####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_60905b _database_code_depnum_ccdc_archive 'CCDC 632456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(n-butylpyridinium) Octamolybdate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Mo8 O26, 4(C9 H14 N)' _chemical_formula_sum 'C36 H56 Mo8 N4 O26' _chemical_formula_weight 1728.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6255(13) _cell_length_b 15.2552(17) _cell_length_c 15.2882(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.341(2) _cell_angle_gamma 90.00 _cell_volume 2709.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6859 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.37 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.873 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15109 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5514 _reflns_number_gt 4582 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker 1997)' _computing_cell_refinement 'SAINT (Bruker 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+1.7951P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5514 _refine_ls_number_parameters 334 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.97246(4) 0.93665(3) 0.17509(3) 0.05704(15) Uani 1 1 d . . . Mo2 Mo 1.07058(4) 0.77480(3) 0.06167(3) 0.06011(15) Uani 1 1 d . . . Mo3 Mo 1.10053(4) 1.07352(3) 0.05116(3) 0.05332(14) Uani 1 1 d . . . Mo4 Mo 0.80048(4) 1.08526(3) 0.06278(3) 0.05660(15) Uani 1 1 d . . . O1 O 1.0981(4) 0.9372(3) 0.2361(3) 0.0706(10) Uani 1 1 d . . . O2 O 0.8672(4) 0.9463(3) 0.2483(3) 0.0698(10) Uani 1 1 d . . . O3 O 0.9603(3) 0.8172(2) 0.1415(2) 0.0594(8) Uani 1 1 d . . . O4 O 1.0354(4) 0.6678(3) 0.0503(3) 0.0768(11) Uani 1 1 d . . . O5 O 1.1904(4) 0.7773(3) 0.1295(3) 0.0741(11) Uani 1 1 d . . . O6 O 1.0651(3) 0.9358(2) 0.0415(3) 0.0562(8) Uani 1 1 d . . . O7 O 1.2174(3) 1.0682(3) 0.1201(3) 0.0675(10) Uani 1 1 d . . . O8 O 1.1650(3) 1.0434(2) -0.0607(2) 0.0565(8) Uani 1 1 d . . . O9 O 1.0818(3) 1.1851(2) 0.0292(3) 0.0598(8) Uani 1 1 d . . . O10 O 0.9797(3) 1.0612(2) 0.1348(2) 0.0552(8) Uani 1 1 d . . . O11 O 0.7481(3) 1.0937(3) 0.1649(3) 0.0651(9) Uani 1 1 d . . . O12 O 0.6813(3) 1.0823(3) -0.0062(3) 0.0694(10) Uani 1 1 d . . . O13 O 0.8556(3) 1.1999(2) 0.0462(3) 0.0608(8) Uani 1 1 d . . . C1 C 0.0246(6) 0.2611(4) 0.4026(4) 0.0733(15) Uani 1 1 d . . . H1 H 0.0976 0.2774 0.4239 0.088 Uiso 1 1 calc R . . C2 C -0.0683(6) 0.3131(4) 0.4181(4) 0.0793(17) Uani 1 1 d . . . H2 H -0.0588 0.3644 0.4504 0.095 Uiso 1 1 calc R . . C3 C -0.1756(7) 0.2892(5) 0.3859(5) 0.089(2) Uani 1 1 d . . . H3 H -0.2391 0.3243 0.3959 0.107 Uiso 1 1 calc R . . C4 C -0.1883(6) 0.2133(5) 0.3390(6) 0.089(2) Uani 1 1 d . . . H4 H -0.2605 0.1962 0.3169 0.106 Uiso 1 1 calc R . . C5 C -0.0934(6) 0.1624(4) 0.3249(5) 0.0779(17) Uani 1 1 d . . . H5 H -0.1014 0.1106 0.2931 0.093 Uiso 1 1 calc R . . N1 N 0.0107(4) 0.1870(3) 0.3567(4) 0.0701(11) Uani 1 1 d U . . C7 C 0.1112(6) 0.1280(5) 0.3473(5) 0.0798(14) Uani 1 1 d U . . H7A H 0.1804 0.1630 0.3430 0.096 Uiso 1 1 calc R . . H7B H 0.1008 0.0945 0.2936 0.096 Uiso 1 1 calc R . . C8 C 0.1258(7) 0.0666(5) 0.4228(6) 0.0984(17) Uani 1 1 d U . . H8A H 0.0607 0.0268 0.4225 0.118 Uiso 1 1 calc R . . H8B H 0.1257 0.1000 0.4768 0.118 Uiso 1 1 calc R . . C9 C 0.2357(8) 0.0135(6) 0.4214(6) 0.108(2) Uani 1 1 d U . . H9A H 0.2364 -0.0198 0.3674 0.129 Uiso 1 1 calc R . . H9B H 0.3012 0.0530 0.4226 0.129 Uiso 1 1 calc R . . C10 C 0.2470(11) -0.0483(8) 0.4980(9) 0.146(3) Uani 1 1 d U . . H10A H 0.2310 -0.0174 0.5508 0.219 Uiso 1 1 calc R . . H10B H 0.3239 -0.0712 0.5023 0.219 Uiso 1 1 calc R . . H10C H 0.1933 -0.0957 0.4897 0.219 Uiso 1 1 calc R . . C11 C 1.0797(6) 0.5460(5) 0.7616(5) 0.0798(17) Uani 1 1 d . . . H11 H 1.1458 0.5127 0.7547 0.096 Uiso 1 1 calc R . . C12 C 1.0840(7) 0.6180(5) 0.8142(5) 0.094(2) Uani 1 1 d . . . H12 H 1.1525 0.6341 0.8434 0.113 Uiso 1 1 calc R . . C13 C 0.9848(7) 0.6670(5) 0.8235(5) 0.091(2) Uani 1 1 d . . . H13 H 0.9858 0.7161 0.8596 0.109 Uiso 1 1 calc R . . C14 C 0.8854(6) 0.6426(5) 0.7792(5) 0.0801(17) Uani 1 1 d . . . H14 H 0.8187 0.6753 0.7849 0.096 Uiso 1 1 calc R . . C15 C 0.8842(5) 0.5698(4) 0.7264(5) 0.0725(16) Uani 1 1 d . . . H15 H 0.8170 0.5534 0.6956 0.087 Uiso 1 1 calc R . . N2 N 0.9806(4) 0.5225(3) 0.7196(3) 0.0642(11) Uani 1 1 d . . . C17 C 0.9771(5) 0.4416(4) 0.6657(4) 0.0642(13) Uani 1 1 d . . . H17A H 1.0520 0.4316 0.6418 0.077 Uiso 1 1 calc R . . H17B H 0.9213 0.4485 0.6173 0.077 Uiso 1 1 calc R . . C18 C 0.9443(6) 0.3634(4) 0.7211(4) 0.0725(15) Uani 1 1 d . . . H18A H 0.8735 0.3767 0.7499 0.087 Uiso 1 1 calc R . . H18B H 1.0040 0.3540 0.7663 0.087 Uiso 1 1 calc R . . C19 C 0.9274(6) 0.2785(4) 0.6679(5) 0.0778(16) Uani 1 1 d . . . H19A H 0.8922 0.2347 0.7042 0.093 Uiso 1 1 calc R . . H19B H 0.8750 0.2900 0.6182 0.093 Uiso 1 1 calc R . . C20 C 1.0381(7) 0.2425(5) 0.6353(5) 0.089(2) Uani 1 1 d . . . H20A H 1.0710 0.2840 0.5964 0.134 Uiso 1 1 calc R . . H20B H 1.0229 0.1885 0.6047 0.134 Uiso 1 1 calc R . . H20C H 1.0909 0.2319 0.6841 0.134 Uiso 1 1 calc R . . 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 Mo1 0.0572(3) 0.0571(3) 0.0567(3) 0.00158(19) 0.0011(2) 0.00072(18) Mo2 0.0600(3) 0.0567(3) 0.0635(3) 0.0022(2) 0.0012(2) 0.00410(19) Mo3 0.0483(2) 0.0542(3) 0.0572(3) -0.00099(18) -0.00052(18) -0.00164(16) Mo4 0.0494(2) 0.0581(3) 0.0624(3) -0.00027(19) 0.00285(19) 0.00317(17) O1 0.071(2) 0.067(2) 0.073(3) -0.0008(19) -0.005(2) -0.0017(18) O2 0.073(2) 0.072(2) 0.065(2) 0.0065(19) 0.0110(19) 0.0060(19) O3 0.060(2) 0.056(2) 0.063(2) 0.0034(16) 0.0047(16) -0.0023(15) O4 0.085(3) 0.060(2) 0.085(3) 0.002(2) 0.006(2) 0.000(2) O5 0.066(2) 0.082(3) 0.074(3) 0.006(2) -0.002(2) 0.0125(19) O6 0.0494(18) 0.057(2) 0.062(2) 0.0002(15) -0.0008(15) -0.0010(14) O7 0.054(2) 0.071(2) 0.077(3) -0.0013(19) -0.0044(19) -0.0033(17) O8 0.0527(18) 0.0548(19) 0.062(2) -0.0007(16) 0.0010(15) -0.0032(15) O9 0.058(2) 0.056(2) 0.066(2) -0.0017(17) 0.0022(16) -0.0024(15) O10 0.0522(19) 0.0582(19) 0.055(2) -0.0013(15) 0.0052(15) 0.0001(14) O11 0.055(2) 0.069(2) 0.071(2) -0.0018(19) 0.0051(17) 0.0022(17) O12 0.054(2) 0.070(2) 0.083(3) -0.004(2) -0.0043(19) 0.0052(17) O13 0.059(2) 0.057(2) 0.067(2) -0.0036(17) 0.0065(17) 0.0028(16) C1 0.078(4) 0.066(3) 0.075(4) -0.002(3) 0.001(3) -0.004(3) C2 0.100(5) 0.068(4) 0.070(4) -0.010(3) 0.002(3) 0.009(3) C3 0.087(5) 0.097(5) 0.084(5) -0.004(4) 0.003(4) 0.024(4) C4 0.073(4) 0.089(5) 0.103(5) -0.009(4) -0.007(4) 0.010(3) C5 0.075(4) 0.072(4) 0.086(4) -0.017(3) -0.003(3) -0.007(3) N1 0.065(3) 0.067(3) 0.079(3) -0.007(2) 0.004(2) -0.001(2) C7 0.073(3) 0.079(3) 0.087(3) -0.013(3) 0.006(3) 0.006(2) C8 0.095(4) 0.096(3) 0.104(4) -0.004(3) 0.005(3) 0.019(3) C9 0.105(4) 0.104(4) 0.115(4) -0.001(4) -0.003(4) 0.020(3) C10 0.147(5) 0.146(5) 0.145(5) 0.011(4) 0.002(4) 0.017(4) C11 0.069(4) 0.082(4) 0.088(4) -0.011(4) -0.008(3) 0.005(3) C12 0.088(5) 0.097(5) 0.095(5) -0.020(4) -0.023(4) -0.005(4) C13 0.111(6) 0.083(5) 0.078(4) -0.024(4) 0.001(4) 0.003(4) C14 0.076(4) 0.080(4) 0.085(4) -0.009(3) 0.008(3) 0.009(3) C15 0.063(3) 0.074(4) 0.081(4) 0.001(3) 0.001(3) 0.006(3) N2 0.060(3) 0.069(3) 0.063(3) -0.001(2) 0.000(2) 0.000(2) C17 0.063(3) 0.068(3) 0.063(3) -0.005(3) 0.004(3) -0.002(2) C18 0.070(3) 0.072(4) 0.076(4) 0.005(3) 0.005(3) 0.002(3) C19 0.078(4) 0.070(4) 0.085(4) 0.007(3) 0.000(3) -0.001(3) C20 0.101(5) 0.078(4) 0.088(5) 0.004(4) 0.003(4) 0.004(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 Mo1 O2 1.698(4) . yes Mo1 O1 1.700(4) . yes Mo1 O3 1.897(4) . yes Mo1 O10 2.000(4) . yes Mo1 O8 2.340(4) 3_775 yes Mo1 O6 2.347(4) . yes Mo2 O4 1.691(4) . yes Mo2 O5 1.702(4) . yes Mo2 O3 1.918(4) . yes Mo2 O13 1.929(4) 3_775 yes Mo2 O9 2.289(4) 3_775 yes Mo2 O6 2.476(3) . yes Mo3 O7 1.687(4) . yes Mo3 O9 1.747(4) . yes Mo3 O10 1.947(4) . yes Mo3 O8 1.950(4) . yes Mo3 O6 2.145(3) . yes Mo3 O6 2.348(4) 3_775 yes Mo4 O11 1.703(4) . yes Mo4 O12 1.707(4) . yes Mo4 O13 1.883(4) . yes Mo4 O8 2.005(4) 3_775 yes Mo4 O6 2.300(4) 3_775 yes? Mo4 O10 2.345(4) . yes C1 N1 1.336(8) . ? C1 C2 1.369(9) . ? C1 H1 0.9300 . ? C2 C3 1.371(10) . ? C2 H2 0.9300 . ? C3 C4 1.367(10) . ? C3 H3 0.9300 . ? C4 C5 1.373(9) . ? C4 H4 0.9300 . ? C5 N1 1.340(8) . ? C5 H5 0.9300 . ? N1 C7 1.487(8) . ? C7 C8 1.492(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.513(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.505(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.345(8) . ? C11 C12 1.361(10) . ? C11 H11 0.9300 . ? C12 C13 1.387(11) . ? C12 H12 0.9300 . ? C13 C14 1.366(10) . ? C13 H13 0.9300 . ? C14 C15 1.373(9) . ? C14 H14 0.9300 . ? C15 N2 1.340(7) . ? C15 H15 0.9300 . ? N2 C17 1.483(7) . ? C17 C18 1.521(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.537(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.502(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 105.3(2) . . ? O2 Mo1 O3 102.38(18) . . ? O1 Mo1 O3 101.89(18) . . ? O2 Mo1 O10 99.26(17) . . ? O1 Mo1 O10 96.79(17) . . ? O3 Mo1 O10 146.37(16) . . ? O2 Mo1 O8 89.60(17) . 3_775 ? O1 Mo1 O8 162.59(18) . 3_775 ? O3 Mo1 O8 83.18(14) . 3_775 ? O10 Mo1 O8 71.49(14) . 3_775 ? O2 Mo1 O6 160.48(17) . . ? O1 Mo1 O6 93.59(18) . . ? O3 Mo1 O6 77.92(14) . . ? O10 Mo1 O6 73.19(14) . . ? O8 Mo1 O6 70.99(13) 3_775 . ? O4 Mo2 O5 105.8(2) . . ? O4 Mo2 O3 103.05(19) . . ? O5 Mo2 O3 98.98(19) . . ? O4 Mo2 O13 102.7(2) . 3_775 ? O5 Mo2 O13 97.75(19) . 3_775 ? O3 Mo2 O13 143.95(16) . 3_775 ? O4 Mo2 O9 91.04(18) . 3_775 ? O5 Mo2 O9 163.13(18) . 3_775 ? O3 Mo2 O9 76.99(15) . 3_775 ? O13 Mo2 O9 77.77(15) 3_775 3_775 ? O4 Mo2 O6 160.15(18) . . ? O5 Mo2 O6 93.99(17) . . ? O3 Mo2 O6 74.33(14) . . ? O13 Mo2 O6 72.85(14) 3_775 . ? O9 Mo2 O6 69.15(13) 3_775 . ? O7 Mo3 O9 104.95(18) . . ? O7 Mo3 O10 99.78(19) . . ? O9 Mo3 O10 97.64(16) . . ? O7 Mo3 O8 101.98(19) . . ? O9 Mo3 O8 96.29(17) . . ? O10 Mo3 O8 150.09(15) . . ? O7 Mo3 O6 98.23(17) . . ? O9 Mo3 O6 156.80(16) . . ? O10 Mo3 O6 78.98(14) . . ? O8 Mo3 O6 77.81(15) . . ? O7 Mo3 O6 173.60(16) . 3_775 ? O9 Mo3 O6 81.38(15) . 3_775 ? O10 Mo3 O6 78.14(15) . 3_775 ? O8 Mo3 O6 77.97(14) . 3_775 ? O6 Mo3 O6 75.46(15) . 3_775 ? O11 Mo4 O12 104.8(2) . . ? O11 Mo4 O13 100.94(17) . . ? O12 Mo4 O13 102.32(18) . . ? O11 Mo4 O8 99.64(17) . 3_775 ? O12 Mo4 O8 97.05(17) . 3_775 ? O13 Mo4 O8 146.93(15) . 3_775 ? O11 Mo4 O6 157.54(16) . 3_775 ? O12 Mo4 O6 97.23(18) . 3_775 ? O13 Mo4 O6 77.98(14) . 3_775 ? O8 Mo4 O6 73.15(14) 3_775 3_775 ? O11 Mo4 O10 85.73(16) . . ? O12 Mo4 O10 165.70(17) . . ? O13 Mo4 O10 84.71(14) . . ? O8 Mo4 O10 71.31(13) 3_775 . ? O6 Mo4 O10 71.82(13) 3_775 . ? Mo1 O3 Mo2 116.88(18) . . ? Mo3 O6 Mo4 92.89(13) . 3_775 ? Mo3 O6 Mo1 91.63(13) . . ? Mo4 O6 Mo1 162.31(18) 3_775 . ? Mo3 O6 Mo3 104.54(15) . 3_775 ? Mo4 O6 Mo3 97.86(14) 3_775 3_775 ? Mo1 O6 Mo3 97.54(13) . 3_775 ? Mo3 O6 Mo2 163.60(18) . . ? Mo4 O6 Mo2 86.16(12) 3_775 . ? Mo1 O6 Mo2 84.71(12) . . ? Mo3 O6 Mo2 91.80(12) 3_775 . ? Mo3 O8 Mo4 109.19(17) . 3_775 ? Mo3 O8 Mo1 110.47(16) . 3_775 ? Mo4 O8 Mo1 104.25(15) 3_775 3_775 ? Mo3 O9 Mo2 117.68(18) . 3_775 ? Mo3 O10 Mo1 109.55(16) . . ? Mo3 O10 Mo4 109.13(16) . . ? Mo1 O10 Mo4 104.21(15) . . ? Mo4 O13 Mo2 117.83(19) . 3_775 ? N1 C1 C2 120.1(6) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C1 C2 C3 119.8(6) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.3(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.4(7) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 120.3(6) . . ? N1 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C1 N1 C5 121.1(6) . . ? C1 N1 C7 119.0(5) . . ? C5 N1 C7 119.8(5) . . ? N1 C7 C8 111.7(6) . . ? N1 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 113.2(7) . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 111.8(9) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 120.5(6) . . ? N2 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 119.0(7) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 119.5(7) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N2 C15 C14 119.5(6) . . ? N2 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 N2 C11 121.5(6) . . ? C15 N2 C17 119.1(5) . . ? C11 N2 C17 119.4(5) . . ? N2 C17 C18 110.2(5) . . ? N2 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N2 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C17 C18 C19 113.3(6) . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C18 113.0(6) . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mo1 O3 Mo2 -177.0(2) . . . . ? O1 Mo1 O3 Mo2 -68.2(3) . . . . ? O10 Mo1 O3 Mo2 54.1(4) . . . . ? O8 Mo1 O3 Mo2 94.9(2) 3_775 . . . ? O6 Mo1 O3 Mo2 22.96(19) . . . . ? O4 Mo2 O3 Mo1 178.3(2) . . . . ? O5 Mo2 O3 Mo1 69.6(2) . . . . ? O13 Mo2 O3 Mo1 -47.1(4) 3_775 . . . ? O9 Mo2 O3 Mo1 -93.7(2) 3_775 . . . ? O6 Mo2 O3 Mo1 -22.06(18) . . . . ? O7 Mo3 O6 Mo4 -82.22(18) . . . 3_775 ? O9 Mo3 O6 Mo4 95.7(4) . . . 3_775 ? O10 Mo3 O6 Mo4 179.34(15) . . . 3_775 ? O8 Mo3 O6 Mo4 18.34(14) . . . 3_775 ? O6 Mo3 O6 Mo4 98.89(17) 3_775 . . 3_775 ? O7 Mo3 O6 Mo1 80.67(19) . . . . ? O9 Mo3 O6 Mo1 -101.4(4) . . . . ? O10 Mo3 O6 Mo1 -17.76(14) . . . . ? O8 Mo3 O6 Mo1 -178.76(14) . . . . ? O6 Mo3 O6 Mo1 -98.22(15) 3_775 . . . ? O7 Mo3 O6 Mo3 178.89(19) . . . 3_775 ? O9 Mo3 O6 Mo3 -3.2(5) . . . 3_775 ? O10 Mo3 O6 Mo3 80.46(16) . . . 3_775 ? O8 Mo3 O6 Mo3 -80.54(16) . . . 3_775 ? O6 Mo3 O6 Mo3 0.0 3_775 . . 3_775 ? O7 Mo3 O6 Mo2 4.0(7) . . . . ? O9 Mo3 O6 Mo2 -178.1(5) . . . . ? O10 Mo3 O6 Mo2 -94.5(7) . . . . ? O8 Mo3 O6 Mo2 104.5(7) . . . . ? O6 Mo3 O6 Mo2 -174.9(8) 3_775 . . . ? O2 Mo1 O6 Mo3 87.3(5) . . . . ? O1 Mo1 O6 Mo3 -78.29(17) . . . . ? O3 Mo1 O6 Mo3 -179.69(16) . . . . ? O10 Mo1 O6 Mo3 17.73(14) . . . . ? O8 Mo1 O6 Mo3 93.45(14) 3_775 . . . ? O2 Mo1 O6 Mo4 -167.9(5) . . . 3_775 ? O1 Mo1 O6 Mo4 26.5(6) . . . 3_775 ? O3 Mo1 O6 Mo4 -74.9(6) . . . 3_775 ? O10 Mo1 O6 Mo4 122.5(6) . . . 3_775 ? O8 Mo1 O6 Mo4 -161.8(6) 3_775 . . 3_775 ? O2 Mo1 O6 Mo3 -17.6(5) . . . 3_775 ? O1 Mo1 O6 Mo3 176.81(16) . . . 3_775 ? O3 Mo1 O6 Mo3 75.41(14) . . . 3_775 ? O10 Mo1 O6 Mo3 -87.17(14) . . . 3_775 ? O8 Mo1 O6 Mo3 -11.45(12) 3_775 . . 3_775 ? O2 Mo1 O6 Mo2 -108.7(5) . . . . ? O1 Mo1 O6 Mo2 85.69(16) . . . . ? O3 Mo1 O6 Mo2 -15.71(13) . . . . ? O10 Mo1 O6 Mo2 -178.29(14) . . . . ? O8 Mo1 O6 Mo2 -102.57(13) 3_775 . . . ? O4 Mo2 O6 Mo3 178.5(6) . . . . ? O5 Mo2 O6 Mo3 -4.8(7) . . . . ? O3 Mo2 O6 Mo3 93.4(7) . . . . ? O13 Mo2 O6 Mo3 -101.7(7) 3_775 . . . ? O9 Mo2 O6 Mo3 175.2(7) 3_775 . . . ? O4 Mo2 O6 Mo4 -94.3(5) . . . 3_775 ? O5 Mo2 O6 Mo4 82.39(18) . . . 3_775 ? O3 Mo2 O6 Mo4 -179.39(16) . . . 3_775 ? O13 Mo2 O6 Mo4 -14.50(14) 3_775 . . 3_775 ? O9 Mo2 O6 Mo4 -97.63(15) 3_775 . . 3_775 ? O4 Mo2 O6 Mo1 100.8(5) . . . . ? O5 Mo2 O6 Mo1 -82.44(18) . . . . ? O3 Mo2 O6 Mo1 15.77(13) . . . . ? O13 Mo2 O6 Mo1 -179.33(15) 3_775 . . . ? O9 Mo2 O6 Mo1 97.54(13) 3_775 . . . ? O4 Mo2 O6 Mo3 3.4(6) . . . 3_775 ? O5 Mo2 O6 Mo3 -179.85(18) . . . 3_775 ? O3 Mo2 O6 Mo3 -81.64(15) . . . 3_775 ? O13 Mo2 O6 Mo3 83.26(15) 3_775 . . 3_775 ? O9 Mo2 O6 Mo3 0.13(12) 3_775 . . 3_775 ? O7 Mo3 O8 Mo4 73.5(2) . . . 3_775 ? O9 Mo3 O8 Mo4 -179.70(17) . . . 3_775 ? O10 Mo3 O8 Mo4 -62.3(4) . . . 3_775 ? O6 Mo3 O8 Mo4 -22.45(17) . . . 3_775 ? O6 Mo3 O8 Mo4 -99.94(17) 3_775 . . 3_775 ? O7 Mo3 O8 Mo1 -172.39(17) . . . 3_775 ? O9 Mo3 O8 Mo1 -65.61(18) . . . 3_775 ? O10 Mo3 O8 Mo1 51.8(4) . . . 3_775 ? O6 Mo3 O8 Mo1 91.64(16) . . . 3_775 ? O6 Mo3 O8 Mo1 14.15(14) 3_775 . . 3_775 ? O7 Mo3 O9 Mo2 -179.2(2) . . . 3_775 ? O10 Mo3 O9 Mo2 -76.9(2) . . . 3_775 ? O8 Mo3 O9 Mo2 76.6(2) . . . 3_775 ? O6 Mo3 O9 Mo2 2.9(5) . . . 3_775 ? O6 Mo3 O9 Mo2 -0.19(18) 3_775 . . 3_775 ? O7 Mo3 O10 Mo1 -74.3(2) . . . . ? O9 Mo3 O10 Mo1 179.05(17) . . . . ? O8 Mo3 O10 Mo1 62.0(4) . . . . ? O6 Mo3 O10 Mo1 22.32(18) . . . . ? O6 Mo3 O10 Mo1 99.58(17) 3_775 . . . ? O7 Mo3 O10 Mo4 172.23(18) . . . . ? O9 Mo3 O10 Mo4 65.54(18) . . . . ? O8 Mo3 O10 Mo4 -51.5(4) . . . . ? O6 Mo3 O10 Mo4 -91.20(16) . . . . ? O6 Mo3 O10 Mo4 -13.93(14) 3_775 . . . ? O2 Mo1 O10 Mo3 177.65(19) . . . . ? O1 Mo1 O10 Mo3 70.9(2) . . . . ? O3 Mo1 O10 Mo3 -52.7(3) . . . . ? O8 Mo1 O10 Mo3 -95.91(19) 3_775 . . . ? O6 Mo1 O10 Mo3 -20.85(16) . . . . ? O2 Mo1 O10 Mo4 -65.7(2) . . . . ? O1 Mo1 O10 Mo4 -172.47(19) . . . . ? O3 Mo1 O10 Mo4 63.9(3) . . . . ? O8 Mo1 O10 Mo4 20.75(13) 3_775 . . . ? O6 Mo1 O10 Mo4 95.82(15) . . . . ? O11 Mo4 O10 Mo3 -165.8(2) . . . . ? O12 Mo4 O10 Mo3 55.9(8) . . . . ? O13 Mo4 O10 Mo3 -64.40(18) . . . . ? O8 Mo4 O10 Mo3 92.49(18) 3_775 . . . ? O6 Mo4 O10 Mo3 14.67(14) 3_775 . . . ? O11 Mo4 O10 Mo1 77.23(19) . . . . ? O12 Mo4 O10 Mo1 -61.1(7) . . . . ? O13 Mo4 O10 Mo1 178.65(18) . . . . ? O8 Mo4 O10 Mo1 -24.46(15) 3_775 . . . ? O6 Mo4 O10 Mo1 -102.28(16) 3_775 . . . ? O11 Mo4 O13 Mo2 178.4(2) . . . 3_775 ? O12 Mo4 O13 Mo2 -73.6(2) . . . 3_775 ? O8 Mo4 O13 Mo2 50.8(4) 3_775 . . 3_775 ? O6 Mo4 O13 Mo2 21.27(19) 3_775 . . 3_775 ? O10 Mo4 O13 Mo2 93.8(2) . . . 3_775 ? N1 C1 C2 C3 -0.5(11) . . . . ? C1 C2 C3 C4 0.4(11) . . . . ? C2 C3 C4 C5 -0.1(12) . . . . ? C3 C4 C5 N1 -0.1(12) . . . . ? C2 C1 N1 C5 0.3(10) . . . . ? C2 C1 N1 C7 -174.8(6) . . . . ? C4 C5 N1 C1 -0.1(11) . . . . ? C4 C5 N1 C7 175.0(7) . . . . ? C1 N1 C7 C8 85.6(8) . . . . ? C5 N1 C7 C8 -89.6(8) . . . . ? N1 C7 C8 C9 -172.6(7) . . . . ? C7 C8 C9 C10 -179.4(9) . . . . ? N2 C11 C12 C13 -0.2(13) . . . . ? C11 C12 C13 C14 -0.7(13) . . . . ? C12 C13 C14 C15 0.4(12) . . . . ? C13 C14 C15 N2 0.8(11) . . . . ? C14 C15 N2 C11 -1.8(10) . . . . ? C14 C15 N2 C17 177.1(6) . . . . ? C12 C11 N2 C15 1.5(11) . . . . ? C12 C11 N2 C17 -177.4(7) . . . . ? C15 N2 C17 C18 -88.7(7) . . . . ? C11 N2 C17 C18 90.2(7) . . . . ? N2 C17 C18 C19 174.5(5) . . . . ? C17 C18 C19 C20 70.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.985 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.127