani 1 1 d . . . O7 O 0.4955(3) 0.2014(3) 0.1992(2) 0.0398(10) Uani 1 1 d . . . O8 O 0.5024(3) 0.3786(4) 0.4827(2) 0.0474(11) Uani 1 1 d . . . O9 O 0.2960(3) 0.2876(3) 0.3620(2) 0.0370(9) Uani 1 1 d . . . O10 O 0.4174(3) 0.2387(3) 0.4184(2) 0.0430(10) Uani 1 1 d . . . O11 O 0.3305(3) 0.0613(3) 0.34124(18) 0.0354(8) Uani 1 1 d . . . O101 O 0.2614(12) 0.1307(6) 0.5833 0.128(5) Uani 1 2 d S . . O102 O 0.5604(7) 0.4951(7) 0.6003(4) 0.043(2) Uani 0.50 1 d P . . O103 O 0.2986(14) -0.0736(15) 0.4574(7) 0.120(6) Uani 0.50 1 d P . . O104 O 0.0219(5) -0.0219(5) 0.4167 0.042(3) Uiso 0.50 2 d SP . . O105 O 0.0222(11) -0.0232(11) 0.3778(7) 0.025(3) Uiso 0.25 1 d P . . N1 N 0.2175(5) 0.0000 0.0000 0.055(2) Uani 1 2 d S . . C1 C 0.3726(4) 0.3637(4) 0.4027(3) 0.0282(12) Uani 1 1 d . . . H1A H 0.4163 0.4191 0.3706 0.034 Uiso 1 1 calc R . . C2 C 0.4029(4) 0.0772(4) 0.2894(3) 0.0305(12) Uani 1 1 d . . . H2A H 0.4627 0.0833 0.3132 0.037 Uiso 1 1 calc R . . C3 C 0.4356(4) 0.3254(5) 0.4387(3) 0.0386(14) Uani 1 1 d . . . C4 C 0.4325(4) 0.1744(4) 0.2491(3) 0.0322(12) 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 Sm 0.0273(2) 0.03096(18) 0.0323(2) 0.00581(15) 0.000 0.01367(11) Mo 0.0426(3) 0.0377(3) 0.0257(2) -0.0013(2) -0.0009(2) 0.0243(2) O1 0.117(5) 0.100(5) 0.060(3) 0.001(3) 0.004(3) 0.087(4) O2 0.046(3) 0.075(4) 0.108(4) 0.054(4) -0.033(3) -0.004(3) O3 0.094(4) 0.050(3) 0.061(3) 0.014(3) -0.031(3) 0.000(3) O4 0.052(3) 0.046(3) 0.046(3) -0.008(2) -0.018(2) 0.024(2) O5 0.058(3) 0.036(2) 0.031(2) 0.0061(17) 0.0083(19) 0.028(2) O6 0.065(3) 0.073(4) 0.039(3) 0.015(2) 0.018(2) 0.045(3) O7 0.041(2) 0.043(2) 0.032(2) 0.0025(17) 0.0056(19) 0.019(2) O8 0.040(2) 0.063(3) 0.043(2) -0.014(2) -0.013(2) 0.029(2) O9 0.045(2) 0.045(2) 0.031(2) -0.0138(19) -0.0095(18) 0.031(2) O10 0.050(3) 0.054(3) 0.042(2) -0.012(2) -0.012(2) 0.038(2) O11 0.052(2) 0.036(2) 0.0257(17) 0.0026(17) 0.0074(18) 0.0273(19) O101 0.250(15) 0.137(6) 0.035(4) 0.017(4) 0.000 0.125(8) O102 0.068(6) 0.057(6) 0.027(4) -0.009(4) -0.010(4) 0.048(5) O103 0.136(15) 0.152(15) 0.067(8) 0.070(9) 0.050(9) 0.067(13) N1 0.049(3) 0.064(6) 0.057(5) 0.027(4) 0.013(2) 0.032(3) C1 0.028(3) 0.034(3) 0.023(3) -0.005(2) 0.001(2) 0.016(2) C2 0.034(3) 0.031(3) 0.026(3) -0.002(2) -0.003(2) 0.016(2) C3 0.033(3) 0.055(4) 0.031(3) -0.003(3) 0.003(2) 0.025(3) C4 0.041(3) 0.032(3) 0.021(2) -0.006(2) -0.006(3) 0.017(2) _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 Sm O7 2.371(4) 12 ? Sm O7 2.371(4) . ? Sm O1 2.407(5) . ? Sm O1 2.407(5) 12 ? Sm O3 2.428(5) . ? Sm O3 2.428(5) 12 ? Sm O2 2.475(5) 12 ? Sm O2 2.475(5) . ? Mo O6 1.706(4) . ? Mo O4 1.719(4) . ? Mo O11 1.950(4) . ? Mo O9 1.959(4) . ? Mo O10 2.221(4) . ? Mo O5 2.234(4) . ? O5 C4 1.250(7) . ? O7 C4 1.255(7) . ? O8 C3 1.247(7) . ? O9 C1 1.396(6) . ? O10 C3 1.272(8) . ? O11 C2 1.399(7) . ? O104 O105 0.727(14) 10 ? O104 O105 0.727(14) . ? O105 O105 1.45(3) 10 ? O105 O105 1.77(3) 9 ? C1 C3 1.516(8) . ? C1 C2 1.519(7) 6 ? C2 C1 1.519(7) 5_554 ? C2 C4 1.523(8) . ? 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 O7 Sm O7 148.3(2) 12 . ? O7 Sm O1 100.69(17) 12 . ? O7 Sm O1 90.04(17) . . ? O7 Sm O1 90.04(17) 12 12 ? O7 Sm O1 100.69(17) . 12 ? O1 Sm O1 140.1(4) . 12 ? O7 Sm O3 80.69(16) 12 . ? O7 Sm O3 74.06(17) . . ? O1 Sm O3 73.0(3) . . ? O1 Sm O3 146.9(3) 12 . ? O7 Sm O3 74.06(17) 12 12 ? O7 Sm O3 80.69(16) . 12 ? O1 Sm O3 146.9(3) . 12 ? O1 Sm O3 73.0(3) 12 12 ? O3 Sm O3 73.9(4) . 12 ? O7 Sm O2 69.05(17) 12 12 ? O7 Sm O2 142.49(17) . 12 ? O1 Sm O2 73.5(2) . 12 ? O1 Sm O2 74.9(3) 12 12 ? O3 Sm O2 128.9(3) . 12 ? O3 Sm O2 130.3(2) 12 12 ? O7 Sm O2 142.49(17) 12 . ? O7 Sm O2 69.05(17) . . ? O1 Sm O2 74.9(3) . . ? O1 Sm O2 73.5(2) 12 . ? O3 Sm O2 130.3(2) . . ? O3 Sm O2 128.9(3) 12 . ? O2 Sm O2 74.1(3) 12 . ? O6 Mo O4 103.7(2) . . ? O6 Mo O11 93.3(2) . . ? O4 Mo O11 104.4(2) . . ? O6 Mo O9 104.9(2) . . ? O4 Mo O9 93.6(2) . . ? O11 Mo O9 150.65(17) . . ? O6 Mo O10 88.4(2) . . ? O4 Mo O10 165.4(2) . . ? O11 Mo O10 82.71(16) . . ? O9 Mo O10 75.10(15) . . ? O6 Mo O5 163.5(2) . . ? O4 Mo O5 90.7(2) . . ? O11 Mo O5 75.00(15) . . ? O9 Mo O5 81.93(16) . . ? O10 Mo O5 78.76(17) . . ? C4 O5 Mo 115.5(4) . . ? C4 O7 Sm 147.6(4) . . ? C1 O9 Mo 122.6(3) . . ? C3 O10 Mo 115.2(4) . . ? C2 O11 Mo 123.4(3) . . ? O105 O104 O105 177(3) 10 . ? O104 O105 O105 1.5(17) . 10 ? O104 O105 O105 160(2) . 9 ? O105 O105 O105 161.1(19) 10 9 ? O9 C1 C3 110.5(5) . . ? O9 C1 C2 108.8(4) . 6 ? C3 C1 C2 112.4(4) . 6 ? O11 C2 C1 111.7(5) . 5_554 ? O11 C2 C4 109.7(5) . . ? C1 C2 C4 108.6(4) 5_554 . ? O8 C3 O10 124.0(6) . . ? O8 C3 C1 120.9(6) . . ? O10 C3 C1 115.1(5) . . ? O5 C4 O7 124.0(5) . . ? O5 C4 C2 116.3(5) . . ? O7 C4 C2 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.623 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.091 data_MoYb _database_code_CSD 200621 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Mo2 N O26 Yb' _chemical_formula_weight 919.23 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.2645(1) _cell_length_b 15.2645(1) _cell_length_c 18.4749(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3728.0(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6058 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 25.05 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2670 _exptl_absorpt_coefficient_mu 4.840 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7653 _exptl_absorpt_correction_T_max .9051 _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 12074 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2194 _reflns_number_gt 1894 _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^)+(0.0348P)^2^+5.2837P] 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 0.00031(12) _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 0.011(16) _refine_ls_number_reflns 2194 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0527 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Yb Yb 0.72762(2) 0.27238(2) 0.0833 0.02452(19) Uani 1 2 d S . . Mo Mo 0.87345(6) 0.15377(6) 0.35485(4) 0.0270(2) Uani 1 1 d . . . O1 O 0.8306(5) 0.2244(5) 0.2654(3) 0.0320(17) Uani 1 1 d . . . O2 O 0.7036(5) 0.2015(5) 0.1945(4) 0.0361(17) Uani 1 1 d . . . O3 O 0.7294(5) 0.0639(4) 0.3406(3) 0.0273(14) Uani 1 1 d . . . O4 O 0.7014(5) -0.0093(5) 0.1939(3) 0.0328(16) Uani 1 1 d . . . O5 O 0.4950(5) -0.1235(5) 0.3178(4) 0.0386(18) Uani 1 1 d . . . O6 O 0.5792(5) -0.1791(5) 0.2504(4) 0.0324(15) Uani 1 1 d . . . O7 O 0.9301(6) 0.1136(5) 0.2942(4) 0.0399(18) Uani 1 1 d . . . O8 O 0.8747(6) 0.0959(6) 0.4339(3) 0.0449(19) Uani 1 1 d . . . O9 O 0.5590(6) 0.1616(7) 0.0577(4) 0.069(3) Uani 1 1 d . . . O10 O 0.7086(9) 0.1121(7) 0.0654(4) 0.081(3) Uani 1 1 d . . . O11 O 0.6349(7) 0.3248(6) 0.1590(5) 0.072(3) Uani 1 1 d . . . O101 O 0.9387(10) 0.4996(12) 0.6015(7) 0.151(6) Uani 1 1 d . . . O102 O 0.8600(15) 0.1400(15) 0.5833 0.112(11) Uani 0.50 2 d SP . . O103 O 0.963(2) -0.0184(10) 0.4167 0.082(8) Uiso 0.50 2 d SP . . O104 O 0.6197(17) -0.0720(18) 0.4612(11) 0.092(7) Uiso 0.50 1 d P . . N1 N 1.0000 0.2209(9) 0.1667 0.053(4) Uani 1 2 d S . . C1 C 0.7406(7) 0.1760(7) 0.2459(5) 0.028(2) Uani 1 1 d . . . C2 C 0.6726(7) 0.0810(7) 0.2878(5) 0.025(2) Uani 1 1 d . . . H2A H 0.6189 0.0880 0.3115 0.030 Uiso 1 1 calc R . . C3 C 0.6257(7) -0.0073(7) 0.2344(4) 0.026(2) Uani 1 1 d . . . H3A H 0.5819 0.0035 0.2013 0.031 Uiso 1 1 calc R . . C4 C 0.5612(7) -0.1104(7) 0.2720(5) 0.029(2) 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 Yb 0.0238(3) 0.0238(3) 0.0278(3) 0.0032(2) 0.0032(2) 0.0133(3) Mo 0.0264(5) 0.0299(5) 0.0245(4) -0.0026(4) -0.0015(4) 0.0138(4) O1 0.031(4) 0.030(4) 0.027(4) -0.002(3) -0.006(3) 0.009(3) O2 0.044(5) 0.038(4) 0.032(4) 0.007(3) -0.001(4) 0.024(4) O3 0.031(4) 0.024(4) 0.021(3) 0.005(3) 0.000(3) 0.009(3) O4 0.038(4) 0.031(4) 0.026(3) -0.005(3) 0.007(3) 0.015(3) O5 0.028(4) 0.034(4) 0.041(4) -0.002(4) 0.009(3) 0.006(3) O6 0.033(4) 0.025(3) 0.037(4) -0.002(3) 0.009(4) 0.012(3) O7 0.047(5) 0.037(4) 0.045(4) -0.006(4) 0.002(4) 0.027(4) O8 0.038(4) 0.063(5) 0.037(4) 0.006(4) -0.003(4) 0.028(4) O9 0.037(5) 0.079(6) 0.054(5) 0.010(5) 0.005(4) 0.002(5) O10 0.145(10) 0.048(5) 0.065(6) 0.014(5) 0.053(7) 0.058(6) O11 0.093(7) 0.060(6) 0.089(6) 0.044(5) 0.060(5) 0.058(6) O101 0.106(10) 0.163(14) 0.107(9) 0.004(9) 0.019(8) 0.009(10) O102 0.15(2) 0.15(2) 0.036(13) 0.008(16) 0.008(16) 0.06(3) N1 0.066(10) 0.050(6) 0.048(8) 0.019(4) 0.039(8) 0.033(5) C1 0.036(6) 0.025(5) 0.017(4) -0.008(5) -0.001(5) 0.011(5) C2 0.023(5) 0.024(5) 0.026(5) -0.010(4) -0.003(4) 0.010(4) C3 0.030(5) 0.024(5) 0.019(5) -0.005(4) -0.005(4) 0.011(4) C4 0.020(5) 0.017(5) 0.035(6) -0.005(4) -0.010(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb O2 2.265(6) 10_665 ? Yb O2 2.265(6) . ? Yb O9 2.315(8) . ? Yb O9 2.315(8) 10_665 ? Yb O10 2.339(8) . ? Yb O10 2.339(8) 10_665 ? Yb O11 2.394(7) 10_665 ? Yb O11 2.394(7) . ? Mo O7 1.705(6) . ? Mo O8 1.711(7) . ? Mo O3 1.941(7) . ? Mo O4 1.946(7) 5_665 ? Mo O6 2.201(6) 5_665 ? Mo O1 2.241(6) . ? O1 C1 1.244(11) . ? O2 C1 1.262(11) . ? O3 C2 1.414(11) . ? O3 O104 2.93(2) . ? O4 C3 1.391(10) . ? O4 Mo 1.946(7) 6_544 ? O5 C4 1.253(11) . ? O6 C4 1.274(11) . ? O6 Mo 2.201(6) 6_544 ? O7 N1 2.762(9) . ? O8 O103 2.708(13) . ? O8 O102 2.877(13) . ? O9 O6 2.956(12) 9_665 ? O11 O5 2.736(10) 6_554 ? O101 O9 2.745(15) 2_655 ? O101 O104 2.88(3) 5_665 ? O101 O1 2.906(19) 12 ? O103 O7 2.891(19) 5_665 ? O104 O9 2.96(2) 4_655 ? N1 O10 2.718(12) 5_665 ? C1 C2 1.508(13) . ? C2 C3 1.529(12) . ? C3 C4 1.542(13) . ? 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 Yb O2 148.2(3) 10_665 . ? O2 Yb O9 101.5(2) 10_665 . ? O2 Yb O9 88.9(3) . . ? O2 Yb O9 88.9(3) 10_665 10_665 ? O2 Yb O9 101.5(2) . 10_665 ? O9 Yb O9 141.4(5) . 10_665 ? O2 Yb O10 80.8(3) 10_665 . ? O2 Yb O10 73.9(3) . . ? O9 Yb O10 72.3(4) . . ? O9 Yb O10 146.3(4) 10_665 . ? O2 Yb O10 73.9(3) 10_665 10_665 ? O2 Yb O10 80.8(3) . 10_665 ? O9 Yb O10 146.3(4) . 10_665 ? O9 Yb O10 72.3(4) 10_665 10_665 ? O10 Yb O10 74.0(6) . 10_665 ? O2 Yb O11 69.4(3) 10_665 10_665 ? O2 Yb O11 142.2(3) . 10_665 ? O9 Yb O11 74.6(3) . 10_665 ? O9 Yb O11 74.7(3) 10_665 10_665 ? O10 Yb O11 129.2(3) . 10_665 ? O10 Yb O11 130.4(3) 10_665 10_665 ? O2 Yb O11 142.2(3) 10_665 . ? O2 Yb O11 69.4(3) . . ? O9 Yb O11 74.7(3) . . ? O9 Yb O11 74.6(3) 10_665 . ? O10 Yb O11 130.4(3) . . ? O10 Yb O11 129.2(3) 10_665 . ? O11 Yb O11 73.5(4) 10_665 . ? O7 Mo O8 103.7(3) . . ? O7 Mo O3 104.8(3) . . ? O8 Mo O3 93.0(3) . . ? O7 Mo O4 93.2(3) . 5_665 ? O8 Mo O4 105.1(3) . 5_665 ? O3 Mo O4 150.8(3) . 5_665 ? O7 Mo O6 165.3(3) . 5_665 ? O8 Mo O6 88.3(3) . 5_665 ? O3 Mo O6 82.7(2) . 5_665 ? O4 Mo O6 75.3(2) 5_665 5_665 ? O7 Mo O1 90.6(3) . . ? O8 Mo O1 163.4(3) . . ? O3 Mo O1 74.9(2) . . ? O4 Mo O1 82.1(2) 5_665 . ? O6 Mo O1 79.0(2) 5_665 . ? C1 O1 Mo 115.4(6) . . ? C1 O2 Yb 147.1(6) . . ? C2 O3 Mo 123.1(5) . . ? C2 O3 O104 118.0(7) . . ? Mo O3 O104 116.2(5) . . ? C3 O4 Mo 123.5(6) . 6_544 ? C4 O6 Mo 115.8(6) . 6_544 ? Mo O7 N1 117.5(4) . . ? Mo O8 O103 111.7(3) . . ? Mo O8 O102 132.5(8) . . ? O103 O8 O102 112.7(8) . . ? Yb O9 O6 115.4(4) . 9_665 ? Yb O11 O5 129.5(3) . 6_554 ? O9 O101 O104 63.4(5) 2_655 5_665 ? O9 O101 O1 100.6(5) 2_655 12 ? O104 O101 O1 147.5(7) 5_665 12 ? O8 O103 O7 70.5(3) . 5_665 ? O3 O104 O9 148.5(9) . 4_655 ? O10 N1 O7 95.0(3) 5_665 . ? O1 C1 O2 124.5(9) . . ? O1 C1 C2 116.6(8) . . ? O2 C1 C2 118.9(8) . . ? O3 C2 C1 109.9(7) . . ? O3 C2 C3 110.0(7) . . ? C1 C2 C3 108.1(7) . . ? O4 C3 C2 109.8(8) . . ? O4 C3 C4 109.5(8) . . ? C2 C3 C4 112.8(7) . . ? O5 C4 O6 124.6(9) . . ? O5 C4 C3 121.3(9) . . ? O6 C4 C3 114.1(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.712 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.128 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 data_K-MoSm _database_code_CSD 208057 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H27 Mo2 O27 Sm' _chemical_formula_weight 897.53 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' 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.374(1) _cell_length_b 15.374(1) _cell_length_c 18.741(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3836.0(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4888 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.01 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2622 _exptl_absorpt_coefficient_mu 3.345 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7209 _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 9952 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2258 _reflns_number_gt 1788 _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^)+(0.0314P)^2^+13.7843P] 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 0.00000(13) _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 -0.01(3) _refine_ls_number_reflns 2258 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0702 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Sm Sm 0.72768(3) 0.27232(3) 0.0833 0.0319(2) Uani 1 2 d S . . Mo Mo 0.87443(7) 0.15181(7) 0.35534(4) 0.0349(3) Uani 1 1 d . . . O1 O 0.8311(6) 0.2228(5) 0.2685(3) 0.0405(19) Uani 1 1 d . . . O2 O 0.7056(5) 0.2011(5) 0.1989(4) 0.0410(18) Uani 1 1 d . . . O3 O 0.7308(5) 0.0614(5) 0.3408(3) 0.0358(16) Uani 1 1 d . . . O4 O 0.7036(5) -0.0090(5) 0.1950(3) 0.0362(17) Uani 1 1 d . . . O5 O 0.4977(6) -0.1239(6) 0.3158(4) 0.046(2) Uani 1 1 d . . . O6 O 0.5826(5) -0.1788(5) 0.2517(4) 0.0446(19) Uani 1 1 d . . . O7 O 0.9305(7) 0.1127(6) 0.2945(4) 0.052(2) Uani 1 1 d . . . O8 O 0.8761(6) 0.0947(7) 0.4316(4) 0.054(2) Uani 1 1 d . . . O9 O 0.5534(7) 0.1591(8) 0.0578(4) 0.081(3) Uani 1 1 d . . . O10 O 0.7069(9) 0.1066(7) 0.0663(5) 0.085(3) Uani 1 1 d . . . O11 O 0.6352(7) 0.3287(7) 0.1618(5) 0.083(3) Uani 1 1 d . . . O101 O 0.9328(9) 0.4961(10) 0.5991(6) 0.031(3) Uani 0.50 1 d P . . O102 O 0.8715(9) 0.1285(9) 0.5833 0.129(7) Uani 1 2 d S . . O103 O 0.9614(9) -0.0188(13) 0.3932(6) 0.051(4) Uiso 0.50 1 d P . . O104 O 0.631(2) -0.073(2) 0.4576(9) 0.111(9) Uani 0.50 1 d P . . O105 O 1.0000 0.2180(8) 0.1667 0.076(4) Uani 1 2 d S . . C1 C 0.7413(8) 0.1740(7) 0.2497(5) 0.033(2) Uani 1 1 d . . . C2 C 0.6736(8) 0.0770(8) 0.2892(5) 0.031(2) Uani 1 1 d . . . H2A H 0.6200 0.0828 0.3131 0.037 Uiso 1 1 calc R . . C3 C 0.6271(7) -0.0092(8) 0.2360(4) 0.029(2) Uani 1 1 d . . . H3A H 0.5838 0.0026 0.2039 0.035 Uiso 1 1 calc R . . C4 C 0.5632(8) -0.1112(8) 0.2713(5) 0.041(3) 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 Sm 0.0340(3) 0.0340(3) 0.0294(4) 0.0052(3) 0.0052(3) 0.0183(4) Mo 0.0354(6) 0.0394(6) 0.0264(4) -0.0016(4) -0.0013(4) 0.0161(5) O1 0.048(5) 0.037(4) 0.028(4) 0.003(3) -0.006(4) 0.015(4) O2 0.043(5) 0.043(4) 0.038(4) 0.004(3) 0.003(4) 0.022(4) O3 0.033(4) 0.033(4) 0.025(3) -0.003(3) -0.007(3) 0.005(4) O4 0.043(5) 0.031(4) 0.026(3) -0.005(3) 0.007(3) 0.013(3) O5 0.043(5) 0.040(5) 0.041(4) -0.008(4) 0.008(4) 0.011(4) O6 0.051(5) 0.032(4) 0.041(4) 0.003(4) 0.014(4) 0.013(4) O7 0.061(6) 0.048(5) 0.045(4) -0.007(4) 0.007(4) 0.025(5) O8 0.054(5) 0.073(6) 0.039(4) 0.006(4) -0.009(4) 0.035(5) O9 0.049(5) 0.091(7) 0.069(6) -0.006(5) -0.010(5) 0.009(5) O10 0.137(10) 0.040(5) 0.072(6) 0.012(5) 0.041(7) 0.038(6) O11 0.111(8) 0.070(6) 0.098(7) 0.049(6) 0.078(6) 0.067(6) O101 0.015(6) 0.055(9) 0.014(6) -0.008(6) -0.002(5) 0.010(6) O102 0.138(9) 0.138(9) 0.027(6) 0.008(7) 0.008(7) 0.006(12) O104 0.15(2) 0.16(2) 0.048(10) 0.070(13) 0.020(12) 0.10(2) O105 0.090(11) 0.065(6) 0.082(9) 0.012(4) 0.023(9) 0.045(5) C1 0.045(7) 0.041(6) 0.014(4) -0.016(5) -0.012(5) 0.022(6) C2 0.031(6) 0.032(6) 0.023(5) 0.003(5) 0.004(5) 0.011(5) C3 0.039(6) 0.038(6) 0.015(5) -0.006(4) -0.009(4) 0.023(5) C4 0.035(6) 0.040(7) 0.031(6) -0.009(5) -0.005(5) 0.007(6) _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 Sm O2 2.374(7) 10_665 ? Sm O2 2.374(7) . ? Sm O9 2.404(9) . ? Sm O9 2.404(9) 10_665 ? Sm O10 2.425(8) . ? Sm O10 2.425(8) 10_665 ? Sm O11 2.483(8) 10_665 ? Sm O11 2.483(8) . ? Mo O8 1.684(7) . ? Mo O7 1.710(7) . ? Mo O3 1.953(7) . ? Mo O4 1.959(7) 5_665 ? Mo O6 2.221(7) 5_665 ? Mo O1 2.237(7) . ? O1 C1 1.249(12) . ? O2 C1 1.267(11) . ? O3 C2 1.407(12) . ? O3 O104 2.874(19) . ? O4 C3 1.404(11) . ? O4 Mo 1.959(7) 6_544 ? O5 C4 1.244(12) . ? O6 C4 1.272(14) . ? O6 Mo 2.221(7) 6_544 ? O7 O105 2.788(9) . ? O8 O103 2.751(19) . ? O8 O102 2.898(8) . ? O9 O6 2.936(13) 9_665 ? O11 O5 2.719(11) 6_554 ? O101 O9 2.783(15) 2_655 ? O101 O1 2.921(14) 12 ? O101 O104 3.07(3) 5_665 ? O103 O103 0.88(2) 12_545 ? O103 O7 3.064(17) 5_665 ? O104 O9 3.09(2) 4_655 ? O105 O10 2.731(13) 5_665 ? C1 C2 1.518(14) . ? C2 C3 1.521(13) . ? C3 C4 1.524(14) . ? 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 Sm O2 148.0(4) 10_665 . ? O2 Sm O9 100.9(3) 10_665 . ? O2 Sm O9 89.8(3) . . ? O2 Sm O9 89.8(3) 10_665 10_665 ? O2 Sm O9 100.9(3) . 10_665 ? O9 Sm O9 140.5(6) . 10_665 ? O2 Sm O10 80.8(3) 10_665 . ? O2 Sm O10 73.8(3) . . ? O9 Sm O10 72.5(4) . . ? O9 Sm O10 147.0(4) 10_665 . ? O2 Sm O10 73.8(3) 10_665 10_665 ? O2 Sm O10 80.8(3) . 10_665 ? O9 Sm O10 147.0(4) . 10_665 ? O9 Sm O10 72.5(4) 10_665 10_665 ? O10 Sm O10 74.5(6) . 10_665 ? O2 Sm O11 69.3(3) 10_665 10_665 ? O2 Sm O11 142.6(3) . 10_665 ? O9 Sm O11 73.4(3) . 10_665 ? O9 Sm O11 75.3(4) 10_665 10_665 ? O10 Sm O11 128.6(4) . 10_665 ? O10 Sm O11 130.3(3) 10_665 10_665 ? O2 Sm O11 142.6(3) 10_665 . ? O2 Sm O11 69.3(3) . . ? O9 Sm O11 75.3(4) . . ? O9 Sm O11 73.4(3) 10_665 . ? O10 Sm O11 130.3(3) . . ? O10 Sm O11 128.6(4) 10_665 . ? O11 Sm O11 74.1(4) 10_665 . ? O8 Mo O7 103.9(4) . . ? O8 Mo O3 93.1(3) . . ? O7 Mo O3 104.2(4) . . ? O8 Mo O4 105.0(3) . 5_665 ? O7 Mo O4 93.5(3) . 5_665 ? O3 Mo O4 150.9(3) . 5_665 ? O8 Mo O6 88.2(3) . 5_665 ? O7 Mo O6 165.4(3) . 5_665 ? O3 Mo O6 82.9(3) . 5_665 ? O4 Mo O6 75.2(3) 5_665 5_665 ? O8 Mo O1 163.1(3) . . ? O7 Mo O1 90.7(3) . . ? O3 Mo O1 74.9(3) . . ? O4 Mo O1 82.1(3) 5_665 . ? O6 Mo O1 78.7(3) 5_665 . ? C1 O1 Mo 115.0(6) . . ? C1 O2 Sm 148.3(7) . . ? C2 O3 Mo 123.7(6) . . ? C2 O3 O104 119.5(7) . . ? Mo O3 O104 114.4(5) . . ? C3 O4 Mo 122.7(6) . 6_544 ? C4 O6 Mo 115.7(7) . 6_544 ? Mo O7 O105 118.9(5) . . ? Mo O8 O103 104.2(4) . . ? Mo O8 O102 137.0(6) . . ? O103 O8 O102 115.6(5) . . ? Sm O9 O6 115.9(4) . 9_665 ? Sm O11 O5 127.8(3) . 6_554 ? O9 O101 O1 104.3(4) 2_655 12 ? O9 O101 O104 63.5(4) 2_655 5_665 ? O1 O101 O104 150.4(7) 12 5_665 ? O103 O103 O8 76(2) 12_545 . ? O103 O103 O7 66.2(17) 12_545 5_665 ? O8 O103 O7 67.3(4) . 5_665 ? O3 O104 O9 144.6(9) . 4_655 ? O10 O105 O7 93.6(3) 5_665 . ? O1 C1 O2 123.1(10) . . ? O1 C1 C2 117.4(9) . . ? O2 C1 C2 119.5(9) . . ? O3 C2 C1 108.9(8) . . ? O3 C2 C3 111.3(8) . . ? C1 C2 C3 109.2(8) . . ? O4 C3 C2 109.2(8) . . ? O4 C3 C4 110.4(9) . . ? C2 C3 C4 113.1(7) . . ? O5 C4 O6 124.6(10) . . ? O5 C4 C3 120.5(11) . . ? O6 C4 C3 114.9(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.731 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.124 data_MoEu _database_code_CSD 208058 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Eu Mo2 N O26' _chemical_formula_weight 898.15 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.3351(2) _cell_length_b 15.3351(2) _cell_length_c 18.7435(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3817.3(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3932 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 25.02 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_absorpt_coefficient_mu 3.517 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3703 _exptl_absorpt_correction_T_max 0.5619 _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 9320 _diffrn_reflns_av_R_equivalents 0.0884 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2253 _reflns_number_gt 1681 _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^)+(0.0305P)^2^+2.7593P] 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 0.00030(16) _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 0.00(3) _refine_ls_number_reflns 2253 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0780 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Eu Eu 0.72747(3) 0.27253(3) 0.0833 0.0271(2) Uani 1 2 d S . . Mo Mo 0.87321(7) 0.15243(7) 0.35449(4) 0.0318(3) Uani 1 1 d . . . O1 O 0.8291(6) 0.2230(6) 0.2680(4) 0.038(2) Uani 1 1 d . . . O2 O 0.7031(6) 0.2000(5) 0.1982(4) 0.0353(19) Uani 1 1 d . . . O3 O 0.7295(6) 0.0612(5) 0.3401(3) 0.0306(17) Uani 1 1 d . . . O4 O 0.7020(6) -0.0109(5) 0.1944(3) 0.0358(19) Uani 1 1 d . . . O5 O 0.4970(6) -0.1255(6) 0.3158(4) 0.040(2) Uani 1 1 d . . . O6 O 0.5816(5) -0.1794(5) 0.2502(4) 0.0372(19) Uani 1 1 d . . . O7 O 0.9291(7) 0.1145(6) 0.2924(4) 0.046(2) Uani 1 1 d . . . O8 O 0.8759(7) 0.0951(7) 0.4308(4) 0.053(2) Uani 1 1 d . . . O9 O 0.5519(6) 0.1582(7) 0.0585(4) 0.065(3) Uani 1 1 d . . . O10 O 0.7066(9) 0.1075(7) 0.0654(5) 0.080(4) Uani 1 1 d . . . O11 O 0.6356(7) 0.3286(6) 0.1610(4) 0.064(3) Uani 1 1 d . . . O101 O 0.9329(8) 0.4949(10) 0.5994(5) 0.113(4) Uani 1 1 d . . . O102 O 0.8558(16) 0.1442(16) 0.5833 0.144(16) Uani 0.50 2 d SP . . O103 O 0.977(4) -0.012(2) 0.4167 0.193(18) Uiso 0.50 2 d SP . . O104 O 0.6360(18) -0.0743(19) 0.4546(9) 0.107(9) Uani 0.50 1 d P . . N1 N 1.0000 0.2187(9) 0.1667 0.052(4) Uani 1 2 d S . . C1 C 0.7379(9) 0.1726(8) 0.2488(6) 0.030(3) Uani 1 1 d . . . C2 C 0.6735(8) 0.0787(8) 0.2879(5) 0.024(2) Uani 1 1 d . . . H2A H 0.6193 0.0840 0.3115 0.029 Uiso 1 1 calc R . . C3 C 0.6269(8) -0.0097(8) 0.2351(5) 0.032(3) Uani 1 1 d . . . H3A H 0.5828 0.0010 0.2028 0.038 Uiso 1 1 calc R . . C4 C 0.5632(9) -0.1127(8) 0.2714(6) 0.033(3) 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 Eu 0.0282(4) 0.0282(4) 0.0262(4) 0.0042(3) 0.0042(3) 0.0150(4) Mo 0.0330(6) 0.0344(7) 0.0277(5) -0.0028(5) -0.0038(5) 0.0166(5) O1 0.036(5) 0.039(5) 0.033(5) -0.001(4) -0.013(4) 0.013(4) O2 0.048(5) 0.037(4) 0.025(4) 0.007(3) 0.006(4) 0.024(4) O3 0.034(4) 0.027(4) 0.021(3) 0.000(3) -0.012(4) 0.008(4) O4 0.048(5) 0.037(5) 0.021(4) -0.002(3) 0.012(4) 0.019(4) O5 0.034(5) 0.028(5) 0.041(5) -0.002(4) 0.012(4) 0.003(4) O6 0.047(5) 0.024(4) 0.037(4) -0.004(4) 0.008(4) 0.014(4) O7 0.054(6) 0.049(6) 0.044(5) -0.014(4) 0.004(4) 0.032(5) O8 0.060(6) 0.069(6) 0.034(5) 0.013(5) -0.012(4) 0.035(5) O9 0.036(5) 0.079(7) 0.061(6) -0.008(5) 0.000(5) 0.014(5) O10 0.133(10) 0.045(6) 0.067(6) 0.024(5) 0.061(7) 0.047(6) O11 0.089(7) 0.055(6) 0.073(6) 0.037(5) 0.058(5) 0.054(6) O101 0.081(8) 0.135(12) 0.090(8) -0.007(8) 0.006(7) 0.029(8) O102 0.23(4) 0.23(4) 0.019(13) 0.02(2) 0.02(2) 0.15(4) O104 0.12(2) 0.12(2) 0.047(11) 0.057(12) -0.021(12) 0.031(17) N1 0.056(11) 0.041(6) 0.064(10) 0.008(4) 0.016(9) 0.028(5) C1 0.055(8) 0.030(6) 0.013(5) -0.012(5) -0.005(6) 0.028(6) C2 0.025(6) 0.025(6) 0.021(5) 0.003(5) -0.001(5) 0.011(5) C3 0.028(7) 0.041(7) 0.026(7) -0.010(5) -0.004(5) 0.018(6) C4 0.044(8) 0.026(7) 0.024(6) -0.010(5) -0.017(5) 0.012(6) _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 Eu O2 2.366(7) 10_665 ? Eu O2 2.366(7) . ? Eu O10 2.410(8) . ? Eu O10 2.410(8) 10_665 ? Eu O9 2.412(8) . ? Eu O9 2.412(8) 10_665 ? Eu O11 2.461(7) 10_665 ? Eu O11 2.461(7) . ? Mo O8 1.691(7) . ? Mo O7 1.710(7) . ? Mo O4 1.942(8) 5_665 ? Mo O3 1.950(7) . ? Mo O6 2.203(7) 5_665 ? Mo O1 2.233(7) . ? O1 C1 1.265(12) . ? O2 C1 1.259(12) . ? O3 C2 1.413(11) . ? O3 O104 2.829(19) . ? O4 C3 1.391(11) . ? O4 Mo 1.942(7) 6_544 ? O5 C4 1.250(13) . ? O6 C4 1.253(13) . ? O6 Mo 2.203(7) 6_544 ? O7 N1 2.749(9) . ? O8 O103 2.77(3) . ? O8 O102 3.011(15) . ? O9 O6 2.912(12) 9_665 ? O11 O5 2.697(10) 6_554 ? O101 O9 2.784(14) 2_655 ? O101 O1 2.927(15) 12 ? O101 O104 3.12(3) 5_665 ? O103 O7 2.80(3) 5_665 ? O104 O9 3.17(2) 4_655 ? N1 O10 2.724(13) 5_665 ? C1 C2 1.472(14) . ? C2 C3 1.535(14) . ? C3 C4 1.540(15) . ? 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 Eu O2 148.6(4) 10_665 . ? O2 Eu O10 81.0(3) 10_665 . ? O2 Eu O10 74.1(3) . . ? O2 Eu O10 74.1(3) 10_665 10_665 ? O2 Eu O10 81.0(3) . 10_665 ? O10 Eu O10 74.8(6) . 10_665 ? O2 Eu O9 101.8(3) 10_665 . ? O2 Eu O9 88.7(3) . . ? O10 Eu O9 72.3(4) . . ? O10 Eu O9 147.1(4) 10_665 . ? O2 Eu O9 88.7(3) 10_665 10_665 ? O2 Eu O9 101.8(3) . 10_665 ? O10 Eu O9 147.1(4) . 10_665 ? O10 Eu O9 72.3(4) 10_665 10_665 ? O9 Eu O9 140.6(5) . 10_665 ? O2 Eu O11 69.1(3) 10_665 10_665 ? O2 Eu O11 142.1(3) . 10_665 ? O10 Eu O11 128.2(3) . 10_665 ? O10 Eu O11 130.6(3) 10_665 10_665 ? O9 Eu O11 73.7(3) . 10_665 ? O9 Eu O11 75.1(3) 10_665 10_665 ? O2 Eu O11 142.1(3) 10_665 . ? O2 Eu O11 69.1(3) . . ? O10 Eu O11 130.6(3) . . ? O10 Eu O11 128.2(3) 10_665 . ? O9 Eu O11 75.1(3) . . ? O9 Eu O11 73.7(3) 10_665 . ? O11 Eu O11 74.0(4) 10_665 . ? O8 Mo O7 104.6(4) . . ? O8 Mo O4 104.6(4) . 5_665 ? O7 Mo O4 93.2(4) . 5_665 ? O8 Mo O3 93.3(4) . . ? O7 Mo O3 103.9(4) . . ? O4 Mo O3 151.3(3) 5_665 . ? O8 Mo O6 88.6(3) . 5_665 ? O7 Mo O6 164.3(3) . 5_665 ? O4 Mo O6 75.0(3) 5_665 5_665 ? O3 Mo O6 83.3(3) . 5_665 ? O8 Mo O1 163.4(3) . . ? O7 Mo O1 89.8(3) . . ? O4 Mo O1 82.4(3) 5_665 . ? O3 Mo O1 74.9(3) . . ? O6 Mo O1 78.6(3) 5_665 . ? C1 O1 Mo 114.9(7) . . ? C1 O2 Eu 148.0(7) . . ? C2 O3 Mo 122.4(6) . . ? C2 O3 O104 122.1(8) . . ? Mo O3 O104 113.5(5) . . ? C3 O4 Mo 123.4(6) . 6_544 ? C4 O6 Mo 116.2(7) . 6_544 ? Mo O7 N1 120.4(5) . . ? Mo O8 O103 113.1(4) . . ? Mo O8 O102 129.8(8) . . ? O103 O8 O102 113.3(8) . . ? Eu O9 O6 115.3(4) . 9_665 ? Eu O11 O5 128.0(3) . 6_554 ? O9 O101 O1 104.0(4) 2_655 12 ? O9 O101 O104 64.7(4) 2_655 5_665 ? O1 O101 O104 149.5(7) 12 5_665 ? O8 O103 O7 71.2(3) . 5_665 ? O3 O104 O9 142.1(10) . 4_655 ? O10 N1 O7 94.1(3) 5_665 . ? O2 C1 O1 122.3(10) . . ? O2 C1 C2 120.8(10) . . ? O1 C1 C2 116.9(9) . . ? O3 C2 C1 110.8(9) . . ? O3 C2 C3 109.8(8) . . ? C1 C2 C3 109.3(8) . . ? O4 C3 C2 110.0(8) . . ? O4 C3 C4 109.5(9) . . ? C2 C3 C4 113.4(8) . . ? O5 C4 O6 125.4(10) . . ? O5 C4 C3 120.3(10) . . ? O6 C4 C3 114.3(10) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.803 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.146 data_MoHo _database_code_CSD 208059 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Ho Mo2 N O26' _chemical_formula_weight 911.12 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.3017(2) _cell_length_b 15.3017(2) _cell_length_c 18.5504(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3761.5(1) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3798 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 23.00 _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2652 _exptl_absorpt_coefficient_mu 4.223 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.0033 _exptl_absorpt_correction_T_max 0.0159 _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 11541 _diffrn_reflns_av_R_equivalents 0.1145 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 23.00 _reflns_number_total 1735 _reflns_number_gt 1330 _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^)+(0.0377P)^2^+3.6256P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 1735 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0809 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Ho Ho 0.72771(4) 0.27229(4) 0.0833 0.0503(3) Uani 1 2 d S . . Mo Mo 0.87330(10) 0.15297(10) 0.35518(6) 0.0514(4) Uani 1 1 d . . . O1 O 0.8298(8) 0.2239(8) 0.2667(5) 0.054(3) Uani 1 1 d . . . O2 O 0.7038(7) 0.1997(7) 0.1960(5) 0.051(3) Uani 1 1 d . . . O3 O 0.7276(8) 0.0624(7) 0.3407(4) 0.050(2) Uani 1 1 d . . . O4 O 0.7014(7) -0.0094(7) 0.1941(5) 0.056(3) Uani 1 1 d . . . O5 O 0.4968(9) -0.1240(9) 0.3173(6) 0.068(3) Uani 1 1 d . . . O6 O 0.5798(7) -0.1799(8) 0.2514(6) 0.060(3) Uani 1 1 d . . . O7 O 0.9303(9) 0.1136(8) 0.2945(5) 0.068(3) Uani 1 1 d . . . O8 O 0.8751(9) 0.0967(9) 0.4337(5) 0.068(3) Uani 1 1 d . . . O9 O 0.5555(9) 0.1583(10) 0.0582(6) 0.092(4) Uani 1 1 d . . . O10 O 0.7073(14) 0.1092(10) 0.0668(7) 0.119(6) Uani 1 1 d . . . O11 O 0.6353(9) 0.3262(9) 0.1613(6) 0.090(4) Uani 1 1 d . . . O101 O 0.9350(14) 0.4974(15) 0.6006(9) 0.160(7) Uani 1 1 d . . . O102 O 0.8587(17) 0.1413(17) 0.5833 0.133(16) Uani 0.50 2 d SP . . O103 O 0.968(3) -0.0160(13) 0.4167 0.15(2) Uani 0.50 2 d SP . . O104 O 0.617(3) -0.076(3) 0.4596(12) 0.138(14) Uani 0.50 1 d P . . N1 N 1.0000 0.2195(13) 0.1667 0.070(6) Uani 1 2 d S . . C1 C 0.7426(13) 0.1777(11) 0.2465(8) 0.054(4) Uani 1 1 d . . . C2 C 0.6712(12) 0.0781(12) 0.2878(8) 0.049(4) Uani 1 1 d . . . H2A H 0.6172 0.0846 0.3111 0.059 Uiso 1 1 calc R . . C3 C 0.6257(11) -0.0080(11) 0.2350(6) 0.043(4) Uani 1 1 d . . . H3A H 0.5821 0.0032 0.2022 0.052 Uiso 1 1 calc R . . C4 C 0.5601(13) -0.1107(12) 0.2732(8) 0.053(4) 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 Ho 0.0495(5) 0.0495(5) 0.0528(5) 0.0032(5) 0.0032(5) 0.0254(6) Mo 0.0504(10) 0.0543(10) 0.0483(6) -0.0026(6) -0.0025(6) 0.0253(8) O1 0.053(8) 0.058(7) 0.048(6) 0.001(5) -0.018(5) 0.026(6) O2 0.058(7) 0.048(6) 0.051(5) 0.010(4) -0.002(5) 0.029(6) O3 0.051(6) 0.044(7) 0.046(5) 0.000(4) -0.007(5) 0.017(6) O4 0.041(7) 0.068(7) 0.046(5) -0.005(5) 0.006(5) 0.016(6) O5 0.057(8) 0.057(8) 0.065(6) -0.001(6) 0.015(6) 0.010(6) O6 0.058(7) 0.048(7) 0.067(6) -0.002(6) 0.001(6) 0.022(6) O7 0.075(8) 0.062(8) 0.068(6) -0.002(6) -0.005(6) 0.034(7) O8 0.067(8) 0.077(9) 0.067(6) 0.010(6) 0.002(6) 0.042(7) O9 0.047(8) 0.098(10) 0.093(8) -0.003(7) -0.008(6) 0.008(7) O10 0.185(16) 0.072(10) 0.105(10) 0.007(8) 0.063(11) 0.067(10) O11 0.116(11) 0.071(9) 0.103(8) 0.032(7) 0.056(7) 0.061(9) O101 0.131(14) 0.18(2) 0.143(14) 0.014(14) -0.003(12) 0.062(14) O102 0.21(4) 0.21(4) 0.046(15) -0.02(2) -0.02(2) 0.15(4) O103 0.07(3) 0.036(15) 0.34(6) -0.03(3) 0.000 0.036(14) O104 0.26(4) 0.15(3) 0.055(13) 0.044(16) 0.041(18) 0.13(3) N1 0.076(15) 0.064(10) 0.074(11) 0.004(6) 0.008(11) 0.038(8) C1 0.075(13) 0.051(10) 0.043(8) 0.000(8) -0.007(9) 0.037(10) C2 0.040(9) 0.061(11) 0.047(8) -0.003(7) 0.001(7) 0.025(9) C3 0.049(10) 0.048(10) 0.038(8) -0.014(7) -0.012(6) 0.029(8) C4 0.046(11) 0.040(11) 0.055(9) -0.008(8) -0.015(8) 0.008(9) _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 Ho O2 2.309(9) 10_665 ? Ho O2 2.309(9) . ? Ho O9 2.368(11) . ? Ho O9 2.368(11) 10_665 ? Ho O10 2.375(12) . ? Ho O10 2.375(12) 10_665 ? Ho O11 2.436(10) 10_665 ? Ho O11 2.436(10) . ? Mo O8 1.700(10) . ? Mo O7 1.706(10) . ? Mo O4 1.959(11) 5_665 ? Mo O3 1.968(11) . ? Mo O6 2.213(11) 5_665 ? Mo O1 2.244(9) . ? O1 C1 1.215(17) . ? O2 C1 1.242(17) . ? O3 C2 1.404(17) . ? O3 O104 2.94(3) . ? O4 C3 1.393(15) . ? O4 Mo 1.959(11) 6_544 ? O5 C4 1.205(18) . ? O6 C4 1.301(18) . ? O6 Mo 2.213(11) 6_544 ? O7 N1 2.768(13) . ? O8 O103 2.748(19) . ? O8 O102 2.898(16) . ? O9 O6 2.941(18) 9_665 ? O11 O5 2.736(15) 6_554 ? O101 O9 2.74(2) 2_655 ? O101 O104 2.87(5) 5_665 ? O101 O1 2.90(2) 12 ? O103 O7 2.86(3) 5_665 ? O104 O9 2.93(3) 4_655 ? N1 O10 2.729(19) 5_665 ? C1 C2 1.56(2) . ? C2 C3 1.504(18) . ? C3 C4 1.55(2) . ? 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 Ho O2 147.5(5) 10_665 . ? O2 Ho O9 102.1(3) 10_665 . ? O2 Ho O9 88.5(4) . . ? O2 Ho O9 88.5(4) 10_665 10_665 ? O2 Ho O9 102.1(3) . 10_665 ? O9 Ho O9 142.0(7) . 10_665 ? O2 Ho O10 81.3(4) 10_665 . ? O2 Ho O10 72.9(4) . . ? O9 Ho O10 71.8(6) . . ? O9 Ho O10 146.2(5) 10_665 . ? O2 Ho O10 72.9(4) 10_665 10_665 ? O2 Ho O10 81.3(4) . 10_665 ? O9 Ho O10 146.2(5) . 10_665 ? O9 Ho O10 71.8(6) 10_665 10_665 ? O10 Ho O10 74.5(9) . 10_665 ? O2 Ho O11 69.3(4) 10_665 10_665 ? O2 Ho O11 143.0(3) . 10_665 ? O9 Ho O11 74.7(4) . 10_665 ? O9 Ho O11 75.3(5) 10_665 10_665 ? O10 Ho O11 128.9(5) . 10_665 ? O10 Ho O11 129.7(4) 10_665 10_665 ? O2 Ho O11 143.0(3) 10_665 . ? O2 Ho O11 69.3(4) . . ? O9 Ho O11 75.3(5) . . ? O9 Ho O11 74.7(4) 10_665 . ? O10 Ho O11 129.7(4) . . ? O10 Ho O11 128.9(5) 10_665 . ? O11 Ho O11 74.6(5) 10_665 . ? O8 Mo O7 104.2(5) . . ? O8 Mo O4 104.8(5) . 5_665 ? O7 Mo O4 93.0(5) . 5_665 ? O8 Mo O3 93.4(5) . . ? O7 Mo O3 105.1(5) . . ? O4 Mo O3 150.4(4) 5_665 . ? O8 Mo O6 87.6(4) . 5_665 ? O7 Mo O6 165.3(5) . 5_665 ? O4 Mo O6 75.3(4) 5_665 5_665 ? O3 Mo O6 82.4(4) . 5_665 ? O8 Mo O1 162.9(4) . . ? O7 Mo O1 90.9(4) . . ? O4 Mo O1 81.9(4) 5_665 . ? O3 Mo O1 74.6(4) . . ? O6 Mo O1 78.8(4) 5_665 . ? C1 O1 Mo 116.7(9) . . ? C1 O2 Ho 146.2(10) . . ? C2 O3 Mo 123.5(8) . . ? C2 O3 O104 117.7(11) . . ? Mo O3 O104 116.6(8) . . ? C3 O4 Mo 123.3(9) . 6_544 ? C4 O6 Mo 116.2(10) . 6_544 ? Mo O7 N1 118.3(6) . . ? Mo O8 O103 111.3(5) . . ? Mo O8 O102 132.6(9) . . ? O103 O8 O102 113.0(9) . . ? Ho O9 O6 114.7(5) . 9_665 ? Ho O11 O5 128.1(5) . 6_554 ? O9 O101 O104 62.8(6) 2_655 5_665 ? O9 O101 O1 102.7(7) 2_655 12 ? O104 O101 O1 148.0(10) 5_665 12 ? O8 O103 O7 70.6(4) . 5_665 ? O9 O104 O3 148.3(13) 4_655 . ? O10 N1 O7 94.0(4) 5_665 . ? O1 C1 O2 127.6(15) . . ? O1 C1 C2 116.4(13) . . ? O2 C1 C2 116.0(15) . . ? O3 C2 C3 111.1(12) . . ? O3 C2 C1 108.7(12) . . ? C3 C2 C1 109.1(11) . . ? O4 C3 C2 110.1(12) . . ? O4 C3 C4 110.7(13) . . ? C2 C3 C4 111.8(11) . . ? O5 C4 O6 124.6(15) . . ? O5 C4 C3 122.6(16) . . ? O6 C4 C3 112.8(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.627 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.108 data_MoY _database_code_CSD 208060 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Mo2 N O26 Y' _chemical_formula_weight 835.10 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5)22 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 15.295(1) _cell_length_b 15.295(1) _cell_length_c 18.597(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3767.8(6) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1821 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 25.05 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 3.388 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3314 _exptl_absorpt_correction_T_max 0.5618 _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 8448 _diffrn_reflns_av_R_equivalents 0.1662 _diffrn_reflns_av_sigmaI/netI 0.1852 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2237 _reflns_number_gt 1220 _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^)+(0.0497P)^2^+4.1390P] 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 0.0000(2) _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 -0.03(3) _refine_ls_number_reflns 2237 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.1583 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.043 _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 Y Y 0.72758(8) 0.27242(8) 0.0833 0.0292(6) Uani 1 2 d S . . Mo Mo 0.87311(11) 0.15302(11) 0.35478(7) 0.0322(4) Uani 1 1 d . . . O1 O 0.8295(8) 0.2226(7) 0.2662(5) 0.033(3) Uani 1 1 d . . . O2 O 0.7037(8) 0.2021(7) 0.1965(5) 0.032(3) Uani 1 1 d . . . O3 O 0.7288(8) 0.0617(7) 0.3402(5) 0.033(3) Uani 1 1 d . . . O4 O 0.7004(8) -0.0105(7) 0.1943(5) 0.030(3) Uani 1 1 d . . . O5 O 0.4970(8) -0.1234(8) 0.3160(5) 0.037(3) Uani 1 1 d . . . O6 O 0.5811(8) -0.1794(7) 0.2512(6) 0.039(3) Uani 1 1 d . . . O7 O 0.9298(9) 0.1132(8) 0.2939(5) 0.042(3) Uani 1 1 d . . . O8 O 0.8741(8) 0.0951(9) 0.4330(5) 0.045(3) Uani 1 1 d . . . O9 O 0.5568(8) 0.1610(10) 0.0569(6) 0.066(4) Uani 1 1 d . . . O10 O 0.7065(11) 0.1083(9) 0.0659(7) 0.075(4) Uani 1 1 d . . . O11 O 0.6358(9) 0.3256(9) 0.1596(6) 0.063(4) Uani 1 1 d . . . O101 O 0.9359(15) 0.4947(17) 0.6016(9) 0.166(9) Uani 1 1 d . . . O102 O 0.8562(17) 0.1438(17) 0.5833 0.099(13) Uiso 0.50 2 d SP . . O103 O 0.959(3) -0.0207(16) 0.4167 0.111(16) Uiso 0.50 2 d SP . . O104 O 0.634(2) -0.065(2) 0.4581(14) 0.087(10) Uiso 0.50 1 d P . . N1 N 1.0000 0.2197(12) 0.1667 0.042(5) Uani 1 2 d S . . C1 C 0.7400(12) 0.1753(12) 0.2475(9) 0.030(4) Uani 1 1 d . . . C2 C 0.6721(12) 0.0784(11) 0.2887(8) 0.032(4) Uani 1 1 d . . . H2A H 0.6180 0.0841 0.3125 0.039 Uiso 1 1 calc R . . C3 C 0.6267(11) -0.0079(10) 0.2349(8) 0.024(4) Uani 1 1 d . . . H3A H 0.5828 0.0034 0.2024 0.029 Uiso 1 1 calc R . . C4 C 0.5612(12) -0.1124(12) 0.2724(8) 0.032(4) 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 Y 0.0307(10) 0.0307(10) 0.0272(12) 0.0048(10) 0.0048(10) 0.0161(12) Mo 0.0330(9) 0.0375(10) 0.0255(7) -0.0030(7) -0.0032(7) 0.0172(8) O1 0.034(7) 0.033(6) 0.026(6) 0.003(5) -0.002(6) 0.011(6) O2 0.034(7) 0.037(7) 0.026(6) 0.013(5) 0.001(6) 0.018(6) O3 0.037(7) 0.031(6) 0.022(5) 0.007(5) -0.006(5) 0.010(6) O4 0.041(7) 0.023(6) 0.022(6) -0.007(5) 0.003(6) 0.013(6) O5 0.034(7) 0.053(8) 0.023(6) -0.006(6) 0.007(6) 0.022(6) O6 0.054(7) 0.030(6) 0.026(6) -0.005(6) 0.008(6) 0.015(6) O7 0.049(8) 0.035(7) 0.040(7) -0.006(6) 0.004(6) 0.019(6) O8 0.053(8) 0.056(8) 0.030(6) -0.002(6) -0.010(6) 0.030(7) O9 0.020(7) 0.087(10) 0.049(8) -0.010(7) -0.009(6) -0.003(7) O10 0.113(12) 0.038(8) 0.065(9) 0.009(7) 0.027(9) 0.031(8) O11 0.074(9) 0.057(8) 0.079(8) 0.036(8) 0.054(7) 0.049(8) O101 0.114(16) 0.23(3) 0.128(15) -0.018(17) 0.015(13) 0.062(17) N1 0.056(14) 0.037(9) 0.040(13) 0.006(5) 0.013(11) 0.028(7) C1 0.037(11) 0.040(10) 0.025(9) -0.009(9) 0.002(9) 0.028(9) C2 0.026(9) 0.025(10) 0.033(10) -0.020(8) -0.007(8) 0.004(8) C3 0.021(9) 0.021(9) 0.021(9) 0.005(7) 0.000(7) 0.003(7) C4 0.033(10) 0.044(12) 0.011(9) -0.017(8) -0.004(8) 0.014(9) _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 Y O2 2.307(10) 10_665 ? Y O2 2.307(10) . ? Y O9 2.349(10) . ? Y O9 2.349(10) 10_665 ? Y O10 2.387(11) . ? Y O10 2.387(11) 10_665 ? Y O11 2.405(10) 10_665 ? Y O11 2.405(10) . ? Mo O8 1.707(10) . ? Mo O7 1.712(10) . ? Mo O4 1.952(10) 5_665 ? Mo O3 1.952(11) . ? Mo O6 2.199(11) 5_665 ? Mo O1 2.235(10) . ? O1 C1 1.236(17) . ? O2 C1 1.267(17) . ? O3 C2 1.398(18) . ? O3 O104 2.81(3) . ? O4 C3 1.374(16) . ? O4 Mo 1.952(10) 6_544 ? O5 C4 1.219(17) . ? O6 C4 1.268(18) . ? O6 Mo 2.199(11) 6_544 ? O7 N1 2.768(13) . ? O8 O103 2.68(2) . ? O8 O102 2.942(16) . ? O9 O6 2.941(17) 9_665 ? O11 O5 2.753(15) 6_554 ? O101 O9 2.72(2) 2_655 ? O101 O1 2.97(2) 12 ? O101 O104 2.98(4) 5_665 ? O103 O7 2.94(3) 5_665 ? O104 O9 3.12(3) 4_655 ? N1 O10 2.720(18) 5_665 ? C1 C2 1.52(2) . ? C2 C3 1.519(18) . ? C3 C4 1.56(2) . ? 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 Y O2 149.1(5) 10_665 . ? O2 Y O9 100.7(4) 10_665 . ? O2 Y O9 89.6(4) . . ? O2 Y O9 89.6(4) 10_665 10_665 ? O2 Y O9 100.7(4) . 10_665 ? O9 Y O9 140.9(7) . 10_665 ? O2 Y O10 81.4(4) 10_665 . ? O2 Y O10 74.1(4) . . ? O9 Y O10 72.1(5) . . ? O9 Y O10 147.0(5) 10_665 . ? O2 Y O10 74.1(4) 10_665 10_665 ? O2 Y O10 81.4(4) . 10_665 ? O9 Y O10 147.0(5) . 10_665 ? O9 Y O10 72.1(5) 10_665 10_665 ? O10 Y O10 75.0(7) . 10_665 ? O2 Y O11 68.7(4) 10_665 10_665 ? O2 Y O11 142.1(4) . 10_665 ? O9 Y O11 73.9(4) . 10_665 ? O9 Y O11 75.1(4) 10_665 10_665 ? O10 Y O11 128.8(4) . 10_665 ? O10 Y O11 129.8(4) 10_665 10_665 ? O2 Y O11 142.1(4) 10_665 . ? O2 Y O11 68.7(4) . . ? O9 Y O11 75.1(4) . . ? O9 Y O11 73.9(4) 10_665 . ? O10 Y O11 129.8(4) . . ? O10 Y O11 128.8(4) 10_665 . ? O11 Y O11 74.1(5) 10_665 . ? O8 Mo O7 103.9(5) . . ? O8 Mo O4 105.3(5) . 5_665 ? O7 Mo O4 93.7(5) . 5_665 ? O8 Mo O3 92.7(5) . . ? O7 Mo O3 104.2(5) . . ? O4 Mo O3 150.8(4) 5_665 . ? O8 Mo O6 87.7(4) . 5_665 ? O7 Mo O6 165.7(4) . 5_665 ? O4 Mo O6 74.9(4) 5_665 5_665 ? O3 Mo O6 83.2(4) . 5_665 ? O8 Mo O1 163.1(4) . . ? O7 Mo O1 90.4(4) . . ? O4 Mo O1 82.3(4) 5_665 . ? O3 Mo O1 74.9(4) . . ? O6 Mo O1 79.7(4) 5_665 . ? C1 O1 Mo 115.8(10) . . ? C1 O2 Y 147.3(10) . . ? C2 O3 Mo 123.2(9) . . ? C2 O3 O104 120.4(11) . . ? Mo O3 O104 113.4(7) . . ? C3 O4 Mo 124.2(9) . 6_544 ? C4 O6 Mo 116.7(10) . 6_544 ? Mo O7 N1 118.2(6) . . ? Mo O8 O103 112.3(5) . . ? Mo O8 O102 130.7(9) . . ? O103 O8 O102 114.3(9) . . ? Y O9 O6 115.8(5) . 9_665 ? Y O11 O5 128.6(4) . 6_554 ? O9 O101 O1 101.4(7) 2_655 12 ? O9 O101 O104 66.2(8) 2_655 5_665 ? O1 O101 O104 150.8(11) 12 5_665 ? O8 O103 O7 70.4(4) . 5_665 ? O3 O104 O9 145.5(12) . 4_655 ? O10 N1 O7 94.3(3) 5_665 . ? O1 C1 O2 123.9(15) . . ? O1 C1 C2 116.4(14) . . ? O2 C1 C2 119.7(14) . . ? O3 C2 C3 110.5(13) . . ? O3 C2 C1 109.7(12) . . ? C3 C2 C1 107.8(12) . . ? O4 C3 C2 111.2(12) . . ? O4 C3 C4 109.3(12) . . ? C2 C3 C4 112.0(12) . . ? O5 C4 O6 126.7(16) . . ? O5 C4 C3 119.9(15) . . ? O6 C4 C3 113.4(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.841 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.166