data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Compain, Jean-Daniel' 'Deniard, Philippe' 'Dessapt, Remi' 'Dolbecq, Anne' 'Oms, Olivier' 'Secheresse, Francis' 'Marrot, Jerome' 'Mialane, Pierre' _publ_contact_author_name 'Mialane, Pierre' _publ_contact_author_email mialane@chimie.uvsq.fr _publ_section_title ; Functionalized polyoxometalates with intrinsic photochromic properties and their association with spiropyran cations ; # Attachment '- CifMo12photochrome' data_1 _database_code_depnum_ccdc_archive 'CCDC 778854' #TrackingRef '- CifMo12photochrome' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Mo12 N6 Na O65 P8' _chemical_formula_weight 2882.71 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' 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' C C 0.0033 0.0016 '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' Na Na 0.0362 0.0249 '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 tetragonal _symmetry_space_group_name_H-M I41/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 19.7317(12) _cell_length_b 19.7317(12) _cell_length_c 29.047(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11309.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15478 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 30.27 _exptl_crystal_description parallelepiped _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5556 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7558 _exptl_absorpt_correction_T_max 0.8659 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCDC area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43623 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 30.27 _reflns_number_total 8382 _reflns_number_gt 4096 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1248P)^2^+50.9975P] 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 8382 _refine_ls_number_parameters 339 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1418 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.2580 _refine_ls_wR_factor_gt 0.1866 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.014 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 0.933823(10) 0.376419(9) 0.051017(6) 0.04882(5) Uani 1 1 d . . . Mo2 Mo 0.812195(12) 0.279156(12) -0.020203(7) 0.06437(7) Uani 1 1 d . . . Mo3 Mo 0.685078(13) 0.245343(17) 0.043201(10) 0.08413(9) Uani 1 1 d . . . P1 P 0.82743(3) 0.26126(3) 0.10100(2) 0.05003(16) Uani 1 1 d . . . P2 P 0.76223(3) 0.39010(4) 0.06944(2) 0.06371(19) Uani 1 1 d . . . Na1 Na 1.0000 0.2500 0.1250 0.0568(5) Uani 1 4 d S . . O1 O 0.60741(11) 0.27748(16) 0.03028(9) 0.1176(10) Uani 1 1 d . . . O2 O 1.00899(8) 0.33269(8) 0.05074(5) 0.0578(5) Uani 1 1 d . . . O3 O 0.82553(8) 0.20519(8) 0.13784(5) 0.0525(4) Uani 1 1 d . . . O4 O 0.80237(8) 0.23204(8) 0.05430(5) 0.0584(5) Uani 1 1 d . . . O5 O 0.95416(9) 0.44610(9) 0.01921(6) 0.0658(5) Uani 1 1 d . . . O6 O 0.89570(7) 0.29629(7) 0.09863(5) 0.0477(4) Uani 1 1 d . . . O7 O 0.74515(9) 0.34717(10) 0.02585(6) 0.0681(5) Uani 1 1 d . . . O8 O 0.69855(9) 0.28575(10) 0.10350(6) 0.0719(6) Uani 1 1 d . . . O9 O 0.83427(8) 0.41868(8) 0.06758(5) 0.0583(5) Uani 1 1 d . . . O10 O 0.88458(9) 0.32710(8) 0.00604(5) 0.0609(5) Uani 1 1 d . . . O11 O 0.72279(10) 0.23478(11) -0.01565(7) 0.0831(7) Uani 1 1 d . . . O12 O 0.66951(12) 0.16293(13) 0.05958(8) 0.1087(9) Uani 1 1 d . . . O13 O 0.85467(11) 0.21012(10) -0.04130(6) 0.0801(7) Uani 1 1 d . . . O14 O 0.79779(11) 0.32681(10) -0.06822(6) 0.0851(7) Uani 1 1 d . . . O15 O 0.71001(10) 0.44260(10) 0.07944(7) 0.0883(7) Uani 1 1 d . . . C1 C 0.75997(12) 0.32219(13) 0.11386(8) 0.0586(7) Uani 1 1 d . . . C2 C 0.75547(12) 0.34650(14) 0.16348(9) 0.0650(8) Uani 1 1 d . . . H2A H 0.7547 0.3073 0.1836 0.078 Uiso 1 1 calc R . . H2B H 0.7130 0.3706 0.1676 0.078 Uiso 1 1 calc R . . C3 C 0.81437(14) 0.39346(14) 0.17830(8) 0.0692(8) Uani 1 1 d . . . H3A H 0.8571 0.3715 0.1713 0.083 Uiso 1 1 calc R . . H3B H 0.8122 0.4351 0.1606 0.083 Uiso 1 1 calc R . . C4 C 0.81237(14) 0.41078(14) 0.22993(8) 0.0673(8) Uani 1 1 d . . . H4A H 0.8437 0.4475 0.2362 0.081 Uiso 1 1 calc R . . H4B H 0.7672 0.4260 0.2381 0.081 Uiso 1 1 calc R . . N1 N 0.83067(11) 0.35135(11) 0.25841(7) 0.0674(7) Uani 1 1 d . . . H1A H 0.7984 0.3200 0.2560 0.101 Uiso 1 1 calc R . . H1B H 0.8347 0.3640 0.2877 0.101 Uiso 1 1 calc R . . H1C H 0.8699 0.3343 0.2486 0.101 Uiso 1 1 calc R . . O1W O 0.85445(13) 0.05134(11) -0.09991(7) 0.0963(8) Uani 1 1 d . . . O2W O 0.6443(5) 0.2762(7) -0.0995(4) 0.162(4) Uani 0.25 1 d P . . N2 N 0.7163(5) 0.5589(4) 0.1091(2) 0.166(7) Uani 0.25 1 d PD . . H2C H 0.7249 0.5224 0.0914 0.199 Uiso 0.25 1 calc PR . . H2D H 0.7567 0.5717 0.1206 0.199 Uiso 0.25 1 calc PR . . C5 C 0.6984(6) 0.5541(7) 0.1749(9) 0.207(9) Uani 0.25 1 d P . . H5A H 0.7392 0.5758 0.1644 0.310 Uiso 0.25 1 calc PR . . H5B H 0.7093 0.5222 0.1987 0.310 Uiso 0.25 1 calc PR . . H5C H 0.6678 0.5876 0.1867 0.310 Uiso 0.25 1 calc PR . . C6 C 0.6778(4) 0.5311(5) 0.1501(3) 0.150(5) Uani 0.25 1 d PD . . H6A H 0.6835 0.4825 0.1528 0.180 Uiso 0.25 1 calc PR . . H6B H 0.6299 0.5417 0.1481 0.180 Uiso 0.25 1 calc PR . . C7 C 0.6595(5) 0.5834(7) 0.0389(2) 0.156(6) Uani 0.25 1 d PD . . H7A H 0.6765 0.5408 0.0279 0.233 Uiso 0.25 1 calc PR . . H7B H 0.6630 0.6168 0.0150 0.233 Uiso 0.25 1 calc PR . . H7C H 0.6128 0.5783 0.0477 0.233 Uiso 0.25 1 calc PR . . C8 C 0.7007(6) 0.6059(6) 0.0804(3) 0.186(11) Uani 0.25 1 d PD . . H8A H 0.6754 0.6406 0.0966 0.223 Uiso 0.25 1 calc PR . . H8B H 0.7423 0.6266 0.0694 0.223 Uiso 0.25 1 calc PR . . N3 N 0.4983(5) 0.2940(4) 0.1162(3) 0.169(7) Uani 0.25 1 d PD . . C9 C 0.5710(5) 0.4257(3) 0.0832(4) 0.139(7) Uani 0.25 1 d PD . . C10 C 0.5476(6) 0.3562(3) 0.1042(4) 0.108(4) Uani 0.25 1 d PD . . C11 C 0.3937(3) 0.2451(6) 0.1753(2) 0.061(3) Uani 0.25 1 d PD . . C12 C 0.4611(3) 0.2438(5) 0.1494(3) 0.191(6) Uani 0.25 1 d PD . . 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 0.06020(10) 0.05177(9) 0.03447(8) 0.00390(7) 0.00107(7) 0.00582(8) Mo2 0.07930(13) 0.07335(13) 0.04047(9) -0.00311(9) -0.01255(9) 0.00758(11) Mo3 0.06772(13) 0.1189(2) 0.06572(14) -0.00707(14) -0.01593(11) -0.01076(14) P1 0.0531(3) 0.0596(3) 0.0374(2) -0.0006(2) -0.0014(2) 0.0005(3) P2 0.0623(3) 0.0779(4) 0.0509(3) -0.0005(3) -0.0046(3) 0.0187(3) Na1 0.0586(6) 0.0586(6) 0.0534(9) 0.000 0.000 0.000 O1 0.0782(13) 0.177(2) 0.0977(16) -0.0101(17) -0.0303(11) 0.0109(16) O2 0.0628(9) 0.0591(8) 0.0514(8) 0.0053(7) 0.0051(7) 0.0046(7) O3 0.0551(8) 0.0621(8) 0.0403(7) -0.0011(7) -0.0010(6) -0.0052(7) O4 0.0663(9) 0.0663(9) 0.0425(8) -0.0040(7) -0.0081(7) -0.0023(8) O5 0.0841(11) 0.0636(9) 0.0496(9) 0.0112(7) 0.0037(8) 0.0042(9) O6 0.0549(8) 0.0515(7) 0.0367(7) 0.0004(6) 0.0014(6) 0.0042(6) O7 0.0646(9) 0.0891(11) 0.0507(9) 0.0020(8) -0.0149(7) 0.0128(9) O8 0.0546(9) 0.0978(12) 0.0632(10) -0.0031(10) -0.0011(8) -0.0010(9) O9 0.0682(9) 0.0635(9) 0.0432(8) -0.0006(7) 0.0015(7) 0.0148(8) O10 0.0801(10) 0.0644(9) 0.0380(7) -0.0049(7) -0.0003(7) 0.0012(8) O11 0.0846(11) 0.1091(14) 0.0557(10) -0.0084(10) -0.0219(9) -0.0086(11) O12 0.1119(15) 0.1364(17) 0.0777(14) -0.0062(14) -0.0121(13) -0.0466(13) O13 0.1101(14) 0.0773(11) 0.0529(10) -0.0118(9) -0.0122(10) 0.0053(11) O14 0.1162(14) 0.0911(13) 0.0479(9) 0.0053(9) -0.0231(10) 0.0095(12) O15 0.0826(11) 0.1000(13) 0.0823(13) -0.0087(11) -0.0036(10) 0.0394(10) C1 0.0538(12) 0.0751(14) 0.0469(11) -0.0029(11) -0.0020(10) -0.0018(11) C2 0.0575(13) 0.0858(16) 0.0518(12) -0.0077(12) 0.0087(11) 0.0028(12) C3 0.0873(16) 0.0702(15) 0.0501(13) -0.0044(12) 0.0151(12) -0.0012(14) C4 0.0752(15) 0.0721(15) 0.0546(13) -0.0164(11) 0.0123(12) -0.0023(13) N1 0.0717(12) 0.0791(13) 0.0514(11) -0.0035(10) 0.0006(10) -0.0126(11) O1W 0.1348(17) 0.0872(13) 0.0668(12) -0.0014(11) -0.0199(12) 0.0076(13) O2W 0.158(6) 0.177(10) 0.150(6) 0.014(7) -0.125(4) 0.005(7) N2 0.295(17) 0.037(5) 0.167(11) -0.035(6) -0.094(11) 0.022(7) C5 0.058(6) 0.111(7) 0.45(3) 0.143(9) -0.003(10) -0.049(5) C6 0.073(4) 0.063(6) 0.313(13) -0.045(8) 0.131(5) -0.039(4) C7 0.137(13) 0.191(12) 0.138(9) 0.118(7) -0.023(9) -0.007(11) C8 0.225(18) 0.053(7) 0.28(3) 0.013(11) 0.053(19) 0.056(9) N3 0.118(10) 0.255(18) 0.132(11) 0.076(10) 0.029(9) 0.020(13) C9 0.044(5) 0.287(19) 0.086(9) -0.044(11) 0.005(6) 0.046(8) C10 0.098(8) 0.131(8) 0.095(7) -0.075(5) 0.020(6) -0.040(7) C11 0.042(4) 0.098(7) 0.042(4) -0.010(4) -0.013(3) -0.013(4) C12 0.272(14) 0.120(11) 0.183(9) 0.037(8) -0.171(7) 0.022(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.7044(17) . ? Mo1 O2 1.7159(16) . ? Mo1 O10 1.8968(16) . ? Mo1 O3 2.0568(15) 15_665 ? Mo1 O9 2.1875(16) . ? Mo1 O6 2.2312(14) . ? Mo1 Na1 3.5420(3) . ? Mo2 O14 1.7060(19) . ? Mo2 O13 1.713(2) . ? Mo2 O10 1.8751(17) . ? Mo2 O11 1.974(2) . ? Mo2 O7 2.3109(18) . ? Mo2 O4 2.3634(16) . ? Mo2 Mo3 3.1825(4) . ? Mo3 O1 1.700(2) . ? Mo3 O12 1.722(3) . ? Mo3 O11 1.876(2) . ? Mo3 O8 1.9427(19) . ? Mo3 O4 2.3515(16) . ? Mo3 O7 2.3866(19) . ? P1 O6 1.5156(15) . ? P1 O3 1.5397(16) . ? P1 O4 1.5545(17) . ? P1 C1 1.832(3) . ? P2 O15 1.490(2) . ? P2 O9 1.5302(18) . ? P2 O7 1.5601(19) . ? P2 C1 1.861(3) . ? Na1 O6 2.3784(14) 15_665 ? Na1 O6 2.3784(14) . ? Na1 O6 2.3784(14) 12_756 ? Na1 O6 2.3784(14) 6_654 ? Na1 O2 2.7105(16) 6_654 ? Na1 O2 2.7105(16) . ? Na1 O2 2.7105(16) 15_665 ? Na1 O2 2.7105(16) 12_756 ? Na1 Mo1 3.5420(3) 6_654 ? Na1 Mo1 3.5420(3) 15_665 ? Na1 Mo1 3.5420(3) 12_756 ? O3 Mo1 2.0568(15) 12_756 ? O8 C1 1.441(3) . ? C1 C2 1.522(3) . ? C2 C3 1.547(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.539(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.480(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 C6 1.515(10) . ? N2 C8 1.285(13) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? C5 C6 0.94(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.520(11) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N3 N3 1.737(18) 6_554 ? N3 C12 1.565(11) . ? N3 C12 1.460(12) 6_554 ? N3 C10 1.605(13) . ? C9 C10 1.569(10) . ? C11 C12 1.527(8) . ? C12 N3 1.460(12) 6_554 ? C12 C12 1.556(13) 6_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 O5 Mo1 O2 101.51(8) . . ? O5 Mo1 O10 99.27(8) . . ? O2 Mo1 O10 100.46(7) . . ? O5 Mo1 O3 92.75(7) . 15_665 ? O2 Mo1 O3 93.36(7) . 15_665 ? O10 Mo1 O3 159.42(7) . 15_665 ? O5 Mo1 O9 91.33(7) . . ? O2 Mo1 O9 165.67(7) . . ? O10 Mo1 O9 83.51(7) . . ? O3 Mo1 O9 79.54(6) 15_665 . ? O5 Mo1 O6 170.75(7) . . ? O2 Mo1 O6 86.45(6) . . ? O10 Mo1 O6 83.72(6) . . ? O3 Mo1 O6 81.99(6) 15_665 . ? O9 Mo1 O6 80.27(6) . . ? O5 Mo1 Na1 144.12(6) . . ? O2 Mo1 Na1 47.94(5) . . ? O10 Mo1 Na1 104.21(5) . . ? O3 Mo1 Na1 74.05(4) 15_665 . ? O9 Mo1 Na1 117.78(4) . . ? O6 Mo1 Na1 41.34(4) . . ? O14 Mo2 O13 103.14(9) . . ? O14 Mo2 O10 100.44(9) . . ? O13 Mo2 O10 100.02(9) . . ? O14 Mo2 O11 98.65(9) . . ? O13 Mo2 O11 96.23(10) . . ? O10 Mo2 O11 151.32(8) . . ? O14 Mo2 O7 93.31(8) . . ? O13 Mo2 O7 161.64(8) . . ? O10 Mo2 O7 84.71(7) . . ? O11 Mo2 O7 72.97(8) . . ? O14 Mo2 O4 162.15(8) . . ? O13 Mo2 O4 93.15(7) . . ? O10 Mo2 O4 83.61(6) . . ? O11 Mo2 O4 71.99(7) . . ? O7 Mo2 O4 69.60(6) . . ? O14 Mo2 Mo3 117.22(7) . . ? O13 Mo2 Mo3 115.21(7) . . ? O10 Mo2 Mo3 118.09(5) . . ? O11 Mo2 Mo3 33.26(6) . . ? O7 Mo2 Mo3 48.36(5) . . ? O4 Mo2 Mo3 47.39(4) . . ? O1 Mo3 O12 104.62(13) . . ? O1 Mo3 O11 101.41(11) . . ? O12 Mo3 O11 102.57(11) . . ? O1 Mo3 O8 99.74(11) . . ? O12 Mo3 O8 99.38(10) . . ? O11 Mo3 O8 144.37(8) . . ? O1 Mo3 O4 163.53(11) . . ? O12 Mo3 O4 91.85(9) . . ? O11 Mo3 O4 73.86(7) . . ? O8 Mo3 O4 77.73(6) . . ? O1 Mo3 O7 95.00(11) . . ? O12 Mo3 O7 160.39(9) . . ? O11 Mo3 O7 72.79(8) . . ? O8 Mo3 O7 77.11(7) . . ? O4 Mo3 O7 68.54(6) . . ? O1 Mo3 Mo2 120.29(9) . . ? O12 Mo3 Mo2 119.90(8) . . ? O11 Mo3 Mo2 35.25(6) . . ? O8 Mo3 Mo2 109.14(5) . . ? O4 Mo3 Mo2 47.70(4) . . ? O7 Mo3 Mo2 46.36(4) . . ? O6 P1 O3 112.40(8) . . ? O6 P1 O4 114.34(9) . . ? O3 P1 O4 109.40(9) . . ? O6 P1 C1 110.84(10) . . ? O3 P1 C1 108.18(10) . . ? O4 P1 C1 100.96(10) . . ? O15 P2 O9 113.15(11) . . ? O15 P2 O7 112.73(11) . . ? O9 P2 O7 111.84(10) . . ? O15 P2 C1 110.43(12) . . ? O9 P2 C1 108.19(10) . . ? O7 P2 C1 99.59(11) . . ? O6 Na1 O6 95.95(2) 15_665 . ? O6 Na1 O6 142.42(7) 15_665 12_756 ? O6 Na1 O6 95.95(2) . 12_756 ? O6 Na1 O6 95.95(2) 15_665 6_654 ? O6 Na1 O6 142.42(7) . 6_654 ? O6 Na1 O6 95.95(2) 12_756 6_654 ? O6 Na1 O2 143.36(5) 15_665 6_654 ? O6 Na1 O2 85.31(5) . 6_654 ? O6 Na1 O2 73.16(5) 12_756 6_654 ? O6 Na1 O2 64.48(5) 6_654 6_654 ? O6 Na1 O2 73.16(5) 15_665 . ? O6 Na1 O2 64.48(5) . . ? O6 Na1 O2 143.36(5) 12_756 . ? O6 Na1 O2 85.31(5) 6_654 . ? O2 Na1 O2 74.53(7) 6_654 . ? O6 Na1 O2 64.48(5) 15_665 15_665 ? O6 Na1 O2 143.36(5) . 15_665 ? O6 Na1 O2 85.31(5) 12_756 15_665 ? O6 Na1 O2 73.16(5) 6_654 15_665 ? O2 Na1 O2 129.30(4) 6_654 15_665 ? O2 Na1 O2 129.30(4) . 15_665 ? O6 Na1 O2 85.31(5) 15_665 12_756 ? O6 Na1 O2 73.16(5) . 12_756 ? O6 Na1 O2 64.48(5) 12_756 12_756 ? O6 Na1 O2 143.36(5) 6_654 12_756 ? O2 Na1 O2 129.30(4) 6_654 12_756 ? O2 Na1 O2 129.30(4) . 12_756 ? O2 Na1 O2 74.53(7) 15_665 12_756 ? O6 Na1 Mo1 131.55(3) 15_665 6_654 ? O6 Na1 Mo1 113.21(3) . 6_654 ? O6 Na1 Mo1 74.19(3) 12_756 6_654 ? O6 Na1 Mo1 38.29(3) 6_654 6_654 ? O2 Na1 Mo1 28.03(3) 6_654 6_654 ? O2 Na1 Mo1 85.24(3) . 6_654 ? O2 Na1 Mo1 102.40(3) 15_665 6_654 ? O2 Na1 Mo1 138.67(3) 12_756 6_654 ? O6 Na1 Mo1 38.29(3) 15_665 15_665 ? O6 Na1 Mo1 131.55(3) . 15_665 ? O6 Na1 Mo1 113.21(3) 12_756 15_665 ? O6 Na1 Mo1 74.19(3) 6_654 15_665 ? O2 Na1 Mo1 138.67(3) 6_654 15_665 ? O2 Na1 Mo1 102.40(3) . 15_665 ? O2 Na1 Mo1 28.03(3) 15_665 15_665 ? O2 Na1 Mo1 85.24(3) 12_756 15_665 ? Mo1 Na1 Mo1 111.599(5) 6_654 15_665 ? O6 Na1 Mo1 74.19(3) 15_665 . ? O6 Na1 Mo1 38.29(3) . . ? O6 Na1 Mo1 131.55(3) 12_756 . ? O6 Na1 Mo1 113.21(3) 6_654 . ? O2 Na1 Mo1 85.24(3) 6_654 . ? O2 Na1 Mo1 28.03(3) . . ? O2 Na1 Mo1 138.67(3) 15_665 . ? O2 Na1 Mo1 102.40(3) 12_756 . ? Mo1 Na1 Mo1 105.295(10) 6_654 . ? Mo1 Na1 Mo1 111.599(5) 15_665 . ? O6 Na1 Mo1 113.21(3) 15_665 12_756 ? O6 Na1 Mo1 74.19(3) . 12_756 ? O6 Na1 Mo1 38.29(3) 12_756 12_756 ? O6 Na1 Mo1 131.55(3) 6_654 12_756 ? O2 Na1 Mo1 102.40(3) 6_654 12_756 ? O2 Na1 Mo1 138.67(3) . 12_756 ? O2 Na1 Mo1 85.24(3) 15_665 12_756 ? O2 Na1 Mo1 28.03(3) 12_756 12_756 ? Mo1 Na1 Mo1 111.599(5) 6_654 12_756 ? Mo1 Na1 Mo1 105.295(10) 15_665 12_756 ? Mo1 Na1 Mo1 111.599(5) . 12_756 ? Mo1 O2 Na1 104.03(7) . . ? P1 O3 Mo1 137.41(9) . 12_756 ? P1 O4 Mo3 113.04(9) . . ? P1 O4 Mo2 128.83(9) . . ? Mo3 O4 Mo2 84.91(5) . . ? P1 O6 Mo1 130.62(8) . . ? P1 O6 Na1 125.40(8) . . ? Mo1 O6 Na1 100.37(5) . . ? P2 O7 Mo2 131.41(10) . . ? P2 O7 Mo3 113.14(9) . . ? Mo2 O7 Mo3 85.28(6) . . ? C1 O8 Mo3 120.54(14) . . ? P2 O9 Mo1 134.55(10) . . ? Mo2 O10 Mo1 158.28(10) . . ? Mo3 O11 Mo2 111.49(10) . . ? O8 C1 C2 107.82(19) . . ? O8 C1 P1 103.96(16) . . ? C2 C1 P1 116.25(17) . . ? O8 C1 P2 103.57(15) . . ? C2 C1 P2 115.54(18) . . ? P1 C1 P2 108.29(12) . . ? C1 C2 C3 114.1(2) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 112.7(2) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N1 C4 C3 111.3(2) . . ? N1 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 N1 H1A 109.5 . . ? C4 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C4 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C6 N2 C8 130.7(9) . . ? C6 N2 H2C 104.6 . . ? C8 N2 H2C 104.6 . . ? C6 N2 H2D 104.6 . . ? C8 N2 H2D 104.6 . . ? H2C N2 H2D 105.7 . . ? C6 C5 H5A 109.6 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C5 102.1(13) . . ? N2 C6 H6A 111.4 . . ? C5 C6 H6A 111.4 . . ? N2 C6 H6B 111.3 . . ? C5 C6 H6B 111.3 . . ? H6A C6 H6B 109.2 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.4 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 N2 115.6(10) . . ? C7 C8 H8A 108.4 . . ? N2 C8 H8A 108.4 . . ? C7 C8 H8B 108.3 . . ? N2 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? N3 N3 C12 52.2(5) 6_554 . ? N3 N3 C12 57.9(6) 6_554 6_554 ? C12 N3 C12 61.8(6) . 6_554 ? N3 N3 C10 137.8(10) 6_554 . ? C12 N3 C10 154.4(8) . . ? C12 N3 C10 101.6(8) 6_554 . ? C9 C10 N3 158.6(10) . . ? C11 C12 N3 134.6(8) . . ? C11 C12 N3 144.3(8) . 6_554 ? N3 C12 N3 70.0(7) . 6_554 ? C11 C12 C12 148.9(5) . 6_554 ? N3 C12 C12 55.8(6) . 6_554 ? N3 C12 C12 62.4(5) 6_554 6_554 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.27 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.137 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.208 #==================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 778855' #TrackingRef '- CifMo12photochrome' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 Mo12 N5 Na7 O98 P8' _chemical_formula_weight 3654.92 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' 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' Na Na 0.0362 0.0249 '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-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 19.6365(15) _cell_length_b 19.6365(15) _cell_length_c 15.5296(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5988.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 29.81 _exptl_crystal_description parallelepiped _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6681 _exptl_absorpt_correction_T_max 0.9438 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 199755 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0118 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 29.86 _reflns_number_total 8610 _reflns_number_gt 8508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0700P)^2^+11.5114P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(3) _refine_ls_number_reflns 8610 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _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 0.686865(15) 0.748307(14) 0.170842(19) 0.01378(7) Uani 1 1 d . . . Mo2 Mo 0.624719(15) 0.623758(15) 0.274433(18) 0.01334(7) Uani 1 1 d . . . Mo3 Mo 0.636567(14) 0.469922(14) 0.137953(18) 0.01118(7) Uani 1 1 d . . . P1 P 0.61231(4) 0.62822(4) 0.05015(6) 0.01058(15) Uani 1 1 d . . . P2 P 0.75149(4) 0.60001(5) 0.11668(6) 0.01197(16) Uani 1 1 d . . . O1 O 0.64548(14) 0.72186(14) 0.27579(19) 0.0170(5) Uani 1 1 d . . . O2 O 0.59939(13) 0.66398(13) 0.13757(18) 0.0141(4) Uani 1 1 d . . . O3 O 0.72335(13) 0.63779(13) 0.19738(17) 0.0138(4) Uani 1 1 d . . . O4 O 0.63642(16) 0.81604(15) 0.1421(2) 0.0217(5) Uani 1 1 d . . . O5 O 0.76198(16) 0.78532(15) 0.2032(2) 0.0206(5) Uani 1 1 d . . . O6 O 0.71029(14) 0.71670(13) 0.05535(17) 0.0140(5) Uani 1 1 d . . . O7 O 0.62412(13) 0.53640(13) 0.22384(17) 0.0144(5) Uani 1 1 d . . . O8 O 0.66670(15) 0.60392(15) 0.36809(19) 0.0200(5) Uani 1 1 d . . . O9 O 0.54099(14) 0.63042(15) 0.30509(18) 0.0190(5) Uani 1 1 d . . . O10 O 0.67962(14) 0.40899(14) 0.19616(18) 0.0165(5) Uani 1 1 d . . . O11 O 0.55587(13) 0.43711(13) 0.13416(18) 0.0151(4) Uani 1 1 d . . . O12 O 0.59949(12) 0.55169(13) 0.05104(16) 0.0117(4) Uani 1 1 d . . . O13 O 0.73103(13) 0.52496(13) 0.11478(17) 0.0131(4) Uani 1 1 d . . . O14 O 0.66438(13) 0.42840(13) 0.02109(17) 0.0124(4) Uani 1 1 d . . . O15 O 0.82709(14) 0.61014(15) 0.10677(18) 0.0176(5) Uani 1 1 d . . . C1 C 0.70369(17) 0.64642(16) 0.0327(2) 0.0115(6) Uani 1 1 d . . . C2 C 0.72874(18) 0.63775(18) -0.0600(2) 0.0139(6) Uani 1 1 d . . . H2A H 0.7753 0.6567 -0.0644 0.017 Uiso 1 1 calc R . . H2B H 0.6990 0.6647 -0.0986 0.017 Uiso 1 1 calc R . . C3 C 0.72988(18) 0.56311(19) -0.0919(2) 0.0153(6) Uani 1 1 d . . . H3A H 0.7622 0.5366 -0.0562 0.018 Uiso 1 1 calc R . . H3B H 0.6841 0.5429 -0.0843 0.018 Uiso 1 1 calc R . . C4 C 0.75068(19) 0.55745(19) -0.1864(2) 0.0163(6) Uani 1 1 d . . . H4A H 0.7916 0.5858 -0.1965 0.020 Uiso 1 1 calc R . . H4B H 0.7628 0.5096 -0.1994 0.020 Uiso 1 1 calc R . . N1 N 0.69556(17) 0.57963(17) -0.2457(2) 0.0176(6) Uani 1 1 d . . . H1A H 0.6606 0.5492 -0.2435 0.026 Uiso 1 1 calc R . . H1B H 0.7120 0.5817 -0.3005 0.026 Uiso 1 1 calc R . . H1C H 0.6803 0.6215 -0.2296 0.026 Uiso 1 1 calc R . . N2 N 0.5000 0.5000 0.5000 0.0131(10) Uani 1 4 d S . . C5 C 0.44364(19) 0.52558(19) 0.4407(2) 0.0148(6) Uani 1 1 d . . . H5A H 0.4609 0.5658 0.4091 0.018 Uiso 1 1 calc R . . H5B H 0.4338 0.4897 0.3977 0.018 Uiso 1 1 calc R . . C6 C 0.37758(19) 0.5450(2) 0.4844(2) 0.0181(7) Uani 1 1 d . . . H6A H 0.3875 0.5693 0.5388 0.022 Uiso 1 1 calc R . . H6B H 0.3514 0.5033 0.4985 0.022 Uiso 1 1 calc R . . C7 C 0.3355(2) 0.5904(2) 0.4257(3) 0.0265(9) Uani 1 1 d . . . H7A H 0.3265 0.5661 0.3710 0.032 Uiso 1 1 calc R . . H7B H 0.3618 0.6320 0.4120 0.032 Uiso 1 1 calc R . . C8 C 0.2672(2) 0.6107(3) 0.4674(3) 0.0321(10) Uani 1 1 d . . . H8A H 0.2756 0.6297 0.5248 0.048 Uiso 1 1 calc R . . H8B H 0.2380 0.5705 0.4724 0.048 Uiso 1 1 calc R . . H8C H 0.2445 0.6450 0.4315 0.048 Uiso 1 1 calc R . . Na1 Na 0.5000 0.5000 0.0000 0.0143(5) Uani 1 4 d S . . Na2 Na 0.5484(2) 0.8904(3) 0.0703(3) 0.0623(11) Uani 0.75 1 d P . . Na3 Na 0.8863(3) 0.3732(4) 0.1302(4) 0.0638(18) Uani 0.50 1 d P . . Na4 Na 0.9107(8) 0.5786(7) 0.2151(14) 0.092(7) Uani 0.25 1 d P . . O1W O 0.5609(2) 0.8202(2) 0.3451(3) 0.0367(8) Uani 1 1 d . . . O2W O 0.8958(3) 0.6840(3) 0.2369(3) 0.0512(12) Uani 1 1 d . . . O3W O 0.7351(5) 0.9366(2) 0.1001(3) 0.089(3) Uani 1 1 d . . . O4W O 0.8163(3) 0.4234(4) 0.0427(4) 0.0690(18) Uani 1 1 d . . . O5W O 0.5295(2) 0.9127(2) 0.2205(4) 0.0476(10) Uani 1 1 d . . . O6W O 0.7781(3) 0.6591(3) 0.4581(4) 0.0558(12) Uani 1 1 d . . . O7W O 0.9097(3) 0.5014(4) 0.1668(5) 0.0319(15) Uani 0.50 1 d P . . O8W O 0.4189(5) 0.9009(3) 0.0357(4) 0.087(3) Uani 1 1 d . . . O9W O 1.0275(5) 0.5958(8) 0.0136(8) 0.073(4) Uani 0.50 1 d P . . O10W O 1.0312(4) 0.6988(6) 0.1591(9) 0.135(4) Uani 1 1 d . . . O11W O 0.9968(4) 0.5296(5) 0.0715(6) 0.0421(19) 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 0.01646(13) 0.01170(12) 0.01318(13) -0.00084(10) 0.00007(10) -0.00153(9) Mo2 0.01719(14) 0.01417(13) 0.00865(13) -0.00097(10) 0.00070(10) -0.00173(10) Mo3 0.01336(13) 0.01146(12) 0.00874(12) 0.00047(9) -0.00059(9) -0.00107(9) P1 0.0117(3) 0.0107(3) 0.0093(3) -0.0002(3) -0.0002(3) -0.0003(3) P2 0.0116(4) 0.0138(4) 0.0105(4) 0.0005(3) -0.0012(3) -0.0014(3) O1 0.0220(12) 0.0155(11) 0.0136(12) -0.0035(10) 0.0015(10) -0.0022(9) O2 0.0173(11) 0.0141(11) 0.0110(11) 0.0004(9) 0.0015(9) -0.0002(9) O3 0.0147(11) 0.0146(11) 0.0121(11) -0.0002(9) -0.0021(9) -0.0027(8) O4 0.0262(14) 0.0180(12) 0.0209(14) -0.0010(11) 0.0031(11) 0.0027(10) O5 0.0234(13) 0.0178(12) 0.0208(14) -0.0050(10) -0.0004(11) -0.0045(10) O6 0.0186(11) 0.0110(11) 0.0125(11) 0.0001(9) 0.0004(9) -0.0041(8) O7 0.0182(11) 0.0154(11) 0.0095(11) -0.0001(9) 0.0004(9) -0.0023(9) O8 0.0254(13) 0.0202(12) 0.0144(12) 0.0000(10) -0.0007(11) -0.0002(10) O9 0.0208(12) 0.0240(13) 0.0122(11) -0.0012(10) 0.0025(10) -0.0018(10) O10 0.0204(12) 0.0160(11) 0.0130(12) 0.0005(9) -0.0021(9) -0.0015(9) O11 0.0137(11) 0.0166(11) 0.0149(11) -0.0015(10) 0.0022(9) -0.0019(9) O12 0.0129(10) 0.0115(10) 0.0105(10) 0.0016(8) -0.0012(9) 0.0007(8) O13 0.0144(11) 0.0137(11) 0.0111(11) 0.0008(8) 0.0006(8) -0.0005(9) O14 0.0132(11) 0.0119(10) 0.0122(11) -0.0009(8) -0.0002(8) -0.0011(8) O15 0.0144(11) 0.0227(13) 0.0157(12) 0.0023(10) -0.0015(9) -0.0030(10) C1 0.0146(14) 0.0086(12) 0.0111(14) -0.0016(11) -0.0012(11) -0.0016(10) C2 0.0178(15) 0.0133(14) 0.0107(14) 0.0020(11) 0.0013(11) -0.0010(11) C3 0.0141(14) 0.0201(16) 0.0117(16) 0.0000(12) 0.0019(12) 0.0023(12) C4 0.0161(15) 0.0219(16) 0.0108(15) -0.0001(12) 0.0027(12) 0.0013(12) N1 0.0185(14) 0.0201(15) 0.0143(14) -0.0004(11) 0.0001(11) -0.0005(11) N2 0.0156(16) 0.0156(16) 0.008(2) 0.000 0.000 0.000 C5 0.0170(15) 0.0192(15) 0.0081(13) 0.0005(12) -0.0031(11) 0.0004(12) C6 0.0188(16) 0.0229(17) 0.0126(15) 0.0030(13) -0.0005(13) 0.0034(13) C7 0.029(2) 0.032(2) 0.0188(19) 0.0080(16) 0.0006(15) 0.0086(17) C8 0.028(2) 0.041(3) 0.027(2) 0.0087(19) 0.0012(17) 0.0149(19) Na1 0.0121(7) 0.0121(7) 0.0187(14) 0.000 0.000 0.000 Na2 0.063(2) 0.077(3) 0.047(2) -0.020(2) 0.0026(18) -0.017(2) Na3 0.051(3) 0.094(5) 0.047(3) -0.011(3) -0.025(3) 0.019(3) Na4 0.081(9) 0.042(6) 0.153(17) -0.002(8) -0.088(11) -0.004(6) O1W 0.0352(18) 0.046(2) 0.0293(19) -0.0019(15) 0.0069(14) 0.0139(16) O2W 0.064(3) 0.045(2) 0.045(2) -0.016(2) -0.024(2) -0.002(2) O3W 0.205(8) 0.030(2) 0.032(2) -0.0055(18) -0.058(4) 0.029(3) O4W 0.037(2) 0.122(5) 0.048(3) -0.032(3) 0.004(2) 0.022(3) O5W 0.049(2) 0.041(2) 0.053(3) 0.004(2) -0.006(2) 0.0127(18) O6W 0.057(3) 0.064(3) 0.047(3) -0.007(2) -0.007(2) -0.004(2) O7W 0.020(3) 0.052(4) 0.023(3) 0.007(3) -0.004(2) 0.020(3) O8W 0.185(8) 0.041(3) 0.034(3) -0.010(2) -0.019(4) 0.005(4) O9W 0.028(4) 0.140(12) 0.051(6) -0.024(7) -0.008(4) -0.003(6) O10W 0.045(4) 0.179(10) 0.180(12) -0.063(9) -0.007(5) -0.005(5) O11W 0.029(3) 0.048(4) 0.049(5) 0.001(4) 0.005(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 1.717(3) . ? Mo1 O5 1.719(3) . ? Mo1 O1 1.894(3) . ? Mo1 O6 1.953(3) . ? Mo1 O3 2.322(3) . ? Mo1 O2 2.441(3) . ? Mo1 Mo2 3.1715(5) . ? Mo2 O9 1.717(3) . ? Mo2 O8 1.717(3) . ? Mo2 O7 1.887(3) . ? Mo2 O1 1.969(3) . ? Mo2 O3 2.293(3) . ? Mo2 O2 2.321(3) . ? Mo3 O11 1.712(3) . ? Mo3 O10 1.721(3) . ? Mo3 O7 1.882(3) . ? Mo3 O14 2.063(3) . ? Mo3 O13 2.177(3) . ? Mo3 O12 2.220(2) . ? Mo3 Na1 3.4828(3) . ? P1 O12 1.524(3) . ? P1 O14 1.538(3) 4_655 ? P1 O2 1.549(3) . ? P1 C1 1.850(4) . ? P1 Na1 3.4364(9) . ? P2 O15 1.506(3) . ? P2 O13 1.528(3) . ? P2 O3 1.558(3) . ? P2 C1 1.848(4) . ? O4 Na2 2.522(6) . ? O6 C1 1.430(4) . ? O11 Na1 2.659(3) . ? O12 Na1 2.340(2) . ? O14 P1 1.538(3) 3_565 ? O15 Na4 2.431(13) . ? C1 C2 1.529(5) . ? C2 C3 1.548(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.528(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.486(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 C5 1.524(4) 3_566 ? N2 C5 1.524(4) 4_656 ? N2 C5 1.524(4) . ? N2 C5 1.524(4) 2_665 ? C5 C6 1.512(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.519(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.543(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? Na1 O12 2.340(2) 4_655 ? Na1 O12 2.340(2) 2_665 ? Na1 O12 2.340(2) 3_565 ? Na1 O11 2.659(3) 3_565 ? Na1 O11 2.659(3) 4_655 ? Na1 O11 2.659(3) 2_665 ? Na1 P1 3.4364(9) 4_655 ? Na1 P1 3.4364(9) 3_565 ? Na1 P1 3.4365(9) 2_665 ? Na2 O9W 2.272(13) 3_575 ? Na2 O4W 2.345(7) 4_655 ? Na2 O5W 2.403(7) . ? Na2 O8W 2.608(10) . ? Na2 Na3 3.474(9) 4_655 ? Na3 O4W 2.170(8) . ? Na3 O10W 2.197(11) 2_765 ? Na3 O6W 2.483(9) 8_645 ? Na3 O2W 2.523(9) 8_645 ? Na3 O9W 2.551(13) 2_765 ? Na3 Na4 2.60(2) 8_645 ? Na3 O7W 2.621(11) . ? Na3 Na2 3.474(9) 3_565 ? Na4 O7W 1.691(17) . ? Na4 O2W 2.118(14) . ? Na4 O7W 2.567(14) 7_565 ? Na4 Na3 2.60(2) 7_565 ? Na4 O11W 2.96(3) . ? Na4 Na4 3.476(18) 8_645 ? Na4 Na4 3.476(18) 7_565 ? O2W Na3 2.523(9) 7_565 ? O4W Na2 2.345(7) 3_565 ? O6W Na3 2.483(9) 7_565 ? O7W Na4 2.567(14) 8_645 ? O9W O11W 1.691(18) . ? O9W Na2 2.272(12) 4_755 ? O9W Na3 2.551(13) 2_765 ? O10W Na3 2.197(11) 2_765 ? O11W O11W 1.169(18) 2_765 ? 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 O5 104.09(15) . . ? O4 Mo1 O1 100.88(14) . . ? O5 Mo1 O1 103.45(14) . . ? O4 Mo1 O6 98.22(13) . . ? O5 Mo1 O6 101.57(13) . . ? O1 Mo1 O6 143.55(11) . . ? O4 Mo1 O3 161.40(12) . . ? O5 Mo1 O3 94.51(12) . . ? O1 Mo1 O3 73.94(11) . . ? O6 Mo1 O3 78.07(10) . . ? O4 Mo1 O2 93.69(12) . . ? O5 Mo1 O2 162.21(12) . . ? O1 Mo1 O2 72.20(11) . . ? O6 Mo1 O2 75.86(10) . . ? O3 Mo1 O2 67.71(9) . . ? O4 Mo1 Mo2 120.48(10) . . ? O5 Mo1 Mo2 120.52(11) . . ? O1 Mo1 Mo2 35.60(8) . . ? O6 Mo1 Mo2 108.14(7) . . ? O3 Mo1 Mo2 46.21(6) . . ? O2 Mo1 Mo2 46.65(7) . . ? O9 Mo2 O8 104.02(14) . . ? O9 Mo2 O7 100.30(13) . . ? O8 Mo2 O7 98.60(13) . . ? O9 Mo2 O1 96.93(13) . . ? O8 Mo2 O1 96.52(13) . . ? O7 Mo2 O1 153.53(12) . . ? O9 Mo2 O3 160.81(12) . . ? O8 Mo2 O3 93.66(12) . . ? O7 Mo2 O3 84.10(10) . . ? O1 Mo2 O3 73.33(10) . . ? O9 Mo2 O2 91.31(12) . . ? O8 Mo2 O2 162.91(12) . . ? O7 Mo2 O2 85.80(10) . . ? O1 Mo2 O2 73.82(11) . . ? O3 Mo2 O2 70.26(9) . . ? O9 Mo2 Mo1 116.77(10) . . ? O8 Mo2 Mo1 114.83(10) . . ? O7 Mo2 Mo1 119.49(8) . . ? O1 Mo2 Mo1 34.04(8) . . ? O3 Mo2 Mo1 46.97(7) . . ? O2 Mo2 Mo1 49.88(6) . . ? O11 Mo3 O10 102.18(13) . . ? O11 Mo3 O7 99.51(12) . . ? O10 Mo3 O7 100.01(12) . . ? O11 Mo3 O14 93.78(12) . . ? O10 Mo3 O14 93.28(12) . . ? O7 Mo3 O14 158.72(11) . . ? O11 Mo3 O13 165.96(12) . . ? O10 Mo3 O13 90.77(12) . . ? O7 Mo3 O13 83.31(10) . . ? O14 Mo3 O13 79.94(10) . . ? O11 Mo3 O12 87.01(11) . . ? O10 Mo3 O12 169.38(11) . . ? O7 Mo3 O12 83.49(11) . . ? O14 Mo3 O12 80.67(10) . . ? O13 Mo3 O12 79.62(9) . . ? O11 Mo3 Na1 47.92(10) . . ? O10 Mo3 Na1 144.98(9) . . ? O7 Mo3 Na1 102.61(8) . . ? O14 Mo3 Na1 74.32(7) . . ? O13 Mo3 Na1 118.05(7) . . ? O12 Mo3 Na1 41.49(6) . . ? O12 P1 O14 112.09(14) . 4_655 ? O12 P1 O2 114.33(15) . . ? O14 P1 O2 109.62(15) 4_655 . ? O12 P1 C1 110.62(14) . . ? O14 P1 C1 108.01(15) 4_655 . ? O2 P1 C1 101.53(15) . . ? O12 P1 Na1 34.26(9) . . ? O14 P1 Na1 80.90(10) 4_655 . ? O2 P1 Na1 115.19(10) . . ? C1 P1 Na1 136.96(11) . . ? O15 P2 O13 112.63(16) . . ? O15 P2 O3 111.66(15) . . ? O13 P2 O3 112.43(14) . . ? O15 P2 C1 111.32(16) . . ? O13 P2 C1 109.18(15) . . ? O3 P2 C1 98.80(15) . . ? Mo1 O1 Mo2 110.36(13) . . ? P1 O2 Mo2 127.81(15) . . ? P1 O2 Mo1 112.20(14) . . ? Mo2 O2 Mo1 83.47(9) . . ? P2 O3 Mo2 131.47(15) . . ? P2 O3 Mo1 114.32(14) . . ? Mo2 O3 Mo1 86.81(9) . . ? Mo1 O4 Na2 163.4(2) . . ? C1 O6 Mo1 120.8(2) . . ? Mo3 O7 Mo2 157.64(16) . . ? Mo3 O11 Na1 103.54(12) . . ? P1 O12 Mo3 131.65(15) . . ? P1 O12 Na1 124.23(14) . . ? Mo3 O12 Na1 99.56(10) . . ? P2 O13 Mo3 134.42(16) . . ? P1 O14 Mo3 135.70(16) 3_565 . ? P2 O15 Na4 124.1(6) . . ? O6 C1 C2 108.1(3) . . ? O6 C1 P2 104.8(2) . . ? C2 C1 P2 116.5(2) . . ? O6 C1 P1 103.8(2) . . ? C2 C1 P1 115.4(2) . . ? P2 C1 P1 107.08(17) . . ? C1 C2 C3 114.3(3) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 112.4(3) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N1 C4 C3 112.3(3) . . ? N1 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C4 N1 H1A 109.5 . . ? C4 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C4 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C5 N2 C5 105.7(3) 3_566 4_656 ? C5 N2 C5 111.37(14) 3_566 . ? C5 N2 C5 111.37(14) 4_656 . ? C5 N2 C5 111.37(14) 3_566 2_665 ? C5 N2 C5 111.37(14) 4_656 2_665 ? C5 N2 C5 105.7(3) . 2_665 ? C6 C5 N2 115.8(3) . . ? C6 C5 H5A 108.3 . . ? N2 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? N2 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 110.2(3) . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 111.9(4) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O12 Na1 O12 96.59(4) 4_655 2_665 ? O12 Na1 O12 140.40(12) 4_655 3_565 ? O12 Na1 O12 96.59(4) 2_665 3_565 ? O12 Na1 O12 96.59(4) 4_655 . ? O12 Na1 O12 140.40(12) 2_665 . ? O12 Na1 O12 96.59(4) 3_565 . ? O12 Na1 O11 82.97(8) 4_655 3_565 ? O12 Na1 O11 72.46(8) 2_665 3_565 ? O12 Na1 O11 65.89(8) 3_565 3_565 ? O12 Na1 O11 146.33(8) . 3_565 ? O12 Na1 O11 146.33(8) 4_655 . ? O12 Na1 O11 82.97(8) 2_665 . ? O12 Na1 O11 72.46(8) 3_565 . ? O12 Na1 O11 65.89(8) . . ? O11 Na1 O11 127.88(7) 3_565 . ? O12 Na1 O11 65.89(8) 4_655 4_655 ? O12 Na1 O11 146.33(8) 2_665 4_655 ? O12 Na1 O11 82.97(8) 3_565 4_655 ? O12 Na1 O11 72.46(8) . 4_655 ? O11 Na1 O11 76.82(12) 3_565 4_655 ? O11 Na1 O11 127.88(7) . 4_655 ? O12 Na1 O11 72.46(8) 4_655 2_665 ? O12 Na1 O11 65.89(8) 2_665 2_665 ? O12 Na1 O11 146.33(8) 3_565 2_665 ? O12 Na1 O11 82.97(8) . 2_665 ? O11 Na1 O11 127.88(7) 3_565 2_665 ? O11 Na1 O11 76.82(12) . 2_665 ? O11 Na1 O11 127.88(7) 4_655 2_665 ? O12 Na1 P1 21.51(6) 4_655 4_655 ? O12 Na1 P1 75.13(6) 2_665 4_655 ? O12 Na1 P1 140.97(6) 3_565 4_655 ? O12 Na1 P1 114.21(6) . 4_655 ? O11 Na1 P1 75.34(6) 3_565 4_655 ? O11 Na1 P1 141.08(6) . 4_655 ? O11 Na1 P1 84.14(6) 4_655 4_655 ? O11 Na1 P1 64.99(6) 2_665 4_655 ? O12 Na1 P1 140.97(6) 4_655 3_565 ? O12 Na1 P1 114.21(6) 2_665 3_565 ? O12 Na1 P1 21.51(6) 3_565 3_565 ? O12 Na1 P1 75.13(6) . 3_565 ? O11 Na1 P1 84.14(6) 3_565 3_565 ? O11 Na1 P1 64.99(6) . 3_565 ? O11 Na1 P1 75.34(6) 4_655 3_565 ? O11 Na1 P1 141.08(6) 2_665 3_565 ? P1 Na1 P1 153.80(3) 4_655 3_565 ? O12 Na1 P1 75.13(6) 4_655 . ? O12 Na1 P1 140.97(6) 2_665 . ? O12 Na1 P1 114.22(6) 3_565 . ? O12 Na1 P1 21.51(6) . . ? O11 Na1 P1 141.07(6) 3_565 . ? O11 Na1 P1 84.14(6) . . ? O11 Na1 P1 64.99(6) 4_655 . ? O11 Na1 P1 75.34(6) 2_665 . ? P1 Na1 P1 92.944(7) 4_655 . ? P1 Na1 P1 92.944(7) 3_565 . ? O12 Na1 P1 114.21(6) 4_655 2_665 ? O12 Na1 P1 21.51(6) 2_665 2_665 ? O12 Na1 P1 75.13(6) 3_565 2_665 ? O12 Na1 P1 140.97(6) . 2_665 ? O11 Na1 P1 64.99(6) 3_565 2_665 ? O11 Na1 P1 75.34(6) . 2_665 ? O11 Na1 P1 141.08(6) 4_655 2_665 ? O11 Na1 P1 84.14(6) 2_665 2_665 ? P1 Na1 P1 92.944(7) 4_655 2_665 ? P1 Na1 P1 92.944(7) 3_565 2_665 ? P1 Na1 P1 153.80(3) . 2_665 ? O9W Na2 O4W 85.1(3) 3_575 4_655 ? O9W Na2 O5W 119.4(4) 3_575 . ? O4W Na2 O5W 151.2(3) 4_655 . ? O9W Na2 O4 112.6(4) 3_575 . ? O4W Na2 O4 79.0(2) 4_655 . ? O5W Na2 O4 77.45(19) . . ? O9W Na2 O8W 103.0(5) 3_575 . ? O4W Na2 O8W 97.2(3) 4_655 . ? O5W Na2 O8W 91.9(2) . . ? O4 Na2 O8W 143.6(3) . . ? O9W Na2 Na3 47.2(3) 3_575 4_655 ? O4W Na2 Na3 37.89(19) 4_655 4_655 ? O5W Na2 Na3 160.6(2) . 4_655 ? O4 Na2 Na3 94.57(19) . 4_655 ? O8W Na2 Na3 104.4(2) . 4_655 ? O4W Na3 O10W 152.5(6) . 2_765 ? O4W Na3 O6W 76.5(3) . 8_645 ? O10W Na3 O6W 83.9(5) 2_765 8_645 ? O4W Na3 O2W 94.9(3) . 8_645 ? O10W Na3 O2W 110.5(5) 2_765 8_645 ? O6W Na3 O2W 112.8(3) 8_645 8_645 ? O4W Na3 O9W 82.4(4) . 2_765 ? O10W Na3 O9W 79.0(5) 2_765 2_765 ? O6W Na3 O9W 91.5(4) 8_645 2_765 ? O2W Na3 O9W 154.4(5) 8_645 2_765 ? O4W Na3 Na4 128.1(5) . 8_645 ? O10W Na3 Na4 78.4(5) 2_765 8_645 ? O6W Na3 Na4 144.8(5) 8_645 8_645 ? O2W Na3 Na4 48.8(3) 8_645 8_645 ? O9W Na3 Na4 114.3(5) 2_765 8_645 ? O4W Na3 O7W 79.1(3) . . ? O10W Na3 O7W 116.4(4) 2_765 . ? O6W Na3 O7W 154.8(3) 8_645 . ? O2W Na3 O7W 75.5(3) 8_645 . ? O9W Na3 O7W 79.0(5) 2_765 . ? Na4 Na3 O7W 58.8(3) 8_645 . ? O4W Na3 Na2 41.6(2) . 3_565 ? O10W Na3 Na2 116.8(4) 2_765 3_565 ? O6W Na3 Na2 81.2(2) 8_645 3_565 ? O2W Na3 Na2 131.9(3) 8_645 3_565 ? O9W Na3 Na2 40.8(3) 2_765 3_565 ? Na4 Na3 Na2 134.1(4) 8_645 3_565 ? O7W Na3 Na2 76.4(3) . 3_565 ? O7W Na4 O2W 160.9(10) . . ? O7W Na4 O15 85.1(6) . . ? O2W Na4 O15 76.6(4) . . ? O7W Na4 O7W 113.9(7) . 7_565 ? O2W Na4 O7W 83.9(5) . 7_565 ? O15 Na4 O7W 160.1(6) . 7_565 ? O7W Na4 Na3 130.0(10) . 7_565 ? O2W Na4 Na3 63.6(6) . 7_565 ? O15 Na4 Na3 112.3(7) . 7_565 ? O7W Na4 Na3 60.9(5) 7_565 7_565 ? O7W Na4 O11W 51.7(7) . . ? O2W Na4 O11W 121.1(9) . . ? O15 Na4 O11W 87.0(7) . . ? O7W Na4 O11W 99.9(6) 7_565 . ? Na3 Na4 O11W 160.4(5) 7_565 . ? O7W Na4 Na4 44.7(4) . 8_645 ? O2W Na4 Na4 152.3(13) . 8_645 ? O15 Na4 Na4 119.9(6) . 8_645 ? O7W Na4 Na4 79.6(5) 7_565 8_645 ? Na3 Na4 Na4 88.9(9) 7_565 8_645 ? O11W Na4 Na4 83.8(6) . 8_645 ? O7W Na4 Na4 101.7(5) . 7_565 ? O2W Na4 Na4 91.3(6) . 7_565 ? O15 Na4 Na4 147.2(12) . 7_565 ? O7W Na4 Na4 27.6(3) 7_565 7_565 ? Na3 Na4 Na4 88.0(7) 7_565 7_565 ? O11W Na4 Na4 73.3(6) . 7_565 ? Na4 Na4 Na4 84.4(4) 8_645 7_565 ? Na4 O2W Na3 67.6(7) . 7_565 ? Na3 O4W Na2 100.5(3) . 3_565 ? Na4 O7W Na4 107.7(5) . 8_645 ? Na4 O7W Na3 163.5(9) . . ? Na4 O7W Na3 60.3(6) 8_645 . ? O11W O9W Na2 104.1(8) . 4_755 ? O11W O9W Na3 92.5(6) . 2_765 ? Na2 O9W Na3 92.0(4) 4_755 2_765 ? O11W O11W O9W 136.5(8) 2_765 . ? O11W O11W Na4 112.6(6) 2_765 . ? O9W O11W Na4 110.7(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.86 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.158 _refine_diff_density_min -2.395 _refine_diff_density_rms 0.534