# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Enbo Wang' _publ_contact_author_email wangeb889@nenu.edu.cn _publ_section_title ; Controllable self-assembly of four new metal-organic frameworks based on different phosphomolybdate clusters by altering molar ratio of H3PO4 and Na2MoO4 ; _publ_author_name 'Enbo Wang' data_92a _database_code_depnum_ccdc_archive 'CCDC 792968' #TrackingRef 'compound 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H57 Co Mo8 N16 O42 P V6' _chemical_formula_weight 2789.24 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.841(3) _cell_length_b 22.841(3) _cell_length_c 15.503(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8088(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30393 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5428 _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.599 _exptl_absorpt_correction_T_max 0.633 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 30393 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3556 _reflns_number_gt 3078 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0400P)^2^+40.6900P] 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 3556 _refine_ls_number_parameters 294 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _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 0.472920(15) 0.862251(15) 0.27913(2) 0.01970(11) Uani 1 1 d . . . Mo2 Mo 0.609800(15) 0.786201(15) 0.27913(2) 0.01955(11) Uani 1 1 d . . . P1 P 0.5000 0.7500 0.1250 0.0164(4) Uani 1 4 d S . . V1 V 0.57682(3) 0.88748(3) 0.13118(4) 0.01441(15) Uani 1 1 d . . . V2 V 0.5000 0.7500 0.38308(6) 0.0176(2) Uani 1 2 d S . . Co1 Co 0.5000 0.7500 0.6250 0.0185(2) Uani 1 4 d S . . O1 O 0.52322(12) 0.91027(11) 0.22263(17) 0.0211(6) Uani 1 1 d . . . O2 O 0.5000 0.7500 0.4881(2) 0.0242(9) Uani 1 2 d S . . O3 O 0.62316(11) 0.85465(12) 0.22394(17) 0.0217(6) Uani 1 1 d . . . O4 O 0.44828(13) 0.90681(13) 0.35812(18) 0.0263(6) Uani 1 1 d . . . O5 O 0.53997(11) 0.82167(11) 0.34454(17) 0.0198(6) Uani 1 1 d . . . O6 O 0.66037(13) 0.78876(13) 0.35803(18) 0.0275(7) Uani 1 1 d . . . O7 O 0.56233(11) 0.71537(11) 0.32081(17) 0.0201(6) Uani 1 1 d . . . O8 O 0.64181(12) 0.73756(12) 0.19922(17) 0.0220(6) Uani 1 1 d . . . O9 O 0.41462(12) 0.86308(11) 0.20021(17) 0.0209(6) Uani 1 1 d . . . O10 O 0.52663(11) 0.79791(11) 0.18183(16) 0.0179(6) Uani 1 1 d . . . O11 O 0.61060(13) 0.94826(13) 0.11512(18) 0.0278(7) Uani 1 1 d . . . N1 N 0.59228(16) 0.76175(16) 0.6253(2) 0.0272(8) Uani 1 1 d . . . N2 N 0.67720(15) 0.79836(16) 0.5863(2) 0.0299(8) Uani 1 1 d . . . N3 N 0.70862(17) 1.11599(16) 0.6488(3) 0.0332(9) Uani 1 1 d . . . N4 N 0.7606(2) 1.1910(2) 0.6219(4) 0.0629(14) Uani 1 1 d U . . C1 C 0.62246(19) 0.78543(19) 0.5620(3) 0.0289(10) Uani 1 1 d . . . H1A H 0.6076 0.7923 0.5071 0.035 Uiso 1 1 calc R . . C2 C 0.6297(2) 0.7589(2) 0.6939(3) 0.0343(10) Uani 1 1 d . . . H2A H 0.6206 0.7434 0.7477 0.041 Uiso 1 1 calc R . . C3 C 0.6825(2) 0.7823(2) 0.6716(3) 0.0397(12) Uani 1 1 d . . . H3A H 0.7153 0.7865 0.7067 0.048 Uiso 1 1 calc R . . C4 C 0.7181(2) 0.8361(2) 0.5396(3) 0.0349(11) Uani 1 1 d . . . H4A H 0.7096 0.8347 0.4784 0.042 Uiso 1 1 calc R . . H4B H 0.7578 0.8222 0.5483 0.042 Uiso 1 1 calc R . . C5 C 0.71275(19) 0.89828(19) 0.5717(3) 0.0296(10) Uani 1 1 d . . . C6 C 0.7599(2) 0.9277(2) 0.6059(3) 0.0335(10) Uani 1 1 d . . . H6A H 0.7969 0.9108 0.6041 0.040 Uiso 1 1 calc R . . C7 C 0.7527(2) 0.9827(2) 0.6432(3) 0.0354(11) Uani 1 1 d . . . H7A H 0.7848 1.0023 0.6662 0.043 Uiso 1 1 calc R . . C8 C 0.6980(2) 1.0081(2) 0.6461(3) 0.0314(10) Uani 1 1 d . . . C9 C 0.6512(2) 0.9800(2) 0.6077(3) 0.0398(12) Uani 1 1 d . . . H9A H 0.6146 0.9978 0.6069 0.048 Uiso 1 1 calc R . . C10 C 0.6587(2) 0.9260(2) 0.5707(3) 0.0417(12) Uani 1 1 d . . . H10A H 0.6270 0.9076 0.5444 0.050 Uiso 1 1 calc R . . C11 C 0.6874(2) 1.0644(2) 0.6957(3) 0.0397(11) Uani 1 1 d . . . H11A H 0.6458 1.0686 0.7066 0.048 Uiso 1 1 calc R . . H11B H 0.7071 1.0621 0.7510 0.048 Uiso 1 1 calc R . . C12 C 0.6898(3) 1.1355(2) 0.5710(4) 0.0542(15) Uani 1 1 d . . . H12A H 0.6602 1.1203 0.5366 0.065 Uiso 1 1 calc R . . C13 C 0.7257(4) 1.1839(3) 0.5548(4) 0.0686(19) Uani 1 1 d U . . H13A H 0.7250 1.2071 0.5055 0.082 Uiso 1 1 calc R . . C14 C 0.7504(2) 1.1505(3) 0.6778(5) 0.0561(15) Uani 1 1 d . . . H14A H 0.7696 1.1463 0.7304 0.067 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 0.02235(19) 0.01967(18) 0.01707(19) -0.00137(13) 0.00011(13) 0.00101(13) Mo2 0.01919(18) 0.02296(19) 0.01650(18) -0.00114(13) -0.00131(13) -0.00100(13) P1 0.0181(6) 0.0181(6) 0.0129(9) 0.000 0.000 0.000 V1 0.0169(3) 0.0140(3) 0.0123(3) -0.0007(2) -0.0001(2) -0.0029(2) V2 0.0198(5) 0.0209(5) 0.0122(4) 0.000 0.000 0.0010(4) Co1 0.0216(3) 0.0216(3) 0.0122(5) 0.000 0.000 0.000 O1 0.0249(14) 0.0182(13) 0.0202(13) -0.0009(11) 0.0006(12) 0.0000(11) O2 0.029(2) 0.028(2) 0.0154(19) 0.000 0.000 -0.0014(17) O3 0.0197(14) 0.0242(14) 0.0212(14) 0.0021(12) -0.0007(11) -0.0022(11) O4 0.0297(16) 0.0275(15) 0.0218(14) -0.0054(12) 0.0001(12) 0.0033(13) O5 0.0225(14) 0.0222(14) 0.0146(13) -0.0016(11) -0.0019(11) -0.0016(11) O6 0.0258(15) 0.0340(17) 0.0225(14) -0.0005(13) -0.0044(12) -0.0003(13) O7 0.0204(14) 0.0230(14) 0.0169(13) -0.0009(11) 0.0019(11) 0.0000(11) O8 0.0213(14) 0.0248(14) 0.0200(14) -0.0005(12) 0.0023(11) -0.0005(11) O9 0.0223(14) 0.0206(14) 0.0198(13) 0.0028(11) -0.0002(11) 0.0015(11) O10 0.0207(13) 0.0186(13) 0.0144(13) -0.0006(11) -0.0019(11) -0.0006(11) O11 0.0347(17) 0.0228(15) 0.0258(15) -0.0023(12) 0.0007(13) -0.0082(13) N1 0.0273(19) 0.032(2) 0.0223(18) -0.0029(16) 0.0016(15) -0.0007(16) N2 0.0262(19) 0.030(2) 0.033(2) -0.0094(17) 0.0027(16) -0.0019(15) N3 0.0279(19) 0.0273(19) 0.044(2) -0.0063(18) 0.0006(17) -0.0006(16) N4 0.044(3) 0.054(3) 0.090(4) -0.003(3) 0.026(3) -0.006(2) C1 0.029(2) 0.034(2) 0.024(2) -0.0081(19) 0.0003(18) -0.0035(18) C2 0.033(2) 0.043(3) 0.027(2) 0.007(2) 0.0001(19) -0.004(2) C3 0.033(3) 0.048(3) 0.038(3) 0.005(2) -0.009(2) -0.001(2) C4 0.029(2) 0.039(3) 0.037(3) -0.008(2) 0.012(2) -0.009(2) C5 0.029(2) 0.032(2) 0.028(2) -0.0016(19) 0.0041(19) -0.0024(19) C6 0.029(2) 0.035(3) 0.037(3) -0.004(2) 0.002(2) 0.002(2) C7 0.037(3) 0.037(3) 0.032(2) -0.004(2) -0.003(2) -0.006(2) C8 0.036(3) 0.029(2) 0.029(2) 0.0021(19) 0.006(2) 0.0023(19) C9 0.030(2) 0.035(3) 0.055(3) -0.001(2) 0.000(2) 0.002(2) C10 0.028(2) 0.045(3) 0.053(3) -0.007(3) 0.000(2) -0.005(2) C11 0.048(3) 0.037(3) 0.034(2) -0.001(2) 0.008(2) 0.000(2) C12 0.074(4) 0.043(3) 0.046(3) 0.006(3) -0.004(3) 0.000(3) C13 0.111(6) 0.036(3) 0.060(4) 0.019(3) 0.039(4) 0.021(3) C14 0.037(3) 0.057(4) 0.075(4) -0.007(3) 0.001(3) -0.010(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 O4 1.689(3) . ? Mo1 O9 1.808(3) . ? Mo1 O1 1.814(3) . ? Mo1 O7 2.052(3) 6_564 ? Mo1 O5 2.057(3) . ? Mo1 O10 2.437(3) . ? Mo1 V2 3.0908(7) . ? Mo2 O6 1.683(3) . ? Mo2 O3 1.808(3) . ? Mo2 O8 1.818(3) . ? Mo2 O7 2.052(3) . ? Mo2 O5 2.056(3) . ? Mo2 O10 2.440(3) . ? Mo2 V2 3.0936(7) . ? P1 O10 1.531(2) 6_564 ? P1 O10 1.531(2) 12_766 ? P1 O10 1.531(3) . ? P1 O10 1.531(3) 15_565 ? V1 O11 1.608(3) . ? V1 O9 1.922(3) 15_565 ? V1 O8 1.930(3) 12_766 ? V1 O3 1.937(3) . ? V1 O1 1.944(3) . ? V2 O2 1.628(4) . ? V2 O7 1.893(3) 6_564 ? V2 O7 1.893(3) . ? V2 O5 1.967(3) 6_564 ? V2 O5 1.967(3) . ? V2 Mo1 3.0908(7) 6_564 ? V2 Mo2 3.0936(7) 6_564 ? Co1 O2 2.122(4) 15_566 ? Co1 O2 2.122(4) . ? Co1 N1 2.125(4) 6_564 ? Co1 N1 2.125(4) . ? Co1 N1 2.125(4) 12_767 ? Co1 N1 2.125(4) 15_566 ? O7 Mo1 2.052(3) 6_564 ? O8 V1 1.930(3) 15_565 ? O9 V1 1.922(3) 12_766 ? N1 C1 1.315(6) . ? N1 C2 1.367(6) . ? N2 C1 1.339(6) . ? N2 C3 1.379(6) . ? N2 C4 1.462(6) . ? N3 C14 1.317(7) . ? N3 C12 1.355(7) . ? N3 C11 1.467(6) . ? N4 C14 1.289(8) . ? N4 C13 1.320(9) . ? C1 H1A 0.9300 . ? C2 C3 1.363(7) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.510(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.376(6) . ? C5 C10 1.387(7) . ? C6 C7 1.392(7) . ? C6 H6A 0.9300 . ? C7 C8 1.378(7) . ? C7 H7A 0.9300 . ? C8 C9 1.381(7) . ? C8 C11 1.518(6) . ? C9 C10 1.371(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.400(9) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? 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 O4 Mo1 O9 103.82(13) . . ? O4 Mo1 O1 101.35(13) . . ? O9 Mo1 O1 97.66(12) . . ? O4 Mo1 O7 99.30(13) . 6_564 ? O9 Mo1 O7 86.17(11) . 6_564 ? O1 Mo1 O7 157.40(11) . 6_564 ? O4 Mo1 O5 99.34(12) . . ? O9 Mo1 O5 152.41(11) . . ? O1 Mo1 O5 92.23(11) . . ? O7 Mo1 O5 75.38(10) 6_564 . ? O4 Mo1 O10 168.49(12) . . ? O9 Mo1 O10 87.61(10) . . ? O1 Mo1 O10 75.34(10) . . ? O7 Mo1 O10 82.61(10) 6_564 . ? O5 Mo1 O10 70.04(9) . . ? O4 Mo1 V2 100.87(10) . . ? O9 Mo1 V2 120.59(8) . . ? O1 Mo1 V2 128.80(9) . . ? O7 Mo1 V2 36.63(7) 6_564 . ? O5 Mo1 V2 38.77(7) . . ? O10 Mo1 V2 73.84(6) . . ? O6 Mo2 O3 101.42(13) . . ? O6 Mo2 O8 103.91(13) . . ? O3 Mo2 O8 97.94(12) . . ? O6 Mo2 O7 99.27(13) . . ? O3 Mo2 O7 156.91(11) . . ? O8 Mo2 O7 86.86(11) . . ? O6 Mo2 O5 99.22(12) . . ? O3 Mo2 O5 91.35(11) . . ? O8 Mo2 O5 152.74(11) . . ? O7 Mo2 O5 75.26(10) . . ? O6 Mo2 O10 168.36(12) . . ? O3 Mo2 O10 75.18(10) . . ? O8 Mo2 O10 87.64(11) . . ? O7 Mo2 O10 82.52(10) . . ? O5 Mo2 O10 70.00(9) . . ? O6 Mo2 V2 100.78(10) . . ? O3 Mo2 V2 127.91(9) . . ? O8 Mo2 V2 121.18(9) . . ? O7 Mo2 V2 36.57(7) . . ? O5 Mo2 V2 38.70(7) . . ? O10 Mo2 V2 73.75(6) . . ? O10 P1 O10 109.34(9) 6_564 12_766 ? O10 P1 O10 109.73(19) 6_564 . ? O10 P1 O10 109.34(9) 12_766 . ? O10 P1 O10 109.34(9) 6_564 15_565 ? O10 P1 O10 109.73(19) 12_766 15_565 ? O10 P1 O10 109.34(9) . 15_565 ? O11 V1 O9 103.07(13) . 15_565 ? O11 V1 O8 102.79(14) . 12_766 ? O9 V1 O8 86.34(11) 15_565 12_766 ? O11 V1 O3 100.77(14) . . ? O9 V1 O3 90.70(12) 15_565 . ? O8 V1 O3 156.31(12) 12_766 . ? O11 V1 O1 100.59(13) . . ? O9 V1 O1 156.34(12) 15_565 . ? O8 V1 O1 88.71(12) 12_766 . ? O3 V1 O1 84.63(12) . . ? O2 V2 O7 120.66(8) . 6_564 ? O2 V2 O7 120.66(8) . . ? O7 V2 O7 118.69(16) 6_564 . ? O2 V2 O5 107.68(8) . 6_564 ? O7 V2 O5 81.02(11) 6_564 6_564 ? O7 V2 O5 81.17(11) . 6_564 ? O2 V2 O5 107.68(8) . . ? O7 V2 O5 81.17(11) 6_564 . ? O7 V2 O5 81.02(11) . . ? O5 V2 O5 144.64(16) 6_564 . ? O2 V2 Mo1 121.424(16) . . ? O7 V2 Mo1 40.28(8) 6_564 . ? O7 V2 Mo1 103.37(8) . . ? O5 V2 Mo1 116.05(8) 6_564 . ? O5 V2 Mo1 40.91(8) . . ? O2 V2 Mo1 121.424(17) . 6_564 ? O7 V2 Mo1 103.37(8) 6_564 6_564 ? O7 V2 Mo1 40.28(8) . 6_564 ? O5 V2 Mo1 40.91(8) 6_564 6_564 ? O5 V2 Mo1 116.05(8) . 6_564 ? Mo1 V2 Mo1 117.15(3) . 6_564 ? O2 V2 Mo2 121.394(16) . 6_564 ? O7 V2 Mo2 40.22(8) 6_564 6_564 ? O7 V2 Mo2 103.43(8) . 6_564 ? O5 V2 Mo2 40.82(8) 6_564 6_564 ? O5 V2 Mo2 116.13(8) . 6_564 ? Mo1 V2 Mo2 77.754(17) . 6_564 ? Mo1 V2 Mo2 70.666(16) 6_564 6_564 ? O2 V2 Mo2 121.394(16) . . ? O7 V2 Mo2 103.43(8) 6_564 . ? O7 V2 Mo2 40.22(8) . . ? O5 V2 Mo2 116.13(8) 6_564 . ? O5 V2 Mo2 40.82(8) . . ? Mo1 V2 Mo2 70.666(16) . . ? Mo1 V2 Mo2 77.754(17) 6_564 . ? Mo2 V2 Mo2 117.21(3) 6_564 . ? O2 Co1 O2 180.000(1) 15_566 . ? O2 Co1 N1 89.88(9) 15_566 6_564 ? O2 Co1 N1 90.12(9) . 6_564 ? O2 Co1 N1 89.88(9) 15_566 . ? O2 Co1 N1 90.12(9) . . ? N1 Co1 N1 179.75(18) 6_564 . ? O2 Co1 N1 90.12(9) 15_566 12_767 ? O2 Co1 N1 89.88(9) . 12_767 ? N1 Co1 N1 90.000(1) 6_564 12_767 ? N1 Co1 N1 90.000(1) . 12_767 ? O2 Co1 N1 90.12(9) 15_566 15_566 ? O2 Co1 N1 89.88(9) . 15_566 ? N1 Co1 N1 90.000(1) 6_564 15_566 ? N1 Co1 N1 90.000(1) . 15_566 ? N1 Co1 N1 179.75(18) 12_767 15_566 ? Mo1 O1 V1 126.09(14) . . ? V2 O2 Co1 180.0 . . ? Mo2 O3 V1 126.43(14) . . ? V2 O5 Mo2 100.48(12) . . ? V2 O5 Mo1 100.32(11) . . ? Mo2 O5 Mo1 120.78(13) . . ? V2 O7 Mo1 103.09(12) . 6_564 ? V2 O7 Mo2 103.21(12) . . ? Mo1 O7 Mo2 142.14(14) 6_564 . ? Mo2 O8 V1 152.27(16) . 15_565 ? Mo1 O9 V1 153.57(16) . 12_766 ? P1 O10 Mo1 125.96(14) . . ? P1 O10 Mo2 125.93(14) . . ? Mo1 O10 Mo2 94.32(9) . . ? C1 N1 C2 105.8(4) . . ? C1 N1 Co1 124.8(3) . . ? C2 N1 Co1 128.1(3) . . ? C1 N2 C3 107.1(4) . . ? C1 N2 C4 126.0(4) . . ? C3 N2 C4 125.1(4) . . ? C14 N3 C12 109.7(5) . . ? C14 N3 C11 123.4(5) . . ? C12 N3 C11 126.9(4) . . ? C14 N4 C13 109.5(5) . . ? N1 C1 N2 111.8(4) . . ? N1 C1 H1A 124.1 . . ? N2 C1 H1A 124.1 . . ? C3 C2 N1 109.8(4) . . ? C3 C2 H2A 125.1 . . ? N1 C2 H2A 125.1 . . ? C2 C3 N2 105.6(4) . . ? C2 C3 H3A 127.2 . . ? N2 C3 H3A 127.2 . . ? N2 C4 C5 109.8(4) . . ? N2 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 118.5(4) . . ? C6 C5 C4 121.6(4) . . ? C10 C5 C4 119.9(4) . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 119.5(4) . . ? C7 C8 C11 121.1(4) . . ? C9 C8 C11 119.3(4) . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C5 121.1(5) . . ? C9 C10 H10A 119.4 . . ? C5 C10 H10A 119.4 . . ? N3 C11 C8 112.2(4) . . ? N3 C11 H11A 109.2 . . ? C8 C11 H11A 109.2 . . ? N3 C11 H11B 109.2 . . ? C8 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N3 C12 C13 103.6(6) . . ? N3 C12 H12A 128.2 . . ? C13 C12 H12A 128.2 . . ? N4 C13 C12 107.9(5) . . ? N4 C13 H13A 126.0 . . ? C12 C13 H13A 126.0 . . ? N4 C14 N3 109.2(6) . . ? N4 C14 H14A 125.4 . . ? N3 C14 H14A 125.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.079 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.098 # Attachment 'compound_2.CIF' data_193a _database_code_depnum_ccdc_archive 'CCDC 792969' #TrackingRef 'compound_2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 Mo5 N8 Na O25 P2' _chemical_formula_weight 1450.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 11.467(2) _cell_length_b 12.372(3) _cell_length_c 16.851(3) _cell_angle_alpha 70.23(3) _cell_angle_beta 81.19(3) _cell_angle_gamma 88.27(3) _cell_volume 2222.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21640 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.711 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 21640 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9995 _reflns_number_gt 7600 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. During the refinement, the restraint command 'DELU' was also used to refine the rigid bond (N1-C2). It makes the two atoms (N1, C2) with more reasonable ADP value. The restraint command 'ISOR' was also used to refine non-H atom (OW1) with NPD and ADP problems. These restraint commands led to a restraint value (7), but it cannot be totally avoided in order to get a reasonable refinement. ; _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^)+(0.0725P)^2^+1.6513P] 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 9995 _refine_ls_number_parameters 631 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.0071(2) -0.2483(2) 0.53814(16) 0.0345(6) Uani 1 1 d . . . Mo1 Mo 0.19248(4) -0.10629(4) 0.35148(3) 0.02218(12) Uani 1 1 d . . . Mo2 Mo 0.15060(5) 0.17720(4) 0.29796(3) 0.02474(13) Uani 1 1 d . . . Mo3 Mo -0.05852(5) -0.23342(4) 0.33788(3) 0.02571(13) Uani 1 1 d . . . Mo4 Mo -0.24298(5) -0.03125(5) 0.24463(3) 0.02885(13) Uani 1 1 d . . . Mo5 Mo -0.10720(5) 0.22918(5) 0.18634(3) 0.03086(14) Uani 1 1 d . . . P1 P -0.08898(13) 0.01449(12) 0.39265(9) 0.0202(3) Uani 1 1 d . . . P2 P 0.06538(14) 0.00825(13) 0.17844(9) 0.0248(3) Uani 1 1 d . . . O23 O 0.2067(4) 0.0363(3) 0.3746(3) 0.0263(9) Uani 1 1 d . . . O22 O 0.1096(4) -0.2062(3) 0.3137(3) 0.0269(9) Uani 1 1 d . . . O21 O -0.2038(4) 0.1203(4) 0.1652(3) 0.0355(10) Uani 1 1 d . . . O20 O -0.0435(4) -0.0744(3) 0.2178(2) 0.0261(9) Uani 1 1 d . . . O19 O 0.1970(4) -0.1950(4) 0.4545(3) 0.0323(10) Uani 1 1 d . . . O18 O -0.2093(4) -0.1665(4) 0.3367(3) 0.0301(9) Uani 1 1 d . . . O17 O -0.0208(4) -0.0963(3) 0.3991(2) 0.0240(8) Uani 1 1 d . . . O16 O 0.1222(4) 0.0256(3) 0.2520(2) 0.0271(9) Uani 1 1 d . . . O15 O 0.1625(4) 0.2654(4) 0.3563(3) 0.0331(10) Uani 1 1 d . . . O14 O -0.0115(4) 0.1070(3) 0.3981(2) 0.0248(8) Uani 1 1 d . . . O13 O -0.1433(4) 0.0578(3) 0.3100(2) 0.0276(9) Uani 1 1 d . . . O12 O -0.1974(4) -0.0130(4) 0.4653(3) 0.0296(9) Uani 1 1 d . . . O11 O 0.0256(4) 0.1265(4) 0.1284(2) 0.0335(10) Uani 1 1 d . . . O10 O 0.0304(4) 0.2466(4) 0.2335(3) 0.0338(10) Uani 1 1 d . . . O9 O 0.3294(4) -0.1097(4) 0.2982(3) 0.0352(10) Uani 1 1 d . . . O8 O -0.0679(4) -0.3223(4) 0.2806(3) 0.0389(11) Uani 1 1 d . . . O7 O -0.0729(5) -0.3273(4) 0.4407(3) 0.0403(11) Uani 1 1 d . . . O6 O -0.2729(5) -0.0938(5) 0.1741(3) 0.0481(13) Uani 1 1 d . . . O5 O 0.1557(4) -0.0397(4) 0.1248(3) 0.0332(10) Uani 1 1 d . . . O4 O -0.3780(4) -0.0060(5) 0.2916(3) 0.0452(12) Uani 1 1 d . . . O3 O -0.0840(5) 0.3333(4) 0.0888(3) 0.0494(13) Uani 1 1 d . . . O2 O 0.2718(5) 0.2171(4) 0.2218(3) 0.0422(12) Uani 1 1 d . . . O1 O -0.2093(5) 0.2892(5) 0.2422(4) 0.0544(14) Uani 1 1 d . . . N1 N 0.0870(9) 0.5720(8) 0.1135(6) 0.081(2) Uani 1 1 d U . . N2 N 0.1648(6) 0.5796(5) 0.2240(4) 0.0426(14) Uani 1 1 d . . . N3 N 0.7678(5) 0.6210(5) 0.1364(4) 0.0374(13) Uani 1 1 d . . . N4 N 0.8539(6) 0.7356(5) 0.0158(4) 0.0436(14) Uani 1 1 d . . . C1 C 0.1618(7) 0.6844(6) 0.1693(5) 0.0442(17) Uani 1 1 d . . . H1A H 0.1882 0.7503 0.1764 0.053 Uiso 1 1 calc R . . C2 C 0.1161(7) 0.6819(6) 0.1036(4) 0.0394(16) Uani 1 1 d U . . H2A H 0.1050 0.7459 0.0569 0.047 Uiso 1 1 calc R . . C3 C 0.1166(8) 0.5030(8) 0.1930(6) 0.062(2) Uani 1 1 d . . . H3A H 0.1061 0.4239 0.2189 0.074 Uiso 1 1 calc R . . C4 C 0.2153(7) 0.5450(7) 0.3047(5) 0.0452(17) Uani 1 1 d . . . H4A H 0.1893 0.4673 0.3396 0.054 Uiso 1 1 calc R . . H4B H 0.1881 0.5957 0.3365 0.054 Uiso 1 1 calc R . . C5 C 0.3477(7) 0.5514(6) 0.2848(4) 0.0360(15) Uani 1 1 d . . . C6 C 0.4102(8) 0.6543(6) 0.2634(5) 0.0477(19) Uani 1 1 d . . . H6A H 0.3693 0.7209 0.2618 0.057 Uiso 1 1 calc R . . C7 C 0.5316(8) 0.6597(7) 0.2445(5) 0.049(2) Uani 1 1 d . . . H7A H 0.5722 0.7294 0.2299 0.059 Uiso 1 1 calc R . . C8 C 0.5930(6) 0.5597(6) 0.2476(4) 0.0341(14) Uani 1 1 d . . . C9 C 0.5333(7) 0.4570(6) 0.2698(5) 0.0441(17) Uani 1 1 d . . . H9A H 0.5750 0.3906 0.2720 0.053 Uiso 1 1 calc R . . C10 C 0.4108(7) 0.4513(6) 0.2889(5) 0.0393(16) Uani 1 1 d . . . H10A H 0.3708 0.3812 0.3044 0.047 Uiso 1 1 calc R . . C11 C 0.7248(7) 0.5672(8) 0.2277(5) 0.053(2) Uani 1 1 d . . . H11A H 0.7545 0.6112 0.2586 0.063 Uiso 1 1 calc R . . H11B H 0.7558 0.4905 0.2473 0.063 Uiso 1 1 calc R . . C12 C 0.8311(7) 0.7161(6) 0.0981(5) 0.0387(15) Uani 1 1 d . . . H12A H 0.8563 0.7629 0.1255 0.046 Uiso 1 1 calc R . . C13 C 0.8023(9) 0.6508(9) -0.0001(6) 0.063(2) Uani 1 1 d . . . H13A H 0.8040 0.6432 -0.0533 0.075 Uiso 1 1 calc R . . C14 C 0.7477(9) 0.5791(9) 0.0743(6) 0.069(3) Uani 1 1 d . . . H14A H 0.7043 0.5130 0.0823 0.083 Uiso 1 1 calc R . . N5 N 0.4965(5) -0.2017(5) 0.5069(4) 0.0378(13) Uani 1 1 d . . . N6 N 0.4236(7) -0.1325(6) 0.6050(5) 0.0560(18) Uani 1 1 d . . . C15 C 0.3991(8) -0.1768(8) 0.5476(6) 0.054(2) Uani 1 1 d . . . H15A H 0.3235 -0.1884 0.5378 0.065 Uiso 1 1 calc R . . C16 C 0.5411(9) -0.1296(7) 0.6004(7) 0.065(3) Uani 1 1 d . . . H16A H 0.5825 -0.1025 0.6335 0.078 Uiso 1 1 calc R . . C17 C 0.5890(8) -0.1728(7) 0.5395(7) 0.060(2) Uani 1 1 d . . . H17A H 0.6689 -0.1814 0.5228 0.072 Uiso 1 1 calc R . . C18 C 0.5063(9) -0.2497(6) 0.4377(4) 0.050(2) Uani 1 1 d . . . H18A H 0.5800 -0.2231 0.3998 0.060 Uiso 1 1 calc R . . H18B H 0.4423 -0.2221 0.4050 0.060 Uiso 1 1 calc R . . C19 C 0.5021(7) -0.3816(6) 0.4714(4) 0.0409(17) Uani 1 1 d . . . C20 C 0.6064(7) -0.4425(7) 0.4746(5) 0.0483(18) Uani 1 1 d . . . H20A H 0.6787 -0.4030 0.4570 0.058 Uiso 1 1 calc R . . C21 C 0.3969(7) -0.4409(7) 0.4969(5) 0.0488(19) Uani 1 1 d . . . H21A H 0.3267 -0.4010 0.4946 0.059 Uiso 1 1 calc R . . N7 N 0.5022(6) 0.1849(5) 0.0529(4) 0.0398(14) Uani 1 1 d . . . N8 N 0.3607(6) 0.0632(6) 0.0699(5) 0.0493(16) Uani 1 1 d . . . C22 C 0.4234(8) 0.1094(7) 0.1093(5) 0.0499(19) Uani 1 1 d . . . H22A H 0.4144 0.0922 0.1681 0.060 Uiso 1 1 calc R . . C23 C 0.4004(8) 0.1093(7) -0.0149(6) 0.052(2) Uani 1 1 d . . . H23A H 0.3719 0.0915 -0.0579 0.062 Uiso 1 1 calc R . . C24 C 0.4871(8) 0.1844(8) -0.0260(5) 0.052(2) Uani 1 1 d . . . H24A H 0.5298 0.2286 -0.0779 0.062 Uiso 1 1 calc R . . C25 C 0.5788(8) 0.2679(7) 0.0682(6) 0.054(2) Uani 1 1 d . . . H25A H 0.5788 0.2478 0.1290 0.065 Uiso 1 1 calc R . . H25B H 0.6591 0.2632 0.0415 0.065 Uiso 1 1 calc R . . C26 C 0.5384(7) 0.3857(6) 0.0339(5) 0.0434(18) Uani 1 1 d . . . C27 C 0.4488(8) 0.4283(7) 0.0790(5) 0.0491(19) Uani 1 1 d . . . H27A H 0.4136 0.3816 0.1327 0.059 Uiso 1 1 calc R . . C28 C 0.5902(7) 0.4579(7) -0.0446(5) 0.0493(19) Uani 1 1 d . . . H28A H 0.6517 0.4316 -0.0756 0.059 Uiso 1 1 calc R . . OW1 O 0.0954(10) 0.8885(7) 0.0034(5) 0.116(3) Uani 1 1 d U . . OW2A O 0.0692(13) -0.4430(10) 0.5941(9) 0.061(3) Uani 0.50 1 d P . . OW2B O 0.0865(14) -0.4002(12) 0.6367(9) 0.074(4) Uani 0.50 1 d P . . 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 Na1 0.0397(16) 0.0304(13) 0.0332(12) -0.0127(10) 0.0004(11) -0.0029(11) Mo1 0.0204(3) 0.0213(2) 0.0266(2) -0.00963(19) -0.00515(19) -0.00007(18) Mo2 0.0257(3) 0.0209(3) 0.0266(2) -0.00841(19) 0.0012(2) -0.00501(19) Mo3 0.0255(3) 0.0247(3) 0.0300(3) -0.0122(2) -0.0056(2) -0.0030(2) Mo4 0.0242(3) 0.0357(3) 0.0317(3) -0.0160(2) -0.0089(2) 0.0010(2) Mo5 0.0341(3) 0.0275(3) 0.0295(3) -0.0065(2) -0.0089(2) 0.0053(2) P1 0.0193(7) 0.0226(7) 0.0196(6) -0.0085(5) -0.0023(5) -0.0017(5) P2 0.0273(8) 0.0285(8) 0.0199(6) -0.0103(6) -0.0020(6) -0.0012(6) O23 0.029(2) 0.022(2) 0.030(2) -0.0107(16) -0.0081(18) 0.0014(17) O22 0.027(2) 0.023(2) 0.034(2) -0.0148(17) -0.0064(18) 0.0010(17) O21 0.040(3) 0.038(3) 0.029(2) -0.0077(19) -0.015(2) 0.002(2) O20 0.025(2) 0.031(2) 0.0233(19) -0.0106(17) -0.0058(17) -0.0005(17) O19 0.031(2) 0.031(2) 0.033(2) -0.0056(18) -0.0110(19) -0.0013(19) O18 0.024(2) 0.032(2) 0.034(2) -0.0120(18) -0.0018(18) -0.0050(18) O17 0.025(2) 0.022(2) 0.0272(19) -0.0108(16) -0.0045(17) -0.0001(16) O16 0.031(2) 0.026(2) 0.0234(19) -0.0078(16) -0.0033(17) -0.0033(18) O15 0.030(3) 0.032(2) 0.038(2) -0.0150(19) 0.000(2) -0.0085(19) O14 0.028(2) 0.026(2) 0.0231(18) -0.0111(16) -0.0021(17) -0.0066(17) O13 0.034(2) 0.025(2) 0.026(2) -0.0075(16) -0.0115(18) 0.0006(18) O12 0.022(2) 0.041(3) 0.027(2) -0.0145(18) 0.0014(17) -0.0053(18) O11 0.041(3) 0.037(3) 0.0204(19) -0.0058(17) -0.0065(19) 0.005(2) O10 0.038(3) 0.030(2) 0.033(2) -0.0088(18) -0.008(2) 0.000(2) O9 0.031(3) 0.037(3) 0.042(2) -0.018(2) -0.006(2) 0.001(2) O8 0.034(3) 0.040(3) 0.053(3) -0.027(2) -0.009(2) 0.000(2) O7 0.048(3) 0.034(3) 0.037(2) -0.009(2) -0.003(2) -0.005(2) O6 0.046(3) 0.064(4) 0.052(3) -0.035(3) -0.025(3) 0.006(3) O5 0.032(3) 0.040(3) 0.030(2) -0.0177(19) 0.0013(19) 0.001(2) O4 0.028(3) 0.056(3) 0.057(3) -0.027(3) -0.007(2) 0.005(2) O3 0.061(4) 0.037(3) 0.039(3) 0.002(2) -0.008(3) 0.009(3) O2 0.038(3) 0.037(3) 0.043(3) -0.011(2) 0.014(2) -0.010(2) O1 0.055(4) 0.044(3) 0.061(3) -0.018(3) -0.001(3) 0.013(3) N1 0.070(6) 0.077(6) 0.091(6) -0.023(5) -0.015(5) 0.007(5) N2 0.034(3) 0.044(4) 0.047(3) -0.016(3) 0.003(3) 0.002(3) N3 0.035(3) 0.037(3) 0.040(3) -0.011(2) -0.005(3) -0.008(3) N4 0.041(4) 0.040(3) 0.045(3) -0.010(3) 0.000(3) 0.003(3) C1 0.042(4) 0.027(4) 0.053(4) -0.005(3) 0.004(3) 0.002(3) C2 0.040(4) 0.037(4) 0.037(3) -0.009(3) -0.001(3) 0.006(3) C3 0.056(6) 0.049(5) 0.089(7) -0.031(5) -0.023(5) 0.009(4) C4 0.047(5) 0.042(4) 0.043(4) -0.014(3) 0.000(3) 0.009(3) C5 0.040(4) 0.039(4) 0.031(3) -0.013(3) -0.007(3) 0.002(3) C6 0.065(6) 0.034(4) 0.047(4) -0.020(3) -0.001(4) -0.004(4) C7 0.061(5) 0.050(5) 0.036(4) -0.014(3) -0.004(4) -0.020(4) C8 0.036(4) 0.039(4) 0.022(3) -0.003(2) -0.005(3) -0.009(3) C9 0.042(4) 0.034(4) 0.048(4) -0.003(3) -0.008(3) 0.003(3) C10 0.042(4) 0.026(3) 0.049(4) -0.009(3) -0.011(3) 0.001(3) C11 0.038(4) 0.068(6) 0.039(4) 0.002(4) -0.011(3) -0.014(4) C12 0.036(4) 0.030(4) 0.051(4) -0.014(3) -0.006(3) 0.001(3) C13 0.059(6) 0.079(7) 0.052(5) -0.026(5) -0.001(4) -0.022(5) C14 0.063(6) 0.083(7) 0.069(6) -0.041(5) 0.011(5) -0.038(5) N5 0.035(3) 0.027(3) 0.048(3) -0.008(2) -0.007(3) 0.001(2) N6 0.060(5) 0.062(5) 0.059(4) -0.033(4) -0.023(4) 0.016(4) C15 0.039(5) 0.071(6) 0.067(5) -0.037(5) -0.025(4) 0.018(4) C16 0.075(7) 0.041(5) 0.086(7) -0.015(4) -0.044(6) -0.013(4) C17 0.032(4) 0.047(5) 0.096(7) -0.014(5) -0.015(5) -0.013(4) C18 0.074(6) 0.033(4) 0.033(3) 0.000(3) -0.002(4) 0.009(4) C19 0.055(5) 0.040(4) 0.027(3) -0.011(3) -0.006(3) 0.010(3) C20 0.038(4) 0.049(5) 0.054(4) -0.017(4) 0.004(4) 0.000(3) C21 0.040(4) 0.047(5) 0.059(5) -0.019(4) -0.010(4) 0.019(4) N7 0.038(3) 0.037(3) 0.046(3) -0.013(3) -0.010(3) -0.004(3) N8 0.038(4) 0.043(4) 0.072(4) -0.031(3) 0.004(3) -0.005(3) C22 0.051(5) 0.054(5) 0.044(4) -0.021(4) 0.006(4) -0.002(4) C23 0.063(6) 0.042(4) 0.059(5) -0.021(4) -0.026(4) 0.008(4) C24 0.050(5) 0.060(5) 0.042(4) -0.010(4) -0.010(4) -0.008(4) C25 0.042(5) 0.061(5) 0.066(5) -0.023(4) -0.023(4) -0.014(4) C26 0.047(5) 0.040(4) 0.046(4) -0.014(3) -0.014(4) -0.014(3) C27 0.052(5) 0.047(5) 0.041(4) -0.008(3) 0.000(4) -0.018(4) C28 0.039(4) 0.051(5) 0.062(5) -0.027(4) 0.003(4) -0.011(4) OW1 0.206(8) 0.091(5) 0.068(4) -0.039(4) -0.038(5) -0.012(5) OW2A 0.073(9) 0.029(6) 0.073(8) -0.009(6) -0.008(7) 0.003(6) OW2B 0.081(11) 0.060(9) 0.067(9) -0.005(7) -0.016(8) 0.016(8) _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 Na1 OW2B 2.317(13) . ? Na1 O14 2.347(4) 2_556 ? Na1 O19 2.384(6) . ? Na1 O15 2.388(5) 2_556 ? Na1 OW2A 2.401(12) . ? Na1 O7 2.468(5) . ? Na1 O17 2.518(5) . ? Na1 Mo2 3.419(3) 2_556 ? Na1 Mo1 3.455(3) . ? Na1 Mo3 3.512(3) . ? Mo1 O9 1.691(5) . ? Mo1 O19 1.719(4) . ? Mo1 O22 1.903(4) . ? Mo1 O23 1.948(4) . ? Mo1 O16 2.146(4) . ? Mo1 O17 2.468(4) . ? Mo2 O2 1.700(5) . ? Mo2 O15 1.717(4) . ? Mo2 O10 1.890(4) . ? Mo2 O23 1.945(4) . ? Mo2 O14 2.281(4) . ? Mo2 O16 2.307(4) . ? Mo2 Na1 3.419(3) 2_556 ? Mo3 O8 1.706(4) . ? Mo3 O7 1.715(5) . ? Mo3 O18 1.894(5) . ? Mo3 O22 1.924(4) . ? Mo3 O20 2.284(4) . ? Mo3 O17 2.344(4) . ? Mo4 O4 1.699(5) . ? Mo4 O6 1.701(4) . ? Mo4 O21 1.918(5) . ? Mo4 O18 1.935(4) . ? Mo4 O13 2.239(4) . ? Mo4 O20 2.344(4) . ? Mo5 O3 1.699(5) . ? Mo5 O1 1.700(6) . ? Mo5 O10 1.920(4) . ? Mo5 O21 1.925(5) . ? Mo5 O11 2.270(5) . ? Mo5 O13 2.410(4) . ? P1 O14 1.505(4) . ? P1 O13 1.536(4) . ? P1 O17 1.537(4) . ? P1 O12 1.562(4) . ? P2 O5 1.511(5) . ? P2 O11 1.517(5) . ? P2 O20 1.552(4) . ? P2 O16 1.563(4) . ? O15 Na1 2.388(5) 2_556 ? O14 Na1 2.347(4) 2_556 ? N1 C2 1.358(11) . ? N1 C3 1.409(12) . ? N2 C1 1.315(9) . ? N2 C3 1.391(10) . ? N2 C4 1.484(9) . ? N3 C12 1.312(9) . ? N3 C14 1.365(10) . ? N3 C11 1.465(9) . ? N4 C12 1.310(9) . ? N4 C13 1.341(10) . ? C1 C2 1.305(10) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.503(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.390(10) . ? C5 C10 1.402(10) . ? C6 C7 1.379(12) . ? C6 H6A 0.9300 . ? C7 C8 1.394(11) . ? C7 H7A 0.9300 . ? C8 C9 1.371(10) . ? C8 C11 1.495(10) . ? C9 C10 1.391(11) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9300 . ? C13 C14 1.338(12) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? N5 C15 1.303(10) . ? N5 C17 1.374(9) . ? N5 C18 1.467(9) . ? N6 C15 1.330(10) . ? N6 C16 1.339(12) . ? C15 H15A 0.9300 . ? C16 C17 1.351(14) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.534(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C21 1.364(11) . ? C19 C20 1.392(11) . ? C20 C21 1.358(11) 2_646 ? C20 H20A 0.9300 . ? C21 C20 1.358(11) 2_646 ? C21 H21A 0.9300 . ? N7 C22 1.335(10) . ? N7 C24 1.368(9) . ? N7 C25 1.481(9) . ? N8 C22 1.309(10) . ? N8 C23 1.357(11) . ? C22 H22A 0.9300 . ? C23 C24 1.330(12) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.464(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C28 1.376(11) . ? C26 C27 1.381(12) . ? C27 C28 1.417(12) 2_665 ? C27 H27A 0.9300 . ? C28 C27 1.417(12) 2_665 ? C28 H28A 0.9300 . ? OW2A OW2B 1.068(16) . ? 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 OW2B Na1 O14 100.0(4) . 2_556 ? OW2B Na1 O19 90.9(4) . . ? O14 Na1 O19 93.92(17) 2_556 . ? OW2B Na1 O15 88.0(4) . 2_556 ? O14 Na1 O15 68.96(16) 2_556 2_556 ? O19 Na1 O15 162.33(18) . 2_556 ? OW2B Na1 OW2A 26.1(4) . . ? O14 Na1 OW2A 126.1(4) 2_556 . ? O19 Na1 OW2A 89.9(4) . . ? O15 Na1 OW2A 96.7(4) 2_556 . ? OW2B Na1 O7 107.0(4) . . ? O14 Na1 O7 150.8(2) 2_556 . ? O19 Na1 O7 96.44(18) . . ? O15 Na1 O7 100.76(18) 2_556 . ? OW2A Na1 O7 81.2(4) . . ? OW2B Na1 O17 160.8(4) . . ? O14 Na1 O17 90.33(15) 2_556 . ? O19 Na1 O17 72.23(15) . . ? O15 Na1 O17 110.86(18) 2_556 . ? OW2A Na1 O17 141.0(4) . . ? O7 Na1 O17 67.28(15) . . ? OW2B Na1 Mo2 89.4(4) . 2_556 ? O14 Na1 Mo2 41.62(11) 2_556 2_556 ? O19 Na1 Mo2 134.59(14) . 2_556 ? O15 Na1 Mo2 27.81(10) 2_556 2_556 ? OW2A Na1 Mo2 108.3(3) . 2_556 ? O7 Na1 Mo2 126.67(16) . 2_556 ? O17 Na1 Mo2 108.80(13) . 2_556 ? OW2B Na1 Mo1 116.6(4) . . ? O14 Na1 Mo1 96.96(13) 2_556 . ? O19 Na1 Mo1 27.08(10) . . ? O15 Na1 Mo1 154.05(15) 2_556 . ? OW2A Na1 Mo1 109.1(4) . . ? O7 Na1 Mo1 80.84(13) . . ? O17 Na1 Mo1 45.53(11) . . ? Mo2 Na1 Mo1 136.35(8) 2_556 . ? OW2B Na1 Mo3 128.0(4) . . ? O14 Na1 Mo3 131.49(14) 2_556 . ? O19 Na1 Mo3 80.13(12) . . ? O15 Na1 Mo3 114.17(14) 2_556 . ? OW2A Na1 Mo3 102.2(3) . . ? O7 Na1 Mo3 26.71(11) . . ? O17 Na1 Mo3 41.81(9) . . ? Mo2 Na1 Mo3 132.04(9) 2_556 . ? Mo1 Na1 Mo3 58.32(4) . . ? O9 Mo1 O19 105.2(2) . . ? O9 Mo1 O22 100.1(2) . . ? O19 Mo1 O22 99.05(19) . . ? O9 Mo1 O23 99.7(2) . . ? O19 Mo1 O23 95.42(19) . . ? O22 Mo1 O23 151.40(18) . . ? O9 Mo1 O16 98.2(2) . . ? O19 Mo1 O16 155.6(2) . . ? O22 Mo1 O16 83.38(16) . . ? O23 Mo1 O16 73.55(16) . . ? O9 Mo1 O17 167.53(17) . . ? O19 Mo1 O17 85.38(18) . . ? O22 Mo1 O17 71.25(16) . . ? O23 Mo1 O17 85.57(16) . . ? O16 Mo1 O17 72.35(15) . . ? O9 Mo1 Na1 142.36(16) . . ? O19 Mo1 Na1 39.16(16) . . ? O22 Mo1 Na1 80.07(14) . . ? O23 Mo1 Na1 96.36(14) . . ? O16 Mo1 Na1 119.04(13) . . ? O17 Mo1 Na1 46.74(10) . . ? O2 Mo2 O15 102.1(2) . . ? O2 Mo2 O10 100.7(2) . . ? O15 Mo2 O10 102.5(2) . . ? O2 Mo2 O23 99.9(2) . . ? O15 Mo2 O23 98.77(19) . . ? O10 Mo2 O23 146.35(18) . . ? O2 Mo2 O14 174.48(19) . . ? O15 Mo2 O14 82.94(18) . . ? O10 Mo2 O14 80.17(18) . . ? O23 Mo2 O14 76.94(17) . . ? O2 Mo2 O16 88.3(2) . . ? O15 Mo2 O16 166.03(18) . . ? O10 Mo2 O16 84.34(17) . . ? O23 Mo2 O16 69.97(15) . . ? O14 Mo2 O16 86.34(14) . . ? O2 Mo2 Na1 142.16(17) . 2_556 ? O15 Mo2 Na1 40.45(16) . 2_556 ? O10 Mo2 Na1 86.78(15) . 2_556 ? O23 Mo2 Na1 92.98(13) . 2_556 ? O14 Mo2 Na1 43.12(10) . 2_556 ? O16 Mo2 Na1 129.46(12) . 2_556 ? O8 Mo3 O7 102.6(2) . . ? O8 Mo3 O18 101.7(2) . . ? O7 Mo3 O18 101.0(2) . . ? O8 Mo3 O22 98.5(2) . . ? O7 Mo3 O22 100.6(2) . . ? O18 Mo3 O22 146.23(17) . . ? O8 Mo3 O20 91.8(2) . . ? O7 Mo3 O20 165.44(19) . . ? O18 Mo3 O20 73.49(17) . . ? O22 Mo3 O20 79.17(17) . . ? O8 Mo3 O17 170.7(2) . . ? O7 Mo3 O17 84.29(18) . . ? O18 Mo3 O17 82.74(16) . . ? O22 Mo3 O17 73.91(15) . . ? O20 Mo3 O17 81.66(14) . . ? O8 Mo3 Na1 139.00(17) . . ? O7 Mo3 Na1 40.32(16) . . ? O18 Mo3 Na1 102.54(14) . . ? O22 Mo3 Na1 78.29(13) . . ? O20 Mo3 Na1 126.68(11) . . ? O17 Mo3 Na1 45.75(10) . . ? O4 Mo4 O6 104.3(3) . . ? O4 Mo4 O21 99.2(2) . . ? O6 Mo4 O21 98.1(2) . . ? O4 Mo4 O18 97.3(2) . . ? O6 Mo4 O18 99.7(2) . . ? O21 Mo4 O18 151.87(18) . . ? O4 Mo4 O13 94.6(2) . . ? O6 Mo4 O13 160.4(2) . . ? O21 Mo4 O13 73.41(16) . . ? O18 Mo4 O13 82.69(16) . . ? O4 Mo4 O20 163.97(19) . . ? O6 Mo4 O20 89.1(2) . . ? O21 Mo4 O20 87.34(18) . . ? O18 Mo4 O20 71.40(17) . . ? O13 Mo4 O20 73.12(15) . . ? O3 Mo5 O1 102.2(3) . . ? O3 Mo5 O10 102.1(2) . . ? O1 Mo5 O10 99.9(2) . . ? O3 Mo5 O21 101.3(2) . . ? O1 Mo5 O21 101.1(3) . . ? O10 Mo5 O21 144.29(19) . . ? O3 Mo5 O11 85.8(2) . . ? O1 Mo5 O11 171.9(2) . . ? O10 Mo5 O11 78.92(18) . . ? O21 Mo5 O11 76.32(19) . . ? O3 Mo5 O13 169.3(2) . . ? O1 Mo5 O13 85.1(2) . . ? O10 Mo5 O13 84.08(17) . . ? O21 Mo5 O13 69.34(15) . . ? O11 Mo5 O13 86.86(15) . . ? O14 P1 O13 110.1(2) . . ? O14 P1 O17 111.6(2) . . ? O13 P1 O17 111.0(2) . . ? O14 P1 O12 110.4(2) . . ? O13 P1 O12 104.4(2) . . ? O17 P1 O12 109.0(2) . . ? O5 P2 O11 112.4(3) . . ? O5 P2 O20 110.9(3) . . ? O11 P2 O20 109.6(3) . . ? O5 P2 O16 109.4(3) . . ? O11 P2 O16 105.2(2) . . ? O20 P2 O16 109.0(2) . . ? Mo2 O23 Mo1 118.85(19) . . ? Mo1 O22 Mo3 125.0(2) . . ? Mo4 O21 Mo5 123.6(2) . . ? P2 O20 Mo3 126.4(2) . . ? P2 O20 Mo4 129.3(2) . . ? Mo3 O20 Mo4 92.83(16) . . ? Mo1 O19 Na1 113.8(2) . . ? Mo3 O18 Mo4 122.2(2) . . ? P1 O17 Mo3 126.4(2) . . ? P1 O17 Mo1 125.5(2) . . ? Mo3 O17 Mo1 89.74(14) . . ? P1 O17 Na1 123.8(2) . . ? Mo3 O17 Na1 92.44(14) . . ? Mo1 O17 Na1 87.73(15) . . ? P2 O16 Mo1 126.3(2) . . ? P2 O16 Mo2 136.0(2) . . ? Mo1 O16 Mo2 97.62(15) . . ? Mo2 O15 Na1 111.7(2) . 2_556 ? P1 O14 Mo2 120.6(2) . . ? P1 O14 Na1 142.7(3) . 2_556 ? Mo2 O14 Na1 95.26(16) . 2_556 ? P1 O13 Mo4 132.6(2) . . ? P1 O13 Mo5 132.1(2) . . ? Mo4 O13 Mo5 93.42(13) . . ? P2 O11 Mo5 123.4(2) . . ? Mo2 O10 Mo5 148.7(3) . . ? Mo3 O7 Na1 113.0(2) . . ? C2 N1 C3 106.5(8) . . ? C1 N2 C3 109.2(7) . . ? C1 N2 C4 126.6(7) . . ? C3 N2 C4 124.1(7) . . ? C12 N3 C14 106.8(6) . . ? C12 N3 C11 128.2(6) . . ? C14 N3 C11 125.0(7) . . ? C12 N4 C13 107.7(7) . . ? N2 C1 C2 109.9(7) . . ? N2 C1 H1A 125.1 . . ? C2 C1 H1A 125.1 . . ? C1 C2 N1 109.9(7) . . ? C1 C2 H2A 125.1 . . ? N1 C2 H2A 125.1 . . ? N1 C3 N2 104.6(8) . . ? N1 C3 H3A 127.7 . . ? N2 C3 H3A 127.7 . . ? N2 C4 C5 109.4(6) . . ? N2 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 118.7(7) . . ? C6 C5 C4 121.6(7) . . ? C10 C5 C4 119.7(7) . . ? C7 C6 C5 121.3(8) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 119.3(7) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 120.3(7) . . ? C9 C8 C11 121.1(7) . . ? C7 C8 C11 118.5(7) . . ? C8 C9 C10 120.4(7) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C5 119.9(7) . . ? C9 C10 H10A 120.0 . . ? C5 C10 H10A 120.0 . . ? N3 C11 C8 112.9(6) . . ? N3 C11 H11A 109.0 . . ? C8 C11 H11A 109.0 . . ? N3 C11 H11B 109.0 . . ? C8 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N4 C12 N3 110.4(6) . . ? N4 C12 H12A 124.8 . . ? N3 C12 H12A 124.8 . . ? N4 C13 C14 107.8(8) . . ? N4 C13 H13A 126.1 . . ? C14 C13 H13A 126.1 . . ? N3 C14 C13 107.3(8) . . ? N3 C14 H14A 126.4 . . ? C13 C14 H14A 126.4 . . ? C15 N5 C17 107.7(7) . . ? C15 N5 C18 126.4(7) . . ? C17 N5 C18 125.9(8) . . ? C15 N6 C16 107.6(8) . . ? N5 C15 N6 110.1(7) . . ? N5 C15 H15A 125.0 . . ? N6 C15 H15A 125.0 . . ? N6 C16 C17 108.1(7) . . ? N6 C16 H16A 125.9 . . ? C17 C16 H16A 125.9 . . ? C16 C17 N5 106.5(8) . . ? C16 C17 H17A 126.7 . . ? N5 C17 H17A 126.7 . . ? N5 C18 C19 112.1(5) . . ? N5 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N5 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C21 C19 C20 119.0(7) . . ? C21 C19 C18 120.9(7) . . ? C20 C19 C18 120.2(8) . . ? C21 C20 C19 120.4(8) 2_646 . ? C21 C20 H20A 119.8 2_646 . ? C19 C20 H20A 119.8 . . ? C20 C21 C19 120.6(7) 2_646 . ? C20 C21 H21A 119.7 2_646 . ? C19 C21 H21A 119.7 . . ? C22 N7 C24 106.6(6) . . ? C22 N7 C25 128.0(7) . . ? C24 N7 C25 124.7(7) . . ? C22 N8 C23 107.5(7) . . ? N8 C22 N7 110.1(7) . . ? N8 C22 H22A 124.9 . . ? N7 C22 H22A 124.9 . . ? C24 C23 N8 108.2(7) . . ? C24 C23 H23A 125.9 . . ? N8 C23 H23A 125.9 . . ? C23 C24 N7 107.6(8) . . ? C23 C24 H24A 126.2 . . ? N7 C24 H24A 126.2 . . ? C26 C25 N7 111.6(6) . . ? C26 C25 H25A 109.3 . . ? N7 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? N7 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C28 C26 C27 118.0(7) . . ? C28 C26 C25 120.4(8) . . ? C27 C26 C25 121.7(7) . . ? C26 C27 C28 121.0(7) . 2_665 ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 2_665 . ? C26 C28 C27 121.0(8) . 2_665 ? C26 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 2_665 . ? OW2B OW2A Na1 72.5(9) . . ? OW2A OW2B Na1 81.4(10) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.379 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.179 # Attachment 'compound_3.CIF' data_77a _database_code_depnum_ccdc_archive 'CCDC 792970' #TrackingRef 'compound_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H52 Cd Mo6 N8 O38 P4' _chemical_formula_weight 1920.70 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' Cd Cd -0.8075 1.2024 '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' P P 0.1023 0.0942 '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' _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 12.578(3) _cell_length_b 15.148(3) _cell_length_c 16.389(3) _cell_angle_alpha 95.96(3) _cell_angle_beta 110.13(3) _cell_angle_gamma 102.95(3) _cell_volume 2800.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21039 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 24.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.684 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 21039 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.1500 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9492 _reflns_number_gt 5649 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. During the refinement, the restraint command 'ISOR' was also used to refine the non-H atoms with NPD and ADP problems. These atoms are as follows: c2 c3 o18 o27 o3w o4w o7w o8w o6w. These restraint commands led to a relative high restraint value (54), but it cannot be totally avoided in order to get a reasonable refinement. ; _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^)+(0.0667P)^2^+55.2359P] 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 9492 _refine_ls_number_parameters 778 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2061 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.5000 0.0000 0.0177(4) Uani 1 2 d S . . Cd2 Cd 0.0000 0.5000 0.5000 0.0489(6) Uani 1 2 d S . . Mo1 Mo 0.14994(13) 0.36163(9) 0.17018(9) 0.0180(3) Uani 1 1 d . . . Mo2 Mo 0.25674(13) 0.71484(9) 0.14184(9) 0.0187(3) Uani 1 1 d . . . Mo3 Mo -0.05610(13) 0.35638(9) 0.17379(9) 0.0172(3) Uani 1 1 d . . . Mo4 Mo -0.15638(13) 0.55557(9) 0.16120(9) 0.0187(3) Uani 1 1 d . . . Mo5 Mo 0.33170(13) 0.56871(9) 0.15246(9) 0.0191(3) Uani 1 1 d . . . Mo6 Mo -0.02532(13) 0.70678(9) 0.14514(9) 0.0198(3) Uani 1 1 d . . . P1 P 0.4328(4) 0.4459(3) 0.3055(3) 0.0293(11) Uani 1 1 d . . . P2 P -0.1937(4) 0.4205(3) 0.3018(3) 0.0198(9) Uani 1 1 d . . . P3 P 0.1406(4) 0.5737(2) 0.2575(3) 0.0153(8) Uani 1 1 d . . . P4 P 0.2163(4) 0.8572(3) 0.2880(3) 0.0255(10) Uani 1 1 d . . . O1 O -0.3255(10) 0.3637(8) 0.2548(8) 0.031(3) Uani 1 1 d . . . O2 O 0.1967(10) 0.6135(7) 0.3557(7) 0.028(3) Uani 1 1 d . . . O3 O 0.2570(13) 0.9591(7) 0.3252(8) 0.040(3) Uani 1 1 d . . . O4 O 0.3145(11) 0.3741(8) 0.2598(8) 0.035(3) Uani 1 1 d . . . O5 O 0.0895(10) 0.7373(6) 0.0764(7) 0.024(3) Uani 1 1 d . . . O6 O -0.1276(11) 0.2462(8) 0.1284(8) 0.033(3) Uani 1 1 d . . . O7 O -0.1616(10) 0.4347(8) 0.4004(7) 0.027(3) Uani 1 1 d . . . O8 O 0.2831(11) 0.8316(7) 0.2326(8) 0.030(3) Uani 1 1 d . . . O9 O 0.4227(11) 0.5843(7) 0.0988(8) 0.030(3) Uani 1 1 d . . . O10 O -0.1212(11) 0.3645(8) 0.2714(7) 0.029(3) Uani 1 1 d . . . O11 O 0.4449(11) 0.5234(7) 0.2543(8) 0.029(3) Uani 1 1 d . . . O12 O 0.0847(11) 0.8277(7) 0.2335(7) 0.030(3) Uani 1 1 d . . . O13 O -0.1297(11) 0.7567(7) 0.0887(7) 0.028(3) Uani 1 1 d . . . O14 O 0.3282(11) 0.7711(7) 0.0855(8) 0.031(3) Uani 1 1 d . . . O15 O -0.1785(10) 0.5131(7) 0.2704(7) 0.023(3) Uani 1 1 d . . . O16 O 0.3736(10) 0.6822(7) 0.2357(7) 0.027(3) Uani 1 1 d . . . O17 O -0.2906(11) 0.5661(8) 0.1123(7) 0.027(3) Uani 1 1 d . . . O18 O -0.0643(11) 0.6717(7) 0.2428(7) 0.025(3) Uani 1 1 d U . . O19 O 0.0131(10) 0.5123(6) 0.2278(7) 0.019(2) Uani 1 1 d . . . O20 O -0.1890(9) 0.4143(7) 0.1080(7) 0.022(2) Uani 1 1 d . . . O21 O 0.1886(9) 0.5893(6) 0.0684(7) 0.021(3) Uani 1 1 d . . . O22 O 0.1344(10) 0.6571(6) 0.2071(7) 0.020(2) Uani 1 1 d . . . O23 O 0.0917(10) 0.3559(7) 0.2661(7) 0.023(3) Uani 1 1 d . . . O24 O 0.2454(9) 0.4254(7) 0.0963(7) 0.022(2) Uani 1 1 d . . . O25 O 0.2117(9) 0.5176(6) 0.2249(7) 0.017(2) Uani 1 1 d . . . O26 O 0.0153(9) 0.3909(6) 0.0890(6) 0.014(2) Uani 1 1 d . . . O27 O -0.0849(9) 0.5811(7) 0.0717(6) 0.018(2) Uani 1 1 d U . . O28 O 0.4416(19) 0.4934(12) 0.3984(11) 0.087(6) Uani 1 1 d . . . O29 O 0.5339(12) 0.4048(10) 0.3249(10) 0.053(4) Uani 1 1 d . . . O30 O 0.1301(11) 0.2523(7) 0.1231(7) 0.028(3) Uani 1 1 d . . . O31 O 0.2422(12) 0.8114(8) 0.3716(7) 0.037(3) Uani 1 1 d . . . N1 N 0.1736(14) 0.0521(11) 1.0922(10) 0.038(4) Uani 1 1 d . . . N2 N 0.1114(15) 0.0101(10) 0.9479(10) 0.037(4) Uani 1 1 d . . . N3 N 0.4264(15) 0.0363(12) 0.6356(10) 0.041(4) Uani 1 1 d . . . N4 N 0.3605(16) 0.0227(12) 0.4937(11) 0.051(5) Uani 1 1 d . . . N5 N 0.3963(15) 0.3254(11) 0.0784(12) 0.043(4) Uani 1 1 d . . . N6 N 0.5109(13) 0.2361(8) 0.0973(9) 0.026(3) Uani 1 1 d . . . N7 N 0.330(2) 0.3419(13) 0.6847(16) 0.065(6) Uani 1 1 d . . . N8 N 0.1614(15) 0.2444(11) 0.6184(12) 0.046(4) Uani 1 1 d . . . C1 C 0.1433(18) 0.0817(11) 1.0116(12) 0.033(4) Uani 1 1 d . . . H1A H 0.1455 0.1434 1.0042 0.039 Uiso 1 1 calc R . . C2 C 0.1576(16) -0.0407(10) 1.0714(12) 0.028(4) Uani 1 1 d U . . H2A H 0.1721 -0.0792 1.1139 0.034 Uiso 1 1 calc R . . C3 C 0.1199(18) -0.0703(12) 0.9860(14) 0.040(5) Uani 1 1 d U . . H3A H 0.1018 -0.1319 0.9556 0.048 Uiso 1 1 calc R . . C4 C 0.074(2) 0.0152(15) 0.8523(12) 0.046(5) Uani 1 1 d . . . H4A H 0.0505 0.0726 0.8432 0.055 Uiso 1 1 calc R . . H4B H 0.0054 -0.0380 0.8169 0.055 Uiso 1 1 calc R . . C5 C 0.1750(18) 0.0142(12) 0.8220(13) 0.037(5) Uani 1 1 d . . . C6 C 0.1632(17) -0.0538(14) 0.7557(14) 0.044(5) Uani 1 1 d . . . H6A H 0.0920 -0.1025 0.7304 0.053 Uiso 1 1 calc R . . C7 C 0.252(2) -0.0543(15) 0.7241(13) 0.051(6) Uani 1 1 d . . . H7A H 0.2428 -0.1042 0.6798 0.062 Uiso 1 1 calc R . . C8 C 0.3538(18) 0.0181(14) 0.7572(12) 0.038(5) Uani 1 1 d . . . C9 C 0.3679(18) 0.0857(13) 0.8240(12) 0.036(5) Uani 1 1 d . . . H9A H 0.4405 0.1328 0.8513 0.043 Uiso 1 1 calc R . . C10 C 0.2764(18) 0.0861(13) 0.8523(13) 0.042(5) Uani 1 1 d . . . H10A H 0.2838 0.1378 0.8940 0.050 Uiso 1 1 calc R . . C11 C 0.455(2) 0.0146(15) 0.7269(14) 0.048(6) Uani 1 1 d . . . H11A H 0.5289 0.0600 0.7688 0.058 Uiso 1 1 calc R . . H11B H 0.4678 -0.0478 0.7261 0.058 Uiso 1 1 calc R . . C12 C 0.376(2) -0.0221(16) 0.5591(15) 0.053(6) Uani 1 1 d . . . H12A H 0.3538 -0.0875 0.5522 0.064 Uiso 1 1 calc R . . C13 C 0.411(2) 0.1137(15) 0.5308(14) 0.051(6) Uani 1 1 d . . . H13A H 0.4184 0.1624 0.4993 0.061 Uiso 1 1 calc R . . C14 C 0.448(2) 0.1239(15) 0.6194(14) 0.051(6) Uani 1 1 d . . . H14A H 0.4815 0.1802 0.6618 0.061 Uiso 1 1 calc R . . C15 C 0.4315(18) 0.2633(13) 0.1223(14) 0.041(5) Uani 1 1 d . . . H15A H 0.4044 0.2408 0.1657 0.049 Uiso 1 1 calc R . . C16 C 0.4601(18) 0.3400(13) 0.0263(12) 0.040(5) Uani 1 1 d . . . H16A H 0.4568 0.3850 -0.0101 0.048 Uiso 1 1 calc R . . C17 C 0.5273(18) 0.2834(12) 0.0330(13) 0.036(5) Uani 1 1 d . . . H17A H 0.5760 0.2767 0.0009 0.043 Uiso 1 1 calc R . . C18 C 0.5743(17) 0.1692(11) 0.1312(12) 0.034(5) Uani 1 1 d . . . H18A H 0.5594 0.1534 0.1841 0.040 Uiso 1 1 calc R . . H18B H 0.6600 0.1974 0.1494 0.040 Uiso 1 1 calc R . . C19 C 0.5356(17) 0.0816(11) 0.0615(11) 0.029(4) Uani 1 1 d . . . C20 C 0.6042(16) 0.0655(11) 0.0152(13) 0.034(5) Uani 1 1 d . . . H20A H 0.6770 0.1096 0.0265 0.041 Uiso 1 1 calc R . . C21 C 0.4324(17) 0.0147(11) 0.0477(12) 0.030(4) Uani 1 1 d . . . H21A H 0.3866 0.0240 0.0817 0.036 Uiso 1 1 calc R . . C22 C 0.231(3) 0.3205(15) 0.612(2) 0.080(9) Uani 1 1 d . . . H22A H 0.2147 0.3534 0.5644 0.096 Uiso 1 1 calc R . . C23 C 0.321(2) 0.2815(16) 0.7372(15) 0.058(7) Uani 1 1 d . . . H23A H 0.3810 0.2816 0.7917 0.070 Uiso 1 1 calc R . . C24 C 0.211(3) 0.2190(18) 0.7001(16) 0.070(8) Uani 1 1 d . . . H24A H 0.1769 0.1707 0.7239 0.085 Uiso 1 1 calc R . . C25 C 0.040(2) 0.1993(12) 0.5559(16) 0.060(7) Uani 1 1 d . . . H25A H 0.0243 0.2274 0.5026 0.072 Uiso 1 1 calc R . . H25B H -0.0154 0.2097 0.5838 0.072 Uiso 1 1 calc R . . C26 C 0.0196(19) 0.0946(14) 0.5280(15) 0.047(6) Uani 1 1 d . . . C27 C 0.066(2) 0.0617(16) 0.4715(17) 0.064(7) Uani 1 1 d . . . H27A H 0.1144 0.1044 0.4512 0.077 Uiso 1 1 calc R . . C28 C -0.046(2) 0.0330(16) 0.5572(16) 0.062(7) Uani 1 1 d . . . H28A H -0.0783 0.0537 0.5976 0.075 Uiso 1 1 calc R . . O1W O -0.0883(15) 0.5863(9) 0.5574(9) 0.055(4) Uani 1 1 d . . . O2W O -0.0305(11) 0.3931(8) 0.5757(8) 0.033(3) Uani 1 1 d . . . O3W O 0.2442(19) 0.1135(12) 1.2641(12) 0.089(6) Uani 1 1 d U . . O4W O 0.187(2) 0.2344(16) 1.3701(17) 0.125(8) Uani 1 1 d U . . O5W O 0.308(2) 0.511(2) 0.489(2) 0.183(14) Uani 1 1 d . . . O6W O -0.253(2) 0.2454(16) 0.4328(16) 0.126(8) Uani 1 1 d U . . O7W O 0.485(4) 0.208(3) 0.325(3) 0.089(12) Uani 0.50 1 d PU . . O8W O 0.461(4) 0.676(3) 0.427(3) 0.117(16) Uani 0.50 1 d PU . . 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 Cd1 0.0204(9) 0.0157(8) 0.0189(9) 0.0006(6) 0.0103(8) 0.0052(6) Cd2 0.0465(15) 0.0554(14) 0.0401(13) 0.0028(10) 0.0145(12) 0.0115(11) Mo1 0.0187(8) 0.0179(7) 0.0211(7) 0.0025(5) 0.0110(6) 0.0073(5) Mo2 0.0216(8) 0.0139(6) 0.0190(7) -0.0007(5) 0.0089(6) 0.0021(5) Mo3 0.0209(8) 0.0153(6) 0.0186(7) 0.0012(5) 0.0126(6) 0.0040(5) Mo4 0.0197(8) 0.0208(7) 0.0184(7) 0.0017(5) 0.0099(6) 0.0078(6) Mo5 0.0178(8) 0.0177(7) 0.0227(8) 0.0032(6) 0.0087(6) 0.0053(6) Mo6 0.0235(8) 0.0172(7) 0.0195(8) -0.0015(5) 0.0091(6) 0.0081(6) P1 0.024(3) 0.047(3) 0.021(2) 0.011(2) 0.011(2) 0.014(2) P2 0.023(2) 0.023(2) 0.015(2) 0.0005(16) 0.0122(19) 0.0042(17) P3 0.020(2) 0.0105(18) 0.017(2) 0.0032(15) 0.0069(18) 0.0077(16) P4 0.035(3) 0.016(2) 0.018(2) -0.0069(17) 0.007(2) 0.0040(18) O1 0.024(7) 0.032(6) 0.033(7) 0.001(5) 0.013(6) -0.002(5) O2 0.029(7) 0.028(6) 0.018(6) -0.008(5) 0.004(6) 0.005(5) O3 0.066(10) 0.018(6) 0.035(8) -0.003(5) 0.023(7) 0.004(6) O4 0.024(7) 0.039(7) 0.042(8) 0.013(6) 0.009(6) 0.012(6) O5 0.034(7) 0.012(5) 0.028(7) 0.003(5) 0.013(6) 0.011(5) O6 0.030(8) 0.035(7) 0.033(7) 0.004(5) 0.016(6) 0.003(5) O7 0.027(7) 0.041(7) 0.019(6) 0.013(5) 0.015(6) 0.010(5) O8 0.037(8) 0.021(6) 0.037(7) 0.002(5) 0.024(6) 0.008(5) O9 0.031(7) 0.025(6) 0.044(8) 0.012(5) 0.022(6) 0.011(5) O10 0.040(8) 0.034(7) 0.025(7) 0.010(5) 0.023(6) 0.013(6) O11 0.036(8) 0.025(6) 0.037(7) 0.020(5) 0.018(6) 0.014(5) O12 0.040(8) 0.017(6) 0.023(6) -0.004(5) 0.000(6) 0.009(5) O13 0.036(8) 0.018(6) 0.029(7) 0.010(5) 0.009(6) 0.012(5) O14 0.048(8) 0.011(5) 0.051(8) 0.005(5) 0.039(7) 0.011(5) O15 0.026(7) 0.029(6) 0.029(7) 0.014(5) 0.019(6) 0.016(5) O16 0.028(7) 0.023(6) 0.030(7) -0.006(5) 0.015(6) 0.005(5) O17 0.037(8) 0.035(6) 0.019(6) 0.004(5) 0.018(6) 0.016(6) O18 0.038(6) 0.020(5) 0.023(5) 0.004(4) 0.010(5) 0.022(5) O19 0.028(7) 0.011(5) 0.019(6) 0.001(4) 0.010(5) 0.007(4) O20 0.016(6) 0.024(6) 0.022(6) -0.007(5) 0.007(5) 0.001(5) O21 0.018(6) 0.015(5) 0.029(7) -0.010(4) 0.017(5) -0.004(4) O22 0.030(7) 0.012(5) 0.014(6) -0.003(4) 0.006(5) 0.004(5) O23 0.021(7) 0.026(6) 0.029(7) 0.013(5) 0.015(5) 0.008(5) O24 0.015(6) 0.028(6) 0.029(7) 0.001(5) 0.018(5) 0.004(5) O25 0.025(6) 0.007(5) 0.019(6) 0.001(4) 0.008(5) 0.006(4) O26 0.025(6) 0.015(5) 0.010(5) 0.010(4) 0.008(5) 0.013(4) O27 0.023(6) 0.026(5) 0.007(5) 0.001(4) 0.007(4) 0.012(4) O28 0.123(18) 0.088(13) 0.048(11) -0.002(9) 0.052(12) -0.002(12) O29 0.037(9) 0.071(10) 0.073(11) 0.045(8) 0.025(8) 0.037(8) O30 0.053(9) 0.020(6) 0.021(6) 0.006(5) 0.026(6) 0.007(5) O31 0.055(9) 0.036(7) 0.011(6) 0.002(5) 0.006(6) 0.005(6) N1 0.037(10) 0.045(9) 0.035(10) 0.007(7) 0.016(8) 0.013(8) N2 0.049(11) 0.037(9) 0.030(9) -0.003(7) 0.023(8) 0.015(8) N3 0.042(11) 0.059(11) 0.013(8) 0.005(7) 0.004(8) 0.009(8) N4 0.055(13) 0.054(11) 0.036(10) -0.003(8) 0.028(10) -0.010(9) N5 0.045(11) 0.036(9) 0.057(12) 0.013(8) 0.022(10) 0.021(8) N6 0.038(9) 0.006(6) 0.039(9) 0.002(6) 0.021(8) 0.008(6) N7 0.060(15) 0.056(12) 0.081(16) 0.031(12) 0.027(13) 0.012(11) N8 0.031(10) 0.041(10) 0.052(12) -0.010(8) 0.004(9) 0.010(8) C1 0.053(13) 0.016(8) 0.038(11) 0.016(8) 0.023(10) 0.012(8) C2 0.034(8) 0.016(6) 0.040(8) 0.007(6) 0.016(6) 0.015(6) C3 0.049(9) 0.023(7) 0.051(9) 0.008(6) 0.020(7) 0.013(6) C4 0.057(15) 0.056(13) 0.023(11) -0.007(9) 0.012(10) 0.027(11) C5 0.044(13) 0.026(9) 0.051(13) 0.004(9) 0.030(11) 0.014(8) C6 0.021(11) 0.053(12) 0.050(13) 0.011(10) 0.016(10) -0.009(9) C7 0.054(16) 0.067(14) 0.017(10) -0.011(9) 0.010(10) 0.001(11) C8 0.038(12) 0.058(12) 0.024(10) 0.012(9) 0.017(10) 0.017(10) C9 0.037(12) 0.042(11) 0.030(11) 0.014(9) 0.014(10) 0.007(9) C10 0.039(13) 0.032(10) 0.045(13) -0.006(9) 0.016(11) 0.000(9) C11 0.059(15) 0.065(14) 0.046(13) 0.044(11) 0.031(12) 0.035(12) C12 0.052(15) 0.059(14) 0.049(14) 0.005(11) 0.031(13) 0.000(11) C13 0.068(17) 0.047(13) 0.034(12) 0.007(10) 0.015(12) 0.015(11) C14 0.050(15) 0.056(14) 0.031(12) -0.004(10) 0.011(11) -0.002(11) C15 0.039(13) 0.044(11) 0.058(14) 0.006(10) 0.038(11) 0.015(9) C16 0.047(14) 0.044(11) 0.023(10) -0.003(8) 0.013(10) 0.006(10) C17 0.043(13) 0.034(10) 0.044(12) 0.014(9) 0.023(10) 0.022(9) C18 0.029(11) 0.021(9) 0.039(11) -0.011(8) 0.002(9) 0.009(8) C19 0.042(12) 0.020(8) 0.017(9) 0.007(7) 0.006(8) 0.002(8) C20 0.026(11) 0.014(8) 0.060(13) 0.016(8) 0.012(10) 0.006(7) C21 0.052(13) 0.022(9) 0.034(10) 0.019(8) 0.030(10) 0.019(8) C22 0.14(3) 0.030(13) 0.10(2) 0.027(14) 0.07(2) 0.039(16) C23 0.039(14) 0.065(15) 0.042(14) -0.014(12) -0.010(11) 0.013(12) C24 0.09(2) 0.073(17) 0.048(16) 0.016(13) 0.016(15) 0.033(16) C25 0.060(16) 0.027(10) 0.074(17) 0.007(11) -0.003(13) 0.020(10) C26 0.038(13) 0.041(11) 0.055(14) -0.009(10) 0.012(12) 0.014(10) C27 0.048(16) 0.053(14) 0.076(18) 0.016(13) 0.020(14) -0.011(11) C28 0.041(15) 0.063(15) 0.075(18) -0.027(13) 0.039(14) -0.005(11) O1W 0.092(13) 0.041(8) 0.037(8) 0.003(6) 0.024(9) 0.032(8) O2W 0.039(8) 0.029(6) 0.032(7) -0.001(5) 0.021(6) 0.003(5) O3W 0.119(10) 0.065(8) 0.073(9) 0.024(7) 0.020(7) 0.028(7) O4W 0.139(12) 0.124(11) 0.129(12) 0.044(9) 0.051(8) 0.061(9) O5W 0.066(18) 0.28(4) 0.18(3) -0.04(3) 0.044(19) 0.06(2) O6W 0.133(12) 0.120(11) 0.118(11) 0.031(9) 0.044(9) 0.023(8) O7W 0.081(15) 0.095(14) 0.095(14) 0.031(10) 0.035(10) 0.022(9) O8W 0.122(18) 0.111(17) 0.116(18) 0.021(10) 0.044(11) 0.029(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 Cd1 O21 2.265(10) 2_565 ? Cd1 O21 2.265(10) . ? Cd1 O27 2.276(10) . ? Cd1 O27 2.276(10) 2_565 ? Cd1 O26 2.312(8) . ? Cd1 O26 2.312(8) 2_565 ? Cd2 O7 2.062(12) . ? Cd2 O7 2.062(12) 2_566 ? Cd2 O2W 2.184(11) . ? Cd2 O2W 2.184(11) 2_566 ? Cd2 O1W 2.224(14) . ? Cd2 O1W 2.224(14) 2_566 ? Mo1 O30 1.678(10) . ? Mo1 O26 1.934(10) . ? Mo1 O23 1.951(11) . ? Mo1 O4 2.037(12) . ? Mo1 O24 2.137(10) . ? Mo1 O25 2.290(9) . ? Mo1 Mo3 2.596(2) . ? Mo2 O14 1.666(11) . ? Mo2 O16 1.922(12) . ? Mo2 O21 1.971(9) . ? Mo2 O8 2.074(11) . ? Mo2 O5 2.130(11) . ? Mo2 O22 2.237(11) . ? Mo2 Mo5 2.5926(19) . ? Mo3 O6 1.660(11) . ? Mo3 O26 1.952(10) . ? Mo3 O23 1.954(11) . ? Mo3 O10 2.038(11) . ? Mo3 O20 2.083(11) . ? Mo3 O19 2.288(9) . ? Mo4 O17 1.654(12) . ? Mo4 O18 1.938(11) . ? Mo4 O27 1.995(10) . ? Mo4 O15 2.049(10) . ? Mo4 O20 2.117(10) . ? Mo4 O19 2.311(11) . ? Mo4 Mo6 2.601(2) . ? Mo5 O9 1.660(12) . ? Mo5 O16 1.925(10) . ? Mo5 O21 1.967(11) . ? Mo5 O11 2.079(11) . ? Mo5 O24 2.140(10) . ? Mo5 O25 2.278(10) . ? Mo6 O13 1.704(11) . ? Mo6 O18 1.919(11) . ? Mo6 O27 1.975(10) . ? Mo6 O12 2.073(11) . ? Mo6 O5 2.120(12) . ? Mo6 O22 2.251(11) . ? P1 O29 1.492(13) . ? P1 O4 1.515(13) . ? P1 O11 1.523(11) . ? P1 O28 1.571(16) . ? P2 O7 1.503(11) . ? P2 O15 1.537(11) . ? P2 O10 1.540(12) . ? P2 O1 1.557(12) . ? P3 O2 1.508(11) . ? P3 O19 1.540(11) . ? P3 O25 1.545(11) . ? P3 O22 1.581(10) . ? P4 O3 1.501(11) . ? P4 O8 1.510(12) . ? P4 O12 1.519(13) . ? P4 O31 1.568(12) . ? N1 C2 1.36(2) . ? N1 C1 1.39(2) . ? N2 C1 1.31(2) . ? N2 C3 1.43(2) . ? N2 C4 1.49(2) . ? N3 C12 1.32(3) . ? N3 C14 1.37(3) . ? N3 C11 1.50(2) . ? N4 C12 1.31(3) . ? N4 C13 1.36(3) . ? N5 C15 1.31(2) . ? N5 C16 1.36(2) . ? N6 C15 1.33(2) . ? N6 C17 1.38(2) . ? N6 C18 1.46(2) . ? N7 C23 1.33(3) . ? N7 C22 1.34(3) . ? N8 C22 1.33(3) . ? N8 C24 1.40(3) . ? N8 C25 1.47(3) . ? C1 H1A 0.9500 . ? C2 C3 1.30(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.51(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.36(3) . ? C5 C10 1.37(3) . ? C6 C7 1.38(3) . ? C6 H6A 0.9500 . ? C7 C8 1.38(3) . ? C7 H7A 0.9500 . ? C8 C9 1.35(3) . ? C8 C11 1.53(3) . ? C9 C10 1.38(3) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9500 . ? C13 C14 1.34(3) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.32(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.52(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.37(3) . ? C19 C21 1.39(2) . ? C20 C21 1.38(2) 2_655 ? C20 H20A 0.9500 . ? C21 C20 1.38(2) 2_655 ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.38(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.54(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C28 1.34(3) . ? C26 C27 1.36(3) . ? C27 C28 1.40(3) 2_556 ? C27 H27A 0.9500 . ? C28 C27 1.40(3) 2_556 ? C28 H28A 0.9500 . ? 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 O21 Cd1 O21 180.000(1) 2_565 . ? O21 Cd1 O27 81.7(4) 2_565 . ? O21 Cd1 O27 98.3(4) . . ? O21 Cd1 O27 98.3(4) 2_565 2_565 ? O21 Cd1 O27 81.7(4) . 2_565 ? O27 Cd1 O27 180.0(4) . 2_565 ? O21 Cd1 O26 83.4(4) 2_565 . ? O21 Cd1 O26 96.6(4) . . ? O27 Cd1 O26 95.4(3) . . ? O27 Cd1 O26 84.6(3) 2_565 . ? O21 Cd1 O26 96.6(4) 2_565 2_565 ? O21 Cd1 O26 83.4(4) . 2_565 ? O27 Cd1 O26 84.6(3) . 2_565 ? O27 Cd1 O26 95.4(3) 2_565 2_565 ? O26 Cd1 O26 180.0(3) . 2_565 ? O7 Cd2 O7 180.000(1) . 2_566 ? O7 Cd2 O2W 89.5(4) . . ? O7 Cd2 O2W 90.5(4) 2_566 . ? O7 Cd2 O2W 90.5(4) . 2_566 ? O7 Cd2 O2W 89.5(4) 2_566 2_566 ? O2W Cd2 O2W 180.000(2) . 2_566 ? O7 Cd2 O1W 88.4(5) . . ? O7 Cd2 O1W 91.6(5) 2_566 . ? O2W Cd2 O1W 92.7(5) . . ? O2W Cd2 O1W 87.3(5) 2_566 . ? O7 Cd2 O1W 91.6(5) . 2_566 ? O7 Cd2 O1W 88.4(5) 2_566 2_566 ? O2W Cd2 O1W 87.3(5) . 2_566 ? O2W Cd2 O1W 92.7(5) 2_566 2_566 ? O1W Cd2 O1W 180.0(6) . 2_566 ? O30 Mo1 O26 101.5(5) . . ? O30 Mo1 O23 107.0(5) . . ? O26 Mo1 O23 95.4(4) . . ? O30 Mo1 O4 94.0(6) . . ? O26 Mo1 O4 161.9(4) . . ? O23 Mo1 O4 88.8(5) . . ? O30 Mo1 O24 96.1(5) . . ? O26 Mo1 O24 86.0(4) . . ? O23 Mo1 O24 156.0(4) . . ? O4 Mo1 O24 83.1(5) . . ? O30 Mo1 O25 167.3(5) . . ? O26 Mo1 O25 83.3(4) . . ? O23 Mo1 O25 84.0(4) . . ? O4 Mo1 O25 79.7(4) . . ? O24 Mo1 O25 72.3(4) . . ? O30 Mo1 Mo3 102.1(4) . . ? O26 Mo1 Mo3 48.4(3) . . ? O23 Mo1 Mo3 48.4(3) . . ? O4 Mo1 Mo3 137.0(4) . . ? O24 Mo1 Mo3 133.2(3) . . ? O25 Mo1 Mo3 89.9(3) . . ? O14 Mo2 O16 106.2(6) . . ? O14 Mo2 O21 102.4(5) . . ? O16 Mo2 O21 95.1(5) . . ? O14 Mo2 O8 95.1(5) . . ? O16 Mo2 O8 86.8(5) . . ? O21 Mo2 O8 161.1(4) . . ? O14 Mo2 O5 97.9(5) . . ? O16 Mo2 O5 154.9(5) . . ? O21 Mo2 O5 86.5(4) . . ? O8 Mo2 O5 84.0(4) . . ? O14 Mo2 O22 167.9(5) . . ? O16 Mo2 O22 84.7(4) . . ? O21 Mo2 O22 81.5(4) . . ? O8 Mo2 O22 79.9(4) . . ? O5 Mo2 O22 70.8(4) . . ? O14 Mo2 Mo5 102.2(4) . . ? O16 Mo2 Mo5 47.7(3) . . ? O21 Mo2 Mo5 48.8(3) . . ? O8 Mo2 Mo5 134.1(3) . . ? O5 Mo2 Mo5 133.8(3) . . ? O22 Mo2 Mo5 89.0(3) . . ? O6 Mo3 O26 100.8(5) . . ? O6 Mo3 O23 105.9(5) . . ? O26 Mo3 O23 94.7(4) . . ? O6 Mo3 O10 96.3(5) . . ? O26 Mo3 O10 161.8(4) . . ? O23 Mo3 O10 86.7(5) . . ? O6 Mo3 O20 98.1(5) . . ? O26 Mo3 O20 87.3(4) . . ? O23 Mo3 O20 155.1(4) . . ? O10 Mo3 O20 84.0(4) . . ? O6 Mo3 O19 170.8(5) . . ? O26 Mo3 O19 81.7(4) . . ? O23 Mo3 O19 82.7(4) . . ? O10 Mo3 O19 80.5(4) . . ? O20 Mo3 O19 73.0(4) . . ? O6 Mo3 Mo1 100.6(4) . . ? O26 Mo3 Mo1 47.8(3) . . ? O23 Mo3 Mo1 48.3(3) . . ? O10 Mo3 Mo1 134.7(4) . . ? O20 Mo3 Mo1 133.7(3) . . ? O19 Mo3 Mo1 87.7(3) . . ? O17 Mo4 O18 106.4(5) . . ? O17 Mo4 O27 102.5(5) . . ? O18 Mo4 O27 94.6(5) . . ? O17 Mo4 O15 97.1(5) . . ? O18 Mo4 O15 84.3(5) . . ? O27 Mo4 O15 159.8(4) . . ? O17 Mo4 O20 98.7(5) . . ? O18 Mo4 O20 154.2(4) . . ? O27 Mo4 O20 85.6(4) . . ? O15 Mo4 O20 86.7(4) . . ? O17 Mo4 O19 169.2(5) . . ? O18 Mo4 O19 82.5(4) . . ? O27 Mo4 O19 82.5(4) . . ? O15 Mo4 O19 77.4(4) . . ? O20 Mo4 O19 72.0(4) . . ? O17 Mo4 Mo6 102.1(4) . . ? O18 Mo4 Mo6 47.3(3) . . ? O27 Mo4 Mo6 48.7(3) . . ? O15 Mo4 Mo6 131.2(3) . . ? O20 Mo4 Mo6 132.8(3) . . ? O19 Mo4 Mo6 88.4(2) . . ? O9 Mo5 O16 106.6(5) . . ? O9 Mo5 O21 102.4(5) . . ? O16 Mo5 O21 95.1(5) . . ? O9 Mo5 O11 93.8(5) . . ? O16 Mo5 O11 87.0(5) . . ? O21 Mo5 O11 162.3(4) . . ? O9 Mo5 O24 97.6(5) . . ? O16 Mo5 O24 155.1(4) . . ? O21 Mo5 O24 84.8(4) . . ? O11 Mo5 O24 85.9(4) . . ? O9 Mo5 O25 168.2(4) . . ? O16 Mo5 O25 82.7(4) . . ? O21 Mo5 O25 83.6(4) . . ? O11 Mo5 O25 79.3(4) . . ? O24 Mo5 O25 72.5(4) . . ? O9 Mo5 Mo2 102.5(4) . . ? O16 Mo5 Mo2 47.6(4) . . ? O21 Mo5 Mo2 48.9(3) . . ? O11 Mo5 Mo2 134.4(3) . . ? O24 Mo5 Mo2 132.3(3) . . ? O25 Mo5 Mo2 89.1(2) . . ? O13 Mo6 O18 106.4(5) . . ? O13 Mo6 O27 101.1(5) . . ? O18 Mo6 O27 95.8(4) . . ? O13 Mo6 O12 95.0(5) . . ? O18 Mo6 O12 85.8(5) . . ? O27 Mo6 O12 162.6(5) . . ? O13 Mo6 O5 98.4(5) . . ? O18 Mo6 O5 154.0(5) . . ? O27 Mo6 O5 86.8(4) . . ? O12 Mo6 O5 84.3(5) . . ? O13 Mo6 O22 168.7(5) . . ? O18 Mo6 O22 84.1(4) . . ? O27 Mo6 O22 81.8(4) . . ? O12 Mo6 O22 81.2(4) . . ? O5 Mo6 O22 70.7(4) . . ? O13 Mo6 Mo4 101.1(4) . . ? O18 Mo6 Mo4 47.9(3) . . ? O27 Mo6 Mo4 49.4(3) . . ? O12 Mo6 Mo4 133.6(3) . . ? O5 Mo6 Mo4 134.6(3) . . ? O22 Mo6 Mo4 89.1(3) . . ? O29 P1 O4 112.7(8) . . ? O29 P1 O11 112.2(8) . . ? O4 P1 O11 111.4(7) . . ? O29 P1 O28 105.3(11) . . ? O4 P1 O28 109.2(9) . . ? O11 P1 O28 105.6(9) . . ? O7 P2 O15 111.5(6) . . ? O7 P2 O10 112.0(7) . . ? O15 P2 O10 109.4(6) . . ? O7 P2 O1 108.7(7) . . ? O15 P2 O1 108.2(7) . . ? O10 P2 O1 106.7(7) . . ? O2 P3 O19 113.3(6) . . ? O2 P3 O25 113.2(6) . . ? O19 P3 O25 108.2(6) . . ? O2 P3 O22 107.8(6) . . ? O19 P3 O22 106.6(6) . . ? O25 P3 O22 107.5(6) . . ? O3 P4 O8 111.1(7) . . ? O3 P4 O12 110.1(7) . . ? O8 P4 O12 110.5(7) . . ? O3 P4 O31 104.5(7) . . ? O8 P4 O31 111.0(7) . . ? O12 P4 O31 109.6(7) . . ? P1 O4 Mo1 139.6(7) . . ? Mo6 O5 Mo2 112.9(5) . . ? P2 O7 Cd2 128.4(7) . . ? P4 O8 Mo2 133.7(7) . . ? P2 O10 Mo3 137.8(7) . . ? P1 O11 Mo5 136.0(7) . . ? P4 O12 Mo6 131.8(7) . . ? P2 O15 Mo4 134.9(7) . . ? Mo2 O16 Mo5 84.7(5) . . ? Mo6 O18 Mo4 84.8(4) . . ? P3 O19 Mo3 127.7(6) . . ? P3 O19 Mo4 126.1(5) . . ? Mo3 O19 Mo4 99.9(4) . . ? Mo3 O20 Mo4 113.9(5) . . ? Mo5 O21 Mo2 82.3(4) . . ? Mo5 O21 Cd1 133.0(5) . . ? Mo2 O21 Cd1 131.9(5) . . ? P3 O22 Mo2 125.9(6) . . ? P3 O22 Mo6 126.7(6) . . ? Mo2 O22 Mo6 104.2(4) . . ? Mo1 O23 Mo3 83.3(4) . . ? Mo1 O24 Mo5 112.1(5) . . ? P3 O25 Mo5 125.4(5) . . ? P3 O25 Mo1 125.2(6) . . ? Mo5 O25 Mo1 101.9(4) . . ? Mo1 O26 Mo3 83.8(3) . . ? Mo1 O26 Cd1 132.2(5) . . ? Mo3 O26 Cd1 133.1(5) . . ? Mo6 O27 Mo4 81.8(4) . . ? Mo6 O27 Cd1 131.1(5) . . ? Mo4 O27 Cd1 133.5(5) . . ? C2 N1 C1 105.8(15) . . ? C1 N2 C3 108.8(15) . . ? C1 N2 C4 123.7(16) . . ? C3 N2 C4 127.5(15) . . ? C12 N3 C14 108.2(17) . . ? C12 N3 C11 127.8(19) . . ? C14 N3 C11 123.9(17) . . ? C12 N4 C13 106.7(18) . . ? C15 N5 C16 105.9(17) . . ? C15 N6 C17 108.4(15) . . ? C15 N6 C18 127.6(16) . . ? C17 N6 C18 124.0(15) . . ? C23 N7 C22 110(2) . . ? C22 N8 C24 111(2) . . ? C22 N8 C25 125(2) . . ? C24 N8 C25 123(2) . . ? N2 C1 N1 108.4(14) . . ? N2 C1 H1A 125.8 . . ? N1 C1 H1A 125.8 . . ? C3 C2 N1 111.8(16) . . ? C3 C2 H2A 124.1 . . ? N1 C2 H2A 124.1 . . ? C2 C3 N2 105.3(15) . . ? C2 C3 H3A 127.4 . . ? N2 C3 H3A 127.4 . . ? N2 C4 C5 109.8(17) . . ? N2 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 116.7(18) . . ? C6 C5 C4 120.8(18) . . ? C10 C5 C4 122.1(17) . . ? C5 C6 C7 122.0(19) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C8 C7 C6 119.8(19) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C9 C8 C7 119.1(19) . . ? C9 C8 C11 121(2) . . ? C7 C8 C11 119.8(19) . . ? C8 C9 C10 119.8(19) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C5 C10 C9 122.2(18) . . ? C5 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? N3 C11 C8 109.4(16) . . ? N3 C11 H11A 109.8 . . ? C8 C11 H11A 109.8 . . ? N3 C11 H11B 109.8 . . ? C8 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? N4 C12 N3 110(2) . . ? N4 C12 H12A 124.9 . . ? N3 C12 H12A 124.9 . . ? C14 C13 N4 109.0(19) . . ? C14 C13 H13A 125.5 . . ? N4 C13 H13A 125.5 . . ? C13 C14 N3 105.5(18) . . ? C13 C14 H14A 127.2 . . ? N3 C14 H14A 127.2 . . ? N5 C15 N6 109.9(17) . . ? N5 C15 H15A 125.0 . . ? N6 C15 H15A 125.0 . . ? C17 C16 N5 111.0(18) . . ? C17 C16 H16A 124.5 . . ? N5 C16 H16A 124.5 . . ? C16 C17 N6 104.5(17) . . ? C16 C17 H17A 127.7 . . ? N6 C17 H17A 127.7 . . ? N6 C18 C19 111.4(14) . . ? N6 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N6 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C21 119.4(16) . . ? C20 C19 C18 121.1(17) . . ? C21 C19 C18 119.5(17) . . ? C19 C20 C21 120.2(17) . 2_655 ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 2_655 . ? C20 C21 C19 120.4(17) 2_655 . ? C20 C21 H21A 119.8 2_655 . ? C19 C21 H21A 119.8 . . ? N8 C22 N7 106(2) . . ? N8 C22 H22A 127.0 . . ? N7 C22 H22A 127.0 . . ? N7 C23 C24 109(2) . . ? N7 C23 H23A 125.4 . . ? C24 C23 H23A 125.4 . . ? C23 C24 N8 103(2) . . ? C23 C24 H24A 128.7 . . ? N8 C24 H24A 128.7 . . ? N8 C25 C26 111.7(17) . . ? N8 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N8 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C28 C26 C27 117.9(19) . . ? C28 C26 C25 121(2) . . ? C27 C26 C25 121(2) . . ? C26 C27 C28 122(2) . 2_556 ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 2_556 . ? C26 C28 C27 120(2) . 2_556 ? C26 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 2_556 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.388 _refine_diff_density_min -3.572 _refine_diff_density_rms 0.286 # Attachment 'compound_4.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 792971' #TrackingRef 'compound_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H30 Co3 Mo4 N6 O28 P4' _chemical_formula_weight 1318.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 17.110(2) _cell_length_b 17.110(2) _cell_length_c 10.740(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3144.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11907 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 3.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.459 _exptl_absorpt_correction_T_max 0.489 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11907 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1385 _reflns_number_gt 1240 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0414P)^2^+56.5893P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1385 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.30926(3) 0.91072(3) 0.05764(5) 0.00795(19) Uani 1 1 d . . . Co1 Co 0.2500 0.7500 0.2500 0.0088(3) Uani 1 2 d S . . Co2 Co 0.5000 0.7500 -0.3750 0.0080(4) Uani 1 4 d S . . P1 P 0.41776(9) 0.88582(9) -0.19687(15) 0.0096(4) Uani 1 1 d . . . O1 O 0.3201(3) 0.8232(3) 0.1407(4) 0.0136(10) Uani 1 1 d . . . O2 O 0.2852(3) 1.0002(3) -0.0846(4) 0.0130(9) Uani 1 1 d . . . O3 O 0.3996(3) 0.9566(3) 0.0818(4) 0.0130(10) Uani 1 1 d . . . O4 O 0.3558(3) 0.8580(2) -0.1020(4) 0.0124(9) Uani 1 1 d . . . O7 O 0.4308(3) 0.8179(3) -0.2844(5) 0.0204(11) Uani 1 1 d . . . C1 C 0.5000 0.7500 -0.8054(14) 0.051(4) Uani 1 2 d S . . C2 C 0.4070(9) 0.9115(9) -0.6044(15) 0.025(3) Uani 0.50 1 d P . . N2 N 0.3471(9) 0.9010(9) -0.5185(14) 0.040(4) Uani 0.50 1 d P . . N1 N 0.4680(9) 0.8231(10) -0.7487(16) 0.047(4) Uani 0.50 1 d P . . C3 C 0.4327(10) 0.9906(10) -0.6082(16) 0.033(4) Uani 0.50 1 d P . . O5 O 0.4929(2) 0.9111(3) -0.1315(4) 0.0148(10) Uani 1 1 d . . . O6 O 0.3833(3) 0.9546(3) -0.2729(4) 0.0123(9) Uani 1 1 d . . . N3 N 0.3817(10) 1.0434(11) -0.6932(17) 0.051(5) Uani 0.50 1 d P . . 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 0.0069(3) 0.0085(3) 0.0085(3) 0.0003(2) 0.0013(2) -0.00079(19) Co1 0.0102(6) 0.0058(6) 0.0105(6) 0.0006(5) 0.0017(5) 0.0013(4) Co2 0.0066(5) 0.0066(5) 0.0110(9) 0.000 0.000 0.000 P1 0.0098(8) 0.0090(8) 0.0098(8) -0.0014(6) 0.0021(6) 0.0015(6) O1 0.014(2) 0.012(2) 0.015(2) 0.0028(19) -0.0006(19) 0.0020(18) O2 0.012(2) 0.013(2) 0.014(2) 0.0002(18) 0.0007(18) -0.0001(18) O3 0.011(2) 0.018(2) 0.011(2) 0.0006(19) -0.0008(18) -0.0030(18) O4 0.016(2) 0.011(2) 0.010(2) -0.0042(18) 0.0054(19) 0.0026(18) O7 0.020(3) 0.021(3) 0.021(3) -0.009(2) 0.005(2) 0.001(2) C1 0.046(8) 0.054(9) 0.053(9) 0.000 0.000 0.004(7) C2 0.030(8) 0.022(8) 0.024(8) 0.001(6) -0.004(7) 0.006(6) N2 0.043(9) 0.051(10) 0.026(8) -0.004(7) -0.018(7) 0.011(8) N1 0.037(9) 0.052(10) 0.053(10) 0.018(8) -0.020(8) -0.012(7) C3 0.035(9) 0.033(9) 0.031(9) -0.008(7) 0.001(8) 0.007(7) O5 0.009(2) 0.018(2) 0.017(2) -0.001(2) -0.0002(19) 0.0035(18) O6 0.015(2) 0.012(2) 0.010(2) 0.0013(18) 0.0006(18) 0.0014(18) N3 0.052(10) 0.053(11) 0.049(11) -0.024(9) 0.006(9) -0.013(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.752(4) . ? Mo1 O3 1.753(4) . ? Mo1 O2 1.794(4) 8_354 ? Mo1 O4 2.095(4) . ? Mo1 O6 2.126(4) 8_354 ? Mo1 O2 2.201(4) . ? Co1 O3 2.067(4) 12_766 ? Co1 O3 2.067(4) 8_354 ? Co1 O5 2.079(5) 8_354 ? Co1 O5 2.079(5) 12_766 ? Co1 O1 2.094(4) . ? Co1 O1 2.094(4) 13_565 ? Co2 O7 1.923(5) . ? Co2 O7 1.923(5) 12_765 ? Co2 O7 1.923(5) 15_564 ? Co2 O7 1.923(5) 6_564 ? P1 O7 1.512(5) . ? P1 O5 1.528(5) . ? P1 O4 1.545(5) . ? P1 O6 1.549(5) . ? O2 Mo1 1.794(4) 7_554 ? O3 Co1 2.067(4) 7_554 ? C1 C1 1.49(3) 15_563 ? C1 N1 1.49(2) . ? C1 N1 1.49(2) 6_564 ? C2 N2 1.39(2) . ? C2 C3 1.42(2) . ? N2 N3 1.35(3) 8_354 ? C3 N3 1.55(3) . ? O5 Co1 2.079(5) 7_554 ? O6 Mo1 2.126(4) 7_554 ? N3 N2 1.35(3) 7_554 ? 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 102.3(2) . . ? O1 Mo1 O2 99.9(2) . 8_354 ? O3 Mo1 O2 99.8(2) . 8_354 ? O1 Mo1 O4 90.52(19) . . ? O3 Mo1 O4 88.75(19) . . ? O2 Mo1 O4 164.67(19) 8_354 . ? O1 Mo1 O6 89.66(19) . 8_354 ? O3 Mo1 O6 164.02(19) . 8_354 ? O2 Mo1 O6 88.29(18) 8_354 8_354 ? O4 Mo1 O6 80.51(17) . 8_354 ? O1 Mo1 O2 165.23(19) . . ? O3 Mo1 O2 87.52(19) . . ? O2 Mo1 O2 89.04(16) 8_354 . ? O4 Mo1 O2 78.59(17) . . ? O6 Mo1 O2 78.81(17) 8_354 . ? O3 Co1 O3 180.000(1) 12_766 8_354 ? O3 Co1 O5 91.31(17) 12_766 8_354 ? O3 Co1 O5 88.69(17) 8_354 8_354 ? O3 Co1 O5 88.69(17) 12_766 12_766 ? O3 Co1 O5 91.31(17) 8_354 12_766 ? O5 Co1 O5 180.00(19) 8_354 12_766 ? O3 Co1 O1 93.05(17) 12_766 . ? O3 Co1 O1 86.95(17) 8_354 . ? O5 Co1 O1 90.20(18) 8_354 . ? O5 Co1 O1 89.80(18) 12_766 . ? O3 Co1 O1 86.95(17) 12_766 13_565 ? O3 Co1 O1 93.05(17) 8_354 13_565 ? O5 Co1 O1 89.80(18) 8_354 13_565 ? O5 Co1 O1 90.20(18) 12_766 13_565 ? O1 Co1 O1 179.999(1) . 13_565 ? O7 Co2 O7 104.82(14) . 12_765 ? O7 Co2 O7 104.82(14) . 15_564 ? O7 Co2 O7 119.2(3) 12_765 15_564 ? O7 Co2 O7 119.2(3) . 6_564 ? O7 Co2 O7 104.82(14) 12_765 6_564 ? O7 Co2 O7 104.82(14) 15_564 6_564 ? O7 P1 O5 112.3(3) . . ? O7 P1 O4 105.9(3) . . ? O5 P1 O4 111.2(3) . . ? O7 P1 O6 108.2(3) . . ? O5 P1 O6 110.4(3) . . ? O4 P1 O6 108.7(2) . . ? Mo1 O1 Co1 137.4(2) . . ? Mo1 O2 Mo1 138.0(2) 7_554 . ? Mo1 O3 Co1 146.2(3) . 7_554 ? P1 O4 Mo1 131.9(3) . . ? P1 O7 Co2 150.4(3) . . ? C1 C1 N1 114.1(8) 15_563 . ? C1 C1 N1 114.1(8) 15_563 6_564 ? N1 C1 N1 131.9(17) . 6_564 ? N2 C2 C3 111.7(14) . . ? N3 N2 C2 162.8(17) 8_354 . ? C2 C3 N3 113.3(14) . . ? P1 O5 Co1 124.6(3) . 7_554 ? P1 O6 Mo1 124.1(3) . 7_554 ? N2 N3 C3 169.7(16) 7_554 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.890 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.188