Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email BARBARA.MODEC@GUEST.ARNES.SI _publ_contact_author_name 'Dr Barbara Modec' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Faculty of Chemistry and Chemical Technology University of Ljubljana Askerceva 5 Ljubljana 1000 SLOVENIA ; _publ_section_title ; Novel Molybdenum(V) Squarato Complexes Based on the Dinuclear Metal-Metal Bonded Unit: Syntheses and Structural Characterization of Dinuclear [Mo2O4(C4O4)(R-Py)4] (R-Py = pyridine) and Tetranuclear [Mo4O8(C4O4)4]4-. ; loop_ _publ_author_name 'Barbara Modec' 'Jurij V. Brencic' 'Eric Burkholder' 'Jon Zubieta' data_1a _database_code_depnum_ccdc_archive 'CCDC 219865' _chemical_name_common ;Tetraoxotetrapyridinesquaratodimolybdenum(V) methanol pyridine (1/2/0.5) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraoxotetrapyridinesquaratodimolybdenum(V) methanol pyridine (1/2/0.5) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.50 H30.50 Mo2 N4.50 O10' _chemical_formula_weight 787.95 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3502(2) _cell_length_b 10.97220(10) _cell_length_c 14.9631(2) _cell_angle_alpha 70.3901(6) _cell_angle_beta 79.9458(6) _cell_angle_gamma 86.4850(6) _cell_volume 1576.13(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13037 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7198 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. One of the two methanol solvent molecules is disordered over two positions, the occupancies factors of each are 0.656(6) and 0.344(6). Carbon atoms of the disordered methanol, C10_a and C10_b, were refined with isotropic displacement parameters. Pyridine solvent molecule was found on a crystallographic inversion centre, its disorder was resolved using PART -1 instruction. ; _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^)+(0.0302P)^2^+1.0855P] 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 7198 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.592954(16) 0.034993(16) 0.669634(12) 0.01272(6) Uani 1 1 d . . . Mo2 Mo 0.468772(16) 0.211921(16) 0.723534(12) 0.01268(6) Uani 1 1 d . . . O1 O 0.48605(14) -0.00589(14) 0.61097(10) 0.0179(3) Uani 1 1 d . . . O2 O 0.32688(14) 0.22126(14) 0.68007(10) 0.0181(3) Uani 1 1 d . . . O3 O 0.61342(14) 0.22059(13) 0.62014(10) 0.0157(3) Uani 1 1 d . . . O4 O 0.50142(14) 0.03314(13) 0.79458(10) 0.0154(3) Uani 1 1 d . . . O5 O 0.77368(14) 0.02876(14) 0.72638(10) 0.0165(3) Uani 1 1 d . . . O6 O 0.61656(14) 0.26682(14) 0.79033(11) 0.0171(3) Uani 1 1 d . . . O7 O 0.88384(17) 0.34040(16) 0.84171(13) 0.0285(4) Uani 1 1 d . . . O8 O 1.03433(16) 0.09961(17) 0.78573(13) 0.0292(4) Uani 1 1 d . . . C1 C 0.8013(2) 0.1158(2) 0.76024(14) 0.0154(4) Uani 1 1 d . . . C2 C 0.7334(2) 0.21976(19) 0.78722(14) 0.0156(4) Uani 1 1 d . . . C3 C 0.8536(2) 0.2555(2) 0.81253(16) 0.0190(4) Uani 1 1 d . . . C4 C 0.9230(2) 0.1448(2) 0.78618(16) 0.0193(4) Uani 1 1 d . . . N1 N 0.61864(18) -0.17961(17) 0.74268(13) 0.0170(4) Uani 1 1 d . . . N2 N 0.74976(17) 0.03722(17) 0.54377(12) 0.0156(3) Uani 1 1 d . . . N3 N 0.34905(17) 0.20956(16) 0.86574(12) 0.0155(3) Uani 1 1 d . . . N4 N 0.46974(18) 0.43017(17) 0.66349(13) 0.0176(4) Uani 1 1 d . . . C11 C 0.5095(2) -0.2483(2) 0.78811(17) 0.0248(5) Uani 1 1 d . . . H11 H 0.4290 -0.2057 0.7887 0.030 Uiso 1 1 calc R . . C12 C 0.5128(3) -0.3806(2) 0.8341(2) 0.0343(6) Uani 1 1 d . . . H12 H 0.4359 -0.4258 0.8662 0.041 Uiso 1 1 calc R . . C13 C 0.6318(3) -0.4448(2) 0.8320(2) 0.0374(6) Uani 1 1 d . . . H13 H 0.6359 -0.5341 0.8609 0.045 Uiso 1 1 calc R . . C14 C 0.7445(3) -0.3740(2) 0.7859(2) 0.0341(6) Uani 1 1 d . . . H14 H 0.8260 -0.4146 0.7844 0.041 Uiso 1 1 calc R . . C15 C 0.7340(2) -0.2419(2) 0.74236(17) 0.0245(5) Uani 1 1 d . . . H15 H 0.8100 -0.1944 0.7116 0.029 Uiso 1 1 calc R . . C21 C 0.7440(2) -0.0443(2) 0.49445(16) 0.0199(4) Uani 1 1 d . . . H21 H 0.6798 -0.1081 0.5178 0.024 Uiso 1 1 calc R . . C22 C 0.8289(2) -0.0375(2) 0.41077(17) 0.0240(5) Uani 1 1 d . . . H22 H 0.8222 -0.0958 0.3788 0.029 Uiso 1 1 calc R . . C23 C 0.9238(2) 0.0573(2) 0.37549(17) 0.0259(5) Uani 1 1 d . . . H23 H 0.9824 0.0642 0.3193 0.031 Uiso 1 1 calc R . . C24 C 0.9301(2) 0.1425(2) 0.42558(17) 0.0255(5) Uani 1 1 d . . . H24 H 0.9928 0.2077 0.4031 0.031 Uiso 1 1 calc R . . C25 C 0.8423(2) 0.1292(2) 0.50907(16) 0.0202(4) Uani 1 1 d . . . H25 H 0.8474 0.1861 0.5425 0.024 Uiso 1 1 calc R . . C31 C 0.2192(2) 0.2331(2) 0.87451(16) 0.0186(4) Uani 1 1 d . . . H31 H 0.1810 0.2615 0.8192 0.022 Uiso 1 1 calc R . . C32 C 0.1401(2) 0.2170(2) 0.96247(16) 0.0235(5) Uani 1 1 d . . . H32 H 0.0509 0.2357 0.9657 0.028 Uiso 1 1 calc R . . C33 C 0.1952(2) 0.1728(2) 1.04540(16) 0.0256(5) Uani 1 1 d . . . H33 H 0.1440 0.1608 1.1053 0.031 Uiso 1 1 calc R . . C34 C 0.3287(2) 0.1467(2) 1.03712(16) 0.0254(5) Uani 1 1 d . . . H34 H 0.3684 0.1161 1.0917 0.031 Uiso 1 1 calc R . . C35 C 0.4018(2) 0.1666(2) 0.94724(16) 0.0204(4) Uani 1 1 d . . . H35 H 0.4915 0.1497 0.9425 0.025 Uiso 1 1 calc R . . C41 C 0.3606(2) 0.4989(2) 0.67611(18) 0.0262(5) Uani 1 1 d . . . H41 H 0.2851 0.4552 0.7130 0.031 Uiso 1 1 calc R . . C42 C 0.3557(3) 0.6323(2) 0.6366(2) 0.0304(5) Uani 1 1 d . . . H42 H 0.2788 0.6770 0.6479 0.036 Uiso 1 1 calc R . . C43 C 0.4660(3) 0.6976(2) 0.58033(17) 0.0268(5) Uani 1 1 d . . . H43 H 0.4650 0.7871 0.5525 0.032 Uiso 1 1 calc R . . C44 C 0.5784(3) 0.6275(2) 0.56593(19) 0.0310(6) Uani 1 1 d . . . H44 H 0.6542 0.6692 0.5275 0.037 Uiso 1 1 calc R . . C45 C 0.5771(2) 0.4946(2) 0.60928(18) 0.0260(5) Uani 1 1 d . . . H45 H 0.6537 0.4483 0.6004 0.031 Uiso 1 1 calc R . . N5 N 1.069(2) 0.4026(18) 0.4639(19) 0.054(6) Uani 0.50 1 d P A -1 C51 C 1.014(3) 0.503(3) 0.4105(18) 0.043(4) Uani 0.50 1 d P A -1 H51 H 1.0281 0.5078 0.3463 0.052 Uiso 0.50 1 calc PR A -1 C52 C 0.946(2) 0.594(3) 0.4245(16) 0.038(4) Uani 0.50 1 d P A -1 H52 H 0.9051 0.6519 0.3768 0.046 Uiso 0.50 1 calc PR A -1 C53 C 0.936(2) 0.6031(15) 0.513(2) 0.042(4) Uani 0.50 1 d P A -1 H53 H 0.8795 0.6652 0.5284 0.050 Uiso 0.50 1 calc PR A -1 C54 C 1.009(3) 0.520(3) 0.587(2) 0.048(5) Uani 0.50 1 d P A -1 H54 H 1.0161 0.5303 0.6447 0.058 Uiso 0.50 1 calc PR A -1 C55 C 1.073(3) 0.413(3) 0.5503(15) 0.042(4) Uani 0.50 1 d P A -1 H55 H 1.1180 0.3493 0.5917 0.051 Uiso 0.50 1 calc PR A -1 O9 O 0.1807(3) -0.1265(2) 0.8477(2) 0.0741(8) Uani 1 1 d . . . H9 H 0.1379 -0.0607 0.8270 0.111 Uiso 1 1 calc R . . C9 C 0.2238(3) -0.1261(3) 0.9305(2) 0.0472(7) Uani 1 1 d . . . H9A H 0.3033 -0.0768 0.9131 0.071 Uiso 1 1 calc R . . H9B H 0.2402 -0.2133 0.9690 0.071 Uiso 1 1 calc R . . H9C H 0.1578 -0.0878 0.9665 0.071 Uiso 1 1 calc R . . O10 O 0.0784(5) -0.3190(4) 0.7985(3) 0.0705(14) Uani 0.656(6) 1 d P B 1 H10 H 0.1147 -0.2596 0.8059 0.106 Uiso 0.656(6) 1 calc PR B 1 C10 C 0.0762(7) -0.4286(7) 0.8803(5) 0.0568(18) Uiso 0.656(6) 1 d P B 1 H10A H 0.1562 -0.4333 0.9055 0.085 Uiso 0.656(6) 1 calc PR B 1 H10B H 0.0679 -0.5046 0.8636 0.085 Uiso 0.656(6) 1 calc PR B 1 H10C H 0.0030 -0.4231 0.9280 0.085 Uiso 0.656(6) 1 calc PR B 1 O10A O 0.0708(6) -0.4678(7) 0.7822(5) 0.051(2) Uani 0.344(6) 1 d P B 2 H10D H 0.0055 -0.5137 0.8052 0.077 Uiso 0.344(6) 1 calc PR B 2 C10A C 0.0997(17) -0.4167(18) 0.8490(13) 0.077(5) Uiso 0.344(6) 1 d P B 2 H10E H 0.1606 -0.3466 0.8177 0.115 Uiso 0.344(6) 1 calc PR B 2 H10F H 0.1381 -0.4826 0.8976 0.115 Uiso 0.344(6) 1 calc PR B 2 H10G H 0.0207 -0.3853 0.8783 0.115 Uiso 0.344(6) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01317(9) 0.01340(9) 0.01240(9) -0.00486(7) -0.00270(7) -0.00083(7) Mo2 0.01280(9) 0.01301(9) 0.01261(9) -0.00419(7) -0.00313(7) -0.00021(7) O1 0.0186(7) 0.0193(7) 0.0173(7) -0.0074(6) -0.0043(6) -0.0006(6) O2 0.0181(7) 0.0202(7) 0.0166(7) -0.0060(6) -0.0046(6) 0.0001(6) O3 0.0165(7) 0.0156(7) 0.0144(7) -0.0043(6) -0.0016(6) -0.0019(6) O4 0.0171(7) 0.0156(7) 0.0133(7) -0.0044(6) -0.0024(6) -0.0001(6) O5 0.0166(7) 0.0176(7) 0.0187(7) -0.0091(6) -0.0058(6) 0.0008(6) O6 0.0162(7) 0.0176(7) 0.0203(8) -0.0090(6) -0.0054(6) 0.0011(6) O7 0.0293(9) 0.0225(8) 0.0433(10) -0.0173(8) -0.0186(8) 0.0011(7) O8 0.0177(8) 0.0394(10) 0.0405(10) -0.0238(8) -0.0115(7) 0.0063(7) C1 0.0159(10) 0.0175(10) 0.0132(9) -0.0042(8) -0.0042(8) -0.0023(8) C2 0.0181(10) 0.0147(9) 0.0141(10) -0.0038(8) -0.0042(8) -0.0019(8) C3 0.0196(11) 0.0192(10) 0.0196(11) -0.0058(9) -0.0076(9) -0.0010(8) C4 0.0169(10) 0.0229(11) 0.0197(11) -0.0077(9) -0.0051(8) -0.0022(9) N1 0.0209(9) 0.0152(8) 0.0160(9) -0.0063(7) -0.0039(7) 0.0005(7) N2 0.0143(8) 0.0172(9) 0.0158(8) -0.0058(7) -0.0036(7) 0.0012(7) N3 0.0166(9) 0.0152(8) 0.0154(8) -0.0057(7) -0.0039(7) 0.0004(7) N4 0.0196(9) 0.0164(9) 0.0174(9) -0.0053(7) -0.0053(7) -0.0001(7) C11 0.0254(12) 0.0212(11) 0.0266(12) -0.0050(9) -0.0054(10) -0.0031(9) C12 0.0400(15) 0.0223(12) 0.0364(14) -0.0037(11) -0.0035(12) -0.0105(11) C13 0.0573(18) 0.0165(12) 0.0370(15) -0.0057(11) -0.0112(13) 0.0010(12) C14 0.0418(15) 0.0236(12) 0.0384(15) -0.0131(11) -0.0096(12) 0.0132(11) C15 0.0255(12) 0.0238(11) 0.0263(12) -0.0120(10) -0.0033(9) 0.0027(9) C21 0.0169(10) 0.0235(11) 0.0235(11) -0.0120(9) -0.0056(9) -0.0004(9) C22 0.0210(11) 0.0318(13) 0.0267(12) -0.0196(10) -0.0048(9) 0.0020(9) C23 0.0205(11) 0.0361(13) 0.0222(12) -0.0139(10) 0.0015(9) 0.0023(10) C24 0.0199(11) 0.0274(12) 0.0284(12) -0.0110(10) 0.0030(9) -0.0051(9) C25 0.0184(10) 0.0210(11) 0.0233(11) -0.0105(9) -0.0025(9) -0.0010(9) C31 0.0173(10) 0.0199(10) 0.0193(11) -0.0063(9) -0.0052(8) 0.0013(8) C32 0.0169(11) 0.0295(12) 0.0233(11) -0.0090(10) -0.0014(9) 0.0024(9) C33 0.0276(12) 0.0313(12) 0.0168(11) -0.0096(10) 0.0020(9) 0.0014(10) C34 0.0287(12) 0.0330(13) 0.0153(11) -0.0078(10) -0.0071(9) 0.0044(10) C35 0.0184(10) 0.0246(11) 0.0189(11) -0.0070(9) -0.0065(8) 0.0040(9) C41 0.0224(12) 0.0215(11) 0.0322(13) -0.0054(10) -0.0054(10) 0.0016(9) C42 0.0296(13) 0.0195(11) 0.0412(15) -0.0060(11) -0.0137(11) 0.0064(10) C43 0.0401(14) 0.0146(11) 0.0263(12) -0.0028(9) -0.0149(11) -0.0011(10) C44 0.0369(14) 0.0213(12) 0.0310(13) -0.0060(10) 0.0017(11) -0.0083(10) C45 0.0249(12) 0.0203(11) 0.0299(13) -0.0077(10) 0.0020(10) -0.0014(9) N5 0.041(5) 0.076(9) 0.053(11) -0.032(7) -0.009(5) 0.007(5) C51 0.042(10) 0.051(10) 0.041(5) -0.020(6) -0.004(5) -0.012(6) C52 0.035(7) 0.034(5) 0.033(10) 0.003(6) 0.000(6) -0.005(4) C53 0.052(7) 0.024(5) 0.050(13) -0.012(4) -0.016(7) 0.018(4) C54 0.038(9) 0.043(9) 0.066(7) -0.015(6) -0.018(5) -0.006(6) C55 0.036(7) 0.042(6) 0.033(11) 0.004(7) 0.001(7) 0.009(5) O9 0.102(2) 0.0467(15) 0.088(2) -0.0301(15) -0.0440(18) 0.0203(15) C9 0.0456(18) 0.0419(17) 0.0454(18) -0.0073(14) 0.0037(14) -0.0077(14) O10 0.099(4) 0.047(2) 0.057(3) 0.0003(19) -0.019(2) -0.021(2) O10A 0.040(4) 0.052(4) 0.063(5) -0.021(3) -0.004(3) -0.011(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 Mo1 O1 1.6913(14) . ? Mo1 O3 1.9303(14) . ? Mo1 O4 1.9370(14) . ? Mo1 O5 2.1736(14) . ? Mo1 N2 2.2557(17) . ? Mo1 N1 2.2599(17) . ? Mo1 Mo2 2.5405(2) . ? Mo2 O2 1.6913(15) . ? Mo2 O4 1.9330(14) . ? Mo2 O3 1.9375(14) . ? Mo2 O6 2.1800(14) . ? Mo2 N4 2.2577(18) . ? Mo2 N3 2.2606(17) . ? O5 C1 1.288(2) . ? O6 C2 1.285(3) . ? O7 C3 1.230(3) . ? O8 C4 1.226(3) . ? C1 C2 1.438(3) . ? C1 C4 1.464(3) . ? C2 C3 1.472(3) . ? C3 C4 1.504(3) . ? N1 C15 1.339(3) . ? N1 C11 1.341(3) . ? N2 C25 1.341(3) . ? N2 C21 1.346(3) . ? N3 C31 1.345(3) . ? N3 C35 1.350(3) . ? N4 C45 1.337(3) . ? N4 C41 1.340(3) . ? C11 C12 1.384(3) . ? C12 C13 1.381(4) . ? C13 C14 1.383(4) . ? C14 C15 1.382(3) . ? C21 C22 1.381(3) . ? C22 C23 1.379(3) . ? C23 C24 1.391(3) . ? C24 C25 1.381(3) . ? C31 C32 1.385(3) . ? C32 C33 1.382(3) . ? C33 C34 1.386(3) . ? C34 C35 1.377(3) . ? C41 C42 1.383(3) . ? C42 C43 1.372(4) . ? C43 C44 1.381(4) . ? C44 C45 1.382(3) . ? N5 C51 1.29(4) . ? N5 C55 1.34(3) . ? C51 C52 1.24(4) . ? C52 C53 1.35(3) . ? C53 C54 1.47(4) . ? C54 C55 1.52(4) . ? O9 C9 1.389(4) . ? O10 C10 1.397(8) . ? O10A C10A 1.380(17) . ? 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 O1 Mo1 O3 108.20(7) . . ? O1 Mo1 O4 108.66(7) . . ? O3 Mo1 O4 94.15(6) . . ? O1 Mo1 O5 157.23(6) . . ? O3 Mo1 O5 86.61(6) . . ? O4 Mo1 O5 86.74(6) . . ? O1 Mo1 N2 87.12(7) . . ? O3 Mo1 N2 84.48(6) . . ? O4 Mo1 N2 163.68(6) . . ? O5 Mo1 N2 76.95(6) . . ? O1 Mo1 N1 86.52(7) . . ? O3 Mo1 N1 164.68(6) . . ? O4 Mo1 N1 84.80(6) . . ? O5 Mo1 N1 78.07(6) . . ? N2 Mo1 N1 92.24(6) . . ? O1 Mo1 Mo2 102.16(5) . . ? O3 Mo1 Mo2 49.06(4) . . ? O4 Mo1 Mo2 48.90(4) . . ? O5 Mo1 Mo2 100.61(4) . . ? N2 Mo1 Mo2 133.37(4) . . ? N1 Mo1 Mo2 133.43(5) . . ? O2 Mo2 O4 108.85(7) . . ? O2 Mo2 O3 108.31(7) . . ? O4 Mo2 O3 94.05(6) . . ? O2 Mo2 O6 157.50(6) . . ? O4 Mo2 O6 88.28(6) . . ? O3 Mo2 O6 84.12(6) . . ? O2 Mo2 N4 85.87(7) . . ? O4 Mo2 N4 164.52(6) . . ? O3 Mo2 N4 85.50(6) . . ? O6 Mo2 N4 76.27(6) . . ? O2 Mo2 N3 88.47(7) . . ? O4 Mo2 N3 83.06(6) . . ? O3 Mo2 N3 162.93(6) . . ? O6 Mo2 N3 78.99(6) . . ? N4 Mo2 N3 92.83(6) . . ? O2 Mo2 Mo1 102.39(5) . . ? O4 Mo2 Mo1 49.04(4) . . ? O3 Mo2 Mo1 48.82(4) . . ? O6 Mo2 Mo1 99.87(4) . . ? N4 Mo2 Mo1 134.07(5) . . ? N3 Mo2 Mo1 131.97(4) . . ? Mo1 O3 Mo2 82.12(5) . . ? Mo2 O4 Mo1 82.06(5) . . ? C1 O5 Mo1 121.80(13) . . ? C2 O6 Mo2 122.49(12) . . ? O5 C1 C2 136.94(19) . . ? O5 C1 C4 131.48(19) . . ? C2 C1 C4 91.59(16) . . ? O6 C2 C1 136.79(18) . . ? O6 C2 C3 132.24(19) . . ? C1 C2 C3 90.97(17) . . ? O7 C3 C2 135.4(2) . . ? O7 C3 C4 135.9(2) . . ? C2 C3 C4 88.68(16) . . ? O8 C4 C1 135.8(2) . . ? O8 C4 C3 135.4(2) . . ? C1 C4 C3 88.74(16) . . ? C15 N1 C11 118.5(2) . . ? C15 N1 Mo1 124.61(15) . . ? C11 N1 Mo1 116.88(15) . . ? C25 N2 C21 117.92(19) . . ? C25 N2 Mo1 120.90(14) . . ? C21 N2 Mo1 120.72(14) . . ? C31 N3 C35 117.45(18) . . ? C31 N3 Mo2 121.23(14) . . ? C35 N3 Mo2 120.67(14) . . ? C45 N4 C41 117.8(2) . . ? C45 N4 Mo2 121.02(15) . . ? C41 N4 Mo2 121.08(15) . . ? N1 C11 C12 122.1(2) . . ? C13 C12 C11 119.2(2) . . ? C12 C13 C14 118.8(2) . . ? C15 C14 C13 118.8(2) . . ? N1 C15 C14 122.6(2) . . ? N2 C21 C22 123.0(2) . . ? C23 C22 C21 118.8(2) . . ? C22 C23 C24 118.7(2) . . ? C25 C24 C23 119.3(2) . . ? N2 C25 C24 122.4(2) . . ? N3 C31 C32 122.7(2) . . ? C33 C32 C31 119.3(2) . . ? C32 C33 C34 118.4(2) . . ? C35 C34 C33 119.3(2) . . ? N3 C35 C34 122.9(2) . . ? N4 C41 C42 122.8(2) . . ? C43 C42 C41 119.1(2) . . ? C42 C43 C44 118.6(2) . . ? C43 C44 C45 119.2(2) . . ? N4 C45 C44 122.5(2) . . ? C51 N5 C55 111(2) . . ? C52 C51 N5 135(3) . . ? C51 C52 C53 116(3) . . ? C52 C53 C54 123(2) . . ? C53 C54 C55 108(2) . . ? N5 C55 C54 126(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.492 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.117 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 219866' _chemical_name_common 'Tetraoxotetrapyridinesquaratodimolybdenum(V) pyridine (1/2)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraoxotetrapyridinesquaratodimolybdenum(V) pyridine (1/2) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Mo2 N6 O8' _chemical_formula_weight 842.5 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1101(7) _cell_length_b 11.1614(5) _cell_length_c 35.7999(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.3470(10) _cell_angle_gamma 90.00 _cell_volume 6834.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89080 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 32.99 _reflns_number_total 24054 _reflns_number_gt 20517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0267P)^2^+6.8029P] 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 24054 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.004 _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 0.270167(8) 0.553950(13) 0.090804(4) 0.01255(3) Uani 1 1 d . . . Mo2 Mo 0.168540(8) 0.602864(13) 0.139159(4) 0.01249(3) Uani 1 1 d . . . O1 O 0.29962(7) 0.69215(12) 0.07793(4) 0.0177(2) Uani 1 1 d . . . O2 O 0.17258(7) 0.75413(12) 0.14075(4) 0.0183(3) Uani 1 1 d . . . O3 O 0.27495(7) 0.54609(11) 0.14476(3) 0.0147(2) Uani 1 1 d . . . O4 O 0.15707(7) 0.55311(12) 0.08744(3) 0.0157(2) Uani 1 1 d . . . O5 O 0.26938(7) 0.36042(12) 0.09236(4) 0.0172(2) Uani 1 1 d . . . O6 O 0.13362(7) 0.42027(11) 0.15316(4) 0.0168(2) Uani 1 1 d . . . O7 O 0.14397(8) 0.14946(12) 0.18323(4) 0.0203(3) Uani 1 1 d . . . O8 O 0.27339(9) 0.08683(13) 0.12043(4) 0.0240(3) Uani 1 1 d . . . N1 N 0.39850(9) 0.50922(14) 0.09541(4) 0.0170(3) Uani 1 1 d . . . N2 N 0.26734(8) 0.50540(14) 0.02980(4) 0.0153(3) Uani 1 1 d . . . N3 N 0.03875(8) 0.61410(14) 0.13895(4) 0.0156(3) Uani 1 1 d . . . N4 N 0.17076(9) 0.60277(14) 0.20208(4) 0.0160(3) Uani 1 1 d . . . N5 N 0.03191(14) 0.8471(2) 0.24047(6) 0.0413(5) Uani 1 1 d . . . N7 N 0.47622(15) 0.1022(2) 0.26338(7) 0.0461(6) Uani 1 1 d . . . N8 N 0.44232(15) 0.7387(2) 0.49249(8) 0.0551(7) Uani 1 1 d . . . C1 C 0.23158(10) 0.30147(16) 0.11683(5) 0.0144(3) Uani 1 1 d . . . C2 C 0.17291(10) 0.32819(16) 0.14355(5) 0.0144(3) Uani 1 1 d . . . C3 C 0.17526(10) 0.20411(16) 0.15786(5) 0.0160(3) Uani 1 1 d . . . C4 C 0.23572(10) 0.17552(16) 0.12909(5) 0.0165(3) Uani 1 1 d . . . C11 C 0.45052(11) 0.5620(2) 0.07327(6) 0.0250(4) Uani 1 1 d . . . H11 H 0.4324 0.6048 0.0525 0.030 Uiso 1 1 calc R . . C12 C 0.53023(12) 0.5545(2) 0.08033(8) 0.0334(5) Uani 1 1 d . . . H12 H 0.5649 0.5919 0.0644 0.040 Uiso 1 1 calc R . . C13 C 0.55814(12) 0.4915(2) 0.11099(7) 0.0298(5) Uani 1 1 d . . . H13 H 0.6115 0.4868 0.1164 0.036 Uiso 1 1 calc R . . C14 C 0.50486(12) 0.4355(2) 0.13350(6) 0.0266(4) Uani 1 1 d . . . H14 H 0.5218 0.3915 0.1542 0.032 Uiso 1 1 calc R . . C15 C 0.42598(11) 0.44573(18) 0.12487(5) 0.0212(4) Uani 1 1 d . . . H15 H 0.3904 0.4072 0.1400 0.025 Uiso 1 1 calc R . . C21 C 0.30008(11) 0.40601(17) 0.01564(5) 0.0189(3) Uani 1 1 d . . . H21 H 0.3242 0.3517 0.0319 0.023 Uiso 1 1 calc R . . C22 C 0.29898(11) 0.38207(18) -0.02227(5) 0.0209(4) Uani 1 1 d . . . H22 H 0.3208 0.3117 -0.0312 0.025 Uiso 1 1 calc R . . C23 C 0.26515(11) 0.46382(18) -0.04679(5) 0.0209(4) Uani 1 1 d . . . H23 H 0.2649 0.4502 -0.0724 0.025 Uiso 1 1 calc R . . C24 C 0.23169(11) 0.56633(18) -0.03241(5) 0.0211(4) Uani 1 1 d . . . H24 H 0.2086 0.6228 -0.0483 0.025 Uiso 1 1 calc R . . C25 C 0.23312(11) 0.58375(17) 0.00590(5) 0.0181(3) Uani 1 1 d . . . H25 H 0.2096 0.6519 0.0155 0.022 Uiso 1 1 calc R . . C31 C -0.00509(11) 0.54286(18) 0.11652(5) 0.0193(3) Uani 1 1 d . . . H31 H 0.0197 0.4864 0.1018 0.023 Uiso 1 1 calc R . . C32 C -0.08568(11) 0.55065(19) 0.11456(6) 0.0229(4) Uani 1 1 d . . . H32 H -0.1145 0.5004 0.0987 0.027 Uiso 1 1 calc R . . C33 C -0.12300(11) 0.63411(19) 0.13641(6) 0.0229(4) Uani 1 1 d . . . H33 H -0.1772 0.6405 0.1356 0.027 Uiso 1 1 calc R . . C34 C -0.07836(11) 0.70789(19) 0.15944(6) 0.0226(4) Uani 1 1 d . . . H34 H -0.1021 0.7650 0.1743 0.027 Uiso 1 1 calc R . . C35 C 0.00217(11) 0.69555(17) 0.16009(5) 0.0194(3) Uani 1 1 d . . . H35 H 0.0320 0.7452 0.1757 0.023 Uiso 1 1 calc R . . C41 C 0.12164(11) 0.53949(18) 0.22310(5) 0.0202(4) Uani 1 1 d . . . H41 H 0.0799 0.4999 0.2115 0.024 Uiso 1 1 calc R . . C42 C 0.13097(13) 0.5310(2) 0.26155(5) 0.0255(4) Uani 1 1 d . . . H42 H 0.0960 0.4865 0.2754 0.031 Uiso 1 1 calc R . . C43 C 0.19286(13) 0.5895(2) 0.27911(6) 0.0284(4) Uani 1 1 d . . . H43 H 0.2009 0.5835 0.3048 0.034 Uiso 1 1 calc R . . C44 C 0.24259(13) 0.6571(2) 0.25767(6) 0.0277(4) Uani 1 1 d . . . H44 H 0.2841 0.6985 0.2688 0.033 Uiso 1 1 calc R . . C45 C 0.22974(11) 0.66212(19) 0.21950(5) 0.0224(4) Uani 1 1 d . . . H45 H 0.2631 0.7083 0.2052 0.027 Uiso 1 1 calc R . . C51 C 0.09219(18) 0.9182(2) 0.23509(7) 0.0416(6) Uani 1 1 d . . . H51 H 0.0996 0.9466 0.2110 0.050 Uiso 1 1 calc R . . C52 C 0.1445(2) 0.9530(3) 0.26230(10) 0.0530(8) Uani 1 1 d . . . H52 H 0.1858 1.0036 0.2567 0.064 Uiso 1 1 calc R . . C53 C 0.1352(2) 0.9124(3) 0.29757(9) 0.0634(11) Uani 1 1 d . . . H53 H 0.1706 0.9338 0.3165 0.076 Uiso 1 1 calc R . . C54 C 0.0740(3) 0.8405(3) 0.30479(8) 0.0677(12) Uani 1 1 d . . . H54 H 0.0662 0.8128 0.3289 0.081 Uiso 1 1 calc R . . C55 C 0.0226(2) 0.8084(3) 0.27571(10) 0.0548(9) Uani 1 1 d . . . H55 H -0.0194 0.7586 0.2808 0.066 Uiso 1 1 calc R . . C71 C 0.41492(18) 0.0315(3) 0.26349(8) 0.0457(7) Uani 1 1 d . . . H71 H 0.4023 -0.0058 0.2858 0.055 Uiso 1 1 calc R . . C72 C 0.3694(2) 0.0101(4) 0.23306(15) 0.0835(15) Uani 1 1 d . . . H72 H 0.3268 -0.0413 0.2345 0.100 Uiso 1 1 calc R . . C73 C 0.3863(4) 0.0644(6) 0.20028(15) 0.126(3) Uani 1 1 d . . . H73 H 0.3549 0.0533 0.1790 0.151 Uiso 1 1 calc R . . C74 C 0.4494(5) 0.1338(5) 0.19965(11) 0.121(3) Uani 1 1 d . . . H74 H 0.4636 0.1700 0.1774 0.145 Uiso 1 1 calc R . . C75 C 0.4927(2) 0.1522(3) 0.23095(14) 0.0752(14) Uani 1 1 d . . . H75 H 0.5360 0.2022 0.2298 0.090 Uiso 1 1 calc R . . C81 C 0.4950(2) 0.6834(3) 0.51317(8) 0.0535(8) Uani 1 1 d . . . H81 H 0.4853 0.6754 0.5385 0.064 Uiso 1 1 calc R . . C82 C 0.56201(19) 0.6372(3) 0.50085(10) 0.0541(9) Uani 1 1 d . . . H82 H 0.5969 0.5993 0.5173 0.065 Uiso 1 1 calc R . . C83 C 0.57799(18) 0.6470(3) 0.46394(12) 0.0606(10) Uani 1 1 d . . . H83 H 0.6244 0.6173 0.4546 0.073 Uiso 1 1 calc R . . C84 C 0.5233(2) 0.7022(3) 0.44062(8) 0.0564(9) Uani 1 1 d . . . H84 H 0.5315 0.7096 0.4151 0.068 Uiso 1 1 calc R . . C85 C 0.45613(18) 0.7460(3) 0.45641(9) 0.0532(8) Uani 1 1 d . . . H85 H 0.4188 0.7824 0.4409 0.064 Uiso 1 1 calc R . . Mo1A Mo 0.222316(8) 0.413775(13) 0.411658(4) 0.01212(3) Uani 1 1 d . . . Mo2A Mo 0.326129(8) 0.356063(13) 0.365065(4) 0.01225(3) Uani 1 1 d . . . O1A O 0.19170(7) 0.27978(12) 0.42786(4) 0.0165(2) Uani 1 1 d . . . O2A O 0.32308(7) 0.20441(12) 0.36668(4) 0.0171(2) Uani 1 1 d . . . O3A O 0.33548(7) 0.41686(12) 0.41579(3) 0.0155(2) Uani 1 1 d . . . O4A O 0.21942(7) 0.40957(11) 0.35768(3) 0.0143(2) Uani 1 1 d . . . O5A O 0.22142(7) 0.60601(11) 0.40666(3) 0.0157(2) Uani 1 1 d . . . O6A O 0.36091(7) 0.53554(11) 0.34828(4) 0.0161(2) Uani 1 1 d . . . O7A O 0.36334(8) 0.80721(13) 0.31927(4) 0.0205(3) Uani 1 1 d . . . O8A O 0.23335(9) 0.88067(12) 0.38061(4) 0.0223(3) Uani 1 1 d . . . N1A N 0.22553(9) 0.47490(14) 0.47169(4) 0.0161(3) Uani 1 1 d . . . N2A N 0.09301(8) 0.45510(14) 0.40345(4) 0.0154(3) Uani 1 1 d . . . N3A N 0.32544(9) 0.34561(14) 0.30217(4) 0.0160(3) Uani 1 1 d . . . N4A N 0.45624(9) 0.34354(14) 0.36444(4) 0.0162(3) Uani 1 1 d . . . C1A C 0.26431(10) 0.66170(16) 0.38315(5) 0.0143(3) Uani 1 1 d . . . C2A C 0.32401(10) 0.63066(16) 0.35745(5) 0.0147(3) Uani 1 1 d . . . C3A C 0.32785(10) 0.75483(16) 0.34388(5) 0.0155(3) Uani 1 1 d . . . C4A C 0.26664(10) 0.78848(16) 0.37173(5) 0.0159(3) Uani 1 1 d . . . C11A C 0.18625(11) 0.41667(19) 0.49838(5) 0.0216(4) Uani 1 1 d . . . H11A H 0.1556 0.3510 0.4916 0.026 Uiso 1 1 calc R . . C12A C 0.18978(13) 0.4509(2) 0.53544(5) 0.0261(4) Uani 1 1 d . . . H12A H 0.1617 0.4088 0.5531 0.031 Uiso 1 1 calc R . . C13A C 0.23510(12) 0.54787(19) 0.54621(5) 0.0225(4) Uani 1 1 d . . . H13A H 0.2373 0.5732 0.5710 0.027 Uiso 1 1 calc R . . C14A C 0.27716(12) 0.60622(18) 0.51919(5) 0.0206(4) Uani 1 1 d . . . H14A H 0.3093 0.6705 0.5256 0.025 Uiso 1 1 calc R . . C15A C 0.27086(11) 0.56790(17) 0.48247(5) 0.0193(3) Uani 1 1 d . . . H15A H 0.2991 0.6081 0.4645 0.023 Uiso 1 1 calc R . . C21A C 0.06952(10) 0.52522(17) 0.37482(5) 0.0185(3) Uani 1 1 d . . . H21A H 0.1069 0.5684 0.3620 0.022 Uiso 1 1 calc R . . C22A C -0.00816(11) 0.53578(18) 0.36359(6) 0.0216(4) Uani 1 1 d . . . H22A H -0.0223 0.5845 0.3435 0.026 Uiso 1 1 calc R . . C23A C -0.06457(11) 0.47286(18) 0.38266(6) 0.0215(4) Uani 1 1 d . . . H23A H -0.1171 0.4782 0.3755 0.026 Uiso 1 1 calc R . . C24A C -0.04097(11) 0.40198(19) 0.41258(6) 0.0233(4) Uani 1 1 d . . . H24A H -0.0775 0.3598 0.4262 0.028 Uiso 1 1 calc R . . C25A C 0.03780(11) 0.39494(18) 0.42191(5) 0.0198(3) Uani 1 1 d . . . H25A H 0.0533 0.3464 0.4419 0.024 Uiso 1 1 calc R . . C31A C 0.37353(11) 0.40785(18) 0.28040(5) 0.0199(3) Uani 1 1 d . . . H31A H 0.4147 0.4501 0.2916 0.024 Uiso 1 1 calc R . . C32A C 0.36417(13) 0.4115(2) 0.24191(6) 0.0262(4) Uani 1 1 d . . . H32A H 0.3987 0.4551 0.2275 0.031 Uiso 1 1 calc R . . C33A C 0.30276(13) 0.3494(2) 0.22514(6) 0.0279(4) Uani 1 1 d . . . H33A H 0.2944 0.3527 0.1994 0.033 Uiso 1 1 calc R . . C34A C 0.25396(12) 0.2824(2) 0.24733(6) 0.0273(4) Uani 1 1 d . . . H34A H 0.2130 0.2382 0.2367 0.033 Uiso 1 1 calc R . . C35A C 0.26745(11) 0.28251(18) 0.28547(5) 0.0211(4) Uani 1 1 d . . . H35A H 0.2350 0.2369 0.3003 0.025 Uiso 1 1 calc R . . C41A C 0.50198(11) 0.41846(18) 0.38480(5) 0.0205(4) Uani 1 1 d . . . H41A H 0.4784 0.4758 0.3997 0.025 Uiso 1 1 calc R . . C42A C 0.58261(11) 0.4131(2) 0.38436(6) 0.0260(4) Uani 1 1 d . . . H42A H 0.6127 0.4655 0.3989 0.031 Uiso 1 1 calc R . . C43A C 0.61816(11) 0.3288(2) 0.36202(6) 0.0270(4) Uani 1 1 d . . . H43A H 0.6723 0.3244 0.3610 0.032 Uiso 1 1 calc R . . C44A C 0.57160(11) 0.2510(2) 0.34119(6) 0.0251(4) Uani 1 1 d . . . H44A H 0.5940 0.1931 0.3261 0.030 Uiso 1 1 calc R . . C45A C 0.49111(11) 0.26086(18) 0.34311(6) 0.0204(4) Uani 1 1 d . . . H45A H 0.4600 0.2084 0.3291 0.025 Uiso 1 1 calc R . . N6 N 0.07193(12) 0.74133(19) -0.00295(7) 0.0373(5) Uani 1 1 d . . . C61 C 0.02107(15) 0.6731(2) 0.01507(7) 0.0327(5) Uani 1 1 d . . . H61 H 0.0340 0.6488 0.0393 0.039 Uiso 1 1 calc R . . C62 C -0.04964(14) 0.6365(2) -0.00025(7) 0.0350(5) Uani 1 1 d . . . H62 H -0.0838 0.5907 0.0136 0.042 Uiso 1 1 calc R . . C63 C -0.06907(15) 0.6690(2) -0.03653(8) 0.0368(5) Uani 1 1 d . . . H63 H -0.1162 0.6449 -0.0476 0.044 Uiso 1 1 calc R . . C64 C -0.01714(16) 0.7377(2) -0.05581(7) 0.0382(6) Uani 1 1 d . . . H64 H -0.0283 0.7607 -0.0803 0.046 Uiso 1 1 calc R . . C65 C 0.05222(15) 0.7723(2) -0.03811(8) 0.0405(6) Uani 1 1 d . . . H65 H 0.0869 0.8194 -0.0513 0.049 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 0.01099(6) 0.01509(7) 0.01155(6) 0.00102(5) -0.00051(5) 0.00045(5) Mo2 0.01079(6) 0.01419(7) 0.01242(6) -0.00042(5) -0.00099(5) 0.00077(5) O1 0.0173(6) 0.0186(6) 0.0171(6) 0.0016(5) -0.0011(5) -0.0002(5) O2 0.0167(6) 0.0168(6) 0.0213(6) -0.0006(5) -0.0012(5) 0.0011(5) O3 0.0122(5) 0.0189(6) 0.0128(5) 0.0013(4) -0.0005(4) 0.0015(4) O4 0.0119(5) 0.0206(6) 0.0146(6) -0.0019(5) -0.0016(4) 0.0007(4) O5 0.0180(6) 0.0172(6) 0.0166(6) 0.0007(5) 0.0024(5) 0.0007(5) O6 0.0150(6) 0.0155(6) 0.0200(6) -0.0008(5) 0.0034(5) 0.0001(5) O7 0.0221(6) 0.0209(7) 0.0177(6) 0.0021(5) -0.0007(5) -0.0062(5) O8 0.0286(7) 0.0186(7) 0.0248(7) -0.0011(5) 0.0004(6) 0.0064(5) N1 0.0127(6) 0.0206(8) 0.0177(7) 0.0004(6) 0.0008(5) 0.0004(5) N2 0.0139(6) 0.0190(7) 0.0130(6) 0.0004(5) 0.0002(5) 0.0000(5) N3 0.0126(6) 0.0186(7) 0.0157(7) -0.0005(5) 0.0000(5) 0.0012(5) N4 0.0158(7) 0.0187(7) 0.0136(6) -0.0018(5) -0.0002(5) 0.0027(5) N5 0.0515(14) 0.0335(11) 0.0385(12) -0.0049(9) -0.0038(10) 0.0015(10) N7 0.0494(14) 0.0394(13) 0.0492(14) -0.0075(11) -0.0067(11) 0.0056(11) N8 0.0462(14) 0.0485(15) 0.0714(18) 0.0244(13) 0.0205(13) 0.0037(11) C1 0.0127(7) 0.0151(8) 0.0154(7) -0.0011(6) -0.0014(6) 0.0006(6) C2 0.0130(7) 0.0143(8) 0.0158(7) 0.0000(6) -0.0013(6) -0.0019(6) C3 0.0151(7) 0.0183(8) 0.0143(7) -0.0007(6) -0.0039(6) -0.0027(6) C4 0.0164(8) 0.0178(8) 0.0153(8) -0.0004(6) -0.0028(6) 0.0006(6) C11 0.0169(8) 0.0288(10) 0.0296(10) 0.0062(8) 0.0056(7) 0.0007(7) C12 0.0162(9) 0.0327(12) 0.0517(15) 0.0056(10) 0.0072(9) -0.0011(8) C13 0.0138(8) 0.0257(10) 0.0497(14) -0.0058(9) -0.0042(8) 0.0025(7) C14 0.0204(9) 0.0273(10) 0.0317(11) -0.0029(8) -0.0068(8) 0.0069(8) C15 0.0167(8) 0.0260(10) 0.0210(9) 0.0022(7) -0.0004(7) 0.0056(7) C21 0.0176(8) 0.0208(9) 0.0184(8) 0.0006(7) 0.0005(6) 0.0021(6) C22 0.0212(9) 0.0226(9) 0.0188(8) -0.0030(7) 0.0025(7) 0.0008(7) C23 0.0225(9) 0.0265(10) 0.0137(8) -0.0018(7) 0.0010(7) -0.0045(7) C24 0.0233(9) 0.0246(9) 0.0153(8) 0.0017(7) -0.0027(7) -0.0010(7) C25 0.0192(8) 0.0194(9) 0.0156(8) 0.0007(6) -0.0019(6) 0.0006(6) C31 0.0154(8) 0.0244(9) 0.0182(8) -0.0023(7) -0.0002(6) -0.0003(7) C32 0.0153(8) 0.0303(11) 0.0230(9) 0.0035(8) -0.0039(7) -0.0036(7) C33 0.0119(8) 0.0298(10) 0.0269(10) 0.0096(8) 0.0012(7) 0.0025(7) C34 0.0175(8) 0.0240(10) 0.0267(10) 0.0038(7) 0.0059(7) 0.0054(7) C35 0.0173(8) 0.0205(9) 0.0204(9) -0.0011(7) 0.0012(6) 0.0029(7) C41 0.0201(8) 0.0241(9) 0.0164(8) -0.0001(7) 0.0009(7) 0.0007(7) C42 0.0288(10) 0.0325(11) 0.0154(8) 0.0014(7) 0.0034(7) 0.0024(8) C43 0.0325(11) 0.0389(12) 0.0137(8) -0.0031(8) -0.0024(8) 0.0082(9) C44 0.0263(10) 0.0380(12) 0.0184(9) -0.0081(8) -0.0064(7) 0.0008(9) C45 0.0211(9) 0.0273(10) 0.0187(9) -0.0046(7) -0.0014(7) -0.0017(7) C51 0.0602(18) 0.0348(13) 0.0298(12) 0.0042(10) 0.0033(11) 0.0001(12) C52 0.0570(19) 0.0343(15) 0.067(2) -0.0146(14) -0.0112(15) 0.0021(13) C53 0.098(3) 0.0437(18) 0.0475(18) -0.0203(14) -0.0308(18) 0.0348(18) C54 0.134(4) 0.0484(19) 0.0218(12) 0.0071(12) 0.0144(17) 0.049(2) C55 0.067(2) 0.0289(14) 0.070(2) 0.0064(13) 0.0338(17) 0.0103(13) C71 0.0604(18) 0.0341(14) 0.0432(15) 0.0082(11) 0.0166(13) 0.0027(12) C72 0.0489(19) 0.054(2) 0.146(4) -0.053(3) -0.033(2) 0.0122(16) C73 0.188(6) 0.117(5) 0.070(3) -0.065(3) -0.082(4) 0.120(4) C74 0.235(8) 0.102(4) 0.0289(19) 0.026(2) 0.049(3) 0.119(5) C75 0.069(2) 0.0300(15) 0.130(4) 0.0161(19) 0.063(3) 0.0126(15) C81 0.090(3) 0.0325(14) 0.0374(15) 0.0048(11) -0.0025(15) -0.0027(15) C82 0.0569(18) 0.0300(14) 0.074(2) -0.0068(14) -0.0359(17) 0.0012(12) C83 0.0408(16) 0.0273(14) 0.114(3) -0.0201(17) 0.0186(18) -0.0029(11) C84 0.098(3) 0.0378(15) 0.0345(14) -0.0040(12) 0.0180(16) -0.0295(17) C85 0.0480(17) 0.0449(17) 0.066(2) 0.0281(15) -0.0221(15) -0.0121(13) Mo1A 0.01131(6) 0.01336(7) 0.01169(6) -0.00005(5) -0.00008(5) -0.00043(5) Mo2A 0.01013(6) 0.01378(7) 0.01281(6) -0.00107(5) -0.00059(5) -0.00003(5) O1A 0.0172(6) 0.0159(6) 0.0165(6) 0.0018(5) -0.0009(5) -0.0011(5) O2A 0.0149(6) 0.0154(6) 0.0211(6) -0.0001(5) -0.0001(5) 0.0002(4) O3A 0.0133(5) 0.0193(6) 0.0138(6) -0.0012(5) -0.0015(4) -0.0009(4) O4A 0.0108(5) 0.0183(6) 0.0138(5) -0.0013(4) -0.0001(4) 0.0009(4) O5A 0.0164(6) 0.0150(6) 0.0157(6) 0.0004(4) 0.0030(5) 0.0004(4) O6A 0.0155(6) 0.0156(6) 0.0174(6) -0.0003(5) 0.0030(5) -0.0006(4) O7A 0.0215(6) 0.0211(7) 0.0190(6) 0.0021(5) 0.0012(5) -0.0055(5) O8A 0.0295(7) 0.0176(6) 0.0199(6) -0.0012(5) 0.0011(5) 0.0044(5) N1A 0.0161(7) 0.0185(7) 0.0137(7) -0.0010(5) 0.0005(5) 0.0000(5) N2A 0.0125(6) 0.0174(7) 0.0164(7) -0.0007(5) 0.0007(5) 0.0004(5) N3A 0.0144(7) 0.0188(7) 0.0149(7) -0.0026(5) -0.0009(5) 0.0019(5) N4A 0.0124(6) 0.0187(7) 0.0175(7) 0.0014(5) -0.0002(5) 0.0003(5) C1A 0.0140(7) 0.0164(8) 0.0123(7) -0.0014(6) -0.0010(6) -0.0003(6) C2A 0.0141(7) 0.0165(8) 0.0134(7) -0.0001(6) -0.0005(6) -0.0027(6) C3A 0.0143(7) 0.0153(8) 0.0168(8) -0.0009(6) -0.0022(6) -0.0032(6) C4A 0.0182(8) 0.0158(8) 0.0134(7) -0.0002(6) -0.0034(6) -0.0008(6) C11A 0.0227(9) 0.0254(10) 0.0167(8) -0.0002(7) 0.0015(7) -0.0063(7) C12A 0.0285(10) 0.0350(12) 0.0151(8) 0.0001(7) 0.0041(7) -0.0073(8) C13A 0.0247(9) 0.0276(10) 0.0152(8) -0.0030(7) 0.0005(7) 0.0006(7) C14A 0.0241(9) 0.0199(9) 0.0176(8) -0.0034(7) -0.0023(7) -0.0005(7) C15A 0.0210(8) 0.0192(9) 0.0176(8) -0.0005(6) 0.0002(7) -0.0030(7) C21A 0.0156(8) 0.0214(9) 0.0186(8) 0.0026(7) 0.0018(6) 0.0016(6) C22A 0.0181(8) 0.0243(10) 0.0224(9) 0.0021(7) -0.0024(7) 0.0044(7) C23A 0.0141(8) 0.0223(9) 0.0279(10) -0.0029(7) -0.0027(7) 0.0014(7) C24A 0.0156(8) 0.0244(10) 0.0300(10) 0.0031(8) 0.0037(7) -0.0013(7) C25A 0.0155(8) 0.0225(9) 0.0214(9) 0.0042(7) 0.0015(7) 0.0002(7) C31A 0.0185(8) 0.0247(9) 0.0166(8) -0.0026(7) 0.0017(6) -0.0005(7) C32A 0.0278(10) 0.0336(11) 0.0173(9) -0.0005(8) 0.0050(7) -0.0004(8) C33A 0.0298(11) 0.0382(12) 0.0157(9) -0.0055(8) -0.0019(7) 0.0031(9) C34A 0.0236(10) 0.0376(12) 0.0204(9) -0.0095(8) -0.0046(7) -0.0019(8) C35A 0.0184(8) 0.0258(10) 0.0190(8) -0.0051(7) -0.0003(7) -0.0012(7) C41A 0.0158(8) 0.0243(9) 0.0214(9) -0.0004(7) -0.0013(7) -0.0019(7) C42A 0.0159(8) 0.0345(11) 0.0274(10) 0.0024(8) -0.0039(7) -0.0058(8) C43A 0.0141(8) 0.0374(12) 0.0297(10) 0.0137(9) 0.0008(7) 0.0022(8) C44A 0.0173(8) 0.0269(10) 0.0313(10) 0.0054(8) 0.0064(7) 0.0063(7) C45A 0.0164(8) 0.0204(9) 0.0246(9) 0.0001(7) 0.0027(7) 0.0028(7) N6 0.0278(10) 0.0297(10) 0.0541(13) 0.0042(9) -0.0062(9) 0.0012(8) C61 0.0400(13) 0.0275(11) 0.0305(11) -0.0025(9) 0.0004(9) 0.0049(9) C62 0.0348(12) 0.0271(11) 0.0438(14) -0.0056(10) 0.0127(10) -0.0034(9) C63 0.0304(12) 0.0300(12) 0.0497(15) -0.0124(11) -0.0054(10) 0.0010(9) C64 0.0450(14) 0.0339(13) 0.0355(13) 0.0043(10) -0.0023(11) 0.0091(11) C65 0.0322(12) 0.0320(13) 0.0577(17) 0.0158(12) 0.0071(11) 0.0016(10) _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 O1 1.6901(13) . ? Mo1 O3 1.9333(12) . ? Mo1 O4 1.9361(12) . ? Mo1 O5 2.1608(13) . ? Mo1 N2 2.2495(15) . ? Mo1 N1 2.2540(15) . ? Mo1 Mo2 2.5416(2) . ? Mo2 O2 1.6906(13) . ? Mo2 O3 1.9338(12) . ? Mo2 O4 1.9386(12) . ? Mo2 O6 2.1854(13) . ? Mo2 N3 2.2241(15) . ? Mo2 N4 2.2521(15) . ? O5 C1 1.283(2) . ? O6 C2 1.280(2) . ? O7 C3 1.227(2) . ? O8 C4 1.225(2) . ? N1 C11 1.342(2) . ? N1 C15 1.346(2) . ? N2 C21 1.347(2) . ? N2 C25 1.348(2) . ? N3 C31 1.346(2) . ? N3 C35 1.347(2) . ? N4 C41 1.342(2) . ? N4 C45 1.348(2) . ? N5 C51 1.319(4) . ? N5 C55 1.347(4) . ? N7 C71 1.313(4) . ? N7 C75 1.324(4) . ? N8 C81 1.308(4) . ? N8 C85 1.321(4) . ? C1 C2 1.434(2) . ? C1 C4 1.474(2) . ? C2 C3 1.477(2) . ? C3 C4 1.511(3) . ? C11 C12 1.384(3) . ? C12 C13 1.380(3) . ? C13 C14 1.381(3) . ? C14 C15 1.382(3) . ? C21 C22 1.383(3) . ? C22 C23 1.384(3) . ? C23 C24 1.384(3) . ? C24 C25 1.385(3) . ? C31 C32 1.382(3) . ? C32 C33 1.382(3) . ? C33 C34 1.383(3) . ? C34 C35 1.384(3) . ? C41 C42 1.385(3) . ? C42 C43 1.382(3) . ? C43 C44 1.383(3) . ? C44 C45 1.380(3) . ? C51 C52 1.364(4) . ? C52 C53 1.354(5) . ? C53 C54 1.349(6) . ? C54 C55 1.394(5) . ? C71 C72 1.346(5) . ? C72 C73 1.358(8) . ? C73 C74 1.328(9) . ? C74 C75 1.345(7) . ? C81 C82 1.340(5) . ? C82 C83 1.360(5) . ? C83 C84 1.384(5) . ? C84 C85 1.383(5) . ? Mo1A O1A 1.6917(13) . ? Mo1A O4A 1.9325(12) . ? Mo1A O3A 1.9387(12) . ? Mo1A O5A 2.1531(13) . ? Mo1A N1A 2.2542(15) . ? Mo1A N2A 2.2723(15) . ? Mo1A Mo2A 2.5479(2) . ? Mo2A O2A 1.6945(13) . ? Mo2A O4A 1.9332(12) . ? Mo2A O3A 1.9417(12) . ? Mo2A O6A 2.1782(13) . ? Mo2A N4A 2.2313(15) . ? Mo2A N3A 2.2544(15) . ? O5A C1A 1.289(2) . ? O6A C2A 1.282(2) . ? O7A C3A 1.230(2) . ? O8A C4A 1.222(2) . ? N1A C15A 1.347(2) . ? N1A C11A 1.348(2) . ? N2A C21A 1.344(2) . ? N2A C25A 1.345(2) . ? N3A C31A 1.341(2) . ? N3A C35A 1.345(2) . ? N4A C45A 1.346(2) . ? N4A C41A 1.348(2) . ? C1A C2A 1.433(2) . ? C1A C4A 1.474(2) . ? C2A C3A 1.471(2) . ? C3A C4A 1.510(3) . ? C11A C12A 1.381(3) . ? C12A C13A 1.381(3) . ? C13A C14A 1.382(3) . ? C14A C15A 1.384(3) . ? C21A C22A 1.384(3) . ? C22A C23A 1.386(3) . ? C23A C24A 1.384(3) . ? C24A C25A 1.383(3) . ? C31A C32A 1.384(3) . ? C32A C33A 1.384(3) . ? C33A C34A 1.385(3) . ? C34A C35A 1.380(3) . ? C41A C42A 1.381(3) . ? C42A C43A 1.385(3) . ? C43A C44A 1.384(3) . ? C44A C45A 1.385(3) . ? N6 C61 1.334(3) . ? N6 C65 1.341(3) . ? C61 C62 1.378(3) . ? C62 C63 1.381(4) . ? C63 C64 1.372(4) . ? C64 C65 1.387(4) . ? 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 O1 Mo1 O3 107.94(6) . . ? O1 Mo1 O4 106.95(6) . . ? O3 Mo1 O4 94.63(5) . . ? O1 Mo1 O5 157.13(6) . . ? O3 Mo1 O5 85.93(5) . . ? O4 Mo1 O5 89.42(5) . . ? O1 Mo1 N2 87.41(6) . . ? O3 Mo1 N2 163.42(6) . . ? O4 Mo1 N2 86.55(5) . . ? O5 Mo1 N2 77.53(5) . . ? O1 Mo1 N1 85.75(6) . . ? O3 Mo1 N1 84.18(5) . . ? O4 Mo1 N1 166.91(6) . . ? O5 Mo1 N1 77.49(5) . . ? N2 Mo1 N1 90.94(5) . . ? O1 Mo1 Mo2 101.70(5) . . ? O3 Mo1 Mo2 48.92(4) . . ? O4 Mo1 Mo2 49.05(4) . . ? O5 Mo1 Mo2 101.10(3) . . ? N2 Mo1 Mo2 135.52(4) . . ? N1 Mo1 Mo2 132.74(4) . . ? O2 Mo2 O3 106.62(6) . . ? O2 Mo2 O4 108.74(6) . . ? O3 Mo2 O4 94.54(5) . . ? O2 Mo2 O6 159.19(6) . . ? O3 Mo2 O6 86.13(5) . . ? O4 Mo2 O6 85.98(5) . . ? O2 Mo2 N3 89.08(6) . . ? O3 Mo2 N3 163.02(6) . . ? O4 Mo2 N3 86.23(5) . . ? O6 Mo2 N3 77.00(5) . . ? O2 Mo2 N4 88.12(6) . . ? O3 Mo2 N4 84.40(5) . . ? O4 Mo2 N4 162.59(6) . . ? O6 Mo2 N4 76.61(5) . . ? N3 Mo2 N4 89.82(5) . . ? O2 Mo2 Mo1 102.08(5) . . ? O3 Mo2 Mo1 48.90(4) . . ? O4 Mo2 Mo1 48.96(4) . . ? O6 Mo2 Mo1 98.69(3) . . ? N3 Mo2 Mo1 135.14(4) . . ? N4 Mo2 Mo1 133.27(4) . . ? Mo1 O3 Mo2 82.18(5) . . ? Mo1 O4 Mo2 81.98(5) . . ? C1 O5 Mo1 122.26(11) . . ? C2 O6 Mo2 122.62(11) . . ? C11 N1 C15 117.99(17) . . ? C11 N1 Mo1 121.22(13) . . ? C15 N1 Mo1 119.71(12) . . ? C21 N2 C25 118.28(16) . . ? C21 N2 Mo1 124.34(12) . . ? C25 N2 Mo1 117.34(12) . . ? C31 N3 C35 118.32(16) . . ? C31 N3 Mo2 120.74(12) . . ? C35 N3 Mo2 120.89(12) . . ? C41 N4 C45 118.11(16) . . ? C41 N4 Mo2 124.41(12) . . ? C45 N4 Mo2 117.22(13) . . ? C51 N5 C55 116.1(3) . . ? C71 N7 C75 116.3(3) . . ? C81 N8 C85 116.5(3) . . ? O5 C1 C2 136.13(16) . . ? O5 C1 C4 132.14(16) . . ? C2 C1 C4 91.68(14) . . ? O6 C2 C1 136.62(16) . . ? O6 C2 C3 132.07(16) . . ? C1 C2 C3 91.29(14) . . ? O7 C3 C2 135.56(18) . . ? O7 C3 C4 135.80(17) . . ? C2 C3 C4 88.57(14) . . ? O8 C4 C1 135.83(18) . . ? O8 C4 C3 135.71(17) . . ? C1 C4 C3 88.43(14) . . ? N1 C11 C12 122.0(2) . . ? C13 C12 C11 119.8(2) . . ? C12 C13 C14 118.32(19) . . ? C13 C14 C15 119.1(2) . . ? N1 C15 C14 122.68(19) . . ? N2 C21 C22 122.15(17) . . ? C21 C22 C23 119.41(18) . . ? C22 C23 C24 118.68(17) . . ? C23 C24 C25 119.11(18) . . ? N2 C25 C24 122.34(18) . . ? N3 C31 C32 122.32(18) . . ? C31 C32 C33 119.16(18) . . ? C32 C33 C34 118.86(17) . . ? C33 C34 C35 119.11(18) . . ? N3 C35 C34 122.22(18) . . ? N4 C41 C42 122.28(18) . . ? C43 C42 C41 119.3(2) . . ? C42 C43 C44 118.66(19) . . ? C45 C44 C43 119.08(19) . . ? N4 C45 C44 122.55(19) . . ? N5 C51 C52 124.7(3) . . ? C53 C52 C51 118.8(3) . . ? C54 C53 C52 119.1(3) . . ? C53 C54 C55 119.3(3) . . ? N5 C55 C54 122.1(3) . . ? N7 C71 C72 123.5(3) . . ? C71 C72 C73 119.3(4) . . ? C74 C73 C72 117.7(4) . . ? C73 C74 C75 120.4(4) . . ? N7 C75 C74 122.8(4) . . ? N8 C81 C82 125.3(3) . . ? C81 C82 C83 118.8(3) . . ? C82 C83 C84 118.2(3) . . ? C85 C84 C83 117.9(3) . . ? N8 C85 C84 123.2(3) . . ? O1A Mo1A O4A 108.70(6) . . ? O1A Mo1A O3A 107.84(6) . . ? O4A Mo1A O3A 94.52(5) . . ? O1A Mo1A O5A 155.21(6) . . ? O4A Mo1A O5A 86.62(5) . . ? O3A Mo1A O5A 89.64(5) . . ? O1A Mo1A N1A 86.65(6) . . ? O4A Mo1A N1A 163.77(6) . . ? O3A Mo1A N1A 85.41(5) . . ? O5A Mo1A N1A 77.15(5) . . ? O1A Mo1A N2A 85.15(6) . . ? O4A Mo1A N2A 82.74(5) . . ? O3A Mo1A N2A 166.88(6) . . ? O5A Mo1A N2A 77.41(5) . . ? N1A Mo1A N2A 93.65(5) . . ? O1A Mo1A Mo2A 103.13(4) . . ? O4A Mo1A Mo2A 48.78(4) . . ? O3A Mo1A Mo2A 49.01(4) . . ? O5A Mo1A Mo2A 101.61(3) . . ? N1A Mo1A Mo2A 134.34(4) . . ? N2A Mo1A Mo2A 131.17(4) . . ? O2A Mo2A O4A 106.47(6) . . ? O2A Mo2A O3A 108.61(6) . . ? O4A Mo2A O3A 94.40(5) . . ? O2A Mo2A O6A 159.54(6) . . ? O4A Mo2A O6A 86.64(5) . . ? O3A Mo2A O6A 85.38(5) . . ? O2A Mo2A N4A 88.24(6) . . ? O4A Mo2A N4A 163.19(6) . . ? O3A Mo2A N4A 88.34(5) . . ? O6A Mo2A N4A 77.04(5) . . ? O2A Mo2A N3A 89.03(6) . . ? O4A Mo2A N3A 84.06(5) . . ? O3A Mo2A N3A 161.91(6) . . ? O6A Mo2A N3A 76.54(5) . . ? N4A Mo2A N3A 88.20(5) . . ? O2A Mo2A Mo1A 101.99(4) . . ? O4A Mo2A Mo1A 48.76(4) . . ? O3A Mo2A Mo1A 48.91(4) . . ? O6A Mo2A Mo1A 98.47(3) . . ? N4A Mo2A Mo1A 137.18(4) . . ? N3A Mo2A Mo1A 132.81(4) . . ? Mo1A O3A Mo2A 82.08(5) . . ? Mo1A O4A Mo2A 82.46(5) . . ? C1A O5A Mo1A 122.12(11) . . ? C2A O6A Mo2A 123.48(11) . . ? C15A N1A C11A 117.51(16) . . ? C15A N1A Mo1A 120.49(12) . . ? C11A N1A Mo1A 121.90(13) . . ? C21A N2A C25A 117.68(16) . . ? C21A N2A Mo1A 119.33(12) . . ? C25A N2A Mo1A 121.87(12) . . ? C31A N3A C35A 117.99(16) . . ? C31A N3A Mo2A 124.40(12) . . ? C35A N3A Mo2A 117.22(12) . . ? C45A N4A C41A 118.21(16) . . ? C45A N4A Mo2A 120.28(12) . . ? C41A N4A Mo2A 121.50(13) . . ? O5A C1A C2A 136.69(17) . . ? O5A C1A C4A 131.57(16) . . ? C2A C1A C4A 91.71(14) . . ? O6A C2A C1A 136.67(16) . . ? O6A C2A C3A 132.06(16) . . ? C1A C2A C3A 91.27(14) . . ? O7A C3A C2A 135.34(17) . . ? O7A C3A C4A 135.78(17) . . ? C2A C3A C4A 88.81(13) . . ? O8A C4A C1A 136.12(17) . . ? O8A C4A C3A 135.71(17) . . ? C1A C4A C3A 88.17(14) . . ? N1A C11A C12A 122.44(18) . . ? C11A C12A C13A 119.79(19) . . ? C12A C13A C14A 118.17(18) . . ? C13A C14A C15A 119.26(18) . . ? N1A C15A C14A 122.80(18) . . ? N2A C21A C22A 122.62(17) . . ? C21A C22A C23A 119.24(18) . . ? C24A C23A C22A 118.49(17) . . ? C25A C24A C23A 118.96(18) . . ? N2A C25A C24A 123.00(18) . . ? N3A C31A C32A 122.40(18) . . ? C33A C32A C31A 119.1(2) . . ? C32A C33A C34A 118.92(19) . . ? C35A C34A C33A 118.54(19) . . ? N3A C35A C34A 123.01(19) . . ? N4A C41A C42A 122.31(19) . . ? C41A C42A C43A 119.21(19) . . ? C44A C43A C42A 118.83(18) . . ? C43A C44A C45A 119.0(2) . . ? N4A C45A C44A 122.48(19) . . ? C61 N6 C65 116.6(2) . . ? N6 C61 C62 123.6(2) . . ? C61 C62 C63 119.1(2) . . ? C64 C63 C62 118.4(2) . . ? C63 C64 C65 118.9(2) . . ? N6 C65 C64 123.4(2) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 32.99 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.231 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.096 #===END data_1c _database_code_depnum_ccdc_archive 'CCDC 219867' _chemical_name_common ;Tetra(3,5-lutidine)tetraoxosquaratodimolybdenum(V) (3,5- lutidine) (1/2) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra(3,5-lutidine)tetraoxosquaratodimolybdenum(V) (3,5-lutidine) (1/2) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 Mo2 N6 O8' _chemical_formula_weight 1010.83 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9594(5) _cell_length_b 11.8057(6) _cell_length_c 21.0573(11) _cell_angle_alpha 90.3260(10) _cell_angle_beta 92.4660(10) _cell_angle_gamma 111.8640(10) _cell_volume 2295.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'Phi and omega scan' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29617 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 31.50 _reflns_number_total 14929 _reflns_number_gt 13130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0379P)^2^+1.4189P] 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 14929 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.779227(13) 0.287118(12) 0.298875(6) 0.01443(3) Uani 1 1 d . . . Mo2 Mo 0.909462(13) 0.253555(11) 0.203023(6) 0.01413(3) Uani 1 1 d . . . O1 O 0.66693(12) 0.14205(10) 0.31315(6) 0.0192(2) Uani 1 1 d . . . O2 O 0.83380(12) 0.09964(10) 0.19287(5) 0.0188(2) Uani 1 1 d . . . O3 O 0.75404(12) 0.31421(11) 0.20933(5) 0.0174(2) Uani 1 1 d . . . O4 O 0.97244(12) 0.28565(10) 0.29204(5) 0.0165(2) Uani 1 1 d . . . O5 O 0.88616(12) 0.48232(10) 0.31323(5) 0.0179(2) Uani 1 1 d . . . O6 O 1.04352(12) 0.44004(10) 0.18414(5) 0.0186(2) Uani 1 1 d . . . O7 O 1.23747(14) 0.72446(11) 0.18492(6) 0.0248(3) Uani 1 1 d . . . O8 O 1.08824(17) 0.76570(12) 0.31552(6) 0.0303(3) Uani 1 1 d . . . N1 N 0.58929(14) 0.34405(13) 0.31390(6) 0.0175(2) Uani 1 1 d . . . N2 N 0.82525(14) 0.30710(12) 0.40540(6) 0.0166(2) Uani 1 1 d . . . N3 N 0.88059(14) 0.26016(12) 0.09586(6) 0.0172(2) Uani 1 1 d . . . N4 N 1.12525(14) 0.23636(12) 0.18745(6) 0.0166(2) Uani 1 1 d . . . N5 N 0.3131(2) 0.35532(16) 0.57593(9) 0.0371(4) Uani 1 1 d . . . N6 N 0.6303(5) 0.7749(4) 0.00405(16) 0.0918(11) Uani 1 1 d . . . C1 C 0.98640(17) 0.54789(14) 0.27739(7) 0.0167(3) Uani 1 1 d . . . C2 C 1.05348(17) 0.52991(14) 0.22136(7) 0.0167(3) Uani 1 1 d . . . C3 C 1.14584(18) 0.66065(14) 0.22011(8) 0.0195(3) Uani 1 1 d . . . C4 C 1.07685(19) 0.67961(15) 0.27989(8) 0.0208(3) Uani 1 1 d . . . C11 C 0.47358(18) 0.26887(16) 0.34364(8) 0.0208(3) Uani 1 1 d . . . H11 H 0.4789 0.1973 0.3621 0.025 Uiso 1 1 calc R . . C12 C 0.34645(18) 0.29112(17) 0.34859(8) 0.0227(3) Uani 1 1 d . . . C13 C 0.34064(18) 0.39628(17) 0.32132(8) 0.0226(3) Uani 1 1 d . . . H13 H 0.2547 0.4132 0.3230 0.027 Uiso 1 1 calc R . . C14 C 0.45972(19) 0.47687(16) 0.29166(8) 0.0227(3) Uani 1 1 d . . . C15 C 0.58214(18) 0.44644(15) 0.28892(8) 0.0207(3) Uani 1 1 d . . . H15 H 0.6640 0.5004 0.2685 0.025 Uiso 1 1 calc R . . C16 C 0.2192(2) 0.2021(2) 0.38123(10) 0.0314(4) Uani 1 1 d . . . H16A H 0.2174 0.2321 0.4246 0.047 Uiso 1 1 calc R . . H16B H 0.2283 0.1223 0.3829 0.047 Uiso 1 1 calc R . . H16C H 0.1292 0.1941 0.3575 0.047 Uiso 1 1 calc R . . C17 C 0.4578(2) 0.59242(19) 0.26244(11) 0.0333(4) Uani 1 1 d . . . H17A H 0.3791 0.5721 0.2296 0.050 Uiso 1 1 calc R . . H17B H 0.5505 0.6357 0.2432 0.050 Uiso 1 1 calc R . . H17C H 0.4426 0.6447 0.2954 0.050 Uiso 1 1 calc R . . C21 C 0.86408(17) 0.22044(15) 0.43301(8) 0.0185(3) Uani 1 1 d . . . H21 H 0.8739 0.1586 0.4067 0.022 Uiso 1 1 calc R . . C22 C 0.89033(19) 0.21739(16) 0.49822(8) 0.0221(3) Uani 1 1 d . . . C23 C 0.8744(2) 0.30855(16) 0.53588(8) 0.0234(3) Uani 1 1 d . . . H23 H 0.8930 0.3100 0.5806 0.028 Uiso 1 1 calc R . . C24 C 0.83144(19) 0.39755(16) 0.50868(8) 0.0211(3) Uani 1 1 d . . . C25 C 0.80904(17) 0.39411(15) 0.44264(8) 0.0186(3) Uani 1 1 d . . . H25 H 0.7814 0.4551 0.4233 0.022 Uiso 1 1 calc R . . C26 C 0.9330(2) 0.11792(18) 0.52631(9) 0.0309(4) Uani 1 1 d . . . H26A H 0.8742 0.0396 0.5055 0.046 Uiso 1 1 calc R . . H26B H 0.9168 0.1135 0.5720 0.046 Uiso 1 1 calc R . . H26C H 1.0356 0.1359 0.5198 0.046 Uiso 1 1 calc R . . C27 C 0.8059(2) 0.49321(18) 0.54901(9) 0.0272(4) Uani 1 1 d . . . H27A H 0.7113 0.4575 0.5678 0.041 Uiso 1 1 calc R . . H27B H 0.8079 0.5617 0.5225 0.041 Uiso 1 1 calc R . . H27C H 0.8820 0.5226 0.5830 0.041 Uiso 1 1 calc R . . C31 C 0.89104(18) 0.17096(15) 0.05856(8) 0.0204(3) Uani 1 1 d . . . H31 H 0.9160 0.1086 0.0780 0.024 Uiso 1 1 calc R . . C32 C 0.86684(19) 0.16622(17) -0.00720(8) 0.0231(3) Uani 1 1 d . . . C33 C 0.8291(2) 0.25776(18) -0.03452(8) 0.0249(3) Uani 1 1 d . . . H33 H 0.8116 0.2571 -0.0793 0.030 Uiso 1 1 calc R . . C34 C 0.8167(2) 0.35036(17) 0.00316(8) 0.0247(3) Uani 1 1 d . . . C35 C 0.84377(19) 0.34794(15) 0.06847(8) 0.0212(3) Uani 1 1 d . . . H35 H 0.8359 0.4107 0.0947 0.025 Uiso 1 1 calc R . . C36 C 0.8796(3) 0.0642(2) -0.04724(10) 0.0347(4) Uani 1 1 d . . . H36A H 0.8303 0.0605 -0.0889 0.052 Uiso 1 1 calc R . . H36B H 0.8346 -0.0136 -0.0260 0.052 Uiso 1 1 calc R . . H36C H 0.9821 0.0797 -0.0527 0.052 Uiso 1 1 calc R . . C37 C 0.7724(3) 0.4482(2) -0.02578(10) 0.0369(5) Uani 1 1 d . . . H37A H 0.6819 0.4453 -0.0079 0.055 Uiso 1 1 calc R . . H37B H 0.7578 0.4346 -0.0719 0.055 Uiso 1 1 calc R . . H37C H 0.8485 0.5283 -0.0163 0.055 Uiso 1 1 calc R . . C41 C 1.14685(18) 0.13942(15) 0.21269(8) 0.0192(3) Uani 1 1 d . . . H41 H 1.0689 0.0798 0.2328 0.023 Uiso 1 1 calc R . . C42 C 1.27748(18) 0.12238(15) 0.21074(8) 0.0214(3) Uani 1 1 d . . . C43 C 1.39000(18) 0.21021(16) 0.18022(8) 0.0210(3) Uani 1 1 d . . . H43 H 1.4806 0.2013 0.1777 0.025 Uiso 1 1 calc R . . C44 C 1.37044(17) 0.31090(16) 0.15343(8) 0.0206(3) Uani 1 1 d . . . C45 C 1.23551(17) 0.31980(15) 0.15790(7) 0.0189(3) Uani 1 1 d . . . H45 H 1.2204 0.3875 0.1394 0.023 Uiso 1 1 calc R . . C46 C 1.2951(2) 0.01369(17) 0.24160(11) 0.0312(4) Uani 1 1 d . . . H46A H 1.2730 -0.0528 0.2100 0.047 Uiso 1 1 calc R . . H46B H 1.2286 -0.0133 0.2763 0.047 Uiso 1 1 calc R . . H46C H 1.3950 0.0364 0.2586 0.047 Uiso 1 1 calc R . . C47 C 1.49105(19) 0.40893(19) 0.12157(9) 0.0288(4) Uani 1 1 d . . . H47A H 1.5841 0.4189 0.1431 0.043 Uiso 1 1 calc R . . H47B H 1.4758 0.4862 0.1240 0.043 Uiso 1 1 calc R . . H47C H 1.4916 0.3855 0.0769 0.043 Uiso 1 1 calc R . . C51 C 0.3926(2) 0.3113(2) 0.54169(11) 0.0375(5) Uani 1 1 d . . . H51 H 0.4446 0.3599 0.5084 0.045 Uiso 1 1 calc R . . C52 C 0.4047(2) 0.1990(2) 0.55117(11) 0.0351(4) Uani 1 1 d . . . C53 C 0.3293(2) 0.12974(19) 0.60056(11) 0.0334(4) Uani 1 1 d . . . H53 H 0.3368 0.0534 0.6095 0.040 Uiso 1 1 calc R . . C54 C 0.2435(2) 0.17122(19) 0.63684(10) 0.0322(4) Uani 1 1 d . . . C55 C 0.2399(2) 0.28567(19) 0.62193(10) 0.0343(4) Uani 1 1 d . . . H55 H 0.1813 0.3154 0.6463 0.041 Uiso 1 1 calc R . . C56 C 0.4918(3) 0.1521(3) 0.50864(14) 0.0516(6) Uani 1 1 d . . . H56A H 0.5551 0.1224 0.5348 0.077 Uiso 1 1 calc R . . H56B H 0.5509 0.2183 0.4821 0.077 Uiso 1 1 calc R . . H56C H 0.4260 0.0851 0.4814 0.077 Uiso 1 1 calc R . . C57 C 0.1533(3) 0.0946(3) 0.68764(12) 0.0488(6) Uani 1 1 d . . . H57A H 0.0630 0.0357 0.6682 0.073 Uiso 1 1 calc R . . H57B H 0.1310 0.1474 0.7181 0.073 Uiso 1 1 calc R . . H57C H 0.2072 0.0508 0.7098 0.073 Uiso 1 1 calc R . . C61 C 0.7136(5) 0.7338(3) 0.0398(2) 0.0839(13) Uani 1 1 d . . . H61 H 0.7568 0.6843 0.0200 0.101 Uiso 1 1 calc R . . C62 C 0.7431(3) 0.7593(2) 0.10715(16) 0.0522(7) Uani 1 1 d . . . C63 C 0.6754(2) 0.83186(19) 0.13219(11) 0.0353(4) Uani 1 1 d . . . H63 H 0.6893 0.8534 0.1762 0.042 Uiso 1 1 calc R . . C64 C 0.5872(2) 0.8735(2) 0.09352(11) 0.0389(5) Uani 1 1 d . . . C65 C 0.5700(4) 0.8411(3) 0.03085(15) 0.0690(9) Uani 1 1 d . . . H65 H 0.5090 0.8693 0.0048 0.083 Uiso 1 1 calc R . . C66 C 0.8385(4) 0.7126(3) 0.1470(2) 0.0844(13) Uani 1 1 d . . . H66A H 0.9206 0.7817 0.1657 0.127 Uiso 1 1 calc R . . H66B H 0.8744 0.6626 0.1205 0.127 Uiso 1 1 calc R . . H66C H 0.7830 0.6630 0.1811 0.127 Uiso 1 1 calc R . . C67 C 0.5140(3) 0.9529(3) 0.11899(17) 0.0577(8) Uani 1 1 d . . . H67A H 0.4622 0.9765 0.0840 0.087 Uiso 1 1 calc R . . H67B H 0.5867 1.0264 0.1393 0.087 Uiso 1 1 calc R . . H67C H 0.4450 0.9080 0.1503 0.087 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 0.01343(6) 0.01667(6) 0.01361(6) 0.00021(4) 0.00091(4) 0.00609(5) Mo2 0.01380(6) 0.01536(6) 0.01337(6) -0.00003(4) 0.00055(4) 0.00561(5) O1 0.0172(5) 0.0188(5) 0.0205(5) 0.0004(4) 0.0026(4) 0.0052(4) O2 0.0191(5) 0.0172(5) 0.0187(5) 0.0003(4) 0.0006(4) 0.0052(4) O3 0.0160(5) 0.0220(5) 0.0158(5) 0.0011(4) 0.0007(4) 0.0088(4) O4 0.0154(5) 0.0198(5) 0.0151(5) -0.0007(4) 0.0005(4) 0.0074(4) O5 0.0181(5) 0.0175(5) 0.0182(5) 0.0004(4) 0.0035(4) 0.0065(4) O6 0.0202(5) 0.0166(5) 0.0186(5) -0.0010(4) 0.0033(4) 0.0061(4) O7 0.0308(7) 0.0192(6) 0.0200(6) 0.0030(4) 0.0046(5) 0.0038(5) O8 0.0469(8) 0.0180(6) 0.0222(6) -0.0018(5) 0.0065(6) 0.0071(6) N1 0.0156(6) 0.0221(6) 0.0164(6) -0.0010(5) 0.0010(4) 0.0089(5) N2 0.0166(6) 0.0184(6) 0.0150(6) -0.0002(5) 0.0009(4) 0.0068(5) N3 0.0170(6) 0.0200(6) 0.0146(6) 0.0007(5) 0.0007(4) 0.0070(5) N4 0.0161(6) 0.0188(6) 0.0150(6) -0.0016(5) 0.0004(4) 0.0066(5) N5 0.0399(10) 0.0295(9) 0.0394(10) 0.0021(7) -0.0078(8) 0.0110(8) N6 0.106(3) 0.086(2) 0.061(2) -0.0240(17) 0.0082(19) 0.010(2) C1 0.0185(7) 0.0164(6) 0.0159(7) 0.0007(5) 0.0001(5) 0.0073(5) C2 0.0168(6) 0.0167(6) 0.0164(7) 0.0014(5) -0.0003(5) 0.0062(5) C3 0.0238(7) 0.0166(7) 0.0169(7) 0.0010(5) -0.0011(6) 0.0063(6) C4 0.0261(8) 0.0181(7) 0.0165(7) 0.0021(5) 0.0015(6) 0.0062(6) C11 0.0183(7) 0.0262(8) 0.0188(7) 0.0026(6) 0.0036(5) 0.0090(6) C12 0.0185(7) 0.0332(9) 0.0182(7) -0.0022(6) 0.0028(6) 0.0115(7) C13 0.0193(7) 0.0324(9) 0.0198(7) -0.0072(6) -0.0014(6) 0.0143(7) C14 0.0216(8) 0.0252(8) 0.0238(8) -0.0044(6) -0.0043(6) 0.0124(6) C15 0.0176(7) 0.0225(7) 0.0223(8) -0.0006(6) -0.0012(6) 0.0083(6) C16 0.0205(8) 0.0451(11) 0.0302(10) 0.0061(8) 0.0088(7) 0.0131(8) C17 0.0289(9) 0.0291(9) 0.0471(12) 0.0031(8) -0.0023(8) 0.0171(8) C21 0.0195(7) 0.0191(7) 0.0178(7) -0.0005(5) 0.0003(5) 0.0084(6) C22 0.0245(8) 0.0232(8) 0.0192(7) 0.0022(6) -0.0008(6) 0.0099(6) C23 0.0284(8) 0.0269(8) 0.0154(7) 0.0007(6) 0.0008(6) 0.0109(7) C24 0.0233(8) 0.0230(7) 0.0174(7) -0.0017(6) 0.0023(6) 0.0089(6) C25 0.0197(7) 0.0192(7) 0.0182(7) -0.0001(5) 0.0019(5) 0.0087(6) C26 0.0418(11) 0.0285(9) 0.0269(9) 0.0035(7) -0.0052(8) 0.0189(8) C27 0.0332(9) 0.0292(9) 0.0213(8) -0.0061(7) 0.0028(7) 0.0140(8) C31 0.0213(7) 0.0229(7) 0.0178(7) -0.0017(6) -0.0005(6) 0.0096(6) C32 0.0219(8) 0.0292(8) 0.0182(7) -0.0044(6) -0.0016(6) 0.0099(7) C33 0.0252(8) 0.0344(9) 0.0148(7) 0.0014(6) 0.0001(6) 0.0109(7) C34 0.0269(8) 0.0278(8) 0.0204(8) 0.0064(6) 0.0014(6) 0.0112(7) C35 0.0250(8) 0.0212(7) 0.0190(7) 0.0014(6) 0.0019(6) 0.0103(6) C36 0.0431(11) 0.0422(11) 0.0244(9) -0.0119(8) -0.0047(8) 0.0233(10) C37 0.0536(13) 0.0378(11) 0.0274(10) 0.0096(8) 0.0016(9) 0.0261(10) C41 0.0194(7) 0.0173(7) 0.0207(7) -0.0010(5) 0.0013(6) 0.0066(6) C42 0.0219(7) 0.0179(7) 0.0254(8) -0.0032(6) -0.0016(6) 0.0090(6) C43 0.0174(7) 0.0243(8) 0.0231(8) -0.0057(6) 0.0005(6) 0.0098(6) C44 0.0174(7) 0.0255(8) 0.0177(7) -0.0014(6) 0.0019(5) 0.0064(6) C45 0.0183(7) 0.0221(7) 0.0168(7) 0.0020(5) 0.0022(5) 0.0079(6) C46 0.0290(9) 0.0205(8) 0.0474(12) 0.0025(8) 0.0013(8) 0.0130(7) C47 0.0194(8) 0.0359(10) 0.0292(9) 0.0078(7) 0.0069(6) 0.0075(7) C51 0.0342(10) 0.0335(10) 0.0370(11) 0.0048(8) -0.0037(8) 0.0040(9) C52 0.0275(9) 0.0332(10) 0.0406(11) -0.0014(8) -0.0007(8) 0.0069(8) C53 0.0306(10) 0.0255(9) 0.0421(11) 0.0015(8) -0.0037(8) 0.0089(8) C54 0.0353(10) 0.0313(10) 0.0275(9) 0.0030(7) -0.0048(8) 0.0100(8) C55 0.0381(11) 0.0332(10) 0.0321(10) -0.0031(8) -0.0056(8) 0.0147(9) C56 0.0408(13) 0.0505(15) 0.0632(17) -0.0017(12) 0.0134(12) 0.0154(11) C57 0.0585(16) 0.0531(15) 0.0387(13) 0.0169(11) 0.0091(11) 0.0242(13) C61 0.090(3) 0.0473(17) 0.106(3) -0.0269(19) 0.048(2) 0.0111(18) C62 0.0422(13) 0.0253(10) 0.084(2) -0.0040(11) 0.0183(13) 0.0046(9) C63 0.0317(10) 0.0274(9) 0.0400(11) -0.0038(8) 0.0016(8) 0.0033(8) C64 0.0263(9) 0.0348(11) 0.0414(12) 0.0034(9) -0.0002(8) -0.0050(8) C65 0.0622(19) 0.075(2) 0.0437(16) -0.0008(15) -0.0036(14) -0.0040(16) C66 0.0588(19) 0.0456(16) 0.160(4) 0.026(2) 0.031(2) 0.0294(15) C67 0.0298(12) 0.0489(15) 0.091(2) 0.0127(15) -0.0002(13) 0.0111(11) _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 O1 1.6978(12) . ? Mo1 O3 1.9355(11) . ? Mo1 O4 1.9423(11) . ? Mo1 O5 2.1616(11) . ? Mo1 N2 2.2634(13) . ? Mo1 N1 2.2641(13) . ? Mo1 Mo2 2.5519(2) . ? Mo2 O2 1.6962(11) . ? Mo2 O4 1.9402(11) . ? Mo2 O3 1.9413(11) . ? Mo2 O6 2.1573(11) . ? Mo2 N3 2.2680(13) . ? Mo2 N4 2.2699(13) . ? O5 C1 1.2889(19) . ? O6 C2 1.2866(19) . ? O7 C3 1.226(2) . ? O8 C4 1.228(2) . ? N1 C15 1.346(2) . ? N1 C11 1.347(2) . ? N2 C21 1.348(2) . ? N2 C25 1.350(2) . ? N3 C35 1.346(2) . ? N3 C31 1.348(2) . ? N4 C41 1.349(2) . ? N4 C45 1.350(2) . ? N5 C51 1.330(3) . ? N5 C55 1.330(3) . ? N6 C65 1.290(5) . ? N6 C61 1.320(6) . ? C1 C2 1.433(2) . ? C1 C4 1.478(2) . ? C2 C3 1.474(2) . ? C3 C4 1.514(2) . ? C11 C12 1.393(2) . ? C12 C13 1.390(3) . ? C12 C16 1.508(3) . ? C13 C14 1.390(3) . ? C14 C15 1.397(2) . ? C14 C17 1.506(3) . ? C21 C22 1.390(2) . ? C22 C23 1.393(2) . ? C22 C26 1.506(2) . ? C23 C24 1.391(2) . ? C24 C25 1.397(2) . ? C24 C27 1.511(2) . ? C31 C32 1.392(2) . ? C32 C33 1.390(3) . ? C32 C36 1.513(3) . ? C33 C34 1.392(3) . ? C34 C35 1.392(2) . ? C34 C37 1.505(3) . ? C41 C42 1.391(2) . ? C42 C43 1.396(2) . ? C42 C46 1.505(2) . ? C43 C44 1.393(2) . ? C44 C45 1.393(2) . ? C44 C47 1.508(2) . ? C51 C52 1.390(3) . ? C52 C53 1.391(3) . ? C52 C56 1.510(3) . ? C53 C54 1.385(3) . ? C54 C55 1.402(3) . ? C54 C57 1.503(3) . ? C61 C62 1.442(5) . ? C62 C63 1.387(3) . ? C62 C66 1.496(5) . ? C63 C64 1.393(3) . ? C64 C65 1.357(4) . ? C64 C67 1.495(4) . ? 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 O1 Mo1 O3 107.12(5) . . ? O1 Mo1 O4 107.27(5) . . ? O3 Mo1 O4 94.47(5) . . ? O1 Mo1 O5 158.22(5) . . ? O3 Mo1 O5 88.60(5) . . ? O4 Mo1 O5 85.84(4) . . ? O1 Mo1 N2 85.94(5) . . ? O3 Mo1 N2 165.53(5) . . ? O4 Mo1 N2 87.31(5) . . ? O5 Mo1 N2 77.20(5) . . ? O1 Mo1 N1 87.39(5) . . ? O3 Mo1 N1 86.89(5) . . ? O4 Mo1 N1 164.06(5) . . ? O5 Mo1 N1 78.31(5) . . ? N2 Mo1 N1 87.54(5) . . ? O1 Mo1 Mo2 101.31(4) . . ? O3 Mo1 Mo2 48.93(3) . . ? O4 Mo1 Mo2 48.87(3) . . ? O5 Mo1 Mo2 100.39(3) . . ? N2 Mo1 Mo2 135.94(3) . . ? N1 Mo1 Mo2 135.71(3) . . ? O2 Mo2 O4 106.68(5) . . ? O2 Mo2 O3 108.00(5) . . ? O4 Mo2 O3 94.36(5) . . ? O2 Mo2 O6 158.40(5) . . ? O4 Mo2 O6 88.58(5) . . ? O3 Mo2 O6 85.40(5) . . ? O2 Mo2 N3 85.74(5) . . ? O4 Mo2 N3 166.03(5) . . ? O3 Mo2 N3 87.61(5) . . ? O6 Mo2 N3 77.78(5) . . ? O2 Mo2 N4 86.69(5) . . ? O4 Mo2 N4 86.89(5) . . ? O3 Mo2 N4 164.12(5) . . ? O6 Mo2 N4 78.80(5) . . ? N3 Mo2 N4 87.51(5) . . ? O2 Mo2 Mo1 101.54(4) . . ? O4 Mo2 Mo1 48.94(3) . . ? O3 Mo2 Mo1 48.74(3) . . ? O6 Mo2 Mo1 100.02(3) . . ? N3 Mo2 Mo1 136.06(3) . . ? N4 Mo2 Mo1 135.72(3) . . ? Mo1 O3 Mo2 82.33(4) . . ? Mo2 O4 Mo1 82.19(4) . . ? C1 O5 Mo1 122.22(10) . . ? C2 O6 Mo2 122.64(10) . . ? C15 N1 C11 118.18(14) . . ? C15 N1 Mo1 121.86(11) . . ? C11 N1 Mo1 119.69(11) . . ? C21 N2 C25 118.75(14) . . ? C21 N2 Mo1 116.14(10) . . ? C25 N2 Mo1 125.00(11) . . ? C35 N3 C31 118.62(14) . . ? C35 N3 Mo2 121.17(11) . . ? C31 N3 Mo2 120.08(11) . . ? C41 N4 C45 118.15(14) . . ? C41 N4 Mo2 117.32(11) . . ? C45 N4 Mo2 124.43(11) . . ? C51 N5 C55 116.99(19) . . ? C65 N6 C61 118.2(3) . . ? O5 C1 C2 137.23(14) . . ? O5 C1 C4 131.38(14) . . ? C2 C1 C4 91.38(13) . . ? O6 C2 C1 137.03(15) . . ? O6 C2 C3 131.22(15) . . ? C1 C2 C3 91.75(13) . . ? O7 C3 C2 134.92(16) . . ? O7 C3 C4 136.69(15) . . ? C2 C3 C4 88.38(12) . . ? O8 C4 C1 134.84(16) . . ? O8 C4 C3 136.68(16) . . ? C1 C4 C3 88.48(12) . . ? N1 C11 C12 123.07(16) . . ? C13 C12 C11 117.67(16) . . ? C13 C12 C16 121.66(16) . . ? C11 C12 C16 120.66(17) . . ? C14 C13 C12 120.42(15) . . ? C13 C14 C15 117.67(16) . . ? C13 C14 C17 121.81(16) . . ? C15 C14 C17 120.51(17) . . ? N1 C15 C14 122.95(16) . . ? N2 C21 C22 122.98(15) . . ? C21 C22 C23 117.50(15) . . ? C21 C22 C26 120.53(16) . . ? C23 C22 C26 121.97(16) . . ? C24 C23 C22 120.63(15) . . ? C23 C24 C25 117.83(15) . . ? C23 C24 C27 121.43(15) . . ? C25 C24 C27 120.72(15) . . ? N2 C25 C24 122.29(15) . . ? N3 C31 C32 122.88(15) . . ? C33 C32 C31 117.58(16) . . ? C33 C32 C36 121.32(16) . . ? C31 C32 C36 121.09(16) . . ? C32 C33 C34 120.51(16) . . ? C33 C34 C35 117.84(16) . . ? C33 C34 C37 120.91(17) . . ? C35 C34 C37 121.23(17) . . ? N3 C35 C34 122.57(16) . . ? N4 C41 C42 123.30(15) . . ? C41 C42 C43 117.46(15) . . ? C41 C42 C46 120.35(16) . . ? C43 C42 C46 122.18(16) . . ? C44 C43 C42 120.46(15) . . ? C43 C44 C45 117.76(15) . . ? C43 C44 C47 121.71(15) . . ? C45 C44 C47 120.52(16) . . ? N4 C45 C44 122.88(15) . . ? N5 C51 C52 124.5(2) . . ? C51 C52 C53 117.0(2) . . ? C51 C52 C56 121.8(2) . . ? C53 C52 C56 121.2(2) . . ? C54 C53 C52 120.4(2) . . ? C53 C54 C55 116.8(2) . . ? C53 C54 C57 121.5(2) . . ? C55 C54 C57 121.6(2) . . ? N5 C55 C54 124.3(2) . . ? N6 C61 C62 124.2(3) . . ? C63 C62 C61 114.1(3) . . ? C63 C62 C66 122.4(3) . . ? C61 C62 C66 123.6(3) . . ? C62 C63 C64 120.7(2) . . ? C65 C64 C63 118.1(3) . . ? C65 C64 C67 120.0(3) . . ? C63 C64 C67 121.9(2) . . ? N6 C65 C64 124.8(4) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.343 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.086 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 219868' _chemical_name_common ; Tetra(N-methylcollidinium) octaoxotetrasquaratotetramolybdate(V) methanol collidine (4/1/2/2) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra(N-methylcollidinium) octaoxotetrasquaratotetramolybdate(V) methanol collidine (4/1/2/2) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H86 Mo4 N6 O26' _chemical_formula_weight 1811.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 14.2914(6) _cell_length_b 17.1820(8) _cell_length_c 30.5418(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.0820(10) _cell_angle_gamma 90.00 _cell_volume 7383.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8897 _exptl_absorpt_correction_T_max 0.9426 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95337 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 31.51 _reflns_number_total 24562 _reflns_number_gt 16327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0425P)^2^+4.2000P] 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 24562 _refine_ls_number_parameters 958 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.020004(18) 0.681177(15) 0.212657(8) 0.01223(6) Uani 1 1 d . . . Mo2 Mo 0.030978(18) 0.686001(15) 0.298286(8) 0.01291(6) Uani 1 1 d . . . Mo3 Mo -0.081751(19) 0.854186(16) 0.256619(8) 0.01376(6) Uani 1 1 d . . . Mo4 Mo 0.095315(19) 0.850164(15) 0.247684(8) 0.01326(6) Uani 1 1 d . . . O1 O -0.02182(15) 0.58368(13) 0.21030(7) 0.0175(5) Uani 1 1 d . . . O2 O 0.03424(16) 0.58904(13) 0.30442(7) 0.0189(5) Uani 1 1 d . . . O3 O -0.08558(16) 0.95141(13) 0.25501(7) 0.0202(5) Uani 1 1 d . . . O4 O 0.10331(17) 0.94721(13) 0.24579(7) 0.0203(5) Uani 1 1 d . . . O5 O -0.09012(15) 0.71312(13) 0.25971(7) 0.0153(4) Uani 1 1 d . . . O6 O 0.10112(15) 0.71185(12) 0.25001(7) 0.0141(4) Uani 1 1 d . . . O7 O -0.02100(15) 0.81778(12) 0.20669(6) 0.0140(4) Uani 1 1 d . . . O8 O 0.03353(15) 0.82230(12) 0.29865(7) 0.0152(4) Uani 1 1 d . . . O9 O 0.0388(3) 0.17537(19) 0.34572(10) 0.0493(8) Uani 1 1 d . . . H9 H 0.0635 0.1487 0.3669 0.074 Uiso 1 1 calc R . . O10 O 0.9508(3) 0.1894(3) 0.16127(14) 0.0835(13) Uani 1 1 d . . . H10 H 0.9430 0.1635 0.1384 0.125 Uiso 1 1 calc R . . O131 O -0.21017(16) 0.83931(14) 0.21695(7) 0.0200(5) Uani 1 1 d . . . O132 O -0.14270(16) 0.69052(13) 0.16579(7) 0.0195(5) Uani 1 1 d . . . O133 O -0.2889(2) 0.73774(17) 0.07694(9) 0.0356(7) Uani 1 1 d . . . O134 O -0.35179(18) 0.89108(16) 0.12693(8) 0.0305(6) Uani 1 1 d . . . O141 O 0.17166(16) 0.83669(13) 0.19723(7) 0.0191(5) Uani 1 1 d . . . O142 O 0.04198(16) 0.68814(13) 0.15704(7) 0.0168(4) Uani 1 1 d . . . O143 O 0.12803(18) 0.69796(15) 0.06713(8) 0.0270(6) Uani 1 1 d . . . O144 O 0.2509(2) 0.85127(15) 0.10548(8) 0.0324(6) Uani 1 1 d . . . O231 O -0.03131(16) 0.70007(13) 0.35368(7) 0.0193(5) Uani 1 1 d . . . O232 O -0.15672(16) 0.84609(14) 0.30722(7) 0.0207(5) Uani 1 1 d . . . O233 O -0.22660(18) 0.88195(15) 0.39928(8) 0.0270(6) Uani 1 1 d . . . O234 O -0.1128(2) 0.72757(16) 0.44313(8) 0.0332(6) Uani 1 1 d . . . O241 O 0.22499(16) 0.84052(13) 0.28842(7) 0.0198(5) Uani 1 1 d . . . O242 O 0.15244(16) 0.69881(13) 0.34490(7) 0.0189(5) Uani 1 1 d . . . O243 O 0.3346(2) 0.72100(17) 0.42135(9) 0.0391(7) Uani 1 1 d . . . O244 O 0.40469(19) 0.86607(16) 0.36650(10) 0.0380(7) Uani 1 1 d . . . N1 N 0.1079(2) 0.07384(18) 0.41562(10) 0.0273(7) Uani 1 1 d . . . N2 N 0.38768(19) -0.03051(16) 0.02802(9) 0.0184(6) Uani 1 1 d . . . N3 N 0.88532(19) 0.49828(16) 0.02775(9) 0.0179(6) Uani 1 1 d . . . N4 N 0.2322(2) 0.54597(17) 0.25540(11) 0.0252(6) Uani 1 1 d . . . N5 N 0.7182(2) 0.58690(18) 0.23797(11) 0.0302(7) Uani 1 1 d . . . N6 N 0.9149(2) 0.0948(2) 0.08618(12) 0.0353(8) Uani 1 1 d . . . C9 C 0.0100(4) 0.2474(3) 0.36141(17) 0.0540(13) Uani 1 1 d . . . H9A H -0.0167 0.2389 0.3878 0.081 Uiso 1 1 calc R . . H9B H -0.0369 0.2708 0.3389 0.081 Uiso 1 1 calc R . . H9C H 0.0640 0.2813 0.3682 0.081 Uiso 1 1 calc R . . C10 C 0.8975(5) 0.2595(4) 0.1538(2) 0.094(2) Uani 1 1 d . . . H10A H 0.8800 0.2767 0.1811 0.141 Uiso 1 1 calc R . . H10B H 0.8412 0.2504 0.1322 0.141 Uiso 1 1 calc R . . H10C H 0.9354 0.2988 0.1429 0.141 Uiso 1 1 calc R . . C11 C 0.1273(3) 0.1014(2) 0.45812(14) 0.0310(9) Uani 1 1 d . . . C12 C 0.1322(3) 0.0531(3) 0.49439(13) 0.0321(9) Uani 1 1 d . . . H12 H 0.1450 0.0741 0.5229 0.039 Uiso 1 1 calc R . . C13 C 0.1184(3) -0.0255(3) 0.48897(13) 0.0324(9) Uani 1 1 d . . . C14 C 0.0999(3) -0.0535(2) 0.44590(14) 0.0334(9) Uani 1 1 d . . . H14 H 0.0903 -0.1065 0.4409 0.040 Uiso 1 1 calc R . . C15 C 0.0955(3) -0.0033(2) 0.41021(12) 0.0271(8) Uani 1 1 d . . . C16 C 0.1430(3) 0.1870(2) 0.46363(16) 0.0442(11) Uani 1 1 d . . . H16A H 0.1918 0.2031 0.4476 0.066 Uiso 1 1 calc R . . H16B H 0.1623 0.1990 0.4946 0.066 Uiso 1 1 calc R . . H16C H 0.0851 0.2141 0.4523 0.066 Uiso 1 1 calc R . . C17 C 0.1222(4) -0.0790(3) 0.52821(17) 0.0571(14) Uani 1 1 d . . . H17A H 0.1824 -0.1053 0.5337 0.086 Uiso 1 1 calc R . . H17B H 0.0719 -0.1166 0.5221 0.086 Uiso 1 1 calc R . . H17C H 0.1148 -0.0491 0.5540 0.086 Uiso 1 1 calc R . . C18 C 0.0783(3) -0.0320(3) 0.36313(14) 0.0451(11) Uani 1 1 d . . . H18A H 0.0746 0.0115 0.3432 0.068 Uiso 1 1 calc R . . H18B H 0.0196 -0.0605 0.3574 0.068 Uiso 1 1 calc R . . H18C H 0.1296 -0.0654 0.3586 0.068 Uiso 1 1 calc R . . C21 C 0.3652(2) 0.0083(2) -0.01148(11) 0.0205(7) Uani 1 1 d . . . C22 C 0.3617(2) 0.0884(2) -0.01094(11) 0.0223(7) Uani 1 1 d . . . H22 H 0.3471 0.1151 -0.0378 0.027 Uiso 1 1 calc R . . C23 C 0.3792(2) 0.1305(2) 0.02850(12) 0.0221(7) Uani 1 1 d . . . C24 C 0.4026(2) 0.0887(2) 0.06762(11) 0.0219(7) Uani 1 1 d . . . H24 H 0.4152 0.1154 0.0945 0.026 Uiso 1 1 calc R . . C25 C 0.4077(2) 0.0088(2) 0.06782(11) 0.0193(7) Uani 1 1 d . . . C26 C 0.3443(3) -0.0361(2) -0.05389(11) 0.0249(8) Uani 1 1 d . . . H26A H 0.3944 -0.0729 -0.0551 0.037 Uiso 1 1 calc R . . H26B H 0.3399 -0.0008 -0.0785 0.037 Uiso 1 1 calc R . . H26C H 0.2852 -0.0633 -0.0554 0.037 Uiso 1 1 calc R . . C27 C 0.3732(3) 0.2173(2) 0.02935(13) 0.0344(9) Uani 1 1 d . . . H27A H 0.3230 0.2327 0.0447 0.052 Uiso 1 1 calc R . . H27B H 0.3604 0.2368 -0.0006 0.052 Uiso 1 1 calc R . . H27C H 0.4324 0.2382 0.0445 0.052 Uiso 1 1 calc R . . C28 C 0.4352(2) -0.0368(2) 0.10973(11) 0.0230(7) Uani 1 1 d . . . H28A H 0.4440 -0.0020 0.1347 0.034 Uiso 1 1 calc R . . H28B H 0.4933 -0.0642 0.1089 0.034 Uiso 1 1 calc R . . H28C H 0.3858 -0.0734 0.1125 0.034 Uiso 1 1 calc R . . C29 C 0.3901(3) -0.1163(2) 0.02930(11) 0.0242(7) Uani 1 1 d . . . H29A H 0.3780 -0.1364 -0.0005 0.036 Uiso 1 1 calc R . . H29B H 0.3423 -0.1351 0.0452 0.036 Uiso 1 1 calc R . . H29C H 0.4515 -0.1334 0.0440 0.036 Uiso 1 1 calc R . . C31 C 0.8744(2) 0.53782(19) -0.01178(11) 0.0184(6) Uani 1 1 d . . . C32 C 0.8797(2) 0.6175(2) -0.01102(11) 0.0206(7) Uani 1 1 d . . . H32 H 0.8726 0.6442 -0.0379 0.025 Uiso 1 1 calc R . . C33 C 0.8952(2) 0.6598(2) 0.02823(11) 0.0213(7) Uani 1 1 d . . . C34 C 0.9046(2) 0.6175(2) 0.06740(11) 0.0218(7) Uani 1 1 d . . . H34 H 0.9141 0.6440 0.0944 0.026 Uiso 1 1 calc R . . C35 C 0.9002(2) 0.5375(2) 0.06758(11) 0.0193(7) Uani 1 1 d . . . C36 C 0.8572(3) 0.4935(2) -0.05431(10) 0.0225(7) Uani 1 1 d . . . H36A H 0.9051 0.4542 -0.0537 0.034 Uiso 1 1 calc R . . H36B H 0.8596 0.5284 -0.0786 0.034 Uiso 1 1 calc R . . H36C H 0.7957 0.4694 -0.0581 0.034 Uiso 1 1 calc R . . C37 C 0.9011(3) 0.7466(2) 0.02887(13) 0.0285(8) Uani 1 1 d . . . H37A H 0.8421 0.7678 0.0344 0.043 Uiso 1 1 calc R . . H37B H 0.9130 0.7648 0.0007 0.043 Uiso 1 1 calc R . . H37C H 0.9518 0.7628 0.0519 0.043 Uiso 1 1 calc R . . C38 C 0.9145(3) 0.4921(2) 0.11003(11) 0.0250(8) Uani 1 1 d . . . H38A H 0.8576 0.4637 0.1121 0.038 Uiso 1 1 calc R . . H38B H 0.9286 0.5272 0.1348 0.038 Uiso 1 1 calc R . . H38C H 0.9663 0.4565 0.1105 0.038 Uiso 1 1 calc R . . C39 C 0.8807(3) 0.41254(19) 0.02925(12) 0.0228(7) Uani 1 1 d . . . H39A H 0.8741 0.3921 -0.0004 0.034 Uiso 1 1 calc R . . H39B H 0.8270 0.3970 0.0422 0.034 Uiso 1 1 calc R . . H39C H 0.9379 0.3927 0.0469 0.034 Uiso 1 1 calc R . . C41 C 0.2398(3) 0.5762(2) 0.21459(13) 0.0294(8) Uani 1 1 d . . . C42 C 0.2959(3) 0.6398(2) 0.21250(14) 0.0334(9) Uani 1 1 d . . . H42 H 0.2998 0.6611 0.1849 0.040 Uiso 1 1 calc R . . C43 C 0.3472(3) 0.6736(2) 0.25036(14) 0.0321(9) Uani 1 1 d . . . C44 C 0.3419(3) 0.6385(2) 0.29023(14) 0.0306(9) Uani 1 1 d . . . H44 H 0.3782 0.6583 0.3161 0.037 Uiso 1 1 calc R . . C45 C 0.2849(3) 0.5753(2) 0.29329(13) 0.0271(8) Uani 1 1 d . . . C46 C 0.1873(3) 0.5388(2) 0.17357(13) 0.0351(9) Uani 1 1 d . . . H46A H 0.1206 0.5491 0.1711 0.053 Uiso 1 1 calc R . . H46B H 0.1981 0.4837 0.1750 0.053 Uiso 1 1 calc R . . H46C H 0.2095 0.5597 0.1481 0.053 Uiso 1 1 calc R . . C47 C 0.4054(3) 0.7462(2) 0.24748(17) 0.0461(12) Uani 1 1 d . . . H47A H 0.4362 0.7611 0.2768 0.069 Uiso 1 1 calc R . . H47B H 0.3644 0.7875 0.2346 0.069 Uiso 1 1 calc R . . H47C H 0.4524 0.7361 0.2293 0.069 Uiso 1 1 calc R . . C48 C 0.2786(3) 0.5378(2) 0.33708(13) 0.0350(9) Uani 1 1 d . . . H48A H 0.2145 0.5410 0.3424 0.052 Uiso 1 1 calc R . . H48B H 0.3203 0.5642 0.3604 0.052 Uiso 1 1 calc R . . H48C H 0.2971 0.4841 0.3364 0.052 Uiso 1 1 calc R . . C49 C 0.1694(3) 0.4785(2) 0.25803(13) 0.0294(8) Uani 1 1 d . . . H49A H 0.1989 0.4440 0.2811 0.044 Uiso 1 1 calc R . . H49B H 0.1589 0.4515 0.2301 0.044 Uiso 1 1 calc R . . H49C H 0.1097 0.4962 0.2646 0.044 Uiso 1 1 calc R . . C51 C 0.7286(3) 0.5429(2) 0.20107(13) 0.0306(9) Uani 1 1 d . . . C52 C 0.7921(3) 0.4830(2) 0.20698(15) 0.0375(10) Uani 1 1 d . . . H52 H 0.8003 0.4534 0.1825 0.045 Uiso 1 1 calc R . . C53 C 0.8454(3) 0.4646(3) 0.24855(17) 0.0410(11) Uani 1 1 d . . . C54 C 0.8308(3) 0.5086(3) 0.28344(16) 0.0412(11) Uani 1 1 d . . . H54 H 0.8645 0.4972 0.3116 0.049 Uiso 1 1 calc R . . C55 C 0.7691(3) 0.5685(2) 0.27867(13) 0.0315(9) Uani 1 1 d . . . C56 C 0.6713(3) 0.5612(3) 0.15713(15) 0.0464(12) Uani 1 1 d . . . H56A H 0.6926 0.6095 0.1465 0.070 Uiso 1 1 calc R . . H56B H 0.6056 0.5657 0.1598 0.070 Uiso 1 1 calc R . . H56C H 0.6785 0.5204 0.1365 0.070 Uiso 1 1 calc R . . C57 C 0.9147(4) 0.3988(3) 0.2534(2) 0.0679(18) Uani 1 1 d . . . H57A H 0.9459 0.3951 0.2839 0.102 Uiso 1 1 calc R . . H57B H 0.9611 0.4078 0.2347 0.102 Uiso 1 1 calc R . . H57C H 0.8816 0.3510 0.2448 0.102 Uiso 1 1 calc R . . C58 C 0.7537(4) 0.6175(3) 0.31773(16) 0.0570(14) Uani 1 1 d . . . H58A H 0.6915 0.6075 0.3243 0.086 Uiso 1 1 calc R . . H58B H 0.7589 0.6716 0.3106 0.086 Uiso 1 1 calc R . . H58C H 0.8008 0.6048 0.3432 0.086 Uiso 1 1 calc R . . C59 C 0.6526(4) 0.6514(3) 0.23395(17) 0.0487(12) Uani 1 1 d . . . H59A H 0.6121 0.6463 0.2558 0.073 Uiso 1 1 calc R . . H59B H 0.6145 0.6513 0.2048 0.073 Uiso 1 1 calc R . . H59C H 0.6874 0.6993 0.2386 0.073 Uiso 1 1 calc R . . C61 C 0.8957(3) 0.1296(2) 0.04561(16) 0.0360(10) Uani 1 1 d . . . C62 C 0.8769(3) 0.0885(3) 0.00695(15) 0.0377(10) Uani 1 1 d . . . H62 H 0.8638 0.1148 -0.0200 0.045 Uiso 1 1 calc R . . C63 C 0.8771(3) 0.0088(2) 0.00748(13) 0.0314(9) Uani 1 1 d . . . C64 C 0.8965(3) -0.0275(2) 0.04828(14) 0.0323(9) Uani 1 1 d . . . H64 H 0.8976 -0.0816 0.0498 0.039 Uiso 1 1 calc R . . C65 C 0.9143(3) 0.0162(2) 0.08708(14) 0.0333(9) Uani 1 1 d . . . C66 C 0.8961(4) 0.2175(3) 0.0452(2) 0.0600(15) Uani 1 1 d . . . H66A H 0.8463 0.2366 0.0597 0.090 Uiso 1 1 calc R . . H66B H 0.8859 0.2357 0.0150 0.090 Uiso 1 1 calc R . . H66C H 0.9563 0.2361 0.0606 0.090 Uiso 1 1 calc R . . C67 C 0.8590(3) -0.0372(3) -0.03518(14) 0.0483(12) Uani 1 1 d . . . H67A H 0.8190 -0.0076 -0.0577 0.073 Uiso 1 1 calc R . . H67B H 0.8281 -0.0853 -0.0304 0.073 Uiso 1 1 calc R . . H67C H 0.9183 -0.0479 -0.0446 0.073 Uiso 1 1 calc R . . C68 C 0.9329(4) -0.0206(3) 0.13245(16) 0.0539(13) Uani 1 1 d . . . H68A H 0.9888 0.0021 0.1498 0.081 Uiso 1 1 calc R . . H68B H 0.9424 -0.0755 0.1295 0.081 Uiso 1 1 calc R . . H68C H 0.8795 -0.0118 0.1470 0.081 Uiso 1 1 calc R . . C131 C -0.2299(2) 0.8126(2) 0.17699(10) 0.0183(6) Uani 1 1 d . . . C132 C -0.2012(2) 0.74687(19) 0.15523(10) 0.0166(6) Uani 1 1 d . . . C133 C -0.2669(2) 0.7659(2) 0.11410(11) 0.0230(7) Uani 1 1 d . . . C134 C -0.2968(2) 0.8368(2) 0.13749(11) 0.0211(7) Uani 1 1 d . . . C141 C 0.1564(2) 0.79842(18) 0.16017(10) 0.0156(6) Uani 1 1 d . . . C142 C 0.1013(2) 0.73403(18) 0.14326(10) 0.0148(6) Uani 1 1 d . . . C143 C 0.1387(2) 0.73641(19) 0.10114(11) 0.0193(7) Uani 1 1 d . . . C144 C 0.1966(2) 0.8070(2) 0.11928(11) 0.0206(7) Uani 1 1 d . . . C231 C -0.0862(2) 0.75107(19) 0.36570(10) 0.0164(6) Uani 1 1 d . . . C232 C -0.1394(2) 0.81528(19) 0.34604(10) 0.0169(6) Uani 1 1 d . . . C233 C -0.1755(2) 0.8326(2) 0.38708(11) 0.0202(7) Uani 1 1 d . . . C234 C -0.1214(3) 0.7618(2) 0.40766(11) 0.0217(7) Uani 1 1 d . . . C241 C 0.2537(2) 0.80790(18) 0.32618(10) 0.0173(6) Uani 1 1 d . . . C242 C 0.2223(2) 0.74640(19) 0.35028(10) 0.0176(6) Uani 1 1 d . . . C243 C 0.3054(3) 0.7541(2) 0.38643(12) 0.0246(7) Uani 1 1 d . . . C244 C 0.3378(3) 0.8212(2) 0.36046(12) 0.0246(7) 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 Mo1 0.01307(12) 0.01122(12) 0.01287(12) -0.00021(9) 0.00360(9) -0.00075(10) Mo2 0.01460(13) 0.01194(12) 0.01277(12) 0.00210(10) 0.00399(9) 0.00218(10) Mo3 0.01754(13) 0.01300(13) 0.01123(11) 0.00115(10) 0.00393(10) 0.00399(10) Mo4 0.01665(13) 0.01142(12) 0.01220(12) -0.00096(9) 0.00386(10) -0.00203(10) O1 0.0196(12) 0.0112(11) 0.0225(12) 0.0006(9) 0.0057(9) -0.0014(9) O2 0.0228(12) 0.0149(11) 0.0192(11) 0.0046(9) 0.0044(9) 0.0031(9) O3 0.0255(13) 0.0172(12) 0.0188(11) 0.0017(9) 0.0060(9) 0.0054(10) O4 0.0258(13) 0.0175(12) 0.0177(11) 0.0009(9) 0.0044(9) -0.0038(10) O5 0.0149(11) 0.0160(11) 0.0154(11) 0.0019(8) 0.0035(9) -0.0004(9) O6 0.0149(11) 0.0138(11) 0.0142(10) -0.0005(8) 0.0045(8) -0.0006(8) O7 0.0175(11) 0.0117(10) 0.0135(10) -0.0002(8) 0.0047(8) -0.0005(8) O8 0.0156(11) 0.0155(11) 0.0143(10) -0.0012(9) 0.0020(8) 0.0014(9) O9 0.065(2) 0.0420(19) 0.0401(18) -0.0023(15) 0.0081(17) 0.0105(17) O10 0.078(3) 0.090(3) 0.074(3) -0.012(2) -0.008(2) 0.031(3) O131 0.0171(11) 0.0274(13) 0.0154(11) 0.0004(9) 0.0025(9) 0.0055(10) O132 0.0173(11) 0.0206(12) 0.0196(11) -0.0036(9) 0.0008(9) 0.0009(9) O133 0.0377(16) 0.0416(17) 0.0228(14) -0.0064(12) -0.0075(12) 0.0037(13) O134 0.0300(14) 0.0334(15) 0.0263(13) 0.0067(11) 0.0000(11) 0.0131(12) O141 0.0216(12) 0.0209(12) 0.0163(11) -0.0047(9) 0.0071(9) -0.0064(9) O142 0.0192(11) 0.0164(11) 0.0159(10) -0.0032(9) 0.0059(9) -0.0052(9) O143 0.0336(15) 0.0295(15) 0.0205(12) -0.0070(10) 0.0115(11) -0.0042(11) O144 0.0421(16) 0.0324(15) 0.0279(14) -0.0029(11) 0.0204(12) -0.0158(13) O231 0.0237(12) 0.0206(12) 0.0159(11) 0.0063(9) 0.0095(9) 0.0064(9) O232 0.0217(12) 0.0263(13) 0.0156(11) 0.0049(9) 0.0074(9) 0.0080(10) O233 0.0322(14) 0.0304(14) 0.0209(12) -0.0012(10) 0.0112(11) 0.0091(11) O234 0.0506(18) 0.0322(16) 0.0207(13) 0.0086(11) 0.0168(12) 0.0086(13) O241 0.0193(12) 0.0228(12) 0.0176(11) -0.0002(9) 0.0040(9) -0.0036(9) O242 0.0211(12) 0.0179(12) 0.0172(11) 0.0024(9) 0.0022(9) 0.0039(9) O243 0.0438(18) 0.0380(17) 0.0280(15) 0.0042(12) -0.0147(13) 0.0024(14) O244 0.0297(15) 0.0313(16) 0.0480(18) -0.0049(13) -0.0075(13) -0.0067(12) N1 0.0264(16) 0.0248(16) 0.0318(17) -0.0032(13) 0.0087(13) 0.0017(13) N2 0.0190(14) 0.0157(14) 0.0217(14) -0.0033(11) 0.0065(11) -0.0024(11) N3 0.0178(13) 0.0181(14) 0.0185(13) -0.0012(11) 0.0045(11) -0.0011(11) N4 0.0204(15) 0.0178(15) 0.0392(18) -0.0011(13) 0.0106(13) 0.0070(12) N5 0.0299(17) 0.0223(16) 0.0385(19) 0.0016(14) 0.0062(14) -0.0085(13) N6 0.0280(18) 0.0319(19) 0.047(2) -0.0106(16) 0.0101(16) -0.0044(14) C9 0.047(3) 0.054(3) 0.061(3) -0.003(3) 0.008(2) 0.014(2) C10 0.100(6) 0.085(5) 0.096(5) -0.001(4) 0.014(4) 0.022(4) C11 0.029(2) 0.027(2) 0.040(2) -0.0135(17) 0.0150(17) -0.0018(16) C12 0.026(2) 0.046(3) 0.0256(19) -0.0108(17) 0.0062(15) 0.0004(17) C13 0.0223(19) 0.042(2) 0.033(2) 0.0054(18) 0.0056(16) 0.0087(17) C14 0.036(2) 0.0174(18) 0.047(2) -0.0029(17) 0.0091(19) 0.0032(16) C15 0.0272(19) 0.0244(19) 0.0289(19) -0.0099(15) 0.0027(15) 0.0024(15) C16 0.055(3) 0.028(2) 0.053(3) -0.016(2) 0.021(2) -0.011(2) C17 0.049(3) 0.069(4) 0.054(3) 0.027(3) 0.011(2) 0.021(3) C18 0.050(3) 0.046(3) 0.040(2) -0.021(2) 0.009(2) -0.001(2) C21 0.0159(15) 0.0248(18) 0.0212(16) -0.0011(13) 0.0044(13) -0.0034(13) C22 0.0192(17) 0.0230(18) 0.0229(17) 0.0037(14) -0.0012(13) -0.0010(13) C23 0.0199(17) 0.0194(17) 0.0251(17) -0.0016(13) -0.0008(14) -0.0036(13) C24 0.0214(17) 0.0244(18) 0.0185(16) -0.0057(13) -0.0004(13) -0.0009(14) C25 0.0141(15) 0.0216(17) 0.0224(16) -0.0053(13) 0.0035(13) -0.0012(12) C26 0.0285(19) 0.029(2) 0.0188(16) -0.0018(14) 0.0087(14) -0.0031(15) C27 0.041(2) 0.0200(19) 0.036(2) -0.0037(16) -0.0113(18) 0.0011(17) C28 0.0223(17) 0.0238(18) 0.0212(17) -0.0036(14) -0.0007(13) 0.0017(14) C29 0.032(2) 0.0211(18) 0.0226(17) -0.0036(14) 0.0123(15) -0.0013(15) C31 0.0150(15) 0.0199(17) 0.0210(16) -0.0016(13) 0.0053(12) -0.0026(12) C32 0.0202(17) 0.0206(17) 0.0208(16) 0.0017(13) 0.0028(13) -0.0001(13) C33 0.0181(16) 0.0190(17) 0.0259(17) -0.0020(13) 0.0014(13) -0.0020(13) C34 0.0217(17) 0.0234(18) 0.0187(16) -0.0041(13) -0.0008(13) 0.0022(14) C35 0.0138(15) 0.0242(18) 0.0196(16) 0.0002(13) 0.0021(12) 0.0005(13) C36 0.0310(19) 0.0223(18) 0.0154(15) -0.0030(13) 0.0073(14) -0.0040(14) C37 0.033(2) 0.0193(18) 0.031(2) -0.0046(15) -0.0023(16) -0.0020(15) C38 0.0248(18) 0.029(2) 0.0208(17) -0.0005(14) 0.0028(14) -0.0052(15) C39 0.0253(18) 0.0184(17) 0.0261(18) -0.0015(14) 0.0087(14) -0.0003(14) C41 0.0249(19) 0.025(2) 0.040(2) -0.0031(17) 0.0121(17) 0.0083(15) C42 0.034(2) 0.026(2) 0.044(2) 0.0016(17) 0.0171(18) 0.0068(17) C43 0.027(2) 0.0215(19) 0.051(2) -0.0058(17) 0.0160(18) 0.0038(15) C44 0.0255(19) 0.0236(19) 0.044(2) -0.0083(17) 0.0101(17) 0.0024(15) C45 0.0248(19) 0.0185(18) 0.040(2) -0.0048(15) 0.0114(16) 0.0074(14) C46 0.037(2) 0.029(2) 0.040(2) -0.0059(18) 0.0094(18) 0.0074(18) C47 0.042(3) 0.029(2) 0.075(3) -0.005(2) 0.030(2) -0.0078(19) C48 0.039(2) 0.029(2) 0.039(2) -0.0005(17) 0.0114(18) 0.0081(18) C49 0.0243(19) 0.0212(18) 0.043(2) -0.0011(16) 0.0073(17) 0.0000(15) C51 0.033(2) 0.030(2) 0.031(2) -0.0034(16) 0.0123(17) -0.0204(17) C52 0.039(2) 0.028(2) 0.053(3) -0.0079(19) 0.028(2) -0.0180(18) C53 0.031(2) 0.033(2) 0.063(3) 0.008(2) 0.018(2) -0.0134(18) C54 0.026(2) 0.044(3) 0.051(3) 0.014(2) 0.0022(19) -0.0165(19) C55 0.029(2) 0.034(2) 0.032(2) 0.0024(17) 0.0056(16) -0.0171(17) C56 0.049(3) 0.045(3) 0.045(3) 0.002(2) 0.009(2) -0.020(2) C57 0.048(3) 0.040(3) 0.121(5) 0.025(3) 0.030(3) 0.004(2) C58 0.073(4) 0.061(3) 0.039(3) -0.009(2) 0.014(3) -0.025(3) C59 0.053(3) 0.031(2) 0.063(3) 0.001(2) 0.012(2) 0.006(2) C61 0.029(2) 0.0199(19) 0.062(3) 0.0040(19) 0.016(2) 0.0004(16) C62 0.029(2) 0.041(3) 0.044(2) 0.012(2) 0.0093(19) -0.0008(18) C63 0.0195(18) 0.038(2) 0.037(2) -0.0036(18) 0.0054(16) -0.0021(16) C64 0.028(2) 0.0188(18) 0.050(3) 0.0004(17) 0.0063(18) -0.0008(15) C65 0.032(2) 0.030(2) 0.038(2) 0.0017(17) 0.0061(17) -0.0031(17) C66 0.056(3) 0.030(3) 0.099(4) 0.007(3) 0.028(3) -0.004(2) C67 0.027(2) 0.079(4) 0.039(3) -0.014(2) 0.0051(19) -0.005(2) C68 0.058(3) 0.057(3) 0.043(3) 0.011(2) -0.001(2) -0.001(3) C131 0.0135(15) 0.0229(17) 0.0187(15) 0.0032(13) 0.0038(12) 0.0001(13) C132 0.0136(15) 0.0199(16) 0.0162(15) 0.0010(12) 0.0023(12) -0.0022(12) C133 0.0224(18) 0.0264(19) 0.0184(16) 0.0006(13) -0.0009(13) 0.0001(14) C134 0.0176(16) 0.0252(18) 0.0202(16) 0.0047(13) 0.0020(13) 0.0006(13) C141 0.0171(15) 0.0153(15) 0.0151(14) -0.0008(11) 0.0043(12) 0.0010(12) C142 0.0160(15) 0.0149(15) 0.0143(14) 0.0002(11) 0.0050(12) 0.0004(11) C143 0.0216(17) 0.0212(17) 0.0165(15) -0.0011(12) 0.0069(13) 0.0015(13) C144 0.0221(17) 0.0243(18) 0.0170(15) -0.0023(13) 0.0078(13) -0.0027(14) C231 0.0180(15) 0.0176(15) 0.0141(14) 0.0000(12) 0.0043(12) 0.0008(12) C232 0.0166(15) 0.0197(16) 0.0158(14) -0.0010(12) 0.0070(12) 0.0015(13) C233 0.0222(17) 0.0232(18) 0.0171(15) -0.0006(12) 0.0085(13) 0.0006(13) C234 0.0271(18) 0.0224(18) 0.0175(16) 0.0010(13) 0.0093(14) 0.0023(14) C241 0.0160(15) 0.0155(15) 0.0202(15) -0.0042(12) 0.0028(12) 0.0024(12) C242 0.0198(16) 0.0181(16) 0.0145(14) -0.0034(12) 0.0014(12) 0.0039(13) C243 0.0262(19) 0.0236(18) 0.0214(17) -0.0038(14) -0.0029(14) 0.0044(15) C244 0.0235(18) 0.0203(17) 0.0273(18) -0.0072(14) -0.0030(14) 0.0030(14) _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 O1 1.677(2) . ? Mo1 O5 1.968(2) . ? Mo1 O6 1.971(2) . ? Mo1 O142 2.052(2) . ? Mo1 O132 2.067(2) . ? Mo1 O7 2.354(2) . ? Mo1 Mo2 2.5904(4) . ? Mo2 O2 1.676(2) . ? Mo2 O5 1.971(2) . ? Mo2 O6 1.973(2) . ? Mo2 O242 2.055(2) . ? Mo2 O231 2.059(2) . ? Mo2 O8 2.342(2) . ? Mo3 O3 1.672(2) . ? Mo3 O8 1.980(2) . ? Mo3 O7 1.983(2) . ? Mo3 O131 2.030(2) . ? Mo3 O232 2.034(2) . ? Mo3 O5 2.429(2) . ? Mo3 Mo4 2.5932(4) . ? Mo4 O4 1.673(2) . ? Mo4 O7 1.978(2) . ? Mo4 O8 1.978(2) . ? Mo4 O241 2.050(2) . ? Mo4 O141 2.051(2) . ? Mo4 O6 2.379(2) . ? O9 C9 1.413(5) . ? O9 H9 0.8200 . ? O10 C10 1.422(7) . ? O10 H10 0.8200 . ? O131 C131 1.288(4) . ? O132 C132 1.283(4) . ? O133 C133 1.223(4) . ? O134 C134 1.225(4) . ? O141 C141 1.294(4) . ? O142 C142 1.281(4) . ? O143 C143 1.218(4) . ? O144 C144 1.214(4) . ? O231 C231 1.272(4) . ? O232 C232 1.282(4) . ? O233 C233 1.220(4) . ? O234 C234 1.220(4) . ? O241 C241 1.283(4) . ? O242 C242 1.279(4) . ? O243 C243 1.216(4) . ? O244 C244 1.216(4) . ? N1 C15 1.343(5) . ? N1 C11 1.364(5) . ? N2 C21 1.367(4) . ? N2 C25 1.376(4) . ? N2 C29 1.476(4) . ? N3 C31 1.370(4) . ? N3 C35 1.374(4) . ? N3 C39 1.476(4) . ? N4 C45 1.362(5) . ? N4 C41 1.372(5) . ? N4 C49 1.476(5) . ? N5 C55 1.363(5) . ? N5 C51 1.386(5) . ? N5 C59 1.443(5) . ? N6 C65 1.351(5) . ? N6 C61 1.360(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.375(6) . ? C11 C16 1.494(5) . ? C12 C13 1.372(6) . ? C12 H12 0.9300 . ? C13 C14 1.382(6) . ? C13 C17 1.503(6) . ? C14 C15 1.383(5) . ? C14 H14 0.9300 . ? C15 C18 1.499(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C22 1.377(5) . ? C21 C26 1.488(5) . ? C22 C23 1.390(5) . ? C22 H22 0.9300 . ? C23 C24 1.384(5) . ? C23 C27 1.494(5) . ? C24 C25 1.374(5) . ? C24 H24 0.9300 . ? C25 C28 1.494(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C32 1.372(4) . ? C31 C36 1.488(4) . ? C32 C33 1.386(5) . ? C32 H32 0.9300 . ? C33 C34 1.386(5) . ? C33 C37 1.492(5) . ? C34 C35 1.376(5) . ? C34 H34 0.9300 . ? C35 C38 1.496(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C41 C42 1.364(5) . ? C41 C46 1.489(5) . ? C42 C43 1.383(6) . ? C42 H42 0.9300 . ? C43 C44 1.373(6) . ? C43 C47 1.510(5) . ? C44 C45 1.371(5) . ? C44 H44 0.9300 . ? C45 C48 1.501(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C51 C52 1.363(6) . ? C51 C56 1.478(6) . ? C52 C53 1.398(6) . ? C52 H52 0.9300 . ? C53 C54 1.352(6) . ? C53 C57 1.493(6) . ? C54 C55 1.346(6) . ? C54 H54 0.9300 . ? C55 C58 1.508(6) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 C62 1.361(6) . ? C61 C66 1.511(6) . ? C62 C63 1.370(6) . ? C62 H62 0.9300 . ? C63 C64 1.378(6) . ? C63 C67 1.507(6) . ? C64 C65 1.388(6) . ? C64 H64 0.9300 . ? C65 C68 1.504(6) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C131 C132 1.407(5) . ? C131 C134 1.463(4) . ? C132 C133 1.468(4) . ? C133 C134 1.511(5) . ? C141 C142 1.403(4) . ? C141 C144 1.470(4) . ? C142 C143 1.478(4) . ? C143 C144 1.517(5) . ? C231 C232 1.413(4) . ? C231 C234 1.468(4) . ? C232 C233 1.467(4) . ? C233 C234 1.516(5) . ? C241 C242 1.405(5) . ? C241 C244 1.467(4) . ? C242 C243 1.478(4) . ? C243 C244 1.518(5) . ? 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 O1 Mo1 O5 107.70(10) . . ? O1 Mo1 O6 107.31(10) . . ? O5 Mo1 O6 90.60(8) . . ? O1 Mo1 O142 91.62(10) . . ? O5 Mo1 O142 159.51(9) . . ? O6 Mo1 O142 90.06(8) . . ? O1 Mo1 O132 92.46(10) . . ? O5 Mo1 O132 90.31(9) . . ? O6 Mo1 O132 158.90(9) . . ? O142 Mo1 O132 81.89(9) . . ? O1 Mo1 O7 173.20(9) . . ? O5 Mo1 O7 77.38(8) . . ? O6 Mo1 O7 76.76(8) . . ? O142 Mo1 O7 82.84(8) . . ? O132 Mo1 O7 82.88(8) . . ? O1 Mo1 Mo2 94.29(8) . . ? O5 Mo1 Mo2 48.94(6) . . ? O6 Mo1 Mo2 48.98(6) . . ? O142 Mo1 Mo2 138.41(6) . . ? O132 Mo1 Mo2 138.72(6) . . ? O7 Mo1 Mo2 92.47(5) . . ? O2 Mo2 O5 107.82(10) . . ? O2 Mo2 O6 107.42(10) . . ? O5 Mo2 O6 90.45(8) . . ? O2 Mo2 O242 91.46(10) . . ? O5 Mo2 O242 159.29(9) . . ? O6 Mo2 O242 90.89(9) . . ? O2 Mo2 O231 91.86(10) . . ? O5 Mo2 O231 90.16(9) . . ? O6 Mo2 O231 159.50(9) . . ? O242 Mo2 O231 81.51(9) . . ? O2 Mo2 O8 173.28(9) . . ? O5 Mo2 O8 77.16(8) . . ? O6 Mo2 O8 76.64(8) . . ? O242 Mo2 O8 83.05(8) . . ? O231 Mo2 O8 83.53(8) . . ? O2 Mo2 Mo1 94.50(8) . . ? O5 Mo2 Mo1 48.84(6) . . ? O6 Mo2 Mo1 48.91(6) . . ? O242 Mo2 Mo1 139.21(6) . . ? O231 Mo2 Mo1 138.38(7) . . ? O8 Mo2 Mo1 92.19(5) . . ? O3 Mo3 O8 108.35(10) . . ? O3 Mo3 O7 107.99(10) . . ? O8 Mo3 O7 89.12(9) . . ? O3 Mo3 O131 94.98(10) . . ? O8 Mo3 O131 156.12(9) . . ? O7 Mo3 O131 88.46(9) . . ? O3 Mo3 O232 94.12(10) . . ? O8 Mo3 O232 88.72(9) . . ? O7 Mo3 O232 157.29(9) . . ? O131 Mo3 O232 84.46(9) . . ? O3 Mo3 O5 175.18(9) . . ? O8 Mo3 O5 74.92(8) . . ? O7 Mo3 O5 75.31(8) . . ? O131 Mo3 O5 81.49(8) . . ? O232 Mo3 O5 82.31(8) . . ? O3 Mo3 Mo4 92.92(8) . . ? O8 Mo3 Mo4 49.04(6) . . ? O7 Mo3 Mo4 49.01(6) . . ? O131 Mo3 Mo4 136.94(6) . . ? O232 Mo3 Mo4 137.04(7) . . ? O5 Mo3 Mo4 91.89(5) . . ? O4 Mo4 O7 108.26(10) . . ? O4 Mo4 O8 108.12(10) . . ? O7 Mo4 O8 89.35(8) . . ? O4 Mo4 O241 92.38(10) . . ? O7 Mo4 O241 158.71(9) . . ? O8 Mo4 O241 89.06(9) . . ? O4 Mo4 O141 92.17(10) . . ? O7 Mo4 O141 89.50(8) . . ? O8 Mo4 O141 158.95(9) . . ? O241 Mo4 O141 84.47(9) . . ? O4 Mo4 O6 174.03(10) . . ? O7 Mo4 O6 76.05(8) . . ? O8 Mo4 O6 75.68(8) . . ? O241 Mo4 O6 82.99(8) . . ? O141 Mo4 O6 83.65(8) . . ? O4 Mo4 Mo3 92.92(8) . . ? O7 Mo4 Mo3 49.20(6) . . ? O8 Mo4 Mo3 49.11(6) . . ? O241 Mo4 Mo3 137.18(6) . . ? O141 Mo4 Mo3 137.67(6) . . ? O6 Mo4 Mo3 93.04(5) . . ? Mo1 O5 Mo2 82.22(8) . . ? Mo1 O5 Mo3 102.42(9) . . ? Mo2 O5 Mo3 102.42(9) . . ? Mo1 O6 Mo2 82.11(8) . . ? Mo1 O6 Mo4 103.14(9) . . ? Mo2 O6 Mo4 103.16(9) . . ? Mo4 O7 Mo3 81.78(8) . . ? Mo4 O7 Mo1 103.80(9) . . ? Mo3 O7 Mo1 104.62(9) . . ? Mo4 O8 Mo3 81.85(8) . . ? Mo4 O8 Mo2 104.30(9) . . ? Mo3 O8 Mo2 105.25(9) . . ? C9 O9 H9 109.5 . . ? C10 O10 H10 109.5 . . ? C131 O131 Mo3 129.4(2) . . ? C132 O132 Mo1 132.0(2) . . ? C141 O141 Mo4 133.2(2) . . ? C142 O142 Mo1 135.5(2) . . ? C231 O231 Mo2 134.0(2) . . ? C232 O232 Mo3 133.5(2) . . ? C241 O241 Mo4 133.9(2) . . ? C242 O242 Mo2 134.7(2) . . ? C15 N1 C11 117.4(3) . . ? C21 N2 C25 121.4(3) . . ? C21 N2 C29 120.8(3) . . ? C25 N2 C29 117.8(3) . . ? C31 N3 C35 120.8(3) . . ? C31 N3 C39 121.6(3) . . ? C35 N3 C39 117.6(3) . . ? C45 N4 C41 120.8(3) . . ? C45 N4 C49 119.6(3) . . ? C41 N4 C49 119.5(3) . . ? C55 N5 C51 119.9(4) . . ? C55 N5 C59 119.4(4) . . ? C51 N5 C59 120.7(4) . . ? C65 N6 C61 117.2(4) . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O10 C10 H10A 109.5 . . ? O10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O10 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 122.0(4) . . ? N1 C11 C16 116.8(4) . . ? C12 C11 C16 121.2(4) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 117.2(4) . . ? C12 C13 C17 121.4(4) . . ? C14 C13 C17 121.4(4) . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N1 C15 C14 122.1(3) . . ? N1 C15 C18 116.0(4) . . ? C14 C15 C18 121.9(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C21 C22 118.7(3) . . ? N2 C21 C26 119.9(3) . . ? C22 C21 C26 121.4(3) . . ? C21 C22 C23 122.0(3) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C22 117.2(3) . . ? C24 C23 C27 120.6(3) . . ? C22 C23 C27 122.2(3) . . ? C25 C24 C23 121.8(3) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 N2 118.9(3) . . ? C24 C25 C28 122.2(3) . . ? N2 C25 C28 118.8(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 109.5 . . ? N2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C31 C32 118.9(3) . . ? N3 C31 C36 119.4(3) . . ? C32 C31 C36 121.7(3) . . ? C31 C32 C33 122.5(3) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C34 C33 C32 116.6(3) . . ? C34 C33 C37 121.0(3) . . ? C32 C33 C37 122.3(3) . . ? C35 C34 C33 122.0(3) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? N3 C35 C34 119.1(3) . . ? N3 C35 C38 119.2(3) . . ? C34 C35 C38 121.6(3) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 H39A 109.5 . . ? N3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 N4 119.1(4) . . ? C42 C41 C46 121.3(4) . . ? N4 C41 C46 119.5(4) . . ? C41 C42 C43 121.8(4) . . ? C41 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C44 C43 C42 117.0(4) . . ? C44 C43 C47 122.1(4) . . ? C42 C43 C47 120.9(4) . . ? C45 C44 C43 122.3(4) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? N4 C45 C44 118.8(4) . . ? N4 C45 C48 119.2(3) . . ? C44 C45 C48 122.0(4) . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N4 C49 H49A 109.5 . . ? N4 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N4 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 N5 117.9(4) . . ? C52 C51 C56 122.1(4) . . ? N5 C51 C56 120.1(4) . . ? C51 C52 C53 122.4(4) . . ? C51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C54 C53 C52 117.0(4) . . ? C54 C53 C57 122.4(5) . . ? C52 C53 C57 120.6(5) . . ? C55 C54 C53 122.0(4) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C54 C55 N5 120.7(4) . . ? C54 C55 C58 121.7(4) . . ? N5 C55 C58 117.6(4) . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N5 C59 H59A 109.5 . . ? N5 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N5 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C61 C62 122.7(4) . . ? N6 C61 C66 116.5(4) . . ? C62 C61 C66 120.8(4) . . ? C61 C62 C63 120.5(4) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C62 C63 C64 117.6(4) . . ? C62 C63 C67 121.0(4) . . ? C64 C63 C67 121.4(4) . . ? C63 C64 C65 120.3(4) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? N6 C65 C64 121.6(4) . . ? N6 C65 C68 116.0(4) . . ? C64 C65 C68 122.4(4) . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C63 C67 H67A 109.5 . . ? C63 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C63 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O131 C131 C132 134.4(3) . . ? O131 C131 C134 133.1(3) . . ? C132 C131 C134 92.4(3) . . ? O132 C132 C131 135.9(3) . . ? O132 C132 C133 132.5(3) . . ? C131 C132 C133 91.7(3) . . ? O133 C133 C132 136.7(3) . . ? O133 C133 C134 135.2(3) . . ? C132 C133 C134 88.1(3) . . ? O134 C134 C131 136.9(3) . . ? O134 C134 C133 135.3(3) . . ? C131 C134 C133 87.8(3) . . ? O141 C141 C142 136.1(3) . . ? O141 C141 C144 131.4(3) . . ? C142 C141 C144 92.5(3) . . ? O142 C142 C141 136.5(3) . . ? O142 C142 C143 131.6(3) . . ? C141 C142 C143 91.9(3) . . ? O143 C143 C142 135.8(3) . . ? O143 C143 C144 136.4(3) . . ? C142 C143 C144 87.8(2) . . ? O144 C144 C141 136.5(3) . . ? O144 C144 C143 135.7(3) . . ? C141 C144 C143 87.8(2) . . ? O231 C231 C232 136.7(3) . . ? O231 C231 C234 131.4(3) . . ? C232 C231 C234 91.8(3) . . ? O232 C232 C231 135.9(3) . . ? O232 C232 C233 131.8(3) . . ? C231 C232 C233 92.2(3) . . ? O233 C233 C232 136.1(3) . . ? O233 C233 C234 136.0(3) . . ? C232 C233 C234 87.8(3) . . ? O234 C234 C231 135.9(3) . . ? O234 C234 C233 136.0(3) . . ? C231 C234 C233 88.1(2) . . ? O241 C241 C242 135.9(3) . . ? O241 C241 C244 131.8(3) . . ? C242 C241 C244 92.3(3) . . ? O242 C242 C241 136.6(3) . . ? O242 C242 C243 131.3(3) . . ? C241 C242 C243 92.1(3) . . ? O243 C243 C242 136.1(4) . . ? O243 C243 C244 136.4(3) . . ? C242 C243 C244 87.5(3) . . ? O244 C244 C241 137.0(4) . . ? O244 C244 C243 134.9(3) . . ? C241 C244 C243 88.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.949 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.132 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 219869' _chemical_name_common ;Tetracollidinium N-ethylpyridinium octaoxotetrasquaratotetramolybdate(V) bromide ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetracollidinium N-ethylpyridinium octaoxotetrasquaratotetramolybdate(V) bromide ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H58 Br Mo4 N5 O24' _chemical_formula_weight 1636.73 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' Mo Mo -1.6832 0.6857 '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' Br Br -0.2901 2.4595 '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/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.05280(10) _cell_length_b 22.6688(2) _cell_length_c 12.1180(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.0427(4) _cell_angle_gamma 90.00 _cell_volume 3019.34(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 1.560 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10451 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5462 _reflns_number_gt 4925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0253P)^2^+4.9927P] 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 5462 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.00502(3) 0.7500 0.13314(3) 0.01214(9) Uani 1 2 d S . . Mo2 Mo -0.15178(3) 0.7500 -0.04866(3) 0.01284(9) Uani 1 2 d S . . Mo3 Mo 0.127867(19) 0.692573(10) -0.086630(18) 0.01266(7) Uani 1 1 d . . . Br Br -0.46929(5) 0.7500 0.35589(4) 0.03865(13) Uani 1 2 d S . . O1 O -0.1179(2) 0.7500 0.2151(2) 0.0159(5) Uani 1 2 d S . . O2 O -0.2754(2) 0.7500 0.0204(2) 0.0173(6) Uani 1 2 d S . . O3 O 0.24451(16) 0.68726(8) -0.16399(16) 0.0192(4) Uani 1 1 d . . . O4 O 0.1703(2) 0.7500 0.0340(2) 0.0132(5) Uani 1 2 d S . . O5 O 0.0108(2) 0.7500 -0.1600(2) 0.0148(5) Uani 1 2 d S . . O6 O -0.04104(16) 0.68833(8) 0.01938(15) 0.0147(4) Uani 1 1 d . . . O131 O 0.19273(17) 0.62615(8) 0.01742(15) 0.0184(4) Uani 1 1 d . . . O132 O 0.09314(16) 0.68997(8) 0.23323(15) 0.0176(4) Uani 1 1 d . . . O133 O 0.27463(18) 0.61223(9) 0.39534(16) 0.0231(4) Uani 1 1 d . . . O134 O 0.38243(17) 0.55154(9) 0.17786(16) 0.0234(4) Uani 1 1 d . . . O231 O -0.22483(17) 0.68989(8) -0.16313(16) 0.0194(4) Uani 1 1 d . . . O232 O 0.03676(16) 0.62374(8) -0.16976(15) 0.0187(4) Uani 1 1 d . . . O233 O -0.09980(18) 0.50892(9) -0.27700(17) 0.0258(5) Uani 1 1 d . . . O234 O -0.36203(17) 0.57681(9) -0.27441(17) 0.0251(5) Uani 1 1 d . . . N1 N 0.4146(2) 0.49289(10) 0.69904(18) 0.0168(5) Uani 1 1 d . . . H1 H 0.4817 0.4788 0.7309 0.020 Uiso 1 1 calc R . . N2 N -0.3197(2) 0.65300(10) 0.2241(2) 0.0221(5) Uani 1 1 d . . . H2 H -0.3595 0.6780 0.2595 0.027 Uiso 1 1 calc R . . N3 N 0.6817(3) 0.2500 0.4358(3) 0.0213(7) Uani 1 2 d S . . C11 C 0.3545(2) 0.53306(12) 0.7545(2) 0.0187(6) Uani 1 1 d . . . C12 C 0.2473(2) 0.55583(12) 0.7037(2) 0.0205(6) Uani 1 1 d . . . H12 H 0.2038 0.5830 0.7413 0.025 Uiso 1 1 calc R . . C13 C 0.2035(2) 0.53871(12) 0.5966(2) 0.0181(6) Uani 1 1 d . . . C14 C 0.2691(2) 0.49699(12) 0.5436(2) 0.0187(6) Uani 1 1 d . . . H14 H 0.2413 0.4847 0.4722 0.022 Uiso 1 1 calc R . . C15 C 0.3753(2) 0.47361(12) 0.5962(2) 0.0182(6) Uani 1 1 d . . . C16 C 0.4090(3) 0.55133(14) 0.8676(2) 0.0267(7) Uani 1 1 d . . . H16A H 0.4557 0.5193 0.9019 0.040 Uiso 1 1 calc R . . H16B H 0.3452 0.5616 0.9121 0.040 Uiso 1 1 calc R . . H16C H 0.4609 0.5848 0.8613 0.040 Uiso 1 1 calc R . . C17 C 0.0881(2) 0.56463(13) 0.5410(3) 0.0247(6) Uani 1 1 d . . . H17A H 0.0809 0.5553 0.4633 0.037 Uiso 1 1 calc R . . H17B H 0.0896 0.6067 0.5504 0.037 Uiso 1 1 calc R . . H17C H 0.0199 0.5485 0.5738 0.037 Uiso 1 1 calc R . . C18 C 0.4508(3) 0.42789(13) 0.5462(2) 0.0249(6) Uani 1 1 d . . . H18A H 0.5353 0.4382 0.5602 0.037 Uiso 1 1 calc R . . H18B H 0.4281 0.4260 0.4676 0.037 Uiso 1 1 calc R . . H18C H 0.4374 0.3902 0.5787 0.037 Uiso 1 1 calc R . . C21 C -0.3662(3) 0.63759(13) 0.1208(2) 0.0217(6) Uani 1 1 d . . . C22 C -0.3029(3) 0.59688(13) 0.0647(2) 0.0246(6) Uani 1 1 d . . . H22 H -0.3332 0.5853 -0.0065 0.029 Uiso 1 1 calc R . . C23 C -0.1941(3) 0.57290(13) 0.1134(3) 0.0260(7) Uani 1 1 d . . . C24 C -0.1516(3) 0.59063(13) 0.2198(3) 0.0259(7) Uani 1 1 d . . . H24 H -0.0796 0.5747 0.2539 0.031 Uiso 1 1 calc R . . C25 C -0.2137(3) 0.63138(13) 0.2758(2) 0.0239(6) Uani 1 1 d . . . C26 C -0.4833(3) 0.66566(13) 0.0734(3) 0.0269(7) Uani 1 1 d . . . H26A H -0.5124 0.6914 0.1277 0.040 Uiso 1 1 calc R . . H26B H -0.5428 0.6355 0.0538 0.040 Uiso 1 1 calc R . . H26C H -0.4697 0.6880 0.0086 0.040 Uiso 1 1 calc R . . C27 C -0.1236(3) 0.52957(15) 0.0516(3) 0.0375(8) Uani 1 1 d . . . H27A H -0.0513 0.5481 0.0309 0.056 Uiso 1 1 calc R . . H27B H -0.1729 0.5166 -0.0139 0.056 Uiso 1 1 calc R . . H27C H -0.1017 0.4962 0.0984 0.056 Uiso 1 1 calc R . . C28 C -0.1721(3) 0.65409(15) 0.3889(3) 0.0340(8) Uani 1 1 d . . . H28A H -0.2279 0.6836 0.4093 0.051 Uiso 1 1 calc R . . H28B H -0.0925 0.6711 0.3890 0.051 Uiso 1 1 calc R . . H28C H -0.1691 0.6222 0.4413 0.051 Uiso 1 1 calc R . . C31 C 0.6309(3) 0.30174(13) 0.4027(2) 0.0249(7) Uani 1 1 d . . . H31 H 0.6666 0.3370 0.4284 0.030 Uiso 1 1 calc R . . C32 C 0.5260(3) 0.30258(15) 0.3310(3) 0.0329(8) Uani 1 1 d . . . H32 H 0.4909 0.3382 0.3068 0.039 Uiso 1 1 calc R . . C33 C 0.4736(4) 0.2500 0.2954(4) 0.0391(12) Uani 1 2 d S . . H33 H 0.4025 0.2500 0.2471 0.047 Uiso 1 2 calc SR . . C34 C 0.7999(4) 0.2500 0.5076(4) 0.0335(11) Uani 1 2 d S . . H34A H 0.8050 0.2153 0.5548 0.040 Uiso 0.50 1 calc PR . . H34B H 0.8050 0.2847 0.5548 0.040 Uiso 0.50 1 calc PR . . C35 C 0.9047(4) 0.2500 0.4357(5) 0.0398(12) Uani 1 2 d S . . H35A H 0.8998 0.2155 0.3895 0.060 Uiso 0.50 1 calc PR . . H35B H 0.9806 0.2499 0.4823 0.060 Uiso 1 2 calc SR . . H35C H 0.9001 0.2846 0.3899 0.060 Uiso 0.50 1 calc PR . . C131 C 0.2155(2) 0.62295(11) 0.1240(2) 0.0154(5) Uani 1 1 d . . . C132 C 0.1715(2) 0.65019(11) 0.2162(2) 0.0155(5) Uani 1 1 d . . . C133 C 0.2544(2) 0.61527(12) 0.2946(2) 0.0175(6) Uani 1 1 d . . . C134 C 0.3018(2) 0.58728(12) 0.1950(2) 0.0182(6) Uani 1 1 d . . . C231 C -0.1881(2) 0.63937(12) -0.1949(2) 0.0169(6) Uani 1 1 d . . . C232 C -0.0751(2) 0.61098(12) -0.1977(2) 0.0159(5) Uani 1 1 d . . . C233 C -0.1341(2) 0.55726(12) -0.2475(2) 0.0186(6) Uani 1 1 d . . . C234 C -0.2552(2) 0.58845(12) -0.2461(2) 0.0185(6) 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 Mo1 0.01232(16) 0.01118(16) 0.01330(17) 0.000 0.00314(12) 0.000 Mo2 0.01073(16) 0.01078(16) 0.01701(17) 0.000 0.00145(12) 0.000 Mo3 0.01194(12) 0.01361(13) 0.01252(13) -0.00089(9) 0.00164(9) 0.00113(8) Br 0.0533(3) 0.0274(2) 0.0398(3) 0.000 0.0265(2) 0.000 O1 0.0173(13) 0.0145(13) 0.0166(14) 0.000 0.0052(11) 0.000 O2 0.0133(13) 0.0140(13) 0.0254(15) 0.000 0.0050(11) 0.000 O3 0.0171(10) 0.0215(10) 0.0195(10) -0.0021(8) 0.0043(8) 0.0005(8) O4 0.0128(12) 0.0143(13) 0.0125(13) 0.000 0.0008(10) 0.000 O5 0.0137(13) 0.0157(13) 0.0147(13) 0.000 0.0008(10) 0.000 O6 0.0151(9) 0.0125(9) 0.0167(9) -0.0005(7) 0.0025(7) 0.0003(7) O131 0.0220(10) 0.0161(10) 0.0166(10) -0.0012(8) 0.0000(8) 0.0056(8) O132 0.0185(10) 0.0180(10) 0.0164(10) 0.0004(8) 0.0025(8) 0.0039(8) O133 0.0270(11) 0.0249(11) 0.0166(10) 0.0044(8) -0.0005(8) 0.0039(9) O134 0.0240(10) 0.0233(11) 0.0229(10) 0.0023(8) 0.0022(8) 0.0111(9) O231 0.0164(9) 0.0151(10) 0.0256(11) -0.0039(8) -0.0027(8) 0.0013(8) O232 0.0162(10) 0.0181(10) 0.0216(10) -0.0051(8) 0.0011(8) 0.0011(8) O233 0.0280(11) 0.0181(11) 0.0313(12) -0.0082(9) 0.0031(9) 0.0003(9) O234 0.0193(11) 0.0218(11) 0.0326(12) -0.0012(9) -0.0049(9) -0.0048(8) N1 0.0155(11) 0.0184(12) 0.0162(11) 0.0006(9) 0.0003(9) 0.0015(9) N2 0.0253(13) 0.0148(12) 0.0273(13) 0.0009(10) 0.0072(10) -0.0032(10) N3 0.0224(18) 0.0244(19) 0.0168(17) 0.000 0.0010(14) 0.000 C11 0.0211(14) 0.0169(14) 0.0184(14) -0.0003(11) 0.0043(11) -0.0014(11) C12 0.0204(14) 0.0159(14) 0.0257(15) -0.0028(12) 0.0055(12) 0.0020(11) C13 0.0163(13) 0.0136(13) 0.0243(15) 0.0039(11) 0.0024(11) -0.0021(11) C14 0.0195(14) 0.0199(14) 0.0166(13) 0.0021(11) 0.0019(11) -0.0019(11) C15 0.0223(14) 0.0150(14) 0.0180(14) 0.0007(11) 0.0054(11) -0.0015(11) C16 0.0295(16) 0.0285(17) 0.0215(15) -0.0064(13) -0.0005(12) 0.0021(13) C17 0.0172(14) 0.0241(16) 0.0325(17) 0.0028(13) 0.0013(12) 0.0029(12) C18 0.0277(16) 0.0253(16) 0.0216(15) -0.0024(12) 0.0021(12) 0.0074(13) C21 0.0226(15) 0.0189(15) 0.0237(15) 0.0028(12) 0.0038(12) -0.0065(12) C22 0.0294(16) 0.0217(15) 0.0230(15) 0.0017(12) 0.0048(12) -0.0035(13) C23 0.0294(16) 0.0216(15) 0.0286(16) 0.0064(13) 0.0106(13) 0.0008(13) C24 0.0223(15) 0.0223(15) 0.0328(17) 0.0095(13) 0.0015(13) -0.0014(12) C25 0.0261(15) 0.0184(14) 0.0267(16) 0.0075(12) 0.0001(12) -0.0075(12) C26 0.0233(15) 0.0221(15) 0.0346(17) 0.0007(13) 0.0008(13) -0.0015(12) C27 0.043(2) 0.0342(19) 0.0371(19) 0.0058(15) 0.0135(16) 0.0126(16) C28 0.0428(19) 0.0279(17) 0.0294(17) 0.0034(14) -0.0054(14) -0.0061(15) C31 0.0302(17) 0.0179(15) 0.0267(16) -0.0005(12) 0.0040(13) 0.0006(12) C32 0.0303(17) 0.0302(18) 0.0378(19) 0.0082(15) 0.0024(14) 0.0073(14) C33 0.024(2) 0.050(3) 0.040(3) 0.000 -0.008(2) 0.000 C34 0.038(3) 0.033(3) 0.025(2) 0.000 -0.014(2) 0.000 C35 0.026(2) 0.040(3) 0.051(3) 0.000 -0.008(2) 0.000 C131 0.0157(13) 0.0117(13) 0.0183(14) 0.0009(11) 0.0000(10) 0.0002(10) C132 0.0146(13) 0.0124(13) 0.0197(14) 0.0030(11) 0.0022(10) -0.0020(11) C133 0.0174(13) 0.0152(13) 0.0199(15) 0.0034(11) 0.0022(11) 0.0001(11) C134 0.0191(14) 0.0154(14) 0.0200(14) 0.0036(11) 0.0024(11) -0.0014(11) C231 0.0205(14) 0.0160(14) 0.0140(13) 0.0012(11) 0.0003(11) -0.0018(11) C232 0.0210(14) 0.0148(13) 0.0117(13) 0.0001(10) 0.0004(10) -0.0016(11) C233 0.0232(14) 0.0179(15) 0.0144(13) 0.0009(11) 0.0011(11) -0.0025(12) C234 0.0232(15) 0.0165(14) 0.0157(14) 0.0014(11) 0.0011(11) -0.0018(11) _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 O1 1.675(2) . ? Mo1 O6 1.9743(18) . ? Mo1 O6 1.9743(18) 4_575 ? Mo1 O132 2.0550(18) 4_575 ? Mo1 O132 2.0550(18) . ? Mo1 O4 2.386(2) . ? Mo1 Mo2 2.5947(4) . ? Mo2 O2 1.676(2) . ? Mo2 O6 1.9800(18) 4_575 ? Mo2 O6 1.9800(18) . ? Mo2 O231 2.0486(18) 4_575 ? Mo2 O231 2.0486(18) . ? Mo2 O5 2.358(2) . ? Mo3 O3 1.6762(18) . ? Mo3 O4 1.9766(18) . ? Mo3 O5 1.9788(19) . ? Mo3 O131 2.0446(18) . ? Mo3 O232 2.0615(18) . ? Mo3 O6 2.3769(17) . ? Mo3 Mo3 2.6036(4) 4_575 ? O4 Mo3 1.9766(18) 4_575 ? O5 Mo3 1.9788(18) 4_575 ? O131 C131 1.291(3) . ? O132 C132 1.282(3) . ? O133 C133 1.220(3) . ? O134 C134 1.238(3) . ? O231 C231 1.287(3) . ? O232 C232 1.280(3) . ? O233 C233 1.225(3) . ? O234 C234 1.223(3) . ? N1 C15 1.348(3) . ? N1 C11 1.348(4) . ? N1 H1 0.8600 . ? N2 C21 1.349(4) . ? N2 C25 1.360(4) . ? N2 H2 0.8600 . ? N3 C31 1.343(3) 4_565 ? N3 C31 1.343(3) . ? N3 C34 1.491(5) . ? C11 C12 1.376(4) . ? C11 C16 1.496(4) . ? C12 C13 1.392(4) . ? C12 H12 0.9300 . ? C13 C14 1.390(4) . ? C13 C17 1.498(4) . ? C14 C15 1.381(4) . ? C14 H14 0.9300 . ? C15 C18 1.499(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C22 1.380(4) . ? C21 C26 1.501(4) . ? C22 C23 1.393(4) . ? C22 H22 0.9300 . ? C23 C24 1.385(4) . ? C23 C27 1.501(4) . ? C24 C25 1.372(4) . ? C24 H24 0.9300 . ? C25 C28 1.491(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C31 C32 1.374(4) . ? C31 H31 0.9300 . ? C32 C33 1.374(4) . ? C32 H32 0.9300 . ? C33 C32 1.374(4) 4_565 ? C33 H33 0.9300 . ? C34 C35 1.522(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C131 C132 1.408(4) . ? C131 C134 1.460(4) . ? C132 C133 1.478(4) . ? C133 C134 1.505(4) . ? C231 C232 1.409(4) . ? C231 C234 1.473(4) . ? C232 C233 1.480(4) . ? C233 C234 1.515(4) . ? 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 O1 Mo1 O6 107.83(8) . . ? O1 Mo1 O6 107.83(8) . 4_575 ? O6 Mo1 O6 90.17(10) . 4_575 ? O1 Mo1 O132 91.71(8) . 4_575 ? O6 Mo1 O132 159.42(7) . 4_575 ? O6 Mo1 O132 89.90(7) 4_575 4_575 ? O1 Mo1 O132 91.71(8) . . ? O6 Mo1 O132 89.90(7) . . ? O6 Mo1 O132 159.42(7) 4_575 . ? O132 Mo1 O132 82.94(10) 4_575 . ? O1 Mo1 O4 173.90(11) . . ? O6 Mo1 O4 76.30(6) . . ? O6 Mo1 O4 76.30(6) 4_575 . ? O132 Mo1 O4 83.73(7) 4_575 . ? O132 Mo1 O4 83.73(7) . . ? O1 Mo1 Mo2 93.76(9) . . ? O6 Mo1 Mo2 49.08(5) . . ? O6 Mo1 Mo2 49.08(5) 4_575 . ? O132 Mo1 Mo2 138.17(5) 4_575 . ? O132 Mo1 Mo2 138.17(5) . . ? O4 Mo1 Mo2 92.34(6) . . ? O2 Mo2 O6 107.03(8) . 4_575 ? O2 Mo2 O6 107.03(8) . . ? O6 Mo2 O6 89.84(10) 4_575 . ? O2 Mo2 O231 93.11(9) . 4_575 ? O6 Mo2 O231 89.69(7) 4_575 4_575 ? O6 Mo2 O231 159.06(8) . 4_575 ? O2 Mo2 O231 93.11(9) . . ? O6 Mo2 O231 159.06(8) 4_575 . ? O6 Mo2 O231 89.69(7) . . ? O231 Mo2 O231 83.38(11) 4_575 . ? O2 Mo2 O5 175.11(11) . . ? O6 Mo2 O5 76.30(7) 4_575 . ? O6 Mo2 O5 76.30(7) . . ? O231 Mo2 O5 83.25(7) 4_575 . ? O231 Mo2 O5 83.25(7) . . ? O2 Mo2 Mo1 92.62(9) . . ? O6 Mo2 Mo1 48.90(5) 4_575 . ? O6 Mo2 Mo1 48.90(5) . . ? O231 Mo2 Mo1 137.86(5) 4_575 . ? O231 Mo2 Mo1 137.86(5) . . ? O5 Mo2 Mo1 92.27(6) . . ? O3 Mo3 O4 108.91(9) . . ? O3 Mo3 O5 107.52(10) . . ? O4 Mo3 O5 89.54(8) . . ? O3 Mo3 O131 92.96(8) . . ? O4 Mo3 O131 89.34(7) . . ? O5 Mo3 O131 158.69(9) . . ? O3 Mo3 O232 92.13(8) . . ? O4 Mo3 O232 157.76(8) . . ? O5 Mo3 O232 90.91(7) . . ? O131 Mo3 O232 82.27(7) . . ? O3 Mo3 O6 173.42(8) . . ? O4 Mo3 O6 76.47(8) . . ? O5 Mo3 O6 75.87(8) . . ? O131 Mo3 O6 83.18(7) . . ? O232 Mo3 O6 82.09(7) . . ? O3 Mo3 Mo3 94.12(6) . 4_575 ? O4 Mo3 Mo3 48.81(5) . 4_575 ? O5 Mo3 Mo3 48.86(5) . 4_575 ? O131 Mo3 Mo3 137.43(5) . 4_575 ? O232 Mo3 Mo3 139.19(5) . 4_575 ? O6 Mo3 Mo3 92.32(4) . 4_575 ? Mo3 O4 Mo3 82.39(9) . 4_575 ? Mo3 O4 Mo1 103.30(9) . . ? Mo3 O4 Mo1 103.30(9) 4_575 . ? Mo3 O5 Mo3 82.28(9) 4_575 . ? Mo3 O5 Mo2 104.16(9) 4_575 . ? Mo3 O5 Mo2 104.16(9) . . ? Mo1 O6 Mo2 82.02(7) . . ? Mo1 O6 Mo3 103.68(7) . . ? Mo2 O6 Mo3 103.45(7) . . ? C131 O131 Mo3 132.59(17) . . ? C132 O132 Mo1 133.98(17) . . ? C231 O231 Mo2 132.83(17) . . ? C232 O232 Mo3 135.14(17) . . ? C15 N1 C11 123.5(2) . . ? C15 N1 H1 118.3 . . ? C11 N1 H1 118.3 . . ? C21 N2 C25 124.0(3) . . ? C21 N2 H2 118.0 . . ? C25 N2 H2 118.0 . . ? C31 N3 C31 121.7(4) 4_565 . ? C31 N3 C34 119.15(18) 4_565 . ? C31 N3 C34 119.15(18) . . ? N1 C11 C12 118.4(2) . . ? N1 C11 C16 118.1(2) . . ? C12 C11 C16 123.4(3) . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 118.2(3) . . ? C14 C13 C17 121.4(3) . . ? C12 C13 C17 120.4(3) . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N1 C15 C14 118.6(2) . . ? N1 C15 C18 117.3(2) . . ? C14 C15 C18 124.1(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C21 C22 117.9(3) . . ? N2 C21 C26 118.3(3) . . ? C22 C21 C26 123.9(3) . . ? C21 C22 C23 120.8(3) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 118.4(3) . . ? C24 C23 C27 120.7(3) . . ? C22 C23 C27 120.9(3) . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? N2 C25 C24 117.8(3) . . ? N2 C25 C28 117.8(3) . . ? C24 C25 C28 124.4(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C31 C32 119.9(3) . . ? N3 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.1(3) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C32 120.3(4) . 4_565 ? C32 C33 H33 119.9 . . ? C32 C33 H33 119.9 4_565 . ? N3 C34 C35 109.8(4) . . ? N3 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? N3 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O131 C131 C132 136.3(2) . . ? O131 C131 C134 131.8(2) . . ? C132 C131 C134 91.9(2) . . ? O132 C132 C131 137.0(2) . . ? O132 C132 C133 131.1(2) . . ? C131 C132 C133 91.9(2) . . ? O133 C133 C132 135.1(3) . . ? O133 C133 C134 137.4(3) . . ? C132 C133 C134 87.4(2) . . ? O134 C134 C131 134.5(3) . . ? O134 C134 C133 136.6(3) . . ? C131 C134 C133 88.8(2) . . ? O231 C231 C232 136.2(2) . . ? O231 C231 C234 131.5(2) . . ? C232 C231 C234 92.3(2) . . ? O232 C232 C231 136.4(3) . . ? O232 C232 C233 131.8(2) . . ? C231 C232 C233 91.8(2) . . ? O233 C233 C232 135.9(3) . . ? O233 C233 C234 136.2(3) . . ? C232 C233 C234 87.9(2) . . ? O234 C234 C231 135.7(3) . . ? O234 C234 C233 136.4(3) . . ? C231 C234 C233 88.0(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.039 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.081 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 219870' _chemical_name_common ;dichlorodimethoxooctaoxotetrapyridinetetramolybdenum(V) acetonitrile (1/1) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichlorodimethoxooctaoxotetrapyridinetetramolybdenum(V) acetonitrile (1/1) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H29 Cl2 Mo4 N5 O10' _chemical_formula_weight 1002.18 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.5660(5) _cell_length_b 12.8020(3) _cell_length_c 10.1968(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.3471(9) _cell_angle_gamma 90.00 _cell_volume 3247.23(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7130 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3725 _reflns_number_gt 3189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0336P)^2^+12.2737P] 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 3725 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.753770(11) 0.29266(2) 0.35117(3) 0.02124(9) Uani 1 1 d . . . Mo2 Mo 0.651240(11) 0.26048(3) 0.51553(3) 0.02731(9) Uani 1 1 d . . . Cl Cl 0.59156(4) 0.40315(12) 0.53790(12) 0.0608(3) Uani 1 1 d . . . O1 O 0.76866(10) 0.39394(19) 0.2618(2) 0.0325(5) Uani 1 1 d . . . O2 O 0.61665(10) 0.1665(2) 0.5748(3) 0.0419(7) Uani 1 1 d . . . O3 O 0.80008(9) 0.1786(2) 0.3302(2) 0.0289(5) Uani 1 1 d . . . O4 O 0.70970(8) 0.18186(17) 0.4572(2) 0.0215(4) Uani 1 1 d . . . O5 O 0.68444(9) 0.36620(17) 0.3841(2) 0.0262(5) Uani 1 1 d . . . C5 C 0.6846(2) 0.4770(3) 0.3913(6) 0.0569(12) Uani 1 1 d . . . H5A H 0.6509 0.5009 0.4064 0.085 Uiso 1 1 calc R . . H5B H 0.6898 0.5055 0.3081 0.085 Uiso 1 1 calc R . . H5C H 0.7133 0.4996 0.4641 0.085 Uiso 1 1 calc R . . N1 N 0.70194(11) 0.2259(2) 0.1657(3) 0.0233(6) Uani 1 1 d . . . C11 C 0.67653(19) 0.2885(3) 0.0666(4) 0.0450(10) Uani 1 1 d . . . H11 H 0.6770 0.3601 0.0822 0.054 Uiso 1 1 calc R . . C12 C 0.64951(18) 0.2517(3) -0.0580(4) 0.0464(11) Uani 1 1 d . . . H12 H 0.6326 0.2978 -0.1249 0.056 Uiso 1 1 calc R . . C13 C 0.64794(17) 0.1479(4) -0.0812(4) 0.0465(10) Uani 1 1 d . . . H13 H 0.6302 0.1212 -0.1644 0.056 Uiso 1 1 calc R . . C14 C 0.6730(2) 0.0830(4) 0.0203(5) 0.084(2) Uani 1 1 d . . . H14 H 0.6724 0.0111 0.0071 0.100 Uiso 1 1 calc R . . C15 C 0.69930(19) 0.1248(3) 0.1426(4) 0.0559(13) Uani 1 1 d . . . H15 H 0.7158 0.0798 0.2113 0.067 Uiso 1 1 calc R . . N2 N 0.59722(12) 0.2220(3) 0.3112(3) 0.0341(7) Uani 1 1 d . . . C21 C 0.5890(3) 0.1237(5) 0.2755(6) 0.084(2) Uani 1 1 d . . . H21 H 0.6077 0.0725 0.3323 0.101 Uiso 1 1 calc R . . C22 C 0.5540(3) 0.0926(6) 0.1576(6) 0.119(3) Uani 1 1 d . . . H22 H 0.5499 0.0221 0.1358 0.143 Uiso 1 1 calc R . . C23 C 0.52599(19) 0.1643(5) 0.0753(5) 0.0663(15) Uani 1 1 d . . . H23 H 0.5015 0.1446 -0.0033 0.080 Uiso 1 1 calc R . . C24 C 0.5340(2) 0.2652(5) 0.1088(5) 0.0636(15) Uani 1 1 d . . . H24 H 0.5151 0.3169 0.0534 0.076 Uiso 1 1 calc R . . C25 C 0.5708(2) 0.2919(4) 0.2269(4) 0.0563(13) Uani 1 1 d . . . H25 H 0.5771 0.3623 0.2473 0.068 Uiso 1 1 calc R . . N3 N 0.5000 0.2127(10) -0.2500 0.127(4) Uani 1 2 d S . . C31 C 0.5000 0.3046(12) -0.2500 0.091(3) Uani 1 2 d S . . C32 C 0.5000 0.4176(10) -0.2500 0.106(4) Uani 1 2 d S . . H32A H 0.5102 0.4426 -0.1589 0.158 Uiso 0.50 1 calc PR . . H32B H 0.4647 0.4426 -0.2916 0.158 Uiso 0.50 1 calc PR . . H32C H 0.5252 0.4426 -0.2996 0.158 Uiso 0.50 1 calc PR . . 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 0.02398(15) 0.02070(15) 0.01920(14) -0.00054(10) 0.00531(10) -0.00089(10) Mo2 0.02181(15) 0.03741(19) 0.02304(15) -0.00311(12) 0.00581(11) 0.00222(12) Cl 0.0371(5) 0.0891(9) 0.0530(6) -0.0153(6) 0.0041(5) 0.0207(6) O1 0.0402(14) 0.0299(13) 0.0267(12) 0.0029(10) 0.0065(11) -0.0075(11) O2 0.0298(13) 0.0645(19) 0.0319(13) 0.0031(13) 0.0084(11) -0.0100(13) O3 0.0284(12) 0.0353(13) 0.0233(11) -0.0053(10) 0.0065(10) 0.0049(10) O4 0.0237(11) 0.0197(11) 0.0209(10) -0.0024(8) 0.0047(9) -0.0016(9) O5 0.0288(12) 0.0205(11) 0.0284(12) -0.0001(9) 0.0047(10) 0.0061(9) C5 0.068(3) 0.023(2) 0.086(4) -0.002(2) 0.031(3) 0.009(2) N1 0.0267(14) 0.0232(14) 0.0200(13) -0.0008(11) 0.0056(11) 0.0012(11) C11 0.067(3) 0.030(2) 0.0293(19) 0.0070(16) -0.0066(19) -0.0105(19) C12 0.057(3) 0.048(2) 0.0267(19) 0.0154(18) -0.0071(18) -0.013(2) C13 0.046(2) 0.057(3) 0.031(2) -0.0160(19) -0.0036(17) 0.006(2) C14 0.111(4) 0.037(3) 0.069(3) -0.027(2) -0.048(3) 0.028(3) C15 0.071(3) 0.030(2) 0.046(2) -0.0080(18) -0.029(2) 0.015(2) N2 0.0230(14) 0.0491(19) 0.0295(16) -0.0034(14) 0.0044(12) 0.0012(13) C21 0.102(5) 0.054(3) 0.067(3) -0.001(3) -0.044(3) -0.016(3) C22 0.156(7) 0.070(4) 0.083(5) -0.005(3) -0.073(5) -0.031(4) C23 0.041(2) 0.107(5) 0.044(3) -0.016(3) -0.006(2) -0.018(3) C24 0.053(3) 0.100(4) 0.031(2) 0.002(3) -0.002(2) 0.028(3) C25 0.067(3) 0.065(3) 0.030(2) -0.004(2) -0.003(2) 0.019(3) N3 0.177(11) 0.144(10) 0.047(5) 0.000 0.002(5) 0.000 C31 0.088(7) 0.139(10) 0.039(4) 0.000 0.001(4) 0.000 C32 0.104(8) 0.131(10) 0.095(8) 0.000 0.051(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.678(2) . ? Mo1 O3 1.923(2) . ? Mo1 O4 1.989(2) 7_656 ? Mo1 O5 2.101(2) . ? Mo1 N1 2.215(3) . ? Mo1 O4 2.239(2) . ? Mo1 Mo2 2.5854(4) 7_656 ? Mo2 O2 1.686(3) . ? Mo2 O3 1.931(2) 7_656 ? Mo2 O4 2.003(2) . ? Mo2 O5 2.207(2) . ? Mo2 N2 2.272(3) . ? Mo2 Cl 2.4242(12) . ? Mo2 Mo1 2.5854(4) 7_656 ? O3 Mo2 1.931(2) 7_656 ? O4 Mo1 1.989(2) 7_656 ? O5 C5 1.420(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? N1 C15 1.314(5) . ? N1 C11 1.334(5) . ? C11 C12 1.382(5) . ? C11 H11 0.9300 . ? C12 C13 1.348(6) . ? C12 H12 0.9300 . ? C13 C14 1.366(7) . ? C13 H13 0.9300 . ? C14 C15 1.381(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? N2 C21 1.313(6) . ? N2 C25 1.314(6) . ? C21 C22 1.382(7) . ? C21 H21 0.9300 . ? C22 C23 1.334(9) . ? C22 H22 0.9300 . ? C23 C24 1.340(8) . ? C23 H23 0.9300 . ? C24 C25 1.390(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? N3 C31 1.177(15) . ? C31 C32 1.447(16) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 O1 Mo1 O3 107.68(12) . . ? O1 Mo1 O4 107.03(10) . 7_656 ? O3 Mo1 O4 94.14(9) . 7_656 ? O1 Mo1 O5 92.64(11) . . ? O3 Mo1 O5 157.19(10) . . ? O4 Mo1 O5 89.52(9) 7_656 . ? O1 Mo1 N1 90.02(11) . . ? O3 Mo1 N1 82.79(10) . . ? O4 Mo1 N1 162.76(9) 7_656 . ? O5 Mo1 N1 87.07(9) . . ? O1 Mo1 O4 162.58(10) . . ? O3 Mo1 O4 87.93(9) . . ? O4 Mo1 O4 78.70(9) 7_656 . ? O5 Mo1 O4 70.71(8) . . ? N1 Mo1 O4 84.22(9) . . ? O1 Mo1 Mo2 100.69(9) . 7_656 ? O3 Mo1 Mo2 47.99(7) . 7_656 ? O4 Mo1 Mo2 49.87(6) 7_656 7_656 ? O5 Mo1 Mo2 139.33(6) . 7_656 ? N1 Mo1 Mo2 130.66(7) . 7_656 ? O4 Mo1 Mo2 95.50(6) . 7_656 ? O2 Mo2 O3 106.80(12) . 7_656 ? O2 Mo2 O4 103.71(12) . . ? O3 Mo2 O4 93.45(9) 7_656 . ? O2 Mo2 O5 164.22(11) . . ? O3 Mo2 O5 88.91(9) 7_656 . ? O4 Mo2 O5 73.14(8) . . ? O2 Mo2 N2 85.17(12) . . ? O3 Mo2 N2 167.36(12) 7_656 . ? O4 Mo2 N2 87.47(10) . . ? O5 Mo2 N2 79.28(10) . . ? O2 Mo2 Cl 96.33(11) . . ? O3 Mo2 Cl 85.43(7) 7_656 . ? O4 Mo2 Cl 159.33(7) . . ? O5 Mo2 Cl 86.20(7) . . ? N2 Mo2 Cl 89.27(8) . . ? O2 Mo2 Mo1 97.49(9) . 7_656 ? O3 Mo2 Mo1 47.73(7) 7_656 7_656 ? O4 Mo2 Mo1 49.40(6) . 7_656 ? O5 Mo2 Mo1 91.97(6) . 7_656 ? N2 Mo2 Mo1 136.33(8) . 7_656 ? Cl Mo2 Mo1 133.16(3) . 7_656 ? Mo1 O3 Mo2 84.28(9) . 7_656 ? Mo1 O4 Mo2 80.73(8) 7_656 . ? Mo1 O4 Mo1 101.30(9) 7_656 . ? Mo2 O4 Mo1 108.56(10) . . ? C5 O5 Mo1 117.6(2) . . ? C5 O5 Mo2 125.3(3) . . ? Mo1 O5 Mo2 106.20(9) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C15 N1 C11 117.4(3) . . ? C15 N1 Mo1 121.9(2) . . ? C11 N1 Mo1 120.4(2) . . ? N1 C11 C12 123.0(4) . . ? N1 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 119.1(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 118.5(4) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C15 119.6(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N1 C15 C14 122.5(4) . . ? N1 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C21 N2 C25 116.5(4) . . ? C21 N2 Mo2 119.1(3) . . ? C25 N2 Mo2 124.3(3) . . ? N2 C21 C22 123.2(5) . . ? N2 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C23 C22 C21 119.7(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 118.3(5) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C23 C24 C25 119.5(5) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N2 C25 C24 122.8(5) . . ? N2 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N3 C31 C32 180.000(1) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.889 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.109 #===END