# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_scmn868f _database_code_depnum_ccdc_archive 'CCDC 293107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.7 H66.8 Ca Cl3.8 Mn4 N3 O19.2' _chemical_formula_weight 1299.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0043 0.0021 http://www.bmsc.washington.edu/scatter/ H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0082 0.0043 http://www.bmsc.washington.edu/scatter/ O O 0.0142 0.0079 http://www.bmsc.washington.edu/scatter/ Cl Cl 0.1776 0.2015 http://www.bmsc.washington.edu/scatter/ Ca Ca 0.2647 0.3862 http://www.bmsc.washington.edu/scatter/ Mn Mn 0.3566 0.9084 http://www.bmsc.washington.edu/scatter/ _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 12.7590(12) _cell_length_b 14.3574(14) _cell_length_c 15.6647(17) _cell_angle_alpha 88.148(9) _cell_angle_beta 83.900(8) _cell_angle_gamma 82.349(8) _cell_volume 2827.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13341 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 29.63 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.012 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details ; XPREP in SHELXTL 5.1 (Bruker AXS Inc., 1997) ; _exptl_special_details ; Data were measured to a resolution of 0.88 \%A with a Stoe IPDS II diffractometer on the ANKA-PX beamline of the ANKA synchrotron source at the Forschungszentrum Karlsruhe, using Si-monochromated radiation of wavelength 0.79999(1) \%A. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.79999 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15575 _diffrn_reflns_av_R_equivalents 0.1136 _diffrn_reflns_av_sigmaI/netI 0.1187 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7959 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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. The methyl groups of the organic ligands showed two-fold disorder; the half-atoms were refined isotropically. Of the two monodentate ligands coordinated to Ca(1), one (the aquo ligand O(13)) was ordered, while the second, involved a threefold disorder of three different ligands: aquo O(14A) (50%), methanol O(14B) (30%) and monodentate acetate O(14C) (20%). The chloride counterion and lattice methanols were also disordered, some badly. ; _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^)+(0.0933P)^2^+5.1485P] 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 7959 _refine_ls_number_parameters 650 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2277 _refine_ls_wR_factor_gt 0.1970 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Mn1 Mn 0.30997(12) 0.14237(9) 0.31004(11) 0.0608(4) Uani 1 1 d . A . Mn2 Mn 0.14351(11) 0.33675(9) 0.32871(10) 0.0560(4) Uani 1 1 d . A . Mn3 Mn 0.39332(11) 0.35659(9) 0.31921(10) 0.0549(4) Uani 1 1 d . A . Mn4 Mn 0.26808(11) 0.25911(9) 0.50677(10) 0.0584(4) Uani 1 1 d . A . Ca1 Ca 0.30275(17) 0.29676(14) 0.13782(15) 0.0672(6) Uani 1 1 d . . . Cl1 Cl 0.09377(19) 0.17748(16) 0.2876(2) 0.0709(7) Uani 1 1 d . . . Cl2 Cl 0.22655(17) 0.48335(14) 0.36479(17) 0.0599(6) Uani 1 1 d . . . Cl3 Cl 0.26677(19) 0.36968(16) 0.62226(18) 0.0655(7) Uani 1 1 d . . . O1 O 0.2886(5) 0.2766(4) 0.3074(4) 0.0540(15) Uani 1 1 d . A . O2 O 0.3466(6) 0.1436(4) 0.1904(5) 0.0728(19) Uani 1 1 d D A . C1A C 0.3279(13) 0.0539(10) 0.1529(9) 0.076(4) Uani 0.75 1 d PDU A 1 H1A H 0.2525 0.0579 0.1395 0.091 Uiso 0.75 1 calc PR A 1 C11A C 0.4024(14) 0.0447(11) 0.0714(10) 0.091(5) Uani 0.75 1 d PD A 1 H11A H 0.3832 0.0974 0.0323 0.136 Uiso 0.75 1 calc PR A 1 H11B H 0.3968 -0.0146 0.0438 0.136 Uiso 0.75 1 calc PR A 1 H11C H 0.4755 0.0452 0.0849 0.136 Uiso 0.75 1 calc PR A 1 C2A C 0.350(2) -0.0218(14) 0.2210(18) 0.108(9) Uani 0.75 1 d PD A 1 H2A1 H 0.3257 -0.0808 0.2048 0.130 Uiso 0.75 1 calc PR A 1 H2A2 H 0.4274 -0.0342 0.2260 0.130 Uiso 0.75 1 calc PR A 1 C1B C 0.403(4) 0.056(2) 0.156(3) 0.088(12) Uiso 0.25 1 d PDU A 2 H1B H 0.4011 0.0605 0.0921 0.106 Uiso 0.25 1 calc PR A 2 C11B C 0.519(4) 0.025(5) 0.171(5) 0.15(3) Uiso 0.25 1 d PD A 2 H11D H 0.5630 0.0726 0.1466 0.232 Uiso 0.25 1 calc PR A 2 H11E H 0.5436 -0.0351 0.1437 0.232 Uiso 0.25 1 calc PR A 2 H11F H 0.5245 0.0188 0.2330 0.232 Uiso 0.25 1 calc PR A 2 C2B C 0.332(4) -0.017(4) 0.190(4) 0.058(15) Uiso 0.25 1 d PD A 2 H2B1 H 0.3706 -0.0812 0.1837 0.070 Uiso 0.25 1 calc PR A 2 H2B2 H 0.2678 -0.0121 0.1589 0.070 Uiso 0.25 1 calc PR A 2 N1 N 0.2971(7) 0.0086(6) 0.2976(8) 0.075(3) Uani 1 1 d . . . C3 C 0.2418(8) -0.0434(7) 0.3452(10) 0.073(3) Uani 1 1 d . A . H3 H 0.2287 -0.1009 0.3226 0.088 Uiso 1 1 calc R . . C4 C 0.1992(8) -0.0215(7) 0.4286(9) 0.070(3) Uani 1 1 d . . . C5 C 0.1379(9) -0.0863(8) 0.4740(12) 0.094(5) Uani 1 1 d . A . H5 H 0.1250 -0.1401 0.4450 0.112 Uiso 1 1 calc R . . C6 C 0.0971(10) -0.0747(9) 0.5566(12) 0.095(5) Uani 1 1 d . . . H6 H 0.0581 -0.1206 0.5852 0.114 Uiso 1 1 calc R A . C7 C 0.1127(8) 0.0061(7) 0.6003(9) 0.080(4) Uani 1 1 d . A . H7 H 0.0821 0.0162 0.6578 0.096 Uiso 1 1 calc R . . C8 C 0.1742(8) 0.0717(7) 0.5578(9) 0.070(3) Uani 1 1 d . . . C9 C 0.2145(7) 0.0610(6) 0.4708(8) 0.065(3) Uani 1 1 d . A . O3 O 0.2687(5) 0.1277(4) 0.4330(5) 0.0607(17) Uani 1 1 d . . . O4 O 0.1986(5) 0.1496(4) 0.5950(5) 0.0678(18) Uani 1 1 d . A . C10 C 0.1740(11) 0.1561(8) 0.6868(9) 0.095(4) Uani 1 1 d . . . H10A H 0.1943 0.2148 0.7062 0.143 Uiso 1 1 calc R A . H10B H 0.2134 0.1026 0.7150 0.143 Uiso 1 1 calc R . . H10C H 0.0975 0.1553 0.7016 0.143 Uiso 1 1 calc R . . O5 O 0.1263(5) 0.3065(4) 0.4491(4) 0.0591(16) Uani 1 1 d . . . C12 C 0.0378(7) 0.3617(6) 0.4953(7) 0.061(3) Uani 1 1 d . A . H12 H 0.0586 0.4243 0.5076 0.073 Uiso 1 1 calc R . . C22 C 0.0014(8) 0.3146(7) 0.5793(7) 0.068(3) Uani 1 1 d . . . H22A H 0.0600 0.3052 0.6157 0.102 Uiso 1 1 calc R A . H22B H -0.0202 0.2537 0.5676 0.102 Uiso 1 1 calc R . . H22C H -0.0590 0.3546 0.6088 0.102 Uiso 1 1 calc R . . C13 C -0.0516(7) 0.3761(6) 0.4366(7) 0.063(3) Uani 1 1 d . . . H13A H -0.0841 0.3176 0.4334 0.076 Uiso 1 1 calc R A . H13B H -0.1076 0.4268 0.4582 0.076 Uiso 1 1 calc R . . N2 N -0.0014(6) 0.4021(5) 0.3514(6) 0.061(2) Uani 1 1 d . A . C14 C -0.0449(8) 0.4713(7) 0.3069(8) 0.066(3) Uani 1 1 d . . . H14 H -0.1115 0.5029 0.3300 0.080 Uiso 1 1 calc R A . C15 C 0.0000(8) 0.5041(7) 0.2247(8) 0.067(3) Uani 1 1 d . A . C16 C -0.0544(10) 0.5856(8) 0.1885(9) 0.085(4) Uani 1 1 d . . . H16 H -0.1176 0.6170 0.2177 0.102 Uiso 1 1 calc R A . C17 C -0.0148(11) 0.6181(8) 0.1116(10) 0.093(4) Uani 1 1 d . A . H17 H -0.0487 0.6749 0.0886 0.112 Uiso 1 1 calc R . . C18 C 0.0738(10) 0.5709(8) 0.0652(9) 0.084(3) Uani 1 1 d . . . H18 H 0.0974 0.5932 0.0096 0.101 Uiso 1 1 calc R A . C19 C 0.1276(9) 0.4916(7) 0.1000(8) 0.071(3) Uani 1 1 d . A . C20 C 0.0908(8) 0.4553(6) 0.1806(7) 0.063(3) Uani 1 1 d . . . O6 O 0.1458(5) 0.3779(4) 0.2103(5) 0.0617(17) Uani 1 1 d . A . O7 O 0.2166(6) 0.4393(5) 0.0596(5) 0.0729(19) Uani 1 1 d . A . C21 C 0.2511(11) 0.4663(10) -0.0257(8) 0.096(4) Uani 1 1 d . . . H21A H 0.3147 0.4241 -0.0469 0.144 Uiso 1 1 calc R B . H21B H 0.2679 0.5310 -0.0265 0.144 Uiso 1 1 calc R . . H21C H 0.1945 0.4624 -0.0627 0.144 Uiso 1 1 calc R . . O8 O 0.3984(5) 0.3985(4) 0.2042(4) 0.0582(16) Uani 1 1 d . A . C23 C 0.4680(10) 0.4660(7) 0.1820(8) 0.079(3) Uani 1 1 d . . . H23 H 0.5387 0.4316 0.1602 0.094 Uiso 1 1 calc R B . C33 C 0.4294(11) 0.5279(9) 0.1116(9) 0.095(4) Uani 1 1 d . B . H33A H 0.4224 0.4897 0.0623 0.143 Uiso 1 1 calc R . . H33B H 0.4802 0.5724 0.0947 0.143 Uiso 1 1 calc R . . H33C H 0.3600 0.5626 0.1311 0.143 Uiso 1 1 calc R . . C24 C 0.4836(9) 0.5192(7) 0.2611(7) 0.072(3) Uani 1 1 d . B . H24A H 0.5498 0.5487 0.2517 0.087 Uiso 1 1 calc R . . H24B H 0.4231 0.5690 0.2744 0.087 Uiso 1 1 calc R . . N3 N 0.4899(6) 0.4505(5) 0.3309(6) 0.062(2) Uani 1 1 d . . . C25 C 0.5522(8) 0.4535(6) 0.3911(7) 0.060(2) Uani 1 1 d . B . H25 H 0.5936 0.5040 0.3900 0.072 Uiso 1 1 calc R . . C26 C 0.5615(7) 0.3835(6) 0.4601(7) 0.057(2) Uani 1 1 d . . . C27 C 0.6451(8) 0.3819(7) 0.5101(8) 0.069(3) Uani 1 1 d . B . H27 H 0.6914 0.4287 0.5006 0.083 Uiso 1 1 calc R . . C28 C 0.6626(8) 0.3149(7) 0.5724(8) 0.075(3) Uani 1 1 d . . . H28 H 0.7226 0.3134 0.6038 0.090 Uiso 1 1 calc R B . C29 C 0.5926(8) 0.2490(7) 0.5897(8) 0.070(3) Uani 1 1 d . B . H29 H 0.6031 0.2037 0.6347 0.083 Uiso 1 1 calc R . . C30 C 0.5074(7) 0.2488(6) 0.5418(7) 0.062(3) Uani 1 1 d . . . C31 C 0.4870(7) 0.3181(6) 0.4783(7) 0.056(2) Uani 1 1 d . A . O9 O 0.4006(5) 0.3173(4) 0.4366(4) 0.0560(16) Uani 1 1 d . . . O10 O 0.4320(5) 0.1882(4) 0.5537(5) 0.0658(18) Uani 1 1 d . A . C32 C 0.4647(10) 0.0957(7) 0.5866(10) 0.097(5) Uani 1 1 d . . . H32A H 0.4045 0.0594 0.5916 0.145 Uiso 1 1 calc R B . H32B H 0.4895 0.1003 0.6432 0.145 Uiso 1 1 calc R . . H32C H 0.5226 0.0642 0.5473 0.145 Uiso 1 1 calc R . . O11 O 0.4710(5) 0.1195(4) 0.3401(5) 0.0669(18) Uani 1 1 d . . . O12 O 0.5332(5) 0.2502(4) 0.2860(5) 0.0609(17) Uani 1 1 d . . . C34 C 0.5442(7) 0.1675(8) 0.3163(8) 0.073(3) Uani 1 1 d . A . C35A C 0.6521(16) 0.1303(13) 0.3444(14) 0.059(5) Uiso 0.50 1 d P A 1 H35A H 0.7038 0.1722 0.3224 0.089 Uiso 0.50 1 calc PR A 1 H35B H 0.6747 0.0672 0.3219 0.089 Uiso 0.50 1 calc PR A 1 H35C H 0.6474 0.1276 0.4073 0.089 Uiso 0.50 1 calc PR A 1 C35B C 0.6558(19) 0.1141(16) 0.2924(17) 0.078(6) Uiso 0.50 1 d P A 2 H35D H 0.7055 0.1592 0.2745 0.118 Uiso 0.50 1 calc PR A 2 H35E H 0.6533 0.0716 0.2452 0.118 Uiso 0.50 1 calc PR A 2 H35F H 0.6795 0.0777 0.3424 0.118 Uiso 0.50 1 calc PR A 2 O13 O 0.4398(6) 0.2841(5) 0.0246(5) 0.082(2) Uani 1 1 d . B . O14A O 0.1826(16) 0.2322(16) 0.0575(12) 0.067(5) Uiso 0.50 1 d P B 1 O14B O 0.213(3) 0.240(2) 0.031(2) 0.065(7) Uiso 0.30 1 d P B 2 C41B C 0.080(7) 0.234(5) 0.076(5) 0.13(3) Uiso 0.30 1 d P B 2 O14C O 0.221(4) 0.211(3) 0.039(4) 0.065(7) Uiso 0.20 1 d P B 3 O15C O 0.127(3) 0.153(3) -0.049(3) 0.080(10) Uiso 0.20 1 d P B 3 C42C C 0.140(4) 0.195(3) 0.010(3) 0.053(11) Uiso 0.20 1 d P B 3 C43C C 0.040(6) 0.234(4) 0.079(4) 0.054(14) Uiso 0.20 1 d P B 3 Cl5A Cl 0.2147(10) 0.0919(11) -0.0957(8) 0.081(3) Uiso 0.30 1 d P C 1 O51B O 0.2008(16) 0.1419(16) -0.1027(13) 0.094(6) Uiso 0.50 1 d P D 2 C51B C 0.258(4) 0.056(3) -0.090(3) 0.125(13) Uiso 0.50 1 d P D 2 O51C O 0.310(5) 0.072(4) -0.146(4) 0.129(18) Uiso 0.20 1 d P E 3 C51C C 0.305(8) -0.031(6) -0.122(6) 0.13(3) Uiso 0.20 1 d P E 3 Cl5B Cl 0.7012(8) 0.3123(6) 0.1938(6) 0.130(3) Uiso 0.50 1 d P F 1 O52A O 0.7760(15) 0.3494(12) 0.2363(12) 0.096(5) Uiso 0.50 1 d PD G 2 C52A C 0.832(8) 0.297(7) 0.294(6) 0.43(6) Uiso 0.50 1 d PD G 2 O53 O -0.0182(12) 0.1056(10) -0.1394(10) 0.170(5) Uiso 1 1 d . . . C53 C -0.0285(19) 0.0081(16) -0.1408(15) 0.169(8) Uiso 1 1 d . . . O54 O -0.1517(11) 0.2042(9) -0.2497(9) 0.148(4) Uiso 1 1 d . . . C54 C -0.2015(14) 0.2908(12) -0.2127(12) 0.128(5) Uiso 1 1 d . . . O55A O 0.4240(11) 0.1885(9) -0.1218(9) 0.104(4) Uiso 0.70 1 d P H 1 C55A C 0.430(2) 0.2446(16) -0.1969(18) 0.108(7) Uiso 0.70 1 d P H 1 O55B O 0.367(4) 0.262(3) -0.155(3) 0.141(14) Uiso 0.30 1 d P I 2 C55B C 0.370(7) 0.239(5) -0.215(5) 0.15(2) Uiso 0.30 1 d P I 2 O56A O 0.6533(12) 0.2852(10) 0.0350(9) 0.051(3) Uiso 0.40 1 d PD J 1 C56A C 0.708(5) 0.204(3) 0.007(4) 0.19(2) Uiso 0.40 1 d PD J 1 O56B O 0.0020(19) 0.2715(17) 0.1063(16) 0.088(6) Uiso 0.40 1 d P B 2 C56B C -0.050(5) 0.210(4) 0.086(4) 0.168(19) Uiso 0.40 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0556(8) 0.0476(7) 0.0830(11) -0.0006(7) -0.0216(8) -0.0090(6) Mn2 0.0440(7) 0.0508(7) 0.0763(10) -0.0001(7) -0.0185(7) -0.0079(6) Mn3 0.0471(8) 0.0499(7) 0.0719(10) 0.0042(7) -0.0162(7) -0.0150(6) Mn4 0.0464(8) 0.0522(8) 0.0800(11) 0.0054(7) -0.0171(7) -0.0124(6) Ca1 0.0638(13) 0.0647(12) 0.0752(14) -0.0031(10) -0.0231(11) -0.0028(10) Cl1 0.0526(13) 0.0551(13) 0.111(2) -0.0066(13) -0.0234(14) -0.0157(10) Cl2 0.0483(12) 0.0476(11) 0.0873(18) -0.0024(11) -0.0169(12) -0.0114(9) Cl3 0.0523(13) 0.0636(14) 0.0827(18) -0.0027(12) -0.0130(13) -0.0107(11) O1 0.047(3) 0.050(3) 0.068(4) 0.004(3) -0.016(3) -0.010(3) O2 0.073(5) 0.063(4) 0.082(5) -0.007(4) -0.019(4) 0.001(3) C1A 0.072(10) 0.079(10) 0.075(10) -0.021(8) -0.021(9) 0.012(7) C11A 0.110(13) 0.082(10) 0.074(11) -0.012(8) -0.013(11) 0.016(9) C2A 0.13(2) 0.073(12) 0.14(2) 0.014(13) -0.062(19) -0.035(12) N1 0.059(5) 0.067(6) 0.096(8) -0.017(6) -0.013(6) 0.003(5) C3 0.053(6) 0.042(5) 0.130(11) 0.004(6) -0.028(7) -0.012(5) C4 0.046(5) 0.057(6) 0.111(10) 0.009(6) -0.025(6) -0.011(5) C5 0.057(7) 0.054(6) 0.175(15) 0.028(8) -0.033(9) -0.016(5) C6 0.054(7) 0.076(8) 0.163(15) 0.043(9) -0.036(8) -0.030(6) C7 0.048(5) 0.064(6) 0.128(11) 0.037(7) -0.019(6) -0.013(5) C8 0.045(5) 0.052(6) 0.113(10) 0.019(6) -0.012(6) -0.004(4) C9 0.042(5) 0.046(5) 0.110(10) 0.016(6) -0.018(6) -0.007(4) O3 0.042(3) 0.049(3) 0.094(5) 0.005(3) -0.014(3) -0.014(3) O4 0.062(4) 0.057(4) 0.085(5) 0.004(4) -0.009(4) -0.013(3) C10 0.113(10) 0.073(7) 0.093(10) 0.011(7) 0.008(8) -0.007(7) O5 0.047(3) 0.051(3) 0.081(5) -0.003(3) -0.011(3) -0.007(3) C12 0.045(5) 0.057(5) 0.083(7) 0.001(5) -0.015(5) -0.009(4) C22 0.047(5) 0.075(6) 0.087(8) 0.008(6) -0.022(5) -0.018(5) C13 0.043(5) 0.053(5) 0.097(8) 0.006(5) -0.020(5) -0.006(4) N2 0.046(4) 0.052(4) 0.089(6) 0.000(4) -0.032(5) -0.004(3) C14 0.053(6) 0.060(6) 0.089(8) -0.016(6) -0.010(6) -0.009(5) C15 0.055(6) 0.054(5) 0.093(8) -0.004(5) -0.025(6) 0.002(5) C16 0.071(7) 0.071(7) 0.111(11) 0.016(7) -0.022(7) 0.007(6) C17 0.107(10) 0.065(7) 0.103(10) 0.016(7) -0.027(9) 0.016(7) C18 0.073(7) 0.078(7) 0.098(9) 0.010(7) -0.009(7) 0.003(6) C19 0.071(7) 0.060(6) 0.085(8) 0.003(6) -0.024(6) -0.003(5) C20 0.065(6) 0.051(5) 0.079(7) -0.001(5) -0.031(6) -0.012(5) O6 0.053(4) 0.056(4) 0.078(5) -0.002(3) -0.020(4) -0.001(3) O7 0.069(5) 0.075(4) 0.075(5) 0.009(4) -0.020(4) -0.005(4) C21 0.088(9) 0.120(10) 0.076(9) 0.015(8) -0.017(7) 0.005(8) O8 0.057(4) 0.060(4) 0.061(4) 0.000(3) -0.007(3) -0.019(3) C23 0.080(7) 0.065(6) 0.092(9) 0.018(6) -0.010(7) -0.017(6) C33 0.107(10) 0.092(8) 0.090(9) 0.017(7) -0.007(8) -0.032(8) C24 0.069(7) 0.060(6) 0.091(8) 0.003(6) -0.010(6) -0.018(5) N3 0.051(4) 0.049(4) 0.087(6) 0.008(4) -0.007(5) -0.012(3) C25 0.053(5) 0.053(5) 0.075(7) -0.006(5) -0.007(5) -0.010(4) C26 0.046(5) 0.057(5) 0.070(6) -0.014(5) -0.017(5) -0.003(4) C27 0.054(6) 0.066(6) 0.093(8) -0.016(6) -0.023(6) -0.013(5) C28 0.054(6) 0.075(7) 0.101(9) -0.010(6) -0.026(6) -0.006(5) C29 0.055(6) 0.067(6) 0.090(8) -0.004(5) -0.030(6) -0.004(5) C30 0.051(5) 0.055(5) 0.083(7) 0.000(5) -0.021(5) -0.006(4) C31 0.036(4) 0.058(5) 0.076(7) -0.011(5) -0.014(5) -0.008(4) O9 0.051(3) 0.054(3) 0.070(4) 0.004(3) -0.026(3) -0.015(3) O10 0.055(4) 0.057(4) 0.090(5) 0.008(3) -0.023(4) -0.014(3) C32 0.079(8) 0.047(6) 0.169(14) 0.027(7) -0.038(8) -0.011(5) O11 0.054(4) 0.054(4) 0.092(5) 0.002(3) -0.010(4) -0.005(3) O12 0.051(4) 0.051(4) 0.083(5) 0.002(3) -0.016(4) -0.007(3) C34 0.037(5) 0.071(7) 0.113(10) 0.004(6) -0.018(6) -0.010(5) O13 0.087(5) 0.080(5) 0.078(5) 0.004(4) -0.008(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.882(8) . ? Mn1 O1 1.910(6) . ? Mn1 O3 1.954(7) . ? Mn1 N1 1.967(9) . ? Mn1 O11 2.137(7) . ? Mn1 Cl1 2.795(3) . ? Mn1 Ca1 3.437(3) . ? Mn2 O5 1.918(7) . ? Mn2 O6 1.927(7) . ? Mn2 O1 1.936(6) . ? Mn2 N2 1.961(8) . ? Mn2 Cl1 2.572(3) . ? Mn2 Cl2 2.583(2) . ? Mn2 Mn3 3.2250(19) . ? Mn2 Ca1 3.451(3) . ? Mn3 O8 1.878(6) . ? Mn3 O1 1.901(5) . ? Mn3 O9 1.914(6) . ? Mn3 N3 1.968(7) . ? Mn3 O12 2.217(7) . ? Mn3 Cl2 2.661(3) . ? Mn3 Ca1 3.357(3) . ? Mn4 O5 2.129(6) . ? Mn4 O9 2.164(6) . ? Mn4 O3 2.243(6) . ? Mn4 O4 2.267(7) . ? Mn4 O10 2.380(6) . ? Mn4 Cl3 2.442(3) . ? Ca1 O2 2.341(7) . ? Ca1 O13 2.347(8) . ? Ca1 O14B 2.35(3) . ? Ca1 O8 2.355(6) . ? Ca1 O6 2.375(7) . ? Ca1 O14A 2.378(17) . ? Ca1 O14C 2.42(4) . ? Ca1 O7 2.535(7) . ? Ca1 O1 2.652(7) . ? O2 C1B 1.45(3) . ? O2 C1A 1.491(15) . ? C1A C11A 1.507(16) . ? C1A C2A 1.518(19) . ? C2A N1 1.37(3) . ? C1B C11B 1.52(2) . ? C1B C2B 1.53(3) . ? C2B N1 1.73(6) . ? N1 C3 1.267(14) . ? C3 C4 1.390(17) . ? C4 C5 1.420(15) . ? C4 C9 1.420(16) . ? C5 C6 1.35(2) . ? C6 C7 1.41(2) . ? C7 C8 1.411(14) . ? C8 O4 1.365(13) . ? C8 C9 1.410(16) . ? C9 O3 1.342(10) . ? O4 C10 1.443(14) . ? O5 C12 1.432(12) . ? C12 C22 1.516(14) . ? C12 C13 1.528(13) . ? C13 N2 1.476(13) . ? N2 C14 1.293(12) . ? C14 C15 1.443(15) . ? C15 C20 1.398(15) . ? C15 C16 1.414(14) . ? C16 C17 1.349(17) . ? C17 C18 1.385(18) . ? C18 C19 1.377(15) . ? C19 O7 1.380(13) . ? C19 C20 1.408(15) . ? C20 O6 1.331(11) . ? O7 C21 1.420(13) . ? O8 C23 1.411(11) . ? C23 C33 1.478(16) . ? C23 C24 1.520(16) . ? C24 N3 1.450(12) . ? N3 C25 1.302(12) . ? C25 C26 1.455(13) . ? C26 C27 1.385(13) . ? C26 C31 1.426(12) . ? C27 C28 1.362(15) . ? C28 C29 1.388(14) . ? C29 C30 1.386(13) . ? C30 O10 1.375(10) . ? C30 C31 1.404(13) . ? C31 O9 1.341(10) . ? O10 C32 1.434(11) . ? O11 C34 1.251(11) . ? O12 C34 1.260(11) . ? C34 C35A 1.51(2) . ? C34 C35B 1.54(3) . ? O14B C41B 1.78(9) . ? C41B O56B 1.13(8) . ? C41B C56B 1.73(9) . ? O14C C42C 1.22(6) . ? O15C C42C 1.16(6) . ? C42C C43C 1.64(10) . ? O51B C51B 1.37(4) . ? O51C C51C 1.52(10) . ? O52A C52A 1.36(3) . ? O53 C53 1.42(2) . ? O54 C54 1.43(2) . ? O55A C55A 1.40(3) . ? O55B C55B 0.99(8) . ? O56A C56A 1.34(3) . ? O56B C56B 1.24(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 89.4(3) . . ? O2 Mn1 O3 174.0(3) . . ? O1 Mn1 O3 96.2(3) . . ? O2 Mn1 N1 85.8(4) . . ? O1 Mn1 N1 164.8(3) . . ? O3 Mn1 N1 88.3(4) . . ? O2 Mn1 O11 94.4(3) . . ? O1 Mn1 O11 99.4(2) . . ? O3 Mn1 O11 86.9(3) . . ? N1 Mn1 O11 95.4(3) . . ? O2 Mn1 Cl1 91.1(2) . . ? O1 Mn1 Cl1 79.08(17) . . ? O3 Mn1 Cl1 87.90(19) . . ? N1 Mn1 Cl1 86.6(3) . . ? O11 Mn1 Cl1 174.3(2) . . ? O2 Mn1 Ca1 40.3(2) . . ? O1 Mn1 Ca1 50.1(2) . . ? O3 Mn1 Ca1 144.65(19) . . ? N1 Mn1 Ca1 121.6(3) . . ? O11 Mn1 Ca1 106.65(19) . . ? Cl1 Mn1 Ca1 76.61(8) . . ? O5 Mn2 O6 173.1(3) . . ? O5 Mn2 O1 96.4(3) . . ? O6 Mn2 O1 90.2(3) . . ? O5 Mn2 N2 83.5(3) . . ? O6 Mn2 N2 89.8(3) . . ? O1 Mn2 N2 177.8(3) . . ? O5 Mn2 Cl1 92.58(19) . . ? O6 Mn2 Cl1 89.9(2) . . ? O1 Mn2 Cl1 84.67(17) . . ? N2 Mn2 Cl1 97.6(2) . . ? O5 Mn2 Cl2 88.64(18) . . ? O6 Mn2 Cl2 90.03(19) . . ? O1 Mn2 Cl2 85.56(17) . . ? N2 Mn2 Cl2 92.2(2) . . ? Cl1 Mn2 Cl2 170.22(10) . . ? O5 Mn2 Mn3 95.89(18) . . ? O6 Mn2 Mn3 88.70(19) . . ? O1 Mn2 Mn3 32.46(16) . . ? N2 Mn2 Mn3 145.3(2) . . ? Cl1 Mn2 Mn3 117.08(8) . . ? Cl2 Mn2 Mn3 53.15(6) . . ? O5 Mn2 Ca1 145.48(19) . . ? O6 Mn2 Ca1 41.4(2) . . ? O1 Mn2 Ca1 49.82(19) . . ? N2 Mn2 Ca1 130.5(3) . . ? Cl1 Mn2 Ca1 79.13(8) . . ? Cl2 Mn2 Ca1 94.41(8) . . ? Mn3 Mn2 Ca1 60.26(5) . . ? O8 Mn3 O1 93.9(3) . . ? O8 Mn3 O9 174.8(2) . . ? O1 Mn3 O9 90.9(2) . . ? O8 Mn3 N3 84.4(3) . . ? O1 Mn3 N3 174.0(3) . . ? O9 Mn3 N3 91.0(3) . . ? O8 Mn3 O12 90.1(3) . . ? O1 Mn3 O12 96.4(2) . . ? O9 Mn3 O12 87.6(3) . . ? N3 Mn3 O12 89.3(3) . . ? O8 Mn3 Cl2 91.9(2) . . ? O1 Mn3 Cl2 84.05(19) . . ? O9 Mn3 Cl2 90.5(2) . . ? N3 Mn3 Cl2 90.3(2) . . ? O12 Mn3 Cl2 178.0(2) . . ? O8 Mn3 Mn2 92.57(19) . . ? O1 Mn3 Mn2 33.13(18) . . ? O9 Mn3 Mn2 92.46(18) . . ? N3 Mn3 Mn2 141.1(2) . . ? O12 Mn3 Mn2 129.50(16) . . ? Cl2 Mn3 Mn2 50.96(5) . . ? O8 Mn3 Ca1 42.83(17) . . ? O1 Mn3 Ca1 52.07(19) . . ? O9 Mn3 Ca1 141.44(17) . . ? N3 Mn3 Ca1 127.0(3) . . ? O12 Mn3 Ca1 86.64(18) . . ? Cl2 Mn3 Ca1 95.15(7) . . ? Mn2 Mn3 Ca1 63.21(5) . . ? O5 Mn4 O9 109.6(2) . . ? O5 Mn4 O3 84.6(2) . . ? O9 Mn4 O3 100.5(2) . . ? O5 Mn4 O4 96.2(2) . . ? O9 Mn4 O4 152.1(2) . . ? O3 Mn4 O4 70.9(3) . . ? O5 Mn4 O10 170.9(3) . . ? O9 Mn4 O10 69.3(2) . . ? O3 Mn4 O10 86.8(2) . . ? O4 Mn4 O10 83.6(2) . . ? O5 Mn4 Cl3 104.02(19) . . ? O9 Mn4 Cl3 90.18(18) . . ? O3 Mn4 Cl3 163.29(19) . . ? O4 Mn4 Cl3 93.7(2) . . ? O10 Mn4 Cl3 85.04(19) . . ? O2 Ca1 O13 94.6(3) . . ? O2 Ca1 O14B 90.7(7) . . ? O13 Ca1 O14B 80.3(11) . . ? O2 Ca1 O8 108.9(2) . . ? O13 Ca1 O8 87.8(3) . . ? O14B Ca1 O8 157.9(7) . . ? O2 Ca1 O6 113.7(3) . . ? O13 Ca1 O6 151.3(3) . . ? O14B Ca1 O6 94.2(11) . . ? O8 Ca1 O6 87.3(2) . . ? O2 Ca1 O14A 86.1(6) . . ? O13 Ca1 O14A 93.5(5) . . ? O14B Ca1 O14A 13.7(10) . . ? O8 Ca1 O14A 164.8(6) . . ? O6 Ca1 O14A 84.2(6) . . ? O2 Ca1 O14C 80.3(11) . . ? O13 Ca1 O14C 81.1(15) . . ? O14B Ca1 O14C 10.4(14) . . ? O8 Ca1 O14C 166.2(15) . . ? O6 Ca1 O14C 98.5(14) . . ? O14A Ca1 O14C 14.3(13) . . ? O2 Ca1 O7 163.2(3) . . ? O13 Ca1 O7 87.6(3) . . ? O14B Ca1 O7 73.2(8) . . ? O8 Ca1 O7 87.8(2) . . ? O6 Ca1 O7 64.0(2) . . ? O14A Ca1 O7 77.1(6) . . ? O14C Ca1 O7 83.5(11) . . ? O2 Ca1 O1 64.2(2) . . ? O13 Ca1 O1 136.4(2) . . ? O14B Ca1 O1 133.6(9) . . ? O8 Ca1 O1 66.63(19) . . ? O6 Ca1 O1 65.7(2) . . ? O14A Ca1 O1 120.4(5) . . ? O14C Ca1 O1 127.2(15) . . ? O7 Ca1 O1 124.0(2) . . ? O2 Ca1 Mn3 83.31(18) . . ? O13 Ca1 Mn3 110.5(2) . . ? O14B Ca1 Mn3 168.0(9) . . ? O8 Ca1 Mn3 32.82(15) . . ? O6 Ca1 Mn3 78.87(17) . . ? O14A Ca1 Mn3 154.4(5) . . ? O14C Ca1 Mn3 160.7(14) . . ? O7 Ca1 Mn3 111.60(19) . . ? O1 Ca1 Mn3 34.42(12) . . ? O2 Ca1 Mn1 31.31(19) . . ? O13 Ca1 Mn1 120.9(2) . . ? O14B Ca1 Mn1 110.3(7) . . ? O8 Ca1 Mn1 91.77(16) . . ? O6 Ca1 Mn1 87.48(17) . . ? O14A Ca1 Mn1 100.4(5) . . ? O14C Ca1 Mn1 100.9(13) . . ? O7 Ca1 Mn1 151.5(2) . . ? O1 Ca1 Mn1 33.52(12) . . ? Mn3 Ca1 Mn1 60.00(5) . . ? O2 Ca1 Mn2 86.4(2) . . ? O13 Ca1 Mn2 166.8(2) . . ? O14B Ca1 Mn2 112.8(11) . . ? O8 Ca1 Mn2 79.42(17) . . ? O6 Ca1 Mn2 32.42(16) . . ? O14A Ca1 Mn2 99.6(5) . . ? O14C Ca1 Mn2 112.0(15) . . ? O7 Ca1 Mn2 95.3(2) . . ? O1 Ca1 Mn2 33.89(13) . . ? Mn3 Ca1 Mn2 56.54(5) . . ? Mn1 Ca1 Mn2 56.79(5) . . ? Mn2 Cl1 Mn1 75.09(7) . . ? Mn2 Cl2 Mn3 75.89(7) . . ? Mn3 O1 Mn1 126.2(3) . . ? Mn3 O1 Mn2 114.4(3) . . ? Mn1 O1 Mn2 116.8(3) . . ? Mn3 O1 Ca1 93.5(2) . . ? Mn1 O1 Ca1 96.4(3) . . ? Mn2 O1 Ca1 96.3(2) . . ? C1B O2 C1A 38.7(19) . . ? C1B O2 Mn1 115(2) . . ? C1A O2 Mn1 110.5(7) . . ? C1B O2 Ca1 136(2) . . ? C1A O2 Ca1 127.8(7) . . ? Mn1 O2 Ca1 108.4(3) . . ? O2 C1A C11A 104.5(12) . . ? O2 C1A C2A 106.0(13) . . ? C11A C1A C2A 115.5(16) . . ? N1 C2A C1A 108.6(18) . . ? O2 C1B C11B 121(5) . . ? O2 C1B C2B 103(4) . . ? C11B C1B C2B 111(4) . . ? C1B C2B N1 105(4) . . ? C3 N1 C2A 121.8(12) . . ? C3 N1 C2B 120.5(17) . . ? C2A N1 C2B 16(2) . . ? C3 N1 Mn1 128.8(9) . . ? C2A N1 Mn1 109.1(10) . . ? C2B N1 Mn1 106.7(18) . . ? N1 C3 C4 124.0(10) . . ? C3 C4 C5 117.6(11) . . ? C3 C4 C9 123.8(10) . . ? C5 C4 C9 118.6(14) . . ? C6 C5 C4 122.8(13) . . ? C5 C6 C7 119.6(11) . . ? C8 C7 C6 119.4(14) . . ? O4 C8 C9 114.6(8) . . ? O4 C8 C7 124.3(12) . . ? C9 C8 C7 121.1(11) . . ? O3 C9 C8 118.3(9) . . ? O3 C9 C4 123.3(12) . . ? C8 C9 C4 118.4(9) . . ? C9 O3 Mn1 126.4(7) . . ? C9 O3 Mn4 117.2(7) . . ? Mn1 O3 Mn4 113.5(3) . . ? C8 O4 C10 116.7(9) . . ? C8 O4 Mn4 117.2(7) . . ? C10 O4 Mn4 126.0(6) . . ? C12 O5 Mn2 113.7(5) . . ? C12 O5 Mn4 121.6(6) . . ? Mn2 O5 Mn4 116.2(3) . . ? O5 C12 C22 112.1(8) . . ? O5 C12 C13 107.0(8) . . ? C22 C12 C13 110.6(7) . . ? N2 C13 C12 105.7(7) . . ? C14 N2 C13 121.0(9) . . ? C14 N2 Mn2 126.4(8) . . ? C13 N2 Mn2 111.7(5) . . ? N2 C14 C15 125.0(10) . . ? C20 C15 C16 121.0(11) . . ? C20 C15 C14 121.7(9) . . ? C16 C15 C14 117.3(11) . . ? C17 C16 C15 118.8(12) . . ? C16 C17 C18 121.9(11) . . ? C19 C18 C17 119.7(12) . . ? C18 C19 O7 124.6(11) . . ? C18 C19 C20 120.7(12) . . ? O7 C19 C20 114.6(9) . . ? O6 C20 C15 124.4(10) . . ? O6 C20 C19 117.8(10) . . ? C15 C20 C19 117.7(9) . . ? C20 O6 Mn2 126.1(7) . . ? C20 O6 Ca1 124.8(7) . . ? Mn2 O6 Ca1 106.2(3) . . ? C19 O7 C21 117.4(9) . . ? C19 O7 Ca1 118.6(6) . . ? C21 O7 Ca1 123.8(7) . . ? C23 O8 Mn3 114.8(6) . . ? C23 O8 Ca1 139.8(6) . . ? Mn3 O8 Ca1 104.3(2) . . ? O8 C23 C33 110.1(10) . . ? O8 C23 C24 110.2(9) . . ? C33 C23 C24 113.4(10) . . ? N3 C24 C23 106.4(8) . . ? C25 N3 C24 122.7(8) . . ? C25 N3 Mn3 127.0(6) . . ? C24 N3 Mn3 110.3(6) . . ? N3 C25 C26 123.2(8) . . ? C27 C26 C31 119.4(9) . . ? C27 C26 C25 118.4(9) . . ? C31 C26 C25 122.1(8) . . ? C28 C27 C26 121.7(9) . . ? C27 C28 C29 119.7(10) . . ? C30 C29 C28 120.3(10) . . ? O10 C30 C29 125.6(9) . . ? O10 C30 C31 113.4(8) . . ? C29 C30 C31 120.8(9) . . ? O9 C31 C30 118.4(7) . . ? O9 C31 C26 123.9(8) . . ? C30 C31 C26 117.7(8) . . ? C31 O9 Mn3 123.7(6) . . ? C31 O9 Mn4 116.3(5) . . ? Mn3 O9 Mn4 119.9(3) . . ? C30 O10 C32 117.3(8) . . ? C30 O10 Mn4 110.8(5) . . ? C32 O10 Mn4 131.8(6) . . ? C34 O11 Mn1 127.9(6) . . ? C34 O12 Mn3 124.6(6) . . ? O11 C34 O12 126.3(9) . . ? O11 C34 C35A 115.6(11) . . ? O12 C34 C35A 116.8(10) . . ? O11 C34 C35B 117.3(12) . . ? O12 C34 C35B 113.1(11) . . ? C35A C34 C35B 32.3(10) . . ? C41B O14B Ca1 107(3) . . ? O56B C41B C56B 46(4) . . ? O56B C41B O14B 149(6) . . ? C56B C41B O14B 160(6) . . ? C42C O14C Ca1 148(5) . . ? O15C C42C O14C 131(6) . . ? O15C C42C C43C 121(5) . . ? O14C C42C C43C 108(5) . . ? C41B O56B C56B 93(6) . . ? O56B C56B C41B 41(4) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.577 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.096 data_scmn97 _database_code_depnum_ccdc_archive 'CCDC 293108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38.60 H55.90 Mn4 N11.10 Na O16.10' _chemical_formula_weight 1175.79 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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 50.422(2) _cell_length_b 50.422(2) _cell_length_c 10.6912(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23540(2) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7482 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.29 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10890 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30242 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1648 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -62 _diffrn_reflns_limit_k_max 60 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.01 _reflns_number_total 10197 _reflns_number_gt 4636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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. The terminal ligand coordinated to Mn4 was three-fold disordered, with two components as azide and one as chelating acetate, with an overall composition of 0.7(azide) and 0.3(acetate). The solvent molecules were badly disordered and was refined as partial C and O atoms; the overall formulation (2MeOH and 0.5H2O per cluster) should be taken as a reasonable approximation, which is consistent with the available solvent volume. ; _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^)+(0.0215P)^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 10197 _refine_ls_number_parameters 656 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.993 _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 Mn1 Mn 0.228093(16) -0.000337(16) 0.55639(7) 0.02616(19) Uani 1 1 d . B . Mn2 Mn 0.183576(16) -0.065812(16) 0.44098(7) 0.0298(2) Uani 1 1 d . B . Mn3 Mn 0.161628(16) -0.054534(17) 0.70131(7) 0.0329(2) Uani 1 1 d . B . Mn4 Mn 0.159157(18) -0.013282(18) 0.44849(8) 0.0467(3) Uani 1 1 d D . . Na1 Na 0.22541(4) -0.06314(4) 0.70312(16) 0.0284(5) Uani 1 1 d . B . O1 O 0.19325(6) -0.03877(6) 0.5800(3) 0.0240(7) Uani 1 1 d . . . O2 O 0.22499(7) 0.02116(7) 0.7270(3) 0.0385(9) Uani 1 1 d . . . O3 O 0.18374(8) -0.01635(8) 0.8241(3) 0.0484(11) Uani 1 1 d . . . C1 C 0.20673(13) 0.00955(14) 0.8190(5) 0.0445(15) Uani 1 1 d . . . C2 C 0.21417(12) 0.02921(13) 0.9363(5) 0.073(2) Uani 1 1 d . . . H2A H 0.1951 0.0246 0.9787 0.110 Uiso 1 1 calc R . . H2B H 0.2254 0.0509 0.9130 0.110 Uiso 1 1 calc R . . H2C H 0.2268 0.0247 0.9927 0.110 Uiso 1 1 calc R . . O4 O 0.20664(7) 0.01511(7) 0.4618(3) 0.0344(9) Uani 1 1 d . B . C3 C 0.22471(12) 0.04621(12) 0.4298(5) 0.0499(16) Uani 1 1 d . . . H3 H 0.2252 0.0585 0.5040 0.060 Uiso 1 1 calc R C . C4 C 0.25700(11) 0.05390(11) 0.4034(4) 0.0347(13) Uani 1 1 d . C . H4A H 0.2586 0.0474 0.3177 0.042 Uiso 1 1 calc R . . H4B H 0.2711 0.0762 0.4109 0.042 Uiso 1 1 calc R . . N1 N 0.26480(9) 0.03739(8) 0.4962(3) 0.0257(10) Uani 1 1 d . . . C5 C 0.29225(11) 0.04685(10) 0.5299(4) 0.0257(12) Uani 1 1 d . C . H5 H 0.3075 0.0652 0.4917 0.031 Uiso 1 1 calc R . . C6 C 0.30296(10) 0.03281(10) 0.6203(4) 0.0221(11) Uani 1 1 d . . . C7 C 0.33363(10) 0.04859(10) 0.6563(4) 0.0236(12) Uani 1 1 d . C . H7 H 0.3473 0.0675 0.6172 0.028 Uiso 1 1 calc R . . C8 C 0.34436(11) 0.03716(10) 0.7478(4) 0.0288(12) Uani 1 1 d . . . H8 H 0.3654 0.0478 0.7707 0.035 Uiso 1 1 calc R C . C9 C 0.32377(10) 0.00950(10) 0.8067(4) 0.0276(12) Uani 1 1 d . C . H9 H 0.3309 0.0015 0.8707 0.033 Uiso 1 1 calc R . . C10 C 0.29368(10) -0.00603(10) 0.7732(4) 0.0215(11) Uani 1 1 d . . . C11 C 0.28207(10) 0.00470(10) 0.6760(4) 0.0211(11) Uani 1 1 d . C . O5 O 0.25329(6) -0.01237(6) 0.6439(3) 0.0226(8) Uani 1 1 d . . . O6 O 0.27186(7) -0.03303(7) 0.8289(3) 0.0275(8) Uani 1 1 d . B . C12 C 0.27775(12) -0.03739(11) 0.9551(4) 0.0485(16) Uani 1 1 d . . . H12A H 0.2611 -0.0571 0.9856 0.073 Uiso 1 1 calc R C . H12B H 0.2790 -0.0208 1.0069 0.073 Uiso 1 1 calc R . . H12C H 0.2972 -0.0373 0.9597 0.073 Uiso 1 1 calc R . . C13 C 0.21162(12) 0.05518(12) 0.3213(5) 0.0549(17) Uani 1 1 d . C . H13A H 0.1907 0.0504 0.3416 0.082 Uiso 1 1 calc R . . H13B H 0.2112 0.0438 0.2466 0.082 Uiso 1 1 calc R . . H13C H 0.2244 0.0772 0.3055 0.082 Uiso 1 1 calc R . . O7 O 0.16089(7) -0.05011(7) 0.3604(3) 0.0379(9) Uani 1 1 d . B . C14 C 0.14836(14) -0.06365(13) 0.2407(5) 0.0595(18) Uani 1 1 d . . . H14 H 0.1294 -0.0626 0.2239 0.071 Uiso 1 1 calc R C . C24 C 0.17287(17) -0.04542(16) 0.1380(6) 0.118(3) Uani 1 1 d . C . H24A H 0.1784 -0.0238 0.1408 0.177 Uiso 1 1 calc R . . H24B H 0.1645 -0.0539 0.0555 0.177 Uiso 1 1 calc R . . H24C H 0.1912 -0.0471 0.1534 0.177 Uiso 1 1 calc R . . C15 C 0.14102(16) -0.09570(14) 0.2428(6) 0.081(2) Uani 1 1 d . C . H15A H 0.1381 -0.1039 0.1567 0.097 Uiso 1 1 calc R . . H15B H 0.1220 -0.1084 0.2911 0.097 Uiso 1 1 calc R . . N2 N 0.16790(10) -0.09576(10) 0.3042(4) 0.0471(13) Uani 1 1 d . . . C16 C 0.17562(12) -0.11597(12) 0.2788(5) 0.0456(15) Uani 1 1 d . C . H16 H 0.1649 -0.1297 0.2124 0.055 Uiso 1 1 calc R . . C17 C 0.19865(11) -0.11972(10) 0.3407(5) 0.0299(13) Uani 1 1 d . . . C18 C 0.20687(12) -0.14026(11) 0.2894(5) 0.0409(15) Uani 1 1 d . C . H18 H 0.1963 -0.1520 0.2179 0.049 Uiso 1 1 calc R . . C19 C 0.22974(13) -0.14344(11) 0.3411(5) 0.0442(16) Uani 1 1 d . . . H19 H 0.2352 -0.1574 0.3062 0.053 Uiso 1 1 calc R C . C20 C 0.24530(12) -0.12596(11) 0.4462(5) 0.0409(15) Uani 1 1 d . C . H20 H 0.2618 -0.1276 0.4805 0.049 Uiso 1 1 calc R . . C21 C 0.23697(11) -0.10654(11) 0.5001(5) 0.0303(13) Uani 1 1 d . . . C22 C 0.21300(11) -0.10284(10) 0.4501(4) 0.0261(12) Uani 1 1 d . C . O8 O 0.20538(7) -0.08465(7) 0.5075(3) 0.0287(8) Uani 1 1 d . . . O9 O 0.25078(7) -0.08867(7) 0.6048(3) 0.0323(8) Uani 1 1 d . B . C23 C 0.27773(10) -0.08824(11) 0.6503(5) 0.0418(14) Uani 1 1 d . . . H23A H 0.2854 -0.0751 0.7245 0.063 Uiso 1 1 calc R C . H23B H 0.2935 -0.0802 0.5852 0.063 Uiso 1 1 calc R . . H23C H 0.2727 -0.1091 0.6725 0.063 Uiso 1 1 calc R . . O10 O 0.14064(7) -0.03766(8) 0.6151(3) 0.0469(10) Uani 1 1 d . B . C25 C 0.10922(17) -0.0502(2) 0.6528(8) 0.100(3) Uani 1 1 d . . . H25 H 0.1037 -0.0337 0.6449 0.120 Uiso 1 1 calc R A 1 C35A C 0.0893(3) -0.0750(3) 0.5731(12) 0.054(3) Uiso 0.50 1 d P B 1 H35A H 0.0925 -0.0680 0.4860 0.081 Uiso 0.50 1 calc PR B 1 H35B H 0.0680 -0.0824 0.5968 0.081 Uiso 0.50 1 calc PR B 1 H35C H 0.0939 -0.0917 0.5817 0.081 Uiso 0.50 1 calc PR B 1 C35B C 0.0899(8) -0.0567(8) 0.550(3) 0.37(2) Uiso 0.50 1 d P B 2 H35D H 0.0941 -0.0687 0.4887 0.554 Uiso 0.50 1 calc PR B 2 H35E H 0.0937 -0.0375 0.5110 0.554 Uiso 0.50 1 calc PR B 2 H35F H 0.0686 -0.0684 0.5770 0.554 Uiso 0.50 1 calc PR B 2 C26 C 0.10598(15) -0.05947(17) 0.7852(7) 0.089(2) Uani 1 1 d . B . H26A H 0.1135 -0.0413 0.8401 0.107 Uiso 1 1 calc R . . H26B H 0.0842 -0.0737 0.8052 0.107 Uiso 1 1 calc R . . N3 N 0.12396(9) -0.07448(11) 0.8047(4) 0.0476(13) Uani 1 1 d . . . C27 C 0.11458(12) -0.09907(14) 0.8685(5) 0.0481(17) Uani 1 1 d . B . H27 H 0.0946 -0.1081 0.9029 0.058 Uiso 1 1 calc R . . C28 C 0.13169(13) -0.11389(13) 0.8918(5) 0.0409(15) Uani 1 1 d . . . C29 C 0.11662(13) -0.14218(13) 0.9535(5) 0.0539(18) Uani 1 1 d . B . H29 H 0.0956 -0.1507 0.9753 0.065 Uiso 1 1 calc R . . C30 C 0.13154(14) -0.15780(13) 0.9831(5) 0.0547(18) Uani 1 1 d . . . H30 H 0.1209 -0.1772 1.0231 0.066 Uiso 1 1 calc R B . C31 C 0.16248(13) -0.14490(11) 0.9539(4) 0.0416(15) Uani 1 1 d . B . H31 H 0.1731 -0.1553 0.9767 0.050 Uiso 1 1 calc R . . C32 C 0.17763(12) -0.11756(12) 0.8930(4) 0.0332(13) Uani 1 1 d . . . C33 C 0.16254(11) -0.10138(11) 0.8567(4) 0.0283(12) Uani 1 1 d . B . O11 O 0.17808(7) -0.07530(7) 0.7960(3) 0.0315(8) Uani 1 1 d . . . O12 O 0.20796(7) -0.10302(7) 0.8596(3) 0.0344(9) Uani 1 1 d . B . C34 C 0.22553(11) -0.11577(11) 0.9097(5) 0.0427(15) Uani 1 1 d . . . H34A H 0.2466 -0.1040 0.8792 0.064 Uiso 1 1 calc R B . H34B H 0.2165 -0.1371 0.8829 0.064 Uiso 1 1 calc R . . H34C H 0.2254 -0.1148 1.0012 0.064 Uiso 1 1 calc R . . N11 N 0.22933(9) -0.02705(9) 0.3721(4) 0.0310(11) Uani 1 1 d . . . N12 N 0.24272(10) -0.01319(10) 0.2796(4) 0.0355(11) Uani 1 1 d . C . N13 N 0.25640(12) 0.00076(11) 0.1919(4) 0.0591(15) Uani 1 1 d . . . N14 N 0.14189(8) -0.09743(9) 0.5629(4) 0.0314(11) Uani 1 1 d . . . N15 N 0.13766(9) -0.12258(10) 0.5861(4) 0.0289(10) Uani 1 1 d . B . N16 N 0.13305(9) -0.14703(10) 0.6078(4) 0.0394(12) Uani 1 1 d . . . N17A N 0.1329(3) -0.0077(3) 0.3047(13) 0.065(5) Uiso 0.56 1 d PDU C 1 N18A N 0.1403(2) 0.0114(3) 0.2111(11) 0.095(3) Uiso 0.56 1 d PDU C 1 N19A N 0.1501(2) 0.0323(2) 0.1251(11) 0.078(3) Uiso 0.56 1 d PDU C 1 N17B N 0.1281(12) 0.0002(12) 0.338(5) 0.128(15) Uiso 0.14 1 d PDU C 2 N18B N 0.1035(10) -0.0048(11) 0.292(6) 0.153(15) Uiso 0.14 1 d PDU C 2 N19B N 0.0797(11) -0.0246(13) 0.236(5) 0.16(2) Uiso 0.14 1 d PDU C 2 O14C O 0.1390(4) -0.0081(4) 0.2699(18) 0.065(7) Uiso 0.30 1 d PDU C 3 C37C C 0.1100(6) -0.0250(5) 0.271(3) 0.169(12) Uiso 0.30 1 d PDU C 3 O15C O 0.1080(6) -0.0257(6) 0.385(3) 0.188(9) Uiso 0.30 1 d PDU C 3 C38C C 0.0767(5) -0.0469(5) 0.219(2) 0.065(6) Uiso 0.30 1 d PD C 3 O13 O 0.15370(10) 0.02380(10) 0.5328(5) 0.0868(15) Uani 1 1 d . C . H13 H 0.1424 0.0310 0.4868 0.104 Uiso 1 1 calc R . . C36 C 0.1661(2) 0.0381(2) 0.6536(8) 0.148(4) Uani 1 1 d . . . H36A H 0.1607 0.0539 0.6697 0.223 Uiso 1 1 calc R C . H36B H 0.1884 0.0473 0.6528 0.223 Uiso 1 1 calc R . . H36C H 0.1574 0.0225 0.7196 0.223 Uiso 1 1 calc R . . O41A O 0.1356(5) 0.0758(5) -0.106(2) 0.211(9) Uiso 0.35 1 d PU . . O41B O 0.1597(4) 0.0595(5) -0.0545(18) 0.192(7) Uiso 0.40 1 d PU C . O41C O 0.1440(8) 0.0325(9) 0.011(4) 0.202(12) Uiso 0.25 1 d PU . . C41A C 0.1188(12) 0.0420(12) -0.071(5) 0.219(19) Uiso 0.25 1 d PU C . C41B C 0.1352(11) 0.0047(12) -0.001(5) 0.203(19) Uiso 0.25 1 d PU C . O42 O 0.0962(3) 0.0209(3) 0.5477(15) 0.349(6) Uiso 1 1 d U . . C42A C 0.0859(6) 0.0134(6) 0.415(3) 0.378(14) Uiso 0.75 1 d PU . . C42B C 0.0843(15) 0.0364(17) 0.678(7) 0.31(3) Uiso 0.25 1 d P . . O43A O 0.0538(10) -0.0191(11) 0.869(5) 0.287(16) Uiso 0.30 1 d PU . . O43B O 0.0701(9) 0.0046(10) 0.770(4) 0.204(15) Uiso 0.20 1 d PU . . C43A C 0.0418(13) -0.0123(14) 0.917(5) 0.27(2) Uiso 0.30 1 d PU . . C43B C 0.0353(16) -0.0388(15) 0.798(6) 0.21(2) Uiso 0.20 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 Mn1 0.0304(4) 0.0268(4) 0.0222(5) 0.0005(4) -0.0022(4) 0.0149(4) Mn2 0.0372(5) 0.0332(5) 0.0200(5) -0.0045(4) -0.0081(4) 0.0183(4) Mn3 0.0278(5) 0.0374(5) 0.0305(5) -0.0058(4) 0.0020(4) 0.0142(4) Mn4 0.0442(6) 0.0448(5) 0.0569(6) -0.0026(5) -0.0161(5) 0.0267(5) Na1 0.0309(11) 0.0290(11) 0.0209(11) 0.0037(9) -0.0024(9) 0.0119(9) O1 0.0222(18) 0.0316(19) 0.0192(18) -0.0047(16) -0.0046(15) 0.0143(16) O2 0.033(2) 0.037(2) 0.035(2) -0.0150(19) 0.0037(19) 0.0105(18) O3 0.039(2) 0.043(2) 0.037(2) -0.016(2) 0.0091(19) 0.001(2) C1 0.040(4) 0.054(4) 0.041(4) -0.017(3) 0.001(3) 0.025(3) C2 0.057(4) 0.071(5) 0.061(5) -0.036(4) 0.013(4) 0.008(4) O4 0.038(2) 0.028(2) 0.039(2) 0.0035(18) -0.0067(18) 0.0173(17) C3 0.055(4) 0.044(4) 0.053(4) 0.020(3) -0.004(3) 0.026(3) C4 0.043(3) 0.039(3) 0.029(3) 0.005(3) -0.008(3) 0.026(3) N1 0.034(3) 0.029(2) 0.017(2) 0.0037(19) 0.002(2) 0.019(2) C5 0.035(3) 0.020(3) 0.019(3) -0.003(2) 0.005(3) 0.012(3) C6 0.030(3) 0.023(3) 0.016(3) -0.002(2) 0.000(2) 0.016(3) C7 0.024(3) 0.015(3) 0.025(3) 0.003(2) 0.010(2) 0.006(2) C8 0.026(3) 0.028(3) 0.032(3) -0.005(3) -0.003(3) 0.013(3) C9 0.033(3) 0.033(3) 0.014(3) -0.002(2) -0.005(2) 0.015(3) C10 0.025(3) 0.022(3) 0.015(3) -0.002(2) 0.001(2) 0.010(2) C11 0.031(3) 0.024(3) 0.013(3) 0.000(2) 0.002(2) 0.017(3) O5 0.0175(18) 0.0235(18) 0.0202(19) 0.0003(15) -0.0040(15) 0.0052(15) O6 0.030(2) 0.0301(19) 0.0152(19) 0.0084(16) -0.0031(16) 0.0101(17) C12 0.060(4) 0.038(3) 0.025(3) 0.007(3) -0.003(3) 0.007(3) C13 0.061(4) 0.055(4) 0.054(4) 0.004(3) -0.008(3) 0.033(3) O7 0.047(2) 0.043(2) 0.030(2) -0.0069(18) -0.0176(18) 0.0272(19) C14 0.081(5) 0.056(4) 0.042(4) -0.010(4) -0.028(4) 0.035(4) C24 0.135(7) 0.115(7) 0.058(5) -0.007(5) -0.034(5) 0.028(6) C15 0.120(6) 0.072(5) 0.055(5) -0.022(4) -0.050(4) 0.051(5) N2 0.075(4) 0.047(3) 0.029(3) -0.014(2) -0.020(3) 0.037(3) C16 0.057(4) 0.039(4) 0.024(3) -0.012(3) 0.002(3) 0.011(3) C17 0.033(3) 0.021(3) 0.028(3) 0.000(3) 0.007(3) 0.007(3) C18 0.047(4) 0.026(3) 0.038(4) 0.004(3) 0.019(3) 0.010(3) C19 0.060(4) 0.032(3) 0.040(4) 0.004(3) 0.029(3) 0.022(3) C20 0.049(4) 0.036(3) 0.045(4) 0.019(3) 0.026(3) 0.027(3) C21 0.032(3) 0.031(3) 0.026(3) 0.013(3) 0.010(3) 0.013(3) C22 0.032(3) 0.021(3) 0.020(3) 0.004(2) 0.012(3) 0.010(2) O8 0.041(2) 0.0289(19) 0.022(2) -0.0049(16) -0.0005(16) 0.0218(17) O9 0.030(2) 0.036(2) 0.032(2) 0.0100(18) 0.0046(18) 0.0168(17) C23 0.031(3) 0.049(4) 0.048(4) 0.016(3) 0.005(3) 0.021(3) O10 0.031(2) 0.054(2) 0.063(3) -0.002(2) 0.004(2) 0.027(2) C25 0.072(6) 0.147(8) 0.107(7) 0.032(7) 0.014(6) 0.075(6) C26 0.064(5) 0.147(7) 0.081(6) 0.021(5) 0.027(5) 0.071(5) N3 0.028(3) 0.059(3) 0.048(3) -0.019(3) 0.004(3) 0.015(3) C27 0.030(4) 0.055(4) 0.029(4) -0.013(3) 0.011(3) -0.001(3) C28 0.040(4) 0.040(4) 0.019(3) -0.014(3) -0.001(3) 0.001(3) C29 0.045(4) 0.047(4) 0.026(4) -0.017(3) 0.011(3) -0.010(3) C30 0.067(5) 0.035(4) 0.021(4) -0.002(3) 0.005(3) -0.006(4) C31 0.055(4) 0.032(3) 0.015(3) -0.001(3) -0.006(3) 0.004(3) C32 0.031(3) 0.035(3) 0.009(3) -0.002(3) -0.002(2) -0.002(3) C33 0.029(3) 0.029(3) 0.010(3) -0.004(2) -0.004(2) 0.001(3) O11 0.0268(19) 0.035(2) 0.020(2) 0.0056(17) 0.0044(16) 0.0057(17) O12 0.042(2) 0.034(2) 0.019(2) 0.0064(16) -0.0042(17) 0.0121(19) C34 0.053(4) 0.041(3) 0.030(3) 0.007(3) -0.006(3) 0.021(3) N11 0.036(3) 0.038(3) 0.020(3) 0.001(2) 0.000(2) 0.020(2) N12 0.047(3) 0.039(3) 0.026(3) -0.006(2) -0.002(3) 0.026(3) N13 0.096(4) 0.063(4) 0.026(3) 0.017(3) 0.029(3) 0.046(3) N14 0.032(3) 0.030(3) 0.029(3) -0.002(2) -0.004(2) 0.014(2) N15 0.027(3) 0.037(3) 0.016(3) -0.009(2) -0.005(2) 0.011(3) N16 0.047(3) 0.036(3) 0.027(3) -0.002(2) 0.006(2) 0.015(3) O13 0.090(4) 0.073(3) 0.119(4) 0.017(3) 0.005(3) 0.057(3) C36 0.206(11) 0.170(10) 0.126(9) -0.021(7) 0.017(8) 0.137(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 Mn1 O1 1.871(3) . ? Mn1 O5 1.905(3) . ? Mn1 O4 1.908(3) . ? Mn1 N1 1.984(4) . ? Mn1 O2 2.167(3) . ? Mn1 N11 2.405(4) . ? Mn1 Mn2 3.1701(10) . ? Mn1 Na1 3.4755(18) . ? Mn2 O7 1.893(3) . ? Mn2 O1 1.908(3) . ? Mn2 O8 1.913(3) . ? Mn2 N2 1.962(4) . ? Mn2 N11 2.275(4) . ? Mn2 N14 2.304(4) . ? Mn2 Mn3 3.1502(10) . ? Mn2 Na1 3.4695(18) . ? Mn3 O1 1.895(3) . ? Mn3 O10 1.896(3) . ? Mn3 O11 1.917(3) . ? Mn3 N3 1.983(4) . ? Mn3 O3 2.128(3) . ? Mn3 N14 2.389(4) . ? Mn3 Na1 3.4535(18) . ? Mn4 O4 2.091(3) . ? Mn4 O10 2.100(4) . ? Mn4 O7 2.122(3) . ? Mn4 N17A 2.138(13) . ? Mn4 O13 2.213(4) . ? Mn4 O14C 2.24(2) . ? Mn4 N17B 2.32(3) . ? Mn4 O15C 2.43(3) . ? Na1 O5 2.309(3) . ? Na1 O8 2.339(3) . ? Na1 O11 2.365(3) . ? Na1 O12 2.418(3) . ? Na1 O6 2.458(3) . ? Na1 O9 2.459(4) . ? Na1 O1 2.805(3) . ? O2 C1 1.272(6) . ? O3 C1 1.240(6) . ? C1 C2 1.525(7) . ? O4 C3 1.406(5) . ? C3 C4 1.500(6) . ? C3 C13 1.511(6) . ? C4 N1 1.469(5) . ? N1 C5 1.270(5) . ? C5 C6 1.452(6) . ? C6 C7 1.394(6) . ? C6 C11 1.407(6) . ? C7 C8 1.376(6) . ? C8 C9 1.404(6) . ? C9 C10 1.362(6) . ? C10 O6 1.385(5) . ? C10 C11 1.426(6) . ? C11 O5 1.310(5) . ? O6 C12 1.422(5) . ? O7 C14 1.440(6) . ? C14 C15 1.466(7) . ? C14 C24 1.562(8) . ? C15 N2 1.508(6) . ? N2 C16 1.289(6) . ? C16 C17 1.429(7) . ? C17 C18 1.405(6) . ? C17 C22 1.415(6) . ? C18 C19 1.359(7) . ? C19 C20 1.402(7) . ? C20 C21 1.370(6) . ? C21 O9 1.387(5) . ? C21 C22 1.416(6) . ? C22 O8 1.311(5) . ? O9 C23 1.433(5) . ? O10 C25 1.439(7) . ? C25 C35B 1.40(3) . ? C25 C35A 1.431(13) . ? C25 C26 1.474(9) . ? C26 N3 1.458(7) . ? N3 C27 1.280(6) . ? C27 C28 1.418(7) . ? C28 C29 1.401(7) . ? C28 C33 1.406(6) . ? C29 C30 1.371(7) . ? C30 C31 1.393(7) . ? C31 C32 1.362(6) . ? C32 O12 1.372(5) . ? C32 C33 1.420(6) . ? C33 O11 1.317(5) . ? O12 C34 1.433(5) . ? N11 N12 1.204(5) . ? N12 N13 1.168(5) . ? N14 N15 1.202(5) . ? N15 N16 1.158(5) . ? N17A N18A 1.307(17) . ? N18A N19A 1.295(12) . ? N19A O41C 1.25(3) . ? N19A C41B 1.81(5) . ? N17B N18B 1.234(19) . ? N18B N19B 1.260(19) . ? O14C C37C 1.27(2) . ? C37C O15C 1.23(3) . ? C37C C38C 1.58(2) . ? C38C O41A 1.36(3) 11 ? O13 C36 1.458(8) . ? O41A C38C 1.36(3) 12 ? O41A C41A 1.52(5) . ? O41B O41C 1.38(3) . ? O41B C41A 1.80(5) . ? O41C C41B 1.25(5) . ? O41C C41A 1.80(5) . ? O42 C42A 1.50(3) . ? O42 C42B 1.84(7) . ? C42B O43B 1.70(6) . ? O43A C43A 0.97(7) . ? O43A C43B 1.22(7) . ? O43A O43B 1.50(5) . ? C43A C43B 1.75(8) . ? 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 Mn1 O5 91.98(12) . . ? O1 Mn1 O4 93.65(13) . . ? O5 Mn1 O4 174.10(14) . . ? O1 Mn1 N1 168.30(14) . . ? O5 Mn1 N1 90.79(14) . . ? O4 Mn1 N1 83.34(15) . . ? O1 Mn1 O2 98.02(12) . . ? O5 Mn1 O2 88.42(12) . . ? O4 Mn1 O2 92.56(13) . . ? N1 Mn1 O2 93.41(14) . . ? O1 Mn1 N11 78.70(13) . . ? O5 Mn1 N11 90.89(12) . . ? O4 Mn1 N11 88.47(13) . . ? N1 Mn1 N11 89.90(14) . . ? O2 Mn1 N11 176.63(14) . . ? O1 Mn1 Mn2 33.34(9) . . ? O5 Mn1 Mn2 95.58(9) . . ? O4 Mn1 Mn2 88.17(9) . . ? N1 Mn1 Mn2 135.02(11) . . ? O2 Mn1 Mn2 131.14(9) . . ? N11 Mn1 Mn2 45.65(10) . . ? O1 Mn1 Na1 53.62(9) . . ? O5 Mn1 Na1 38.41(9) . . ? O4 Mn1 Na1 147.06(10) . . ? N1 Mn1 Na1 127.79(12) . . ? O2 Mn1 Na1 95.52(10) . . ? N11 Mn1 Na1 81.92(10) . . ? Mn2 Mn1 Na1 62.75(3) . . ? O7 Mn2 O1 92.71(13) . . ? O7 Mn2 O8 173.84(14) . . ? O1 Mn2 O8 93.45(12) . . ? O7 Mn2 N2 83.55(16) . . ? O1 Mn2 N2 172.36(16) . . ? O8 Mn2 N2 90.32(16) . . ? O7 Mn2 N11 93.38(14) . . ? O1 Mn2 N11 81.43(13) . . ? O8 Mn2 N11 87.66(13) . . ? N2 Mn2 N11 105.38(16) . . ? O7 Mn2 N14 90.79(14) . . ? O1 Mn2 N14 82.69(13) . . ? O8 Mn2 N14 89.87(13) . . ? N2 Mn2 N14 90.68(16) . . ? N11 Mn2 N14 163.76(14) . . ? O7 Mn2 Mn3 89.20(10) . . ? O1 Mn2 Mn3 33.93(8) . . ? O8 Mn2 Mn3 95.85(9) . . ? N2 Mn2 Mn3 139.00(14) . . ? N11 Mn2 Mn3 115.33(10) . . ? N14 Mn2 Mn3 48.99(10) . . ? O7 Mn2 Mn1 90.16(10) . . ? O1 Mn2 Mn1 32.62(8) . . ? O8 Mn2 Mn1 95.09(9) . . ? N2 Mn2 Mn1 153.45(13) . . ? N11 Mn2 Mn1 49.12(10) . . ? N14 Mn2 Mn1 115.24(10) . . ? Mn3 Mn2 Mn1 66.29(2) . . ? O7 Mn2 Na1 146.52(10) . . ? O1 Mn2 Na1 53.84(9) . . ? O8 Mn2 Na1 39.63(9) . . ? N2 Mn2 Na1 129.43(14) . . ? N11 Mn2 Na1 83.82(10) . . ? N14 Mn2 Na1 84.06(10) . . ? Mn3 Mn2 Na1 62.67(3) . . ? Mn1 Mn2 Na1 62.94(3) . . ? O1 Mn3 O10 91.16(14) . . ? O1 Mn3 O11 95.03(12) . . ? O10 Mn3 O11 173.03(14) . . ? O1 Mn3 N3 170.54(16) . . ? O10 Mn3 N3 83.72(18) . . ? O11 Mn3 N3 89.70(18) . . ? O1 Mn3 O3 95.31(13) . . ? O10 Mn3 O3 92.94(15) . . ? O11 Mn3 O3 89.68(14) . . ? N3 Mn3 O3 92.90(16) . . ? O1 Mn3 N14 80.66(13) . . ? O10 Mn3 N14 91.83(14) . . ? O11 Mn3 N14 86.03(13) . . ? N3 Mn3 N14 91.52(15) . . ? O3 Mn3 N14 173.82(13) . . ? O1 Mn3 Mn2 34.19(8) . . ? O10 Mn3 Mn2 88.67(11) . . ? O11 Mn3 Mn2 94.65(9) . . ? N3 Mn3 Mn2 137.31(12) . . ? O3 Mn3 Mn2 129.49(10) . . ? N14 Mn3 Mn2 46.69(9) . . ? O1 Mn3 Na1 54.23(9) . . ? O10 Mn3 Na1 145.39(11) . . ? O11 Mn3 Na1 40.91(9) . . ? N3 Mn3 Na1 130.48(16) . . ? O3 Mn3 Na1 90.61(10) . . ? N14 Mn3 Na1 83.23(10) . . ? Mn2 Mn3 Na1 63.19(3) . . ? O4 Mn4 O10 111.39(13) . . ? O4 Mn4 O7 95.46(12) . . ? O10 Mn4 O7 93.72(13) . . ? O4 Mn4 N17A 122.1(4) . . ? O10 Mn4 N17A 124.3(4) . . ? O7 Mn4 N17A 95.5(4) . . ? O4 Mn4 O13 88.71(14) . . ? O10 Mn4 O13 86.69(15) . . ? O7 Mn4 O13 175.33(15) . . ? N17A Mn4 O13 80.5(4) . . ? O4 Mn4 O14C 114.1(5) . . ? O10 Mn4 O14C 134.2(5) . . ? O7 Mn4 O14C 86.7(5) . . ? N17A Mn4 O14C 12.6(6) . . ? O13 Mn4 O14C 89.7(5) . . ? O4 Mn4 N17B 122.9(15) . . ? O10 Mn4 N17B 115.9(17) . . ? O7 Mn4 N17B 111.0(14) . . ? N17A Mn4 N17B 16.4(16) . . ? O13 Mn4 N17B 64.7(14) . . ? O14C Mn4 N17B 28.2(16) . . ? O4 Mn4 O15C 154.3(6) . . ? O10 Mn4 O15C 88.9(7) . . ? O7 Mn4 O15C 98.9(6) . . ? N17A Mn4 O15C 35.5(7) . . ? O13 Mn4 O15C 76.4(6) . . ? O14C Mn4 O15C 46.2(8) . . ? N17B Mn4 O15C 31.5(15) . . ? O5 Na1 O8 98.69(11) . . ? O5 Na1 O11 112.24(12) . . ? O8 Na1 O11 96.27(12) . . ? O5 Na1 O12 151.45(13) . . ? O8 Na1 O12 109.86(12) . . ? O11 Na1 O12 66.03(12) . . ? O5 Na1 O6 66.50(10) . . ? O8 Na1 O6 146.34(13) . . ? O11 Na1 O6 117.18(12) . . ? O12 Na1 O6 88.47(12) . . ? O5 Na1 O9 105.98(12) . . ? O8 Na1 O9 65.95(11) . . ? O11 Na1 O9 139.96(13) . . ? O12 Na1 O9 85.91(12) . . ? O6 Na1 O9 88.43(12) . . ? O5 Na1 O1 63.28(9) . . ? O8 Na1 O1 64.74(10) . . ? O11 Na1 O1 65.23(10) . . ? O12 Na1 O1 129.76(12) . . ? O6 Na1 O1 124.55(11) . . ? O9 Na1 O1 126.51(12) . . ? O5 Na1 Mn3 87.03(8) . . ? O8 Na1 Mn3 80.79(8) . . ? O11 Na1 Mn3 32.07(8) . . ? O12 Na1 Mn3 97.70(10) . . ? O6 Na1 Mn3 125.80(9) . . ? O9 Na1 Mn3 145.53(10) . . ? O1 Na1 Mn3 33.24(6) . . ? O5 Na1 Mn2 80.95(8) . . ? O8 Na1 Mn2 31.44(8) . . ? O11 Na1 Mn2 79.28(9) . . ? O12 Na1 Mn2 124.42(10) . . ? O6 Na1 Mn2 147.01(9) . . ? O9 Na1 Mn2 95.73(9) . . ? O1 Na1 Mn2 33.31(6) . . ? Mn3 Na1 Mn2 54.13(3) . . ? O5 Na1 Mn1 30.83(7) . . ? O8 Na1 Mn1 80.21(8) . . ? O11 Na1 Mn1 90.01(9) . . ? O12 Na1 Mn1 154.45(10) . . ? O6 Na1 Mn1 95.34(8) . . ? O9 Na1 Mn1 119.38(9) . . ? O1 Na1 Mn1 32.49(6) . . ? Mn3 Na1 Mn1 59.83(3) . . ? Mn2 Na1 Mn1 54.32(3) . . ? Mn1 O1 Mn3 133.17(16) . . ? Mn1 O1 Mn2 114.05(14) . . ? Mn3 O1 Mn2 111.88(14) . . ? Mn1 O1 Na1 93.89(11) . . ? Mn3 O1 Na1 92.54(11) . . ? Mn2 O1 Na1 92.85(11) . . ? C1 O2 Mn1 129.6(3) . . ? C1 O3 Mn3 135.8(4) . . ? O3 C1 O2 126.8(5) . . ? O3 C1 C2 116.4(5) . . ? O2 C1 C2 116.8(5) . . ? C3 O4 Mn1 113.6(3) . . ? C3 O4 Mn4 128.9(3) . . ? Mn1 O4 Mn4 116.44(15) . . ? O4 C3 C4 110.4(4) . . ? O4 C3 C13 112.6(4) . . ? C4 C3 C13 111.0(5) . . ? N1 C4 C3 106.9(4) . . ? C5 N1 C4 121.9(4) . . ? C5 N1 Mn1 125.9(3) . . ? C4 N1 Mn1 112.1(3) . . ? N1 C5 C6 127.4(5) . . ? C7 C6 C11 121.1(4) . . ? C7 C6 C5 118.8(4) . . ? C11 C6 C5 119.9(4) . . ? C8 C7 C6 120.9(4) . . ? C7 C8 C9 119.0(4) . . ? C10 C9 C8 120.7(4) . . ? C9 C10 O6 124.1(4) . . ? C9 C10 C11 121.6(4) . . ? O6 C10 C11 114.3(4) . . ? O5 C11 C6 125.2(4) . . ? O5 C11 C10 118.2(4) . . ? C6 C11 C10 116.6(4) . . ? C11 O5 Mn1 128.0(3) . . ? C11 O5 Na1 121.1(3) . . ? Mn1 O5 Na1 110.76(13) . . ? C10 O6 C12 115.8(3) . . ? C10 O6 Na1 114.5(2) . . ? C12 O6 Na1 129.2(3) . . ? C14 O7 Mn2 114.8(3) . . ? C14 O7 Mn4 127.5(3) . . ? Mn2 O7 Mn4 117.52(15) . . ? O7 C14 C15 108.6(5) . . ? O7 C14 C24 108.4(5) . . ? C15 C14 C24 110.4(6) . . ? C14 C15 N2 106.1(5) . . ? C16 N2 C15 122.5(5) . . ? C16 N2 Mn2 126.9(4) . . ? C15 N2 Mn2 109.9(3) . . ? N2 C16 C17 126.4(5) . . ? C18 C17 C22 121.0(5) . . ? C18 C17 C16 118.4(5) . . ? C22 C17 C16 120.6(5) . . ? C19 C18 C17 120.6(5) . . ? C18 C19 C20 119.5(5) . . ? C21 C20 C19 120.8(5) . . ? C20 C21 O9 124.7(5) . . ? C20 C21 C22 121.5(5) . . ? O9 C21 C22 113.8(4) . . ? O8 C22 C17 124.6(5) . . ? O8 C22 C21 118.9(4) . . ? C17 C22 C21 116.5(5) . . ? C22 O8 Mn2 128.0(3) . . ? C22 O8 Na1 122.2(3) . . ? Mn2 O8 Na1 108.93(14) . . ? C21 O9 C23 116.6(4) . . ? C21 O9 Na1 117.5(3) . . ? C23 O9 Na1 125.8(3) . . ? C25 O10 Mn3 114.0(4) . . ? C25 O10 Mn4 124.3(4) . . ? Mn3 O10 Mn4 119.39(16) . . ? C35B C25 C35A 39.0(15) . . ? C35B C25 O10 111.5(16) . . ? C35A C25 O10 110.6(8) . . ? C35B C25 C26 136.9(17) . . ? C35A C25 C26 112.1(9) . . ? O10 C25 C26 109.3(6) . . ? N3 C26 C25 107.7(5) . . ? C27 N3 C26 123.7(5) . . ? C27 N3 Mn3 125.8(4) . . ? C26 N3 Mn3 110.1(4) . . ? N3 C27 C28 125.2(5) . . ? C29 C28 C33 119.8(6) . . ? C29 C28 C27 117.2(6) . . ? C33 C28 C27 123.0(5) . . ? C30 C29 C28 121.3(6) . . ? C29 C30 C31 119.2(5) . . ? C32 C31 C30 120.7(6) . . ? C31 C32 O12 125.2(5) . . ? C31 C32 C33 121.5(5) . . ? O12 C32 C33 113.4(4) . . ? O11 C33 C28 123.5(5) . . ? O11 C33 C32 119.1(4) . . ? C28 C33 C32 117.4(5) . . ? C33 O11 Mn3 127.0(3) . . ? C33 O11 Na1 119.0(3) . . ? Mn3 O11 Na1 107.02(14) . . ? C32 O12 C34 115.9(4) . . ? C32 O12 Na1 118.0(3) . . ? C34 O12 Na1 125.6(3) . . ? N12 N11 Mn2 142.9(3) . . ? N12 N11 Mn1 120.8(3) . . ? Mn2 N11 Mn1 85.23(14) . . ? N13 N12 N11 178.1(6) . . ? N15 N14 Mn2 117.8(3) . . ? N15 N14 Mn3 127.0(3) . . ? Mn2 N14 Mn3 84.32(13) . . ? N16 N15 N14 178.8(5) . . ? N18A N17A Mn4 133.0(10) . . ? N19A N18A N17A 174.0(13) . . ? O41C N19A N18A 134(2) . . ? O41C N19A C41B 44(2) . . ? N18A N19A C41B 93.5(18) . . ? N18B N17B Mn4 154(5) . . ? N17B N18B N19B 144(4) . . ? C37C O14C Mn4 110.6(18) . . ? O15C C37C O14C 95(3) . . ? O15C C37C C38C 107(3) . . ? O14C C37C C38C 158(3) . . ? C37C O15C Mn4 102(2) . . ? O41A C38C C37C 115(2) 11 . ? C36 O13 Mn4 125.0(4) . . ? C38C O41A C41A 104(3) 12 . ? O41C O41B C41A 67(2) . . ? C41B O41C N19A 93(4) . . ? C41B O41C O41B 140(4) . . ? N19A O41C O41B 119(3) . . ? C41B O41C C41A 110(4) . . ? N19A O41C C41A 133(3) . . ? O41B O41C C41A 68(2) . . ? O41A C41A O41C 110(4) . . ? O41A C41A O41B 67(2) . . ? O41C C41A O41B 45.0(18) . . ? O41C C41B N19A 44(3) . . ? C42A O42 C42B 133(3) . . ? O43B C42B O42 96(4) . . ? C43A O43A C43B 105(7) . . ? C43A O43A O43B 106(7) . . ? C43B O43A O43B 96(5) . . ? O43A O43B C42B 164(5) . . ? O43A C43A C43B 42(4) . . ? O43A C43B C43A 33(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.806 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.077 data_scmn116s _database_code_depnum_ccdc_archive 'CCDC 293109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H132 Cl Mn8 N23 Na2 O39' _chemical_formula_weight 2717.17 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' Na Na 0.0362 0.0249 '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' Cl Cl 0.1484 0.1585 '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 13.7526(6) _cell_length_b 14.1250(7) _cell_length_c 15.6463(7) _cell_angle_alpha 90.093(1) _cell_angle_beta 94.081(1) _cell_angle_gamma 110.122(1) _cell_volume 2845.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5173 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1402 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12204 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10325 _reflns_number_gt 6826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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. The counterion and lattice solvent were badly disordered and could not be successfully refined; they were handled using the SQUEEZE option in PLATON (A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13). 79 electrons were corrected for in an available solvent volume of 325 \%A^3^. These were assigned as a chloride anion (no linear azide could be seen in the difference maps) and 3 methanols (calc. 75 electrons in total), which is consistent with the available solvent volume. ; # SQUEEZE RESULTS (APPEND TO CIF) 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 0.000 0.000 0.005 325.8 78.8 _platon_squeeze_details ; A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13 ; _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^)+(0.1404P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10325 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2138 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 Mn1 Mn 0.16079(6) 0.40705(6) 0.31494(4) 0.0372(2) Uani 1 1 d . A . Mn2 Mn 0.22707(6) 0.22455(6) 0.31686(5) 0.0356(2) Uani 1 1 d . A . Mn3 Mn 0.22821(7) 0.30340(7) 0.13205(4) 0.0401(2) Uani 1 1 d . A . Mn4 Mn 0.43875(6) 0.44489(7) 0.28747(5) 0.0418(2) Uani 1 1 d . A . Na1 Na -0.00577(18) 0.18633(19) 0.20926(13) 0.0495(6) Uani 1 1 d . A . O1 O 0.1847(3) 0.3116(3) 0.24076(19) 0.0344(8) Uani 1 1 d . . . O2 O 0.1815(3) 0.3241(3) 0.40289(19) 0.0348(8) Uani 1 1 d . . . C1 C 0.2207(5) 0.3792(5) 0.4801(3) 0.0438(13) Uani 1 1 d . . . H1A H 0.2944 0.4216 0.4765 0.053 Uiso 1 1 calc R . . H1B H 0.2166 0.3326 0.5280 0.053 Uiso 1 1 calc R . . C2 C 0.1569(5) 0.4448(5) 0.4956(3) 0.0450(13) Uani 1 1 d . . . H2 H 0.0861 0.3986 0.5078 0.054 Uiso 1 1 calc R . . C11 C 0.1965(6) 0.5170(6) 0.5702(4) 0.0652(19) Uani 1 1 d . . . H11A H 0.1451 0.5498 0.5803 0.078 Uiso 1 1 calc R . . H11B H 0.2044 0.4794 0.6221 0.078 Uiso 1 1 calc R . . O5 O 0.2942(5) 0.5928(4) 0.5566(4) 0.0801(15) Uani 1 1 d . . . H5 H 0.3403 0.5663 0.5563 0.120 Uiso 1 1 calc R . . N1 N 0.1459(4) 0.4906(4) 0.4117(2) 0.0442(11) Uani 1 1 d . . . C3 C 0.1296(5) 0.5743(5) 0.4065(4) 0.0552(16) Uani 1 1 d . . . H3 H 0.1212 0.6045 0.4585 0.066 Uiso 1 1 calc R . . C4 C 0.1231(5) 0.6266(5) 0.3288(4) 0.0545(16) Uani 1 1 d . . . C5 C 0.1113(8) 0.7188(6) 0.3374(5) 0.083(3) Uani 1 1 d . . . H5 H 0.1014 0.7415 0.3922 0.099 Uiso 1 1 calc R . . C6 C 0.1137(9) 0.7777(7) 0.2687(5) 0.093(3) Uani 1 1 d . . . H6 H 0.1063 0.8417 0.2754 0.112 Uiso 1 1 calc R . . C7 C 0.1270(7) 0.7446(7) 0.1898(5) 0.080(2) Uani 1 1 d . A . H7 H 0.1293 0.7861 0.1418 0.096 Uiso 1 1 calc R . . C8 C 0.1369(6) 0.6522(6) 0.1791(4) 0.0604(17) Uani 1 1 d . . . C9 C 0.1329(5) 0.5874(5) 0.2476(4) 0.0496(14) Uani 1 1 d . A . O3 O 0.1459(4) 0.5021(3) 0.2337(2) 0.0502(10) Uani 1 1 d . . . O4A O 0.1659(8) 0.6227(7) 0.1052(5) 0.057(2) Uani 0.62 1 d P A 1 C10A C 0.1989(13) 0.6919(12) 0.0391(8) 0.081(4) Uani 0.62 1 d P A 1 H10A H 0.2214 0.6596 -0.0074 0.121 Uiso 0.62 1 calc PR A 1 H10B H 0.2571 0.7510 0.0617 0.121 Uiso 0.62 1 calc PR A 1 H10C H 0.1413 0.7131 0.0171 0.121 Uiso 0.62 1 calc PR A 1 O4B O 0.1188(12) 0.5975(14) 0.0995(11) 0.062(5) Uiso 0.38 1 d P A 2 C10B C 0.122(3) 0.656(3) 0.024(2) 0.129(12) Uiso 0.38 1 d P A 2 H10D H 0.1129 0.6129 -0.0272 0.194 Uiso 0.38 1 calc PR A 2 H10E H 0.1897 0.7109 0.0248 0.194 Uiso 0.38 1 calc PR A 2 H10F H 0.0668 0.6850 0.0227 0.194 Uiso 0.38 1 calc PR A 2 O6 O 0.3732(3) 0.3099(3) 0.3310(2) 0.0407(8) Uani 1 1 d . . . C12 C 0.4368(5) 0.2505(5) 0.3487(4) 0.0481(13) Uani 1 1 d . . . H12A H 0.5076 0.2943 0.3701 0.058 Uiso 1 1 calc R . . H12B H 0.4422 0.2148 0.2957 0.058 Uiso 1 1 calc R . . C13 C 0.3891(4) 0.1754(5) 0.4152(4) 0.0497(14) Uani 1 1 d . . . H13 H 0.4183 0.1196 0.4149 0.060 Uiso 1 1 calc R . . C22 C 0.4112(6) 0.2274(5) 0.5047(4) 0.0610(17) Uani 1 1 d . . . H22A H 0.4872 0.2555 0.5186 0.073 Uiso 1 1 calc R . . H22B H 0.3846 0.2843 0.5036 0.073 Uiso 1 1 calc R . . O9 O 0.3652(4) 0.1613(5) 0.5690(3) 0.0874(18) Uani 1 1 d . . . H9 H 0.4115 0.1482 0.5995 0.131 Uiso 1 1 calc R . . N2 N 0.2758(4) 0.1346(4) 0.3909(3) 0.0425(10) Uani 1 1 d . . . C14 C 0.2210(5) 0.0483(5) 0.4180(3) 0.0485(14) Uani 1 1 d . . . H14 H 0.2567 0.0119 0.4504 0.058 Uiso 1 1 calc R . . C15 C 0.1100(5) 0.0021(4) 0.4033(3) 0.0456(13) Uani 1 1 d . . . C16 C 0.0610(6) -0.0871(5) 0.4459(4) 0.0544(15) Uani 1 1 d . . . H16 H 0.1015 -0.1168 0.4808 0.065 Uiso 1 1 calc R . . C17 C -0.0430(6) -0.1307(5) 0.4375(4) 0.0617(18) Uani 1 1 d . . . H17 H -0.0750 -0.1908 0.4671 0.074 Uiso 1 1 calc R . . C18 C -0.1046(5) -0.0901(5) 0.3867(4) 0.0581(17) Uani 1 1 d . . . H18 H -0.1780 -0.1220 0.3819 0.070 Uiso 1 1 calc R . . C19 C -0.0596(5) -0.0039(5) 0.3435(3) 0.0475(14) Uani 1 1 d . . . C20 C 0.0500(4) 0.0452(4) 0.3518(3) 0.0410(12) Uani 1 1 d . . . O7 O 0.0904(3) 0.1296(3) 0.3095(2) 0.0465(9) Uani 1 1 d . . . O8 O -0.1123(3) 0.0436(4) 0.2921(3) 0.0596(11) Uani 1 1 d . . . C21 C -0.2216(6) 0.0186(8) 0.3025(6) 0.092(3) Uani 1 1 d . . . H21A H -0.2539 -0.0546 0.3072 0.138 Uiso 1 1 calc R . . H21B H -0.2544 0.0411 0.2528 0.138 Uiso 1 1 calc R . . H21C H -0.2306 0.0522 0.3547 0.138 Uiso 1 1 calc R . . O10 O 0.3618(3) 0.3973(3) 0.1570(2) 0.0493(10) Uani 1 1 d . . . C23 C 0.4161(5) 0.4337(6) 0.0822(3) 0.0577(17) Uani 1 1 d . . . H23A H 0.4916 0.4647 0.0979 0.069 Uiso 1 1 calc R . . H23B H 0.3914 0.4853 0.0548 0.069 Uiso 1 1 calc R . . C24 C 0.3946(5) 0.3434(5) 0.0207(4) 0.0553(16) Uani 1 1 d . B . H24 H 0.4117 0.3673 -0.0383 0.066 Uiso 1 1 calc R . . C33 C 0.4559(6) 0.2744(7) 0.0499(4) 0.075(2) Uani 1 1 d . . . O13A O 0.5578(7) 0.3201(11) 0.0334(5) 0.101(4) Uani 0.62 1 d P B 1 H13A H 0.5955 0.3296 0.0795 0.152 Uiso 0.62 1 calc PR B 1 O13B O 0.4381(15) 0.1940(14) -0.0021(9) 0.093(5) Uani 0.38 1 d P B 2 H13B H 0.4025 0.1993 -0.0466 0.139 Uiso 0.38 1 calc PR B 2 N3 N 0.2823(4) 0.2871(4) 0.0216(3) 0.0489(12) Uani 1 1 d . . . C25 C 0.2299(6) 0.2304(5) -0.0432(3) 0.0588(18) Uani 1 1 d . B . H25 H 0.2669 0.2281 -0.0917 0.071 Uiso 1 1 calc R . . C26 C 0.1224(5) 0.1712(5) -0.0486(3) 0.0475(14) Uani 1 1 d . . . C27 C 0.0790(7) 0.1108(5) -0.1250(4) 0.0612(18) Uani 1 1 d . B . H27 H 0.1220 0.1106 -0.1699 0.073 Uiso 1 1 calc R . . C28 C -0.0227(7) 0.0545(5) -0.1334(4) 0.066(2) Uani 1 1 d . . . H28 H -0.0506 0.0152 -0.1845 0.079 Uiso 1 1 calc R B . C29 C -0.0875(6) 0.0525(5) -0.0691(4) 0.0582(17) Uani 1 1 d . B . H29 H -0.1587 0.0114 -0.0758 0.070 Uiso 1 1 calc R . . C30 C -0.0477(5) 0.1113(5) 0.0056(3) 0.0492(14) Uani 1 1 d . . . C31 C 0.0586(5) 0.1686(5) 0.0178(3) 0.0456(13) Uani 1 1 d . B . O11 O 0.0924(3) 0.2179(3) 0.0916(2) 0.0503(10) Uani 1 1 d . . . O12 O -0.1058(3) 0.1159(3) 0.0716(3) 0.0553(11) Uani 1 1 d . A . C32 C -0.2149(5) 0.0622(7) 0.0602(5) 0.077(2) Uani 1 1 d . . . H32A H -0.2444 0.0877 0.0102 0.115 Uiso 1 1 calc R B . H32B H -0.2478 0.0718 0.1114 0.115 Uiso 1 1 calc R . . H32C H -0.2273 -0.0098 0.0510 0.115 Uiso 1 1 calc R . . O14 O 0.3359(3) 0.4938(3) 0.3211(2) 0.0408(8) Uani 1 1 d . . . C34 C 0.3755(4) 0.5971(4) 0.3456(3) 0.0437(13) Uani 1 1 d . A . H34A H 0.4064 0.6051 0.4054 0.052 Uiso 1 1 calc R . . H34B H 0.3183 0.6248 0.3427 0.052 Uiso 1 1 calc R . . C35 C 0.4572(5) 0.6548(5) 0.2868(4) 0.0522(15) Uani 1 1 d . . . H35 H 0.5024 0.7209 0.3138 0.063 Uiso 1 1 calc R A . C44 C 0.4047(7) 0.6698(7) 0.1993(5) 0.077(2) Uani 1 1 d . A . H44A H 0.3640 0.6037 0.1713 0.093 Uiso 1 1 calc R . . H44B H 0.3573 0.7077 0.2074 0.093 Uiso 1 1 calc R . . O17 O 0.4847(6) 0.7242(8) 0.1487(5) 0.138(3) Uani 1 1 d . . . H17A H 0.4603 0.7243 0.0979 0.207 Uiso 1 1 calc R A . N4 N 0.5182(4) 0.5889(4) 0.2718(3) 0.0455(11) Uani 1 1 d . A . C36 C 0.6155(5) 0.6285(6) 0.2610(4) 0.0618(18) Uani 1 1 d . . . H36 H 0.6455 0.7000 0.2650 0.074 Uiso 1 1 calc R A . C37 C 0.6824(5) 0.5737(6) 0.2436(4) 0.0582(17) Uani 1 1 d . A . C38 C 0.7880(6) 0.6270(9) 0.2313(6) 0.096(3) Uani 1 1 d . . . H38 H 0.8134 0.6985 0.2363 0.115 Uiso 1 1 calc R A . C39 C 0.8526(7) 0.5793(11) 0.2128(6) 0.105(4) Uani 1 1 d . A . H39 H 0.9241 0.6167 0.2080 0.126 Uiso 1 1 calc R . . C40 C 0.8162(7) 0.4756(12) 0.2004(6) 0.106(4) Uani 1 1 d . . . H40 H 0.8612 0.4417 0.1843 0.128 Uiso 1 1 calc R A . C41 C 0.7144(7) 0.4229(7) 0.2119(5) 0.073(2) Uani 1 1 d . A . C42 C 0.6457(5) 0.4706(6) 0.2357(4) 0.0582(18) Uani 1 1 d . . . O15 O 0.5501(3) 0.4134(4) 0.2488(3) 0.0567(11) Uani 1 1 d . A . O16 O 0.6764(6) 0.3255(7) 0.1967(5) 0.124(3) Uani 1 1 d . . . C43A C 0.6915(17) 0.2680(17) 0.2559(13) 0.119(6) Uiso 0.62 1 d P A 1 H43A H 0.7658 0.2788 0.2646 0.179 Uiso 0.62 1 calc PR A 1 H43B H 0.6534 0.1974 0.2389 0.179 Uiso 0.62 1 calc PR A 1 H43C H 0.6667 0.2841 0.3094 0.179 Uiso 0.62 1 calc PR A 1 C43B C 0.713(3) 0.239(3) 0.205(2) 0.123(10) Uiso 0.38 1 d P A 2 H43D H 0.7161 0.2211 0.2653 0.185 Uiso 0.38 1 calc PR A 2 H43E H 0.7831 0.2580 0.1843 0.185 Uiso 0.38 1 calc PR A 2 H43F H 0.6659 0.1816 0.1708 0.185 Uiso 0.38 1 calc PR A 2 N11 N 0.5273(4) 0.4802(5) 0.4340(4) 0.0570(13) Uani 1 1 d . . . N12 N 0.5000 0.5000 0.5000 0.0538(19) Uani 1 2 d S . . N13 N -0.0204(3) 0.3249(4) 0.2975(3) 0.0493(13) Uani 1 1 d . . . N14 N -0.0584(4) 0.2976(5) 0.3640(4) 0.0632(15) Uani 1 1 d . A . N15 N -0.0989(6) 0.2775(7) 0.4281(4) 0.094(2) Uani 1 1 d . . . N16 N 0.2604(4) 0.1623(4) 0.1904(3) 0.0396(10) Uani 1 1 d . . . N17 N 0.2977(6) 0.1118(6) 0.1765(4) 0.0770(18) Uani 1 1 d . B . N18A N 0.3236(18) 0.0294(19) 0.1784(15) 0.125(7) Uiso 0.50 1 d P . . N18B N 0.3515(15) 0.0650(16) 0.1502(12) 0.097(5) Uiso 0.50 1 d P B . O18 O 0.1799(5) 0.4308(4) 0.0773(3) 0.0768(15) Uani 1 1 d . . . H18A H 0.1815 0.4793 0.1200 0.092 Uiso 1 1 calc R B 3 C45A C 0.149(3) 0.454(3) -0.002(3) 0.212(17) Uiso 0.50 1 d P B 3 H45A H 0.1424 0.5208 0.0007 0.318 Uiso 0.50 1 calc PR B 3 H45B H 0.0822 0.4035 -0.0214 0.318 Uiso 0.50 1 calc PR B 3 H45C H 0.2012 0.4547 -0.0418 0.318 Uiso 0.50 1 calc PR B 3 C45B C 0.081(2) 0.411(2) 0.0254(16) 0.120(8) Uiso 0.50 1 d P B 4 H45D H 0.0747 0.4755 0.0074 0.181 Uiso 0.50 1 calc PR B 4 H45E H 0.0230 0.3755 0.0596 0.181 Uiso 0.50 1 calc PR B 4 H45F H 0.0793 0.3698 -0.0253 0.181 Uiso 0.50 1 calc PR B 4 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 Mn1 0.0501(5) 0.0399(5) 0.0243(4) -0.0010(3) 0.0013(3) 0.0195(4) Mn2 0.0394(4) 0.0329(5) 0.0311(4) -0.0003(3) -0.0014(3) 0.0087(4) Mn3 0.0457(5) 0.0460(5) 0.0249(4) -0.0056(3) 0.0025(3) 0.0112(4) Mn4 0.0418(5) 0.0418(5) 0.0382(4) -0.0017(3) 0.0056(3) 0.0094(4) Na1 0.0514(13) 0.0525(15) 0.0385(11) -0.0012(9) -0.0023(9) 0.0114(11) O1 0.0439(19) 0.033(2) 0.0233(15) -0.0025(13) -0.0006(13) 0.0109(16) O2 0.046(2) 0.034(2) 0.0239(15) -0.0010(13) -0.0038(14) 0.0151(17) C1 0.049(3) 0.050(4) 0.030(2) 0.001(2) -0.001(2) 0.015(3) C2 0.057(3) 0.053(4) 0.029(2) 0.002(2) 0.005(2) 0.024(3) C11 0.082(5) 0.074(5) 0.042(3) -0.013(3) -0.003(3) 0.033(4) O5 0.088(4) 0.072(4) 0.074(3) -0.014(3) -0.010(3) 0.023(3) N1 0.058(3) 0.058(3) 0.024(2) -0.0035(19) 0.0025(19) 0.029(3) C3 0.074(4) 0.068(5) 0.037(3) -0.003(3) 0.004(3) 0.041(4) C4 0.076(4) 0.056(4) 0.043(3) -0.005(3) -0.001(3) 0.038(4) C5 0.153(8) 0.059(5) 0.056(4) -0.014(3) -0.009(4) 0.065(6) C6 0.168(10) 0.059(5) 0.072(5) -0.011(4) -0.013(5) 0.068(6) C7 0.116(7) 0.080(6) 0.068(5) 0.022(4) 0.010(4) 0.061(6) C8 0.081(5) 0.068(5) 0.041(3) 0.004(3) 0.001(3) 0.038(4) C9 0.060(4) 0.055(4) 0.042(3) 0.003(3) 0.001(3) 0.030(3) O3 0.082(3) 0.050(3) 0.0310(18) 0.0040(16) 0.0051(18) 0.039(2) O4A 0.074(6) 0.068(6) 0.039(4) 0.026(4) 0.020(4) 0.034(5) C10A 0.110(11) 0.092(11) 0.053(7) 0.037(7) 0.029(7) 0.047(9) O6 0.0369(19) 0.045(2) 0.0371(18) 0.0014(15) -0.0015(15) 0.0112(18) C12 0.045(3) 0.048(4) 0.051(3) -0.005(3) -0.002(2) 0.016(3) C13 0.043(3) 0.058(4) 0.048(3) 0.007(3) -0.002(2) 0.018(3) C22 0.072(4) 0.048(4) 0.054(4) 0.005(3) -0.013(3) 0.013(4) O9 0.080(4) 0.109(5) 0.051(3) 0.013(3) -0.007(3) 0.006(4) N2 0.050(3) 0.040(3) 0.034(2) 0.0007(19) -0.0035(19) 0.013(2) C14 0.069(4) 0.047(4) 0.031(3) 0.000(2) -0.004(3) 0.024(3) C15 0.064(4) 0.034(3) 0.033(3) -0.006(2) 0.007(2) 0.010(3) C16 0.072(4) 0.037(4) 0.049(3) -0.001(2) 0.003(3) 0.013(3) C17 0.082(5) 0.038(4) 0.059(4) 0.004(3) 0.020(4) 0.010(4) C18 0.058(4) 0.048(4) 0.055(4) -0.004(3) 0.018(3) 0.000(3) C19 0.055(3) 0.042(3) 0.038(3) -0.009(2) 0.007(2) 0.006(3) C20 0.052(3) 0.035(3) 0.027(2) -0.006(2) 0.004(2) 0.004(3) O7 0.046(2) 0.045(2) 0.0388(19) 0.0062(16) -0.0036(16) 0.0048(19) O8 0.047(2) 0.062(3) 0.058(3) 0.007(2) 0.003(2) 0.005(2) C21 0.054(4) 0.119(8) 0.094(6) 0.025(6) 0.010(4) 0.019(5) O10 0.045(2) 0.061(3) 0.0325(18) -0.0001(17) 0.0079(16) 0.006(2) C23 0.059(4) 0.073(5) 0.031(3) 0.007(3) 0.012(3) 0.008(3) C24 0.065(4) 0.065(5) 0.032(3) -0.001(3) 0.014(3) 0.015(3) C33 0.065(5) 0.115(7) 0.051(4) 0.005(4) 0.016(3) 0.037(5) O13A 0.069(6) 0.184(12) 0.054(5) 0.004(6) 0.009(4) 0.048(7) O13B 0.121(14) 0.113(14) 0.065(9) 0.004(9) 0.034(9) 0.060(12) N3 0.065(3) 0.049(3) 0.031(2) -0.001(2) 0.010(2) 0.017(3) C25 0.097(5) 0.059(4) 0.024(3) 0.000(2) 0.013(3) 0.030(4) C26 0.069(4) 0.042(4) 0.030(3) -0.003(2) -0.001(2) 0.017(3) C27 0.101(6) 0.055(4) 0.030(3) 0.000(3) -0.008(3) 0.034(4) C28 0.104(6) 0.051(4) 0.038(3) -0.015(3) -0.025(3) 0.028(4) C29 0.072(4) 0.045(4) 0.049(3) -0.009(3) -0.021(3) 0.016(3) C30 0.069(4) 0.037(4) 0.040(3) -0.002(2) -0.015(3) 0.020(3) C31 0.064(4) 0.040(3) 0.030(3) -0.006(2) -0.008(2) 0.016(3) O11 0.057(2) 0.057(3) 0.0286(18) -0.0087(16) -0.0020(16) 0.010(2) O12 0.053(2) 0.053(3) 0.049(2) -0.0107(18) -0.0096(19) 0.008(2) C32 0.055(4) 0.082(6) 0.079(5) -0.011(4) -0.008(4) 0.008(4) O14 0.048(2) 0.032(2) 0.0378(18) -0.0071(14) 0.0042(16) 0.0087(18) C34 0.050(3) 0.036(3) 0.039(3) -0.003(2) 0.003(2) 0.007(3) C35 0.060(4) 0.047(4) 0.045(3) 0.006(3) 0.006(3) 0.012(3) C44 0.091(5) 0.093(6) 0.063(4) 0.036(4) 0.017(4) 0.048(5) O17 0.144(6) 0.199(9) 0.095(5) 0.093(6) 0.060(5) 0.080(6) N4 0.046(3) 0.045(3) 0.037(2) 0.004(2) 0.000(2) 0.006(2) C36 0.053(4) 0.070(5) 0.055(4) 0.025(3) 0.003(3) 0.011(3) C37 0.051(4) 0.070(5) 0.046(3) 0.018(3) 0.005(3) 0.011(3) C38 0.044(4) 0.139(9) 0.095(6) 0.059(6) 0.018(4) 0.017(5) C39 0.046(5) 0.170(12) 0.091(6) 0.028(7) 0.018(4) 0.024(6) C40 0.061(6) 0.178(13) 0.091(6) 0.003(7) 0.014(5) 0.053(7) C41 0.073(5) 0.081(6) 0.068(5) -0.018(4) 0.002(4) 0.032(5) C42 0.046(3) 0.095(6) 0.036(3) 0.005(3) 0.005(2) 0.027(4) O15 0.049(2) 0.063(3) 0.056(2) -0.008(2) 0.0105(19) 0.016(2) O16 0.098(5) 0.144(8) 0.153(7) -0.043(6) -0.032(4) 0.080(6) N11 0.055(3) 0.053(3) 0.053(3) -0.006(2) -0.015(3) 0.010(3) N12 0.050(4) 0.061(5) 0.046(4) 0.008(4) -0.009(3) 0.017(4) N13 0.034(2) 0.075(4) 0.027(2) -0.004(2) 0.0055(18) 0.002(2) N14 0.056(3) 0.065(4) 0.072(4) -0.012(3) -0.006(3) 0.027(3) N15 0.101(5) 0.120(7) 0.066(4) 0.011(4) 0.036(4) 0.039(5) N16 0.049(3) 0.042(3) 0.031(2) -0.0016(18) 0.0015(18) 0.019(2) N17 0.082(5) 0.075(5) 0.065(4) -0.026(3) -0.012(3) 0.020(4) O18 0.115(4) 0.075(4) 0.052(3) -0.011(2) -0.009(3) 0.051(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.878(3) . ? Mn1 O3 1.902(4) . ? Mn1 O1 1.905(3) . ? Mn1 N1 1.983(4) . ? Mn1 O14 2.290(4) . ? Mn1 N13 2.354(5) . ? Mn1 Mn2 3.0150(11) . ? Mn1 Na1 3.497(3) . ? Mn2 O7 1.892(4) . ? Mn2 O1 1.915(3) . ? Mn2 O6 1.952(4) . ? Mn2 N2 1.972(4) . ? Mn2 O2 2.214(3) . ? Mn2 N16 2.301(5) . ? Mn2 Mn3 3.0996(10) . ? Mn2 Na1 3.379(2) . ? Mn3 O1 1.859(3) . ? Mn3 O10 1.873(4) . ? Mn3 O11 1.904(4) . ? Mn3 N3 1.974(4) . ? Mn3 O18 2.272(5) . ? Mn3 N16 2.357(5) . ? Mn3 Na1 3.383(2) . ? Mn4 O15 1.873(4) . ? Mn4 O14 1.880(4) . ? Mn4 O6 1.955(4) . ? Mn4 N4 1.975(5) . ? Mn4 O10 2.223(4) . ? Mn4 N11 2.483(5) . ? Na1 O7 2.300(4) . ? Na1 O11 2.314(4) . ? Na1 N13 2.465(6) . ? Na1 O8 2.477(5) . ? Na1 O12 2.480(4) . ? Na1 O1 2.619(4) . ? O2 C1 1.405(6) . ? C1 C2 1.509(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.486(7) . ? C2 C11 1.490(8) . ? C2 H2 1.0000 . ? C11 O5 1.432(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O5 H5 0.8400 . ? N1 C3 1.278(8) . ? C3 C4 1.438(8) . ? C3 H3 0.9500 . ? C4 C5 1.374(9) . ? C4 C9 1.418(8) . ? C5 C6 1.357(10) . ? C5 H5 0.9500 . ? C6 C7 1.365(11) . ? C6 H6 0.9500 . ? C7 C8 1.369(11) . ? C7 H7 0.9500 . ? C8 O4A 1.359(10) . ? C8 C9 1.402(8) . ? C8 O4B 1.42(2) . ? C9 O3 1.298(7) . ? O4A C10A 1.414(12) . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? O4B C10B 1.44(4) . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? O6 C12 1.420(7) . ? C12 C13 1.504(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N2 1.484(7) . ? C13 C22 1.541(9) . ? C13 H13 1.0000 . ? C22 O9 1.404(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O9 H9 0.8400 . ? N2 C14 1.283(7) . ? C14 C15 1.441(9) . ? C14 H14 0.9500 . ? C15 C20 1.397(8) . ? C15 C16 1.403(8) . ? C16 C17 1.346(10) . ? C16 H16 0.9500 . ? C17 C18 1.385(10) . ? C17 H17 0.9500 . ? C18 C19 1.365(8) . ? C18 H18 0.9500 . ? C19 O8 1.370(7) . ? C19 C20 1.423(8) . ? C20 O7 1.329(6) . ? O8 C21 1.443(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O10 C23 1.433(6) . ? C23 C24 1.528(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N3 1.474(8) . ? C24 C33 1.543(11) . ? C24 H24 1.0000 . ? C33 O13B 1.338(18) . ? C33 O13A 1.370(11) . ? O13A H13A 0.8400 . ? O13B H13B 0.8400 . ? N3 C25 1.298(8) . ? C25 C26 1.422(9) . ? C25 H25 0.9500 . ? C26 C31 1.399(8) . ? C26 C27 1.435(8) . ? C27 C28 1.347(11) . ? C27 H27 0.9500 . ? C28 C29 1.385(10) . ? C28 H28 0.9500 . ? C29 C30 1.396(8) . ? C29 H29 0.9500 . ? C30 O12 1.364(7) . ? C30 C31 1.405(9) . ? C31 O11 1.316(6) . ? O12 C32 1.427(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O14 C34 1.413(7) . ? C34 C35 1.513(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N4 1.480(8) . ? C35 C44 1.552(9) . ? C35 H35 1.0000 . ? C44 O17 1.404(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O17 H17A 0.8400 . ? N4 C36 1.285(8) . ? C36 C37 1.431(10) . ? C36 H36 0.9500 . ? C37 C42 1.370(11) . ? C37 C38 1.414(9) . ? C38 C39 1.333(15) . ? C38 H38 0.9500 . ? C39 C40 1.384(16) . ? C39 H39 0.9500 . ? C40 C41 1.366(13) . ? C40 H40 0.9500 . ? C41 O16 1.307(11) . ? C41 C42 1.404(10) . ? C42 O15 1.316(8) . ? O16 C43A 1.286(19) . ? O16 C43B 1.48(3) . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? N11 N12 1.189(6) . ? N12 N11 1.189(6) 2_666 ? N13 N14 1.202(7) . ? N14 N15 1.170(8) . ? N16 N17 1.042(8) . ? N17 N18B 1.24(2) . ? N17 N18A 1.33(2) . ? N18A N18B 0.70(3) . ? O18 C45A 1.36(4) . ? O18 C45B 1.47(2) . ? O18 H18A 0.9500 . ? C45A H45A 0.9800 . ? C45A H45B 0.9800 . ? C45A H45C 0.9800 . ? C45B H45D 0.9800 . ? C45B H45E 0.9800 . ? C45B H45F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O3 174.31(17) . . ? O2 Mn1 O1 84.64(14) . . ? O3 Mn1 O1 100.12(15) . . ? O2 Mn1 N1 83.34(17) . . ? O3 Mn1 N1 91.77(18) . . ? O1 Mn1 N1 167.81(16) . . ? O2 Mn1 O14 90.09(14) . . ? O3 Mn1 O14 87.06(17) . . ? O1 Mn1 O14 87.31(14) . . ? N1 Mn1 O14 90.67(17) . . ? O2 Mn1 N13 94.71(17) . . ? O3 Mn1 N13 88.25(19) . . ? O1 Mn1 N13 92.08(17) . . ? N1 Mn1 N13 90.93(19) . . ? O14 Mn1 N13 175.09(15) . . ? O2 Mn1 Mn2 47.05(10) . . ? O3 Mn1 Mn2 137.25(12) . . ? O1 Mn1 Mn2 38.00(9) . . ? N1 Mn1 Mn2 129.82(13) . . ? O14 Mn1 Mn2 83.51(10) . . ? N13 Mn1 Mn2 98.99(15) . . ? O2 Mn1 Na1 86.76(12) . . ? O3 Mn1 Na1 98.73(14) . . ? O1 Mn1 Na1 47.50(11) . . ? N1 Mn1 Na1 133.46(16) . . ? O14 Mn1 Na1 134.81(10) . . ? N13 Mn1 Na1 44.73(14) . . ? Mn2 Mn1 Na1 62.00(4) . . ? O7 Mn2 O1 90.89(16) . . ? O7 Mn2 O6 173.12(16) . . ? O1 Mn2 O6 95.83(15) . . ? O7 Mn2 N2 90.60(18) . . ? O1 Mn2 N2 177.03(17) . . ? O6 Mn2 N2 82.61(17) . . ? O7 Mn2 O2 90.87(16) . . ? O1 Mn2 O2 75.80(13) . . ? O6 Mn2 O2 92.18(15) . . ? N2 Mn2 O2 106.75(16) . . ? O7 Mn2 N16 91.01(18) . . ? O1 Mn2 N16 82.22(15) . . ? O6 Mn2 N16 88.47(16) . . ? N2 Mn2 N16 95.19(18) . . ? O2 Mn2 N16 157.96(14) . . ? O7 Mn2 Mn1 95.08(13) . . ? O1 Mn2 Mn1 37.76(10) . . ? O6 Mn2 Mn1 91.14(12) . . ? N2 Mn2 Mn1 144.56(14) . . ? O2 Mn2 Mn1 38.39(8) . . ? N16 Mn2 Mn1 119.59(12) . . ? O7 Mn2 Mn3 98.39(11) . . ? O1 Mn2 Mn3 34.20(10) . . ? O6 Mn2 Mn3 86.45(10) . . ? N2 Mn2 Mn3 142.94(14) . . ? O2 Mn2 Mn3 108.97(8) . . ? N16 Mn2 Mn3 49.07(12) . . ? Mn1 Mn2 Mn3 70.60(3) . . ? O7 Mn2 Na1 40.58(12) . . ? O1 Mn2 Na1 50.53(11) . . ? O6 Mn2 Na1 145.92(11) . . ? N2 Mn2 Na1 130.70(15) . . ? O2 Mn2 Na1 85.00(10) . . ? N16 Mn2 Na1 82.21(12) . . ? Mn1 Mn2 Na1 66.03(5) . . ? Mn3 Mn2 Na1 62.79(4) . . ? O1 Mn3 O10 94.82(16) . . ? O1 Mn3 O11 91.14(16) . . ? O10 Mn3 O11 171.68(17) . . ? O1 Mn3 N3 174.47(18) . . ? O10 Mn3 N3 83.73(19) . . ? O11 Mn3 N3 90.87(19) . . ? O1 Mn3 O18 95.64(17) . . ? O10 Mn3 O18 88.2(2) . . ? O11 Mn3 O18 85.4(2) . . ? N3 Mn3 O18 89.65(19) . . ? O1 Mn3 N16 81.85(15) . . ? O10 Mn3 N16 97.15(18) . . ? O11 Mn3 N16 89.43(18) . . ? N3 Mn3 N16 93.02(18) . . ? O18 Mn3 N16 174.20(19) . . ? O1 Mn3 Mn2 35.38(10) . . ? O10 Mn3 Mn2 90.51(11) . . ? O11 Mn3 Mn2 97.71(12) . . ? N3 Mn3 Mn2 139.16(15) . . ? O18 Mn3 Mn2 130.68(13) . . ? N16 Mn3 Mn2 47.53(11) . . ? O1 Mn3 Na1 50.25(12) . . ? O10 Mn3 Na1 145.02(12) . . ? O11 Mn3 Na1 41.04(11) . . ? N3 Mn3 Na1 131.21(16) . . ? O18 Mn3 Na1 93.01(16) . . ? N16 Mn3 Na1 81.36(12) . . ? Mn2 Mn3 Na1 62.65(4) . . ? O15 Mn4 O14 172.44(19) . . ? O15 Mn4 O6 93.00(18) . . ? O14 Mn4 O6 94.56(16) . . ? O15 Mn4 N4 88.6(2) . . ? O14 Mn4 N4 83.94(19) . . ? O6 Mn4 N4 166.49(17) . . ? O15 Mn4 O10 86.15(17) . . ? O14 Mn4 O10 93.86(16) . . ? O6 Mn4 O10 91.90(15) . . ? N4 Mn4 O10 101.59(17) . . ? O15 Mn4 N11 90.17(19) . . ? O14 Mn4 N11 90.44(18) . . ? O6 Mn4 N11 83.35(17) . . ? N4 Mn4 N11 83.24(19) . . ? O10 Mn4 N11 173.84(19) . . ? O7 Na1 O11 103.83(17) . . ? O7 Na1 N13 97.34(17) . . ? O11 Na1 N13 121.39(18) . . ? O7 Na1 O8 66.48(15) . . ? O11 Na1 O8 140.6(2) . . ? N13 Na1 O8 98.02(18) . . ? O7 Na1 O12 134.12(19) . . ? O11 Na1 O12 65.66(15) . . ? N13 Na1 O12 126.94(18) . . ? O8 Na1 O12 93.09(17) . . ? O7 Na1 O1 66.58(13) . . ? O11 Na1 O1 65.68(13) . . ? N13 Na1 O1 74.55(14) . . ? O8 Na1 O1 130.91(15) . . ? O12 Na1 O1 130.67(15) . . ? O7 Na1 Mn2 32.36(10) . . ? O11 Na1 Mn2 82.80(12) . . ? N13 Na1 Mn2 87.78(12) . . ? O8 Na1 Mn2 98.37(12) . . ? O12 Na1 Mn2 141.46(14) . . ? O1 Na1 Mn2 34.36(8) . . ? O7 Na1 Mn3 83.22(11) . . ? O11 Na1 Mn3 32.70(10) . . ? N13 Na1 Mn3 100.10(13) . . ? O8 Na1 Mn3 146.36(14) . . ? O12 Na1 Mn3 98.25(12) . . ? O1 Na1 Mn3 33.08(7) . . ? Mn2 Na1 Mn3 54.56(4) . . ? O7 Na1 Mn1 76.19(12) . . ? O11 Na1 Mn1 91.49(13) . . ? N13 Na1 Mn1 42.23(11) . . ? O8 Na1 Mn1 120.35(13) . . ? O12 Na1 Mn1 144.11(14) . . ? O1 Na1 Mn1 32.43(8) . . ? Mn2 Na1 Mn1 51.97(4) . . ? Mn3 Na1 Mn1 61.79(4) . . ? Mn3 O1 Mn1 139.75(19) . . ? Mn3 O1 Mn2 110.41(17) . . ? Mn1 O1 Mn2 104.24(14) . . ? Mn3 O1 Na1 96.67(14) . . ? Mn1 O1 Na1 100.07(15) . . ? Mn2 O1 Na1 95.11(14) . . ? C1 O2 Mn1 111.5(3) . . ? C1 O2 Mn2 137.3(3) . . ? Mn1 O2 Mn2 94.56(13) . . ? O2 C1 C2 108.4(4) . . ? O2 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O2 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C11 115.6(5) . . ? N1 C2 C1 105.0(4) . . ? C11 C2 C1 114.9(5) . . ? N1 C2 H2 106.9 . . ? C11 C2 H2 106.9 . . ? C1 C2 H2 106.9 . . ? O5 C11 C2 112.0(5) . . ? O5 C11 H11A 109.2 . . ? C2 C11 H11A 109.2 . . ? O5 C11 H11B 109.2 . . ? C2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 O5 H5 109.5 . . ? C3 N1 C2 121.7(5) . . ? C3 N1 Mn1 126.7(4) . . ? C2 N1 Mn1 111.7(4) . . ? N1 C3 C4 125.5(5) . . ? N1 C3 H3 117.2 . . ? C4 C3 H3 117.2 . . ? C5 C4 C9 121.6(6) . . ? C5 C4 C3 116.5(6) . . ? C9 C4 C3 121.9(6) . . ? C6 C5 C4 120.8(7) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.6(7) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 120.8(7) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? O4A C8 C7 122.7(7) . . ? O4A C8 C9 114.7(6) . . ? C7 C8 C9 122.0(6) . . ? O4A C8 O4B 25.7(6) . . ? C7 C8 O4B 124.8(9) . . ? C9 C8 O4B 110.3(9) . . ? O3 C9 C8 119.0(5) . . ? O3 C9 C4 125.7(5) . . ? C8 C9 C4 115.2(6) . . ? C9 O3 Mn1 128.4(3) . . ? C8 O4A C10A 120.3(10) . . ? O4A C10A H10A 109.5 . . ? O4A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? O4A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C8 O4B C10B 116(2) . . ? O4B C10B H10D 109.5 . . ? O4B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? O4B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12 O6 Mn2 110.5(3) . . ? C12 O6 Mn4 117.7(3) . . ? Mn2 O6 Mn4 128.04(18) . . ? O6 C12 C13 108.7(5) . . ? O6 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? O6 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? N2 C13 C12 106.6(4) . . ? N2 C13 C22 110.7(5) . . ? C12 C13 C22 110.2(6) . . ? N2 C13 H13 109.8 . . ? C12 C13 H13 109.8 . . ? C22 C13 H13 109.8 . . ? O9 C22 C13 112.6(6) . . ? O9 C22 H22A 109.1 . . ? C13 C22 H22A 109.1 . . ? O9 C22 H22B 109.1 . . ? C13 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C22 O9 H9 109.5 . . ? C14 N2 C13 119.6(5) . . ? C14 N2 Mn2 127.2(4) . . ? C13 N2 Mn2 113.2(4) . . ? N2 C14 C15 125.5(5) . . ? N2 C14 H14 117.2 . . ? C15 C14 H14 117.2 . . ? C20 C15 C16 119.6(6) . . ? C20 C15 C14 122.4(5) . . ? C16 C15 C14 117.9(6) . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.6(6) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 119.8(6) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 O8 125.1(6) . . ? C18 C19 C20 120.3(6) . . ? O8 C19 C20 114.6(5) . . ? O7 C20 C15 123.3(5) . . ? O7 C20 C19 118.2(5) . . ? C15 C20 C19 118.5(5) . . ? C20 O7 Mn2 130.2(4) . . ? C20 O7 Na1 122.7(4) . . ? Mn2 O7 Na1 107.05(17) . . ? C19 O8 C21 117.1(5) . . ? C19 O8 Na1 116.6(3) . . ? C21 O8 Na1 125.2(5) . . ? O8 C21 H21A 109.5 . . ? O8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 O10 Mn3 113.4(4) . . ? C23 O10 Mn4 120.9(4) . . ? Mn3 O10 Mn4 125.60(17) . . ? O10 C23 C24 107.3(5) . . ? O10 C23 H23A 110.2 . . ? C24 C23 H23A 110.2 . . ? O10 C23 H23B 110.2 . . ? C24 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? N3 C24 C23 105.3(5) . . ? N3 C24 C33 109.5(6) . . ? C23 C24 C33 112.2(6) . . ? N3 C24 H24 109.9 . . ? C23 C24 H24 109.9 . . ? C33 C24 H24 109.9 . . ? O13B C33 O13A 95.8(10) . . ? O13B C33 C24 113.7(9) . . ? O13A C33 C24 108.9(8) . . ? C33 O13A H13A 109.5 . . ? C33 O13B H13B 109.5 . . ? C25 N3 C24 121.6(5) . . ? C25 N3 Mn3 126.1(5) . . ? C24 N3 Mn3 112.2(4) . . ? N3 C25 C26 126.3(5) . . ? N3 C25 H25 116.8 . . ? C26 C25 H25 116.8 . . ? C31 C26 C25 122.7(5) . . ? C31 C26 C27 119.2(6) . . ? C25 C26 C27 118.0(6) . . ? C28 C27 C26 120.1(6) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 121.4(6) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C30 119.7(6) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? O12 C30 C29 124.0(6) . . ? O12 C30 C31 115.6(5) . . ? C29 C30 C31 120.4(6) . . ? O11 C31 C26 123.6(6) . . ? O11 C31 C30 117.5(5) . . ? C26 C31 C30 118.9(5) . . ? C31 O11 Mn3 130.3(4) . . ? C31 O11 Na1 122.4(4) . . ? Mn3 O11 Na1 106.27(16) . . ? C30 O12 C32 117.3(5) . . ? C30 O12 Na1 115.4(3) . . ? C32 O12 Na1 126.0(4) . . ? O12 C32 H32A 109.5 . . ? O12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 O14 Mn4 112.9(3) . . ? C34 O14 Mn1 120.2(3) . . ? Mn4 O14 Mn1 126.61(19) . . ? O14 C34 C35 110.2(5) . . ? O14 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? O14 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? N4 C35 C34 105.5(5) . . ? N4 C35 C44 107.9(5) . . ? C34 C35 C44 110.1(5) . . ? N4 C35 H35 111.1 . . ? C34 C35 H35 111.1 . . ? C44 C35 H35 111.1 . . ? O17 C44 C35 106.9(7) . . ? O17 C44 H44A 110.3 . . ? C35 C44 H44A 110.3 . . ? O17 C44 H44B 110.3 . . ? C35 C44 H44B 110.3 . . ? H44A C44 H44B 108.6 . . ? C44 O17 H17A 109.5 . . ? C36 N4 C35 119.7(6) . . ? C36 N4 Mn4 127.2(5) . . ? C35 N4 Mn4 112.6(4) . . ? N4 C36 C37 125.2(7) . . ? N4 C36 H36 117.4 . . ? C37 C36 H36 117.4 . . ? C42 C37 C38 119.2(8) . . ? C42 C37 C36 121.4(6) . . ? C38 C37 C36 119.4(8) . . ? C39 C38 C37 121.6(11) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 120.3(9) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 118.8(10) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? O16 C41 C40 120.3(9) . . ? O16 C41 C42 117.5(8) . . ? C40 C41 C42 122.2(10) . . ? O15 C42 C37 124.2(6) . . ? O15 C42 C41 117.9(8) . . ? C37 C42 C41 117.8(7) . . ? C42 O15 Mn4 131.5(5) . . ? C43A O16 C41 117.7(12) . . ? C43A O16 C43B 42.0(14) . . ? C41 O16 C43B 137.1(16) . . ? O16 C43A H43A 109.5 . . ? O16 C43A H43B 109.5 . . ? O16 C43A H43C 109.5 . . ? O16 C43B H43D 109.5 . . ? O16 C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? O16 C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? N12 N11 Mn4 131.8(4) . . ? N11 N12 N11 180.000(2) 2_666 . ? N14 N13 Mn1 112.9(4) . . ? N14 N13 Na1 113.4(5) . . ? Mn1 N13 Na1 93.04(18) . . ? N15 N14 N13 174.3(7) . . ? N17 N16 Mn2 133.0(5) . . ? N17 N16 Mn3 140.0(5) . . ? Mn2 N16 Mn3 83.40(17) . . ? N16 N17 N18B 168.5(13) . . ? N16 N17 N18A 160.2(14) . . ? N18B N17 N18A 31.3(11) . . ? N18B N18A N17 67(3) . . ? N18A N18B N17 82(3) . . ? C45A O18 C45B 43.2(17) . . ? C45A O18 Mn3 135.2(19) . . ? C45B O18 Mn3 121.8(11) . . ? C45A O18 H18A 112.4 . . ? C45B O18 H18A 105.4 . . ? Mn3 O18 H18A 112.4 . . ? O18 C45A H45A 109.5 . . ? O18 C45A H45B 109.5 . . ? H45A C45A H45B 109.5 . . ? O18 C45A H45C 109.5 . . ? H45A C45A H45C 109.5 . . ? H45B C45A H45C 109.5 . . ? O18 C45B H45D 109.5 . . ? O18 C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? O18 C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 N11 0.84 2.13 2.967(8) 171.0 2_666 O13A H13A O16 0.84 2.09 2.918(11) 169.7 . O17 H17A O13A 0.84 2.12 2.890(12) 152.4 2_665 O18 H18A O3 0.95 1.93 2.775(6) 146.3 . _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.861 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.110