# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cyy _database_code_depnum_ccdc_archive 'CCDC 897841' #TrackingRef '897841.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Ce3 Mn2 Na O31' _chemical_formula_weight 1289.75 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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 Orthorhombic _symmetry_space_group_name_H-M 'Pnma ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 16.681(6) _cell_length_b 18.988(6) _cell_length_c 15.587(7) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 4937(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description tetragonal-prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284.0 _exptl_absorpt_coefficient_mu 3.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.631 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27837 _diffrn_reflns_av_R_equivalents 0.1579 _diffrn_reflns_av_sigmaI/netI 0.1121 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4492 _reflns_number_gt 2926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.0000P] 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 4492 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.241 0.528 0.027 1998.6 421.9 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 Ce2 Ce -0.06238(3) 0.65140(3) 0.10066(3) 0.02759(18) Uani 1 1 d . . . Ce1 Ce 0.05452(5) 0.7500 -0.06736(5) 0.0323(2) Uani 1 2 d S . . Mn2 Mn -0.13703(13) 0.7500 -0.04711(13) 0.0313(5) Uani 1 2 d S . . Mn1 Mn 0.09110(12) 0.7500 0.13551(13) 0.0270(5) Uani 1 2 d S . . Na1 Na -0.2545(4) 0.7500 0.2302(4) 0.0514(16) Uani 1 2 d S . . C10 C 0.0891(7) 0.6244(6) 0.2441(7) 0.042(3) Uani 1 1 d . . . C9 C -0.2343(6) 0.6254(6) -0.0130(7) 0.038(3) Uani 1 1 d . . . O1 O -0.0157(6) 0.7500 -0.2072(7) 0.056(3) Uani 1 2 d S . . O2 O -0.0598(4) 0.6838(4) -0.0453(4) 0.0338(16) Uani 1 1 d . . . O9W O -0.3225(9) 0.7500 0.0977(9) 0.089(4) Uani 1 2 d S . . O5 O 0.1974(6) 0.7500 -0.0336(7) 0.061(4) Uani 1 2 d S . . O8W O -0.0217(5) 0.5423(4) 0.0374(5) 0.0468(19) Uani 1 1 d . . . O7 O -0.1537(4) 0.6640(4) 0.2232(5) 0.0425(18) Uani 1 1 d . . . O8 O -0.2260(4) 0.6823(4) -0.0579(4) 0.0398(17) Uani 1 1 d . . . O9 O 0.0265(5) 0.6044(4) 0.2106(5) 0.0469(19) Uani 1 1 d . . . O10 O -0.1388(5) 0.7500 0.0704(5) 0.030(2) Uani 1 2 d S . . O11 O -0.1875(4) 0.6049(4) 0.0432(5) 0.0463(19) Uani 1 1 d . . . O12 O 0.2070(5) 0.7500 0.1084(6) 0.037(2) Uani 1 2 d S . . O13 O 0.0640(4) 0.6840(3) 0.0557(4) 0.0331(16) Uani 1 1 d . . . O14 O -0.1447(6) 0.7500 -0.1744(6) 0.044(3) Uani 1 2 d S . . O15 O -0.1216(5) 0.5554(4) 0.1961(5) 0.048(2) Uani 1 1 d . . . O16 O -0.0126(5) 0.7500 0.1723(6) 0.032(2) Uani 1 2 d S . . O7W O 0.1041(7) 0.6408(5) -0.1343(6) 0.096(4) Uani 1 1 d . . . C8 C -0.3069(8) 0.5803(6) -0.0333(9) 0.065(4) Uani 1 1 d . . . H8A H -0.3080 0.5404 0.0045 0.098 Uiso 1 1 calc R . . H8B H -0.3038 0.5643 -0.0916 0.098 Uiso 1 1 calc R . . H8C H -0.3548 0.6076 -0.0256 0.098 Uiso 1 1 calc R . . C7 C 0.1303(9) 0.5803(8) 0.3102(8) 0.090(5) Uani 1 1 d . . . H7A H 0.1784 0.6036 0.3287 0.134 Uiso 1 1 calc R . . H7B H 0.1437 0.5353 0.2859 0.134 Uiso 1 1 calc R . . H7C H 0.0953 0.5736 0.3584 0.134 Uiso 1 1 calc R . . C6 C -0.1555(7) 0.5998(7) 0.2440(8) 0.048(3) Uani 1 1 d . . . C5 C 0.2375(10) 0.7500 0.0305(11) 0.054(5) Uani 1 2 d S . . C4 C 0.3242(11) 0.7500 0.0301(13) 0.117(11) Uani 1 2 d S . . H4A H 0.3432 0.7500 -0.0280 0.176 Uiso 1 2 calc SR . . H4B H 0.3435 0.7087 0.0591 0.176 Uiso 0.50 1 calc PR . . H4C H 0.3435 0.7913 0.0591 0.176 Uiso 0.50 1 calc PR . . C3 C -0.1918(10) 0.5767(7) 0.3233(9) 0.087(5) Uani 1 1 d . . . H3A H -0.2434 0.5565 0.3115 0.130 Uiso 1 1 calc R . . H3B H -0.1980 0.6162 0.3611 0.130 Uiso 1 1 calc R . . H3C H -0.1581 0.5420 0.3499 0.130 Uiso 1 1 calc R . . C2 C -0.1079(14) 0.7500 -0.3184(14) 0.129(11) Uani 1 2 d S . . H2A H -0.1651 0.7500 -0.3253 0.194 Uiso 1 2 calc SR . . H2B H -0.0857 0.7087 -0.3449 0.194 Uiso 0.50 1 calc PR . . H2C H -0.0857 0.7913 -0.3449 0.194 Uiso 0.50 1 calc PR . . C1 C -0.0880(11) 0.7500 -0.2262(10) 0.047(4) Uani 1 2 d S . . O3 O 0.1271(4) 0.6808(4) 0.2229(4) 0.0376(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce2 0.0303(3) 0.0239(3) 0.0286(3) -0.0013(2) 0.0007(3) -0.0003(2) Ce1 0.0312(5) 0.0419(5) 0.0237(4) 0.000 0.0011(4) 0.000 Mn2 0.0303(12) 0.0348(12) 0.0289(12) 0.000 -0.0077(9) 0.000 Mn1 0.0229(11) 0.0346(12) 0.0235(11) 0.000 -0.0005(9) 0.000 Na1 0.039(4) 0.049(4) 0.066(4) 0.000 -0.002(3) 0.000 C10 0.058(7) 0.036(6) 0.034(7) 0.011(5) -0.002(6) 0.003(5) C9 0.032(6) 0.035(6) 0.046(7) -0.003(5) 0.004(5) -0.012(5) O1 0.034(7) 0.097(9) 0.036(7) 0.000 -0.006(5) 0.000 O2 0.029(4) 0.036(4) 0.037(4) -0.005(3) -0.002(3) 0.001(3) O9W 0.085(10) 0.103(11) 0.080(10) 0.000 0.014(9) 0.000 O5 0.036(7) 0.131(11) 0.017(6) 0.000 0.007(5) 0.000 O8W 0.044(4) 0.039(4) 0.058(5) 0.000(3) -0.005(4) 0.002(4) O7 0.050(5) 0.030(4) 0.048(5) 0.005(3) 0.012(4) -0.003(3) O8 0.034(4) 0.045(4) 0.040(4) -0.007(4) -0.014(3) -0.005(3) O9 0.046(5) 0.048(5) 0.047(5) 0.010(4) -0.010(4) -0.007(4) O10 0.022(5) 0.044(6) 0.023(5) 0.000 0.003(4) 0.000 O11 0.042(5) 0.044(4) 0.053(5) 0.007(4) -0.014(4) -0.007(4) O12 0.016(5) 0.063(7) 0.032(6) 0.000 -0.004(4) 0.000 O13 0.041(4) 0.025(3) 0.034(4) -0.005(3) 0.008(3) 0.004(3) O14 0.029(6) 0.071(8) 0.033(6) 0.000 -0.003(5) 0.000 O15 0.052(5) 0.031(4) 0.061(5) 0.004(4) 0.006(4) -0.003(4) O16 0.016(5) 0.044(6) 0.036(6) 0.000 0.009(4) 0.000 O7W 0.139(9) 0.074(7) 0.076(7) -0.034(5) -0.055(7) 0.043(6) C8 0.056(9) 0.059(8) 0.081(10) -0.004(7) -0.012(7) -0.019(7) C7 0.101(12) 0.105(12) 0.064(10) 0.048(9) -0.046(9) -0.022(10) C6 0.037(7) 0.057(8) 0.050(8) -0.003(6) -0.001(6) -0.001(6) C5 0.029(9) 0.096(15) 0.038(11) 0.000 0.012(8) 0.000 C4 0.026(10) 0.28(4) 0.048(13) 0.000 -0.004(9) 0.000 C3 0.112(13) 0.070(10) 0.079(11) 0.026(8) 0.045(10) -0.003(9) C2 0.070(17) 0.25(4) 0.064(16) 0.000 -0.023(13) 0.000 C1 0.058(11) 0.061(11) 0.021(8) 0.000 -0.025(8) 0.000 O3 0.034(4) 0.046(4) 0.033(4) 0.014(3) -0.007(3) -0.001(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 Ce2 O13 2.306(6) . ? Ce2 O10 2.313(5) . ? Ce2 O16 2.332(5) . ? Ce2 O2 2.358(7) . ? Ce2 O8W 2.392(7) . ? Ce2 O11 2.437(7) . ? Ce2 O9 2.436(7) . ? Ce2 O7 2.455(7) . ? Ce2 O15 2.551(7) . ? Ce2 C6 2.892(12) . ? Ce2 Mn1 3.2179(18) . ? Ce2 Mn2 3.2188(18) . ? Ce1 O13 2.297(7) 8_575 ? Ce1 O13 2.297(7) . ? Ce1 O2 2.310(6) . ? Ce1 O2 2.310(6) 8_575 ? Ce1 O5 2.441(11) . ? Ce1 O7W 2.464(9) . ? Ce1 O7W 2.464(9) 8_575 ? Ce1 O1 2.474(10) . ? Ce1 Mn2 3.211(2) . ? Ce1 Mn1 3.221(2) . ? Ce1 Ce2 3.7638(11) 8_575 ? Mn2 O2 1.800(7) 8_575 ? Mn2 O2 1.800(7) . ? Mn2 O10 1.832(9) . ? Mn2 O8 1.971(7) . ? Mn2 O8 1.971(7) 8_575 ? Mn2 O14 1.988(10) . ? Mn2 Ce2 3.2188(18) 8_575 ? Mn1 O16 1.823(8) . ? Mn1 O13 1.822(6) . ? Mn1 O13 1.822(6) 8_575 ? Mn1 O12 1.980(9) . ? Mn1 O3 1.986(7) 8_575 ? Mn1 O3 1.986(7) . ? Mn1 Ce2 3.2179(18) 8_575 ? Mn1 Na1 3.318(7) 6_656 ? Na1 O9W 2.356(16) . ? Na1 O7 2.347(8) 8_575 ? Na1 O7 2.347(8) . ? Na1 O3 2.482(8) 6_556 ? Na1 O3 2.482(8) 3_465 ? Na1 O12 2.597(12) 6_556 ? Na1 Mn1 3.318(7) 6_556 ? C10 O9 1.227(13) . ? C10 O3 1.288(12) . ? C10 C7 1.495(15) . ? C9 O11 1.235(12) . ? C9 O8 1.295(12) . ? C9 C8 1.517(14) . ? O1 C1 1.243(19) . ? O5 C5 1.203(18) . ? O7 C6 1.261(13) . ? O10 Ce2 2.313(5) 8_575 ? O12 C5 1.315(17) . ? O12 Na1 2.597(12) 6_656 ? O14 C1 1.243(19) . ? O15 C6 1.261(13) . ? O16 Ce2 2.332(5) 8_575 ? C6 C3 1.444(16) . ? C5 C4 1.45(2) . ? C2 C1 1.47(2) . ? O3 Na1 2.482(8) 6_656 ? 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 O13 Ce2 O10 103.0(2) . . ? O13 Ce2 O16 66.7(3) . . ? O10 Ce2 O16 69.1(3) . . ? O13 Ce2 O2 67.7(2) . . ? O10 Ce2 O2 66.6(3) . . ? O16 Ce2 O2 104.3(3) . . ? O13 Ce2 O8W 81.3(2) . . ? O10 Ce2 O8W 140.6(3) . . ? O16 Ce2 O8W 142.3(3) . . ? O2 Ce2 O8W 79.8(2) . . ? O13 Ce2 O11 140.2(2) . . ? O10 Ce2 O11 75.3(2) . . ? O16 Ce2 O11 140.5(3) . . ? O2 Ce2 O11 75.8(2) . . ? O8W Ce2 O11 77.2(3) . . ? O13 Ce2 O9 75.8(2) . . ? O10 Ce2 O9 140.8(3) . . ? O16 Ce2 O9 75.0(3) . . ? O2 Ce2 O9 139.8(2) . . ? O8W Ce2 O9 78.5(3) . . ? O11 Ce2 O9 130.3(2) . . ? O13 Ce2 O7 141.0(2) . . ? O10 Ce2 O7 74.8(3) . . ? O16 Ce2 O7 76.7(3) . . ? O2 Ce2 O7 137.5(2) . . ? O8W Ce2 O7 125.5(2) . . ? O11 Ce2 O7 77.9(3) . . ? O9 Ce2 O7 82.3(3) . . ? O13 Ce2 O15 136.3(2) . . ? O10 Ce2 O15 118.9(3) . . ? O16 Ce2 O15 115.6(3) . . ? O2 Ce2 O15 139.1(2) . . ? O8W Ce2 O15 74.4(2) . . ? O11 Ce2 O15 67.9(2) . . ? O9 Ce2 O15 64.1(2) . . ? O7 Ce2 O15 51.4(2) . . ? O13 Ce2 C6 144.7(3) . . ? O10 Ce2 C6 97.8(3) . . ? O16 Ce2 C6 95.3(3) . . ? O2 Ce2 C6 147.5(3) . . ? O8W Ce2 C6 100.2(3) . . ? O11 Ce2 C6 72.6(3) . . ? O9 Ce2 C6 70.1(3) . . ? O7 Ce2 C6 25.6(3) . . ? O15 Ce2 C6 25.8(3) . . ? O13 Ce2 Mn1 33.67(16) . . ? O10 Ce2 Mn1 90.10(17) . . ? O16 Ce2 Mn1 33.8(2) . . ? O2 Ce2 Mn1 89.82(16) . . ? O8W Ce2 Mn1 110.35(18) . . ? O11 Ce2 Mn1 162.60(17) . . ? O9 Ce2 Mn1 67.05(17) . . ? O7 Ce2 Mn1 107.79(17) . . ? O15 Ce2 Mn1 128.69(18) . . ? C6 Ce2 Mn1 119.6(2) . . ? O13 Ce2 Mn2 88.87(17) . . ? O10 Ce2 Mn2 33.9(2) . . ? O16 Ce2 Mn2 90.76(18) . . ? O2 Ce2 Mn2 33.34(16) . . ? O8W Ce2 Mn2 108.55(18) . . ? O11 Ce2 Mn2 67.43(17) . . ? O9 Ce2 Mn2 162.21(18) . . ? O7 Ce2 Mn2 105.08(18) . . ? O15 Ce2 Mn2 133.08(18) . . ? C6 Ce2 Mn2 122.8(2) . . ? Mn1 Ce2 Mn2 95.18(5) . . ? O13 Ce1 O13 66.1(3) 8_575 . ? O13 Ce1 O2 103.3(2) 8_575 . ? O13 Ce1 O2 68.7(2) . . ? O13 Ce1 O2 68.7(2) 8_575 8_575 ? O13 Ce1 O2 103.3(2) . 8_575 ? O2 Ce1 O2 65.9(3) . 8_575 ? O13 Ce1 O5 75.7(2) 8_575 . ? O13 Ce1 O5 75.7(2) . . ? O2 Ce1 O5 140.7(2) . . ? O2 Ce1 O5 140.7(2) 8_575 . ? O13 Ce1 O7W 142.2(3) 8_575 . ? O13 Ce1 O7W 82.6(3) . . ? O2 Ce1 O7W 83.2(3) . . ? O2 Ce1 O7W 142.9(3) 8_575 . ? O5 Ce1 O7W 76.3(3) . . ? O13 Ce1 O7W 82.6(3) 8_575 8_575 ? O13 Ce1 O7W 142.2(3) . 8_575 ? O2 Ce1 O7W 142.9(3) . 8_575 ? O2 Ce1 O7W 83.2(3) 8_575 8_575 ? O5 Ce1 O7W 76.3(3) . 8_575 ? O7W Ce1 O7W 114.6(6) . 8_575 ? O13 Ce1 O1 140.2(2) 8_575 . ? O13 Ce1 O1 140.2(2) . . ? O2 Ce1 O1 74.9(3) . . ? O2 Ce1 O1 74.9(3) 8_575 . ? O5 Ce1 O1 130.7(3) . . ? O7W Ce1 O1 77.6(2) . . ? O7W Ce1 O1 77.6(2) 8_575 . ? O13 Ce1 Mn2 89.23(16) 8_575 . ? O13 Ce1 Mn2 89.23(16) . . ? O2 Ce1 Mn2 33.24(16) . . ? O2 Ce1 Mn2 33.24(16) 8_575 . ? O5 Ce1 Mn2 161.9(2) . . ? O7W Ce1 Mn2 112.1(3) . . ? O7W Ce1 Mn2 112.1(3) 8_575 . ? O1 Ce1 Mn2 67.4(2) . . ? O13 Ce1 Mn1 33.57(16) 8_575 . ? O13 Ce1 Mn1 33.57(16) . . ? O2 Ce1 Mn1 90.60(16) . . ? O2 Ce1 Mn1 90.60(16) 8_575 . ? O5 Ce1 Mn1 66.6(2) . . ? O7W Ce1 Mn1 110.6(2) . . ? O7W Ce1 Mn1 110.6(2) 8_575 . ? O1 Ce1 Mn1 162.7(2) . . ? Mn2 Ce1 Mn1 95.28(6) . . ? O13 Ce1 Ce2 35.24(16) 8_575 8_575 ? O13 Ce1 Ce2 74.09(15) . 8_575 ? O2 Ce1 Ce2 74.90(16) . 8_575 ? O2 Ce1 Ce2 36.69(16) 8_575 8_575 ? O5 Ce1 Ce2 110.8(2) . 8_575 ? O7W Ce1 Ce2 152.5(3) . 8_575 ? O7W Ce1 Ce2 92.9(3) 8_575 8_575 ? O1 Ce1 Ce2 111.6(2) . 8_575 ? Mn2 Ce1 Ce2 54.27(3) . 8_575 ? Mn1 Ce1 Ce2 54.20(3) . 8_575 ? O13 Ce1 Ce2 74.09(15) 8_575 . ? O13 Ce1 Ce2 35.24(16) . . ? O2 Ce1 Ce2 36.69(16) . . ? O2 Ce1 Ce2 74.90(16) 8_575 . ? O5 Ce1 Ce2 110.8(2) . . ? O7W Ce1 Ce2 92.9(3) . . ? O7W Ce1 Ce2 152.5(3) 8_575 . ? O1 Ce1 Ce2 111.6(2) . . ? Mn2 Ce1 Ce2 54.27(3) . . ? Mn1 Ce1 Ce2 54.20(3) . . ? Ce2 Ce1 Ce2 59.66(3) 8_575 . ? O2 Mn2 O2 88.6(4) 8_575 . ? O2 Mn2 O10 89.8(3) 8_575 . ? O2 Mn2 O10 89.8(3) . . ? O2 Mn2 O8 174.7(3) 8_575 . ? O2 Mn2 O8 94.9(3) . . ? O10 Mn2 O8 94.2(3) . . ? O2 Mn2 O8 94.9(3) 8_575 8_575 ? O2 Mn2 O8 174.7(3) . 8_575 ? O10 Mn2 O8 94.2(3) . 8_575 ? O8 Mn2 O8 81.4(4) . 8_575 ? O2 Mn2 O14 93.5(3) 8_575 . ? O2 Mn2 O14 93.5(3) . . ? O10 Mn2 O14 175.4(4) . . ? O8 Mn2 O14 82.3(3) . . ? O8 Mn2 O14 82.3(3) 8_575 . ? O2 Mn2 Ce1 44.7(2) 8_575 . ? O2 Mn2 Ce1 44.7(2) . . ? O10 Mn2 Ce1 96.5(3) . . ? O8 Mn2 Ce1 137.8(2) . . ? O8 Mn2 Ce1 137.8(2) 8_575 . ? O14 Mn2 Ce1 88.1(3) . . ? O2 Mn2 Ce2 46.0(2) 8_575 8_575 ? O2 Mn2 Ce2 96.8(2) . 8_575 ? O10 Mn2 Ce2 44.81(15) . 8_575 ? O8 Mn2 Ce2 137.0(2) . 8_575 ? O8 Mn2 Ce2 88.5(2) 8_575 8_575 ? O14 Mn2 Ce2 137.65(15) . 8_575 ? Ce1 Mn2 Ce2 71.66(4) . 8_575 ? O2 Mn2 Ce2 96.8(2) 8_575 . ? O2 Mn2 Ce2 46.0(2) . . ? O10 Mn2 Ce2 44.81(15) . . ? O8 Mn2 Ce2 88.5(2) . . ? O8 Mn2 Ce2 137.0(2) 8_575 . ? O14 Mn2 Ce2 137.65(15) . . ? Ce1 Mn2 Ce2 71.66(4) . . ? Ce2 Mn2 Ce2 71.13(5) 8_575 . ? O16 Mn1 O13 88.8(3) . . ? O16 Mn1 O13 88.8(3) . 8_575 ? O13 Mn1 O13 86.9(4) . 8_575 ? O16 Mn1 O12 174.0(4) . . ? O13 Mn1 O12 95.5(3) . . ? O13 Mn1 O12 95.5(3) 8_575 . ? O16 Mn1 O3 94.1(3) . 8_575 ? O13 Mn1 O3 176.5(3) . 8_575 ? O13 Mn1 O3 95.1(3) 8_575 8_575 ? O12 Mn1 O3 81.5(3) . 8_575 ? O16 Mn1 O3 94.1(3) . . ? O13 Mn1 O3 95.1(3) . . ? O13 Mn1 O3 176.5(3) 8_575 . ? O12 Mn1 O3 81.5(3) . . ? O3 Mn1 O3 82.8(4) 8_575 . ? O16 Mn1 Ce2 45.40(17) . 8_575 ? O13 Mn1 Ce2 95.0(2) . 8_575 ? O13 Mn1 Ce2 44.6(2) 8_575 8_575 ? O12 Mn1 Ce2 137.83(14) . 8_575 ? O3 Mn1 Ce2 88.4(2) 8_575 8_575 ? O3 Mn1 Ce2 137.8(2) . 8_575 ? O16 Mn1 Ce2 45.40(17) . . ? O13 Mn1 Ce2 44.6(2) . . ? O13 Mn1 Ce2 95.0(2) 8_575 . ? O12 Mn1 Ce2 137.83(14) . . ? O3 Mn1 Ce2 137.8(2) 8_575 . ? O3 Mn1 Ce2 88.4(2) . . ? Ce2 Mn1 Ce2 71.15(5) 8_575 . ? O16 Mn1 Ce1 97.4(3) . . ? O13 Mn1 Ce1 44.2(2) . . ? O13 Mn1 Ce1 44.2(2) 8_575 . ? O12 Mn1 Ce1 88.6(3) . . ? O3 Mn1 Ce1 137.0(2) 8_575 . ? O3 Mn1 Ce1 137.0(2) . . ? Ce2 Mn1 Ce1 71.55(4) 8_575 . ? Ce2 Mn1 Ce1 71.55(4) . . ? O16 Mn1 Na1 122.6(3) . 6_656 ? O13 Mn1 Na1 128.5(2) . 6_656 ? O13 Mn1 Na1 128.5(2) 8_575 6_656 ? O12 Mn1 Na1 51.5(3) . 6_656 ? O3 Mn1 Na1 48.1(2) 8_575 6_656 ? O3 Mn1 Na1 48.1(2) . 6_656 ? Ce2 Mn1 Na1 136.38(7) 8_575 6_656 ? Ce2 Mn1 Na1 136.38(7) . 6_656 ? Ce1 Mn1 Na1 140.02(13) . 6_656 ? O9W Na1 O7 107.7(4) . 8_575 ? O9W Na1 O7 107.7(4) . . ? O7 Na1 O7 88.2(4) 8_575 . ? O9W Na1 O3 82.8(4) . 6_556 ? O7 Na1 O3 162.2(4) 8_575 6_556 ? O7 Na1 O3 102.5(2) . 6_556 ? O9W Na1 O3 82.8(4) . 3_465 ? O7 Na1 O3 102.5(2) 8_575 3_465 ? O7 Na1 O3 162.2(4) . 3_465 ? O3 Na1 O3 63.9(3) 6_556 3_465 ? O9W Na1 O12 136.9(5) . 6_556 ? O7 Na1 O12 102.8(3) 8_575 6_556 ? O7 Na1 O12 102.8(3) . 6_556 ? O3 Na1 O12 61.2(3) 6_556 6_556 ? O3 Na1 O12 61.2(3) 3_465 6_556 ? O9W Na1 Mn1 100.3(4) . 6_556 ? O7 Na1 Mn1 125.8(2) 8_575 6_556 ? O7 Na1 Mn1 125.8(2) . 6_556 ? O3 Na1 Mn1 36.57(17) 6_556 6_556 ? O3 Na1 Mn1 36.57(17) 3_465 6_556 ? O12 Na1 Mn1 36.6(2) 6_556 6_556 ? O9 C10 O3 124.5(10) . . ? O9 C10 C7 120.7(11) . . ? O3 C10 C7 114.6(11) . . ? O11 C9 O8 125.4(9) . . ? O11 C9 C8 118.3(10) . . ? O8 C9 C8 116.3(10) . . ? C1 O1 Ce1 132.0(10) . . ? Mn2 O2 Ce1 102.0(3) . . ? Mn2 O2 Ce2 100.6(3) . . ? Ce1 O2 Ce2 107.5(2) . . ? C5 O5 Ce1 136.3(10) . . ? C6 O7 Na1 130.0(7) . . ? C6 O7 Ce2 96.9(7) . . ? Na1 O7 Ce2 123.3(3) . . ? C9 O8 Mn2 125.3(6) . . ? C10 O9 Ce2 134.7(7) . . ? Mn2 O10 Ce2 101.2(3) . 8_575 ? Mn2 O10 Ce2 101.2(3) . . ? Ce2 O10 Ce2 108.1(3) 8_575 . ? C9 O11 Ce2 133.4(6) . . ? C5 O12 Mn1 125.1(9) . . ? C5 O12 Na1 143.0(9) . 6_656 ? Mn1 O12 Na1 91.9(4) . 6_656 ? Mn1 O13 Ce1 102.2(3) . . ? Mn1 O13 Ce2 101.8(3) . . ? Ce1 O13 Ce2 109.7(3) . . ? C1 O14 Mn2 126.8(9) . . ? C6 O15 Ce2 92.4(7) . . ? Mn1 O16 Ce2 100.8(3) . . ? Mn1 O16 Ce2 100.8(3) . 8_575 ? Ce2 O16 Ce2 106.8(4) . 8_575 ? O7 C6 O15 118.9(11) . . ? O7 C6 C3 121.6(11) . . ? O15 C6 C3 119.4(12) . . ? O7 C6 Ce2 57.4(6) . . ? O15 C6 Ce2 61.8(6) . . ? C3 C6 Ce2 171.5(9) . . ? O5 C5 O12 123.5(14) . . ? O5 C5 C4 123.5(16) . . ? O12 C5 C4 113.0(15) . . ? O14 C1 O1 125.8(14) . . ? O14 C1 C2 117.5(16) . . ? O1 C1 C2 116.7(17) . . ? C10 O3 Mn1 125.3(7) . . ? C10 O3 Na1 139.2(7) . 6_656 ? Mn1 O3 Na1 95.3(3) . 6_656 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.000 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.190 data_yy _database_code_depnum_ccdc_archive 'CCDC 897842' #TrackingRef '897842.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H38 Mn Na2 Nd2 O24' _chemical_formula_weight 1003.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 8.255(1) _cell_length_b 10.394(1) _cell_length_c 11.550(1) _cell_angle_alpha 111.477(1) _cell_angle_beta 107.859(1) _cell_angle_gamma 93.506(1) _cell_volume 860.78(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 479.0 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.618 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7357 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4264 _reflns_number_gt 3656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.0799P] 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 4264 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Nd1 Nd -0.08449(3) 0.08088(2) -0.33222(2) 0.01878(7) Uani 1 1 d . . . Mn1 Mn 0.0000 0.0000 0.0000 0.01991(17) Uani 1 2 d S . . O8 O 0.1444(4) 0.2254(3) -0.1302(3) 0.0376(8) Uani 1 1 d . . . O7 O -0.1735(4) 0.0509(3) -0.1548(3) 0.0272(6) Uani 1 1 d . . . O6 O 0.1121(4) 0.1303(3) -0.4346(3) 0.0316(7) Uani 1 1 d . . . O5 O 0.1043(4) -0.0810(3) -0.2904(3) 0.0315(7) Uani 1 1 d . . . O4W O -0.2859(4) 0.1098(4) -0.5299(3) 0.0339(7) Uani 1 1 d . . . O4 O -0.3841(4) 0.0825(4) -0.3043(3) 0.0362(8) Uani 1 1 d . . . C8 C 0.1010(5) -0.1771(4) -0.2483(4) 0.0250(8) Uani 1 1 d . . . C7 C -0.4467(7) 0.0610(7) -0.1221(6) 0.0476(14) Uani 1 1 d . . . H7A H -0.5586 0.0762 -0.1657 0.071 Uiso 1 1 calc R . . H7B H -0.3967 0.1332 -0.0335 0.071 Uiso 1 1 calc R . . H7C H -0.4593 -0.0296 -0.1181 0.071 Uiso 1 1 calc R . . C6 C 0.2314(6) 0.2060(4) -0.4418(4) 0.0276(9) Uani 1 1 d . . . C5 C 0.3247(8) 0.3427(6) -0.3314(6) 0.0557(16) Uani 1 1 d . . . H5A H 0.3283 0.3393 -0.2487 0.084 Uiso 1 1 calc R . . H5B H 0.2656 0.4159 -0.3441 0.084 Uiso 1 1 calc R . . H5C H 0.4409 0.3618 -0.3296 0.084 Uiso 1 1 calc R . . O2 O 0.2116(4) 0.1689(3) 0.0444(3) 0.0315(7) Uani 1 1 d . . . O1 O 0.0667(4) -0.1662(3) -0.1473(3) 0.0325(7) Uani 1 1 d . . . C4 C 0.2340(5) 0.2462(4) -0.0136(4) 0.0246(8) Uani 1 1 d . . . O3W O -0.1113(5) 0.3328(4) -0.2606(4) 0.0569(11) Uani 1 1 d . . . C3 C 0.3776(7) 0.3744(5) 0.0617(5) 0.0478(14) Uani 1 1 d . . . H3A H 0.4191 0.3956 0.0004 0.072 Uiso 1 1 calc R . . H3B H 0.4709 0.3563 0.1239 0.072 Uiso 1 1 calc R . . H3C H 0.3344 0.4530 0.1089 0.072 Uiso 1 1 calc R . . C2 C 0.1436(11) -0.3134(6) -0.3231(7) 0.069(2) Uani 1 1 d . . . H2A H 0.2669 -0.3074 -0.2910 0.104 Uiso 1 1 calc R . . H2B H 0.1037 -0.3325 -0.4161 0.104 Uiso 1 1 calc R . . H2C H 0.0875 -0.3881 -0.3102 0.104 Uiso 1 1 calc R . . C1 C -0.3311(5) 0.0659(4) -0.1982(4) 0.0245(8) Uani 1 1 d . . . O2W O 0.0917(6) 0.5991(4) -0.0666(4) 0.0617(12) Uani 1 1 d . . . O1W O -0.3045(6) 0.4436(4) -0.4208(4) 0.0610(12) Uani 1 1 d . . . O3 O 0.2732(4) 0.1606(3) -0.5438(3) 0.0372(8) Uani 1 1 d . . . Na1 Na 0.3935(5) 0.2945(4) -0.6744(4) 0.0936(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02014(11) 0.02172(11) 0.01336(11) 0.00765(8) 0.00452(8) 0.00025(7) Mn1 0.0234(4) 0.0206(4) 0.0141(4) 0.0072(3) 0.0048(3) 0.0013(3) O8 0.0426(19) 0.0369(18) 0.0195(16) 0.0121(14) -0.0048(14) -0.0105(15) O7 0.0214(14) 0.0452(18) 0.0210(15) 0.0198(14) 0.0075(12) 0.0075(13) O6 0.0337(17) 0.0316(16) 0.0266(17) 0.0092(14) 0.0127(14) -0.0076(13) O5 0.0349(17) 0.0358(17) 0.0299(17) 0.0191(14) 0.0117(14) 0.0113(14) O4W 0.0308(16) 0.0458(19) 0.0241(16) 0.0181(15) 0.0040(13) 0.0048(14) O4 0.0285(16) 0.060(2) 0.0310(18) 0.0294(17) 0.0106(14) 0.0158(15) C8 0.027(2) 0.026(2) 0.023(2) 0.0090(17) 0.0118(17) 0.0072(16) C7 0.032(3) 0.084(4) 0.039(3) 0.032(3) 0.019(2) 0.016(3) C6 0.035(2) 0.023(2) 0.020(2) 0.0066(17) 0.0087(18) -0.0037(17) C5 0.070(4) 0.038(3) 0.036(3) -0.008(2) 0.023(3) -0.025(3) O2 0.0329(16) 0.0334(16) 0.0234(16) 0.0127(13) 0.0049(13) -0.0063(13) O1 0.049(2) 0.0299(16) 0.0238(16) 0.0106(13) 0.0198(15) 0.0097(14) C4 0.027(2) 0.0200(18) 0.018(2) 0.0026(16) 0.0046(16) -0.0013(15) O3W 0.057(2) 0.0281(18) 0.065(3) 0.0120(18) 0.001(2) 0.0116(17) C3 0.050(3) 0.038(3) 0.034(3) 0.013(2) -0.005(2) -0.023(2) C2 0.123(6) 0.045(3) 0.074(5) 0.028(3) 0.073(5) 0.039(4) C1 0.0222(19) 0.029(2) 0.021(2) 0.0092(17) 0.0069(16) 0.0054(16) O2W 0.086(3) 0.036(2) 0.054(3) 0.0157(19) 0.018(2) 0.006(2) O1W 0.057(3) 0.051(2) 0.057(3) 0.014(2) 0.005(2) 0.021(2) O3 0.0421(19) 0.0380(18) 0.0251(17) 0.0053(14) 0.0164(15) -0.0128(15) Na1 0.105(3) 0.086(2) 0.083(2) 0.0349(19) 0.028(2) 0.0030(19) _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 Nd1 O8 2.378(3) . ? Nd1 O6 2.411(3) . ? Nd1 O5 2.439(3) . ? Nd1 O3W 2.487(4) . ? Nd1 O7 2.489(3) . ? Nd1 O3 2.510(3) 2_554 ? Nd1 O4W 2.511(3) . ? Nd1 O4 2.591(3) . ? Nd1 O6 2.712(3) 2_554 ? Nd1 C1 2.938(4) . ? Nd1 C6 3.015(4) 2_554 ? Mn1 O1 2.172(3) 2 ? Mn1 O1 2.172(3) . ? Mn1 O7 2.178(3) 2 ? Mn1 O7 2.178(3) . ? Mn1 O2 2.193(3) . ? Mn1 O2 2.193(3) 2 ? O8 C4 1.250(5) . ? O7 C1 1.284(5) . ? O6 C6 1.264(5) . ? O6 Nd1 2.712(3) 2_554 ? O5 C8 1.263(5) . ? O4 C1 1.247(5) . ? C8 O1 1.250(5) . ? C8 C2 1.493(7) . ? C7 C1 1.493(6) . ? C6 O3 1.261(5) . ? C6 C5 1.475(6) . ? C6 Nd1 3.015(4) 2_554 ? O2 C4 1.258(5) . ? O2 Na1 2.858(5) 1_556 ? C4 C3 1.504(6) . ? O1W Na1 2.776(6) 2_564 ? O1W Na1 2.987(6) 1_455 ? O3 Nd1 2.510(3) 2_554 ? O3 Na1 2.736(5) . ? Na1 O1W 2.776(6) 2_564 ? Na1 O2 2.858(5) 1_554 ? Na1 O1W 2.987(6) 1_655 ? 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 O8 Nd1 O6 83.94(12) . . ? O8 Nd1 O5 76.32(12) . . ? O6 Nd1 O5 83.01(11) . . ? O8 Nd1 O3W 68.68(12) . . ? O6 Nd1 O3W 87.69(14) . . ? O5 Nd1 O3W 144.52(12) . . ? O8 Nd1 O7 75.26(11) . . ? O6 Nd1 O7 157.04(10) . . ? O5 Nd1 O7 82.71(10) . . ? O3W Nd1 O7 93.61(13) . . ? O8 Nd1 O3 142.67(11) . 2_554 ? O6 Nd1 O3 114.35(10) . 2_554 ? O5 Nd1 O3 74.25(12) . 2_554 ? O3W Nd1 O3 139.78(13) . 2_554 ? O7 Nd1 O3 78.69(10) . 2_554 ? O8 Nd1 O4W 137.30(11) . . ? O6 Nd1 O4W 77.87(11) . . ? O5 Nd1 O4W 137.61(11) . . ? O3W Nd1 O4W 72.26(12) . . ? O7 Nd1 O4W 124.32(11) . . ? O3 Nd1 O4W 79.80(11) 2_554 . ? O8 Nd1 O4 111.70(12) . . ? O6 Nd1 O4 150.20(10) . . ? O5 Nd1 O4 124.45(10) . . ? O3W Nd1 O4 75.73(13) . . ? O7 Nd1 O4 50.77(9) . . ? O3 Nd1 O4 68.88(11) 2_554 . ? O4W Nd1 O4 73.59(10) . . ? O8 Nd1 O6 136.24(12) . 2_554 ? O6 Nd1 O6 65.37(11) . 2_554 ? O5 Nd1 O6 69.90(11) . 2_554 ? O3W Nd1 O6 135.31(12) . 2_554 ? O7 Nd1 O6 125.22(10) . 2_554 ? O3 Nd1 O6 49.01(9) 2_554 2_554 ? O4W Nd1 O6 67.76(11) . 2_554 ? O4 Nd1 O6 110.14(10) . 2_554 ? O8 Nd1 C1 93.46(13) . . ? O6 Nd1 C1 171.12(11) . . ? O5 Nd1 C1 104.67(11) . . ? O3W Nd1 C1 83.46(14) . . ? O7 Nd1 C1 25.71(10) . . ? O3 Nd1 C1 72.62(11) 2_554 . ? O4W Nd1 C1 98.66(11) . . ? O4 Nd1 C1 25.07(10) . . ? O6 Nd1 C1 121.14(11) 2_554 . ? O8 Nd1 C6 147.44(12) . 2_554 ? O6 Nd1 C6 90.16(11) . 2_554 ? O5 Nd1 C6 71.19(12) . 2_554 ? O3W Nd1 C6 143.23(13) . 2_554 ? O7 Nd1 C6 102.10(11) . 2_554 ? O3 Nd1 C6 24.26(10) 2_554 2_554 ? O4W Nd1 C6 71.41(12) . 2_554 ? O4 Nd1 C6 88.78(12) . 2_554 ? O6 Nd1 C6 24.79(10) 2_554 2_554 ? C1 Nd1 C6 96.51(12) . 2_554 ? O1 Mn1 O1 180.0 2 . ? O1 Mn1 O7 90.92(12) 2 2 ? O1 Mn1 O7 89.08(12) . 2 ? O1 Mn1 O7 89.08(12) 2 . ? O1 Mn1 O7 90.92(12) . . ? O7 Mn1 O7 180.0 2 . ? O1 Mn1 O2 83.06(13) 2 . ? O1 Mn1 O2 96.94(13) . . ? O7 Mn1 O2 88.09(12) 2 . ? O7 Mn1 O2 91.91(12) . . ? O1 Mn1 O2 96.94(13) 2 2 ? O1 Mn1 O2 83.06(13) . 2 ? O7 Mn1 O2 91.91(12) 2 2 ? O7 Mn1 O2 88.09(12) . 2 ? O2 Mn1 O2 180.0 . 2 ? C4 O8 Nd1 148.6(3) . . ? C1 O7 Mn1 140.6(3) . . ? C1 O7 Nd1 97.1(2) . . ? Mn1 O7 Nd1 122.13(13) . . ? C6 O6 Nd1 154.2(3) . . ? C6 O6 Nd1 91.1(3) . 2_554 ? Nd1 O6 Nd1 114.63(11) . 2_554 ? C8 O5 Nd1 135.9(3) . . ? C1 O4 Nd1 93.2(2) . . ? O1 C8 O5 124.9(4) . . ? O1 C8 C2 117.3(4) . . ? O5 C8 C2 117.9(4) . . ? O3 C6 O6 118.8(4) . . ? O3 C6 C5 120.2(4) . . ? O6 C6 C5 120.9(4) . . ? O3 C6 Nd1 54.8(2) . 2_554 ? O6 C6 Nd1 64.1(2) . 2_554 ? C5 C6 Nd1 172.9(4) . 2_554 ? C4 O2 Mn1 133.4(3) . . ? C4 O2 Na1 113.8(3) . 1_556 ? Mn1 O2 Na1 108.34(13) . 1_556 ? C8 O1 Mn1 134.6(3) . . ? O8 C4 O2 124.8(4) . . ? O8 C4 C3 116.8(4) . . ? O2 C4 C3 118.4(4) . . ? O4 C1 O7 118.9(4) . . ? O4 C1 C7 121.7(4) . . ? O7 C1 C7 119.4(4) . . ? O4 C1 Nd1 61.7(2) . . ? O7 C1 Nd1 57.2(2) . . ? C7 C1 Nd1 176.3(3) . . ? Na1 O1W Na1 100.69(15) 2_564 1_455 ? C6 O3 Nd1 100.9(2) . 2_554 ? C6 O3 Na1 132.3(3) . . ? Nd1 O3 Na1 121.00(14) 2_554 . ? O3 Na1 O1W 101.88(18) . 2_564 ? O3 Na1 O2 112.75(15) . 1_554 ? O1W Na1 O2 106.81(16) 2_564 1_554 ? O3 Na1 O1W 86.73(16) . 1_655 ? O1W Na1 O1W 79.31(15) 2_564 1_655 ? O2 Na1 O1W 157.07(18) 1_554 1_655 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.900 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.139