Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Qiutian Liu' _publ_contact_author_address ; Chinese Academy of Science Fujian Institute of Research on the Structure of Matter Fuzhou 350002 CHINA ; _publ_contact_author_email LQT@MS.FJIRSM.AC.CN _publ_section_title ; Aggregation of Tetranuclear Mn Building Blocks with Alkali Ion. Syntheses, Crystal Structures and Chemical Behaviors of Monomer, Dimer and Polymer Containing [Mn4(?3-O)2]8+ units ; loop_ _publ_author_name 'Qiutian Liu' 'Hui Chen' 'Changneng Chen' 'Deguang Huang' 'Licun Li' ; DaiZheng Liao ; 'Chengbing Ma' 'Xiaofeng Zhang' 'Chunxi Zhang' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 614091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(NBu4)[Mn4O2(AcO)7(pyz)2] 4(C2H5O)' _chemical_formula_sum 'C48 H87 Mn4 N5 O24' _chemical_formula_weight 1337.99 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 11.53670(10) _cell_length_b 12.4167(2) _cell_length_c 23.1596(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.4220(10) _cell_angle_gamma 90.00 _cell_volume 3316.54(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5552 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 24.97 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max .24 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11311 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6047 _reflns_number_gt 4925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+5.8736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(8) _refine_ls_number_reflns 5759 _refine_ls_number_parameters 738 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.291 _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 0.47628(13) 0.67373(12) 0.14978(7) 0.0531(4) Uani 1 1 d . . . Mn2 Mn 0.68013(13) 0.57809(13) 0.05843(7) 0.0522(4) Uani 1 1 d . . . Mn3 Mn 0.44306(12) 0.56100(13) 0.02101(7) 0.0514(4) Uani 1 1 d . . . Mn4 Mn 0.63916(13) 0.63279(11) -0.08087(7) 0.0464(4) Uani 1 1 d . . . O1 O 0.4254(7) 0.7478(6) 0.2186(3) 0.065(2) Uani 1 1 d . . . O2 O 0.3899(10) 0.7359(9) 0.3122(4) 0.105(3) Uani 1 1 d . . . O3 O 0.6516(8) 0.7083(7) 0.1788(4) 0.071(2) Uani 1 1 d . . . O4 O 0.7608(7) 0.5856(7) 0.1332(3) 0.066(2) Uani 1 1 d . . . O5 O 0.4449(7) 0.8038(6) 0.1052(3) 0.068(2) Uani 1 1 d . . . O6 O 0.3954(8) 0.7327(6) 0.0188(3) 0.068(2) Uani 1 1 d . . . O7 O 0.2998(7) 0.6130(6) 0.1405(3) 0.066(2) Uani 1 1 d . . . O8 O 0.2957(7) 0.5240(6) 0.0568(3) 0.064(2) Uani 1 1 d . . . O9 O 0.7071(8) 0.7506(6) 0.0437(3) 0.071(2) Uani 1 1 d . . . O10 O 0.6688(8) 0.7782(6) -0.0513(3) 0.067(2) Uani 1 1 d . . . O11 O 0.8344(7) 0.5508(7) 0.0279(3) 0.070(2) Uani 1 1 d . . . O12 O 0.8129(6) 0.5810(7) -0.0667(3) 0.066(2) Uani 1 1 d . . . O13 O 0.3620(7) 0.5491(6) -0.0535(3) 0.063(2) Uani 1 1 d . . . O14 O 0.4641(7) 0.6635(6) -0.1081(3) 0.0618(19) Uani 1 1 d . . . O15 O 0.6586(8) 0.3972(6) 0.0669(4) 0.066(2) Uani 1 1 d . . . O16 O 0.4823(7) 0.3840(6) 0.0253(3) 0.0612(19) Uani 1 1 d . . . O17 O 0.5292(6) 0.5872(5) 0.0913(3) 0.0497(17) Uani 1 1 d . . . O18 O 0.5928(6) 0.5732(5) -0.0118(3) 0.0459(16) Uani 1 1 d . . . O19 O 0.6870(6) 0.6753(5) -0.1577(3) 0.0531(16) Uani 1 1 d . . . O20 O 0.7342(8) 0.6173(7) -0.2453(3) 0.078(2) Uani 1 1 d . . . O21 O 0.3488(15) 0.2470(14) -0.0584(8) 0.184(7) Uani 1 1 d D . . H21A H 0.3773 0.2881 -0.0342 0.276 Uiso 1 1 calc R . . O22 O 0.6478(17) 0.1319(15) 0.2085(10) 0.225(9) Uani 1 1 d D . . H22A H 0.6622 0.1953 0.2019 0.337 Uiso 1 1 calc R . . O23 O 0.310(2) 0.8146(18) 0.4216(9) 0.230(10) Uani 1 1 d D . . H23A H 0.2809 0.7806 0.3947 0.345 Uiso 1 1 calc R . . O24 O 0.787(2) 0.2956(14) 0.1491(10) 0.239(11) Uani 1 1 d D . . H24A H 0.7535 0.3323 0.1245 0.359 Uiso 1 1 calc R . . N1 N 0.4933(7) 0.5485(7) 0.2110(3) 0.053(2) Uani 1 1 d . . . N2 N 0.5039(10) 0.4116(10) 0.3052(5) 0.081(3) Uani 1 1 d . . . N3 N 0.6147(8) 0.4855(7) -0.1266(4) 0.053(2) Uani 1 1 d . . . N4 N 0.6027(10) 0.3095(8) -0.2008(4) 0.075(3) Uani 1 1 d . . . N5 N 0.7270(8) 0.9659(7) -0.2435(4) 0.066(2) Uani 1 1 d . . . C1 C 0.5271(11) 0.4501(10) 0.2053(5) 0.065(3) Uani 1 1 d . . . H1A H 0.5458 0.4249 0.1689 0.078 Uiso 1 1 calc R . . C2 C 0.5363(11) 0.3798(10) 0.2531(6) 0.073(3) Uani 1 1 d . . . H2B H 0.5652 0.3106 0.2482 0.087 Uiso 1 1 calc R . . C3 C 0.4663(11) 0.5113(12) 0.3093(5) 0.078(4) Uani 1 1 d . . . H3A H 0.4421 0.5351 0.3451 0.093 Uiso 1 1 calc R . . C4 C 0.4607(11) 0.5819(10) 0.2641(4) 0.063(3) Uani 1 1 d . . . C5 C 0.4227(10) 0.6963(10) 0.2669(5) 0.064(3) Uani 1 1 d . . . C6 C 0.7396(13) 0.6536(11) 0.1739(5) 0.067(3) Uani 1 1 d . . . C7 C 0.8353(14) 0.6581(14) 0.2220(6) 0.103(5) Uani 1 1 d . . . H7A H 0.8344 0.7275 0.2403 0.154 Uiso 1 1 calc R . . H7B H 0.9097 0.6464 0.2053 0.154 Uiso 1 1 calc R . . H7C H 0.8213 0.6032 0.2502 0.154 Uiso 1 1 calc R . . C8 C 0.4074(11) 0.8081(9) 0.0520(5) 0.062(3) Uani 1 1 d . . . C9 C 0.3761(16) 0.9204(11) 0.0318(6) 0.100(5) Uani 1 1 d . . . H9A H 0.4196 0.9378 -0.0018 0.150 Uiso 1 1 calc R . . H9B H 0.3941 0.9711 0.0620 0.150 Uiso 1 1 calc R . . H9C H 0.2947 0.9235 0.0223 0.150 Uiso 1 1 calc R . . C10 C 0.2546(10) 0.5521(10) 0.1053(4) 0.056(3) Uani 1 1 d . . . C11 C 0.1387(11) 0.5062(12) 0.1190(5) 0.080(4) Uani 1 1 d . . . H11A H 0.1429 0.4721 0.1562 0.120 Uiso 1 1 calc R . . H11B H 0.1165 0.4541 0.0902 0.120 Uiso 1 1 calc R . . H11C H 0.0822 0.5630 0.1195 0.120 Uiso 1 1 calc R . . C12 C 0.6954(10) 0.8086(9) 0.0000(5) 0.062(3) Uani 1 1 d . . . C13 C 0.7153(16) 0.9280(10) 0.0065(6) 0.107(5) Uani 1 1 d . . . H13A H 0.6670 0.9557 0.0363 0.160 Uiso 1 1 calc R . . H13B H 0.6964 0.9634 -0.0293 0.160 Uiso 1 1 calc R . . H13C H 0.7952 0.9410 0.0168 0.160 Uiso 1 1 calc R . . C14 C 0.8734(11) 0.5620(10) -0.0232(5) 0.063(3) Uani 1 1 d . . . C15 C 1.0022(13) 0.5459(15) -0.0274(6) 0.103(5) Uani 1 1 d . . . H15A H 1.0246 0.5565 -0.0667 0.154 Uiso 1 1 calc R . . H15B H 1.0221 0.4741 -0.0154 0.154 Uiso 1 1 calc R . . H15C H 1.0421 0.5969 -0.0029 0.154 Uiso 1 1 calc R . . C16 C 0.3735(11) 0.6126(12) -0.0970(5) 0.067(3) Uani 1 1 d . . . C17 C 0.2710(14) 0.6208(19) -0.1358(7) 0.133(8) Uani 1 1 d . . . H17A H 0.2954 0.6256 -0.1751 0.200 Uiso 1 1 calc R . . H17B H 0.2274 0.6839 -0.1263 0.200 Uiso 1 1 calc R . . H17C H 0.2233 0.5581 -0.1315 0.200 Uiso 1 1 calc R . . C18 C 0.5762(13) 0.3446(9) 0.0436(5) 0.063(3) Uani 1 1 d . . . C19 C 0.5924(13) 0.2234(10) 0.0365(8) 0.099(5) Uani 1 1 d . . . H19A H 0.5182 0.1884 0.0370 0.148 Uiso 1 1 calc R . . H19B H 0.6407 0.1964 0.0676 0.148 Uiso 1 1 calc R . . H19C H 0.6284 0.2091 0.0003 0.148 Uiso 1 1 calc R . . C20 C 0.5733(11) 0.3931(8) -0.1094(5) 0.061(3) Uani 1 1 d . . . H20A H 0.5494 0.3856 -0.0715 0.074 Uiso 1 1 calc R . . C21 C 0.5645(12) 0.3065(10) -0.1468(5) 0.075(3) Uani 1 1 d . . . H21B H 0.5305 0.2433 -0.1338 0.090 Uiso 1 1 calc R . . C22 C 0.6474(10) 0.4032(9) -0.2168(5) 0.061(3) Uani 1 1 d . . . H22B H 0.6758 0.4090 -0.2539 0.073 Uiso 1 1 calc R . . C23 C 0.6538(9) 0.4932(8) -0.1808(4) 0.047(2) Uani 1 1 d . . . C24 C 0.6946(11) 0.6019(9) -0.1972(4) 0.057(3) Uani 1 1 d . . . C25 C 0.6204(11) 0.9373(9) -0.2063(5) 0.073(3) Uani 1 1 d . . . H25A H 0.5555 0.9210 -0.2322 0.088 Uiso 1 1 calc R . . H25B H 0.6385 0.8723 -0.1847 0.088 Uiso 1 1 calc R . . C26 C 0.5830(15) 1.0210(11) -0.1650(6) 0.094(4) Uani 1 1 d . . . H26A H 0.5554 1.0835 -0.1864 0.113 Uiso 1 1 calc R . . H26B H 0.6489 1.0431 -0.1411 0.113 Uiso 1 1 calc R . . C27 C 0.4887(16) 0.9812(13) -0.1271(7) 0.102(5) Uani 1 1 d . . . H27A H 0.5165 0.9179 -0.1065 0.122 Uiso 1 1 calc R . . H27B H 0.4728 1.0362 -0.0986 0.122 Uiso 1 1 calc R . . C28 C 0.380(2) 0.954(2) -0.1576(11) 0.182(11) Uani 1 1 d . . . H28A H 0.3247 0.9290 -0.1304 0.272 Uiso 1 1 calc R . . H28B H 0.3943 0.8980 -0.1853 0.272 Uiso 1 1 calc R . . H28C H 0.3503 1.0164 -0.1772 0.272 Uiso 1 1 calc R . . C29 C 0.7417(11) 0.8691(9) -0.2824(5) 0.074(3) Uani 1 1 d . . . H29A H 0.6707 0.8596 -0.3051 0.089 Uiso 1 1 calc R . . H29B H 0.7515 0.8058 -0.2582 0.089 Uiso 1 1 calc R . . C30 C 0.8420(15) 0.8741(14) -0.3233(7) 0.105(5) Uani 1 1 d . . . H30A H 0.9147 0.8768 -0.3013 0.126 Uiso 1 1 calc R . . H30B H 0.8360 0.9387 -0.3467 0.126 Uiso 1 1 calc R . . C31 C 0.8399(18) 0.7735(16) -0.3626(8) 0.122(6) Uani 1 1 d . . . H31A H 0.9148 0.7653 -0.3802 0.147 Uiso 1 1 calc R . . H31B H 0.8258 0.7100 -0.3395 0.147 Uiso 1 1 calc R . . C32 C 0.750(2) 0.7825(18) -0.4079(9) 0.146(8) Uani 1 1 d . . . H32A H 0.7498 0.7189 -0.4315 0.218 Uiso 1 1 calc R . . H32B H 0.7645 0.8444 -0.4314 0.218 Uiso 1 1 calc R . . H32C H 0.6753 0.7901 -0.3906 0.218 Uiso 1 1 calc R . . C33 C 0.7042(13) 1.0690(9) -0.2783(6) 0.077(3) Uani 1 1 d . . . H33A H 0.6878 1.1266 -0.2514 0.092 Uiso 1 1 calc R . . H33B H 0.7748 1.0880 -0.2977 0.092 Uiso 1 1 calc R . . C34 C 0.6063(13) 1.0647(11) -0.3231(7) 0.093(4) Uani 1 1 d . . . H34A H 0.6208 1.0073 -0.3504 0.112 Uiso 1 1 calc R . . H34B H 0.5339 1.0491 -0.3043 0.112 Uiso 1 1 calc R . . C35 C 0.5961(16) 1.1700(12) -0.3547(7) 0.099(5) Uani 1 1 d . . . H35A H 0.6698 1.1865 -0.3719 0.118 Uiso 1 1 calc R . . H35B H 0.5795 1.2266 -0.3272 0.118 Uiso 1 1 calc R . . C36 C 0.502(2) 1.1697(17) -0.4018(8) 0.155(8) Uani 1 1 d . . . H36A H 0.4999 1.2387 -0.4205 0.233 Uiso 1 1 calc R . . H36B H 0.4285 1.1554 -0.3850 0.233 Uiso 1 1 calc R . . H36C H 0.5188 1.1149 -0.4296 0.233 Uiso 1 1 calc R . . C37 C 0.8333(13) 0.9873(11) -0.2065(6) 0.082(4) Uani 1 1 d . . . H37A H 0.8193 1.0512 -0.1835 0.098 Uiso 1 1 calc R . . H37B H 0.8969 1.0035 -0.2317 0.098 Uiso 1 1 calc R . . C38 C 0.8719(13) 0.8970(12) -0.1657(6) 0.090(4) Uani 1 1 d . . . H38A H 0.8116 0.8835 -0.1382 0.108 Uiso 1 1 calc R . . H38B H 0.8832 0.8316 -0.1877 0.108 Uiso 1 1 calc R . . C39 C 0.9807(16) 0.9246(16) -0.1342(8) 0.120(6) Uani 1 1 d . . . H39A H 0.9701 0.9930 -0.1148 0.144 Uiso 1 1 calc R . . H39B H 1.0412 0.9343 -0.1621 0.144 Uiso 1 1 calc R . . C40 C 1.021(2) 0.844(2) -0.0909(10) 0.177(11) Uani 1 1 d . . . H40A H 1.0913 0.8689 -0.0724 0.266 Uiso 1 1 calc R . . H40B H 1.0346 0.7767 -0.1097 0.266 Uiso 1 1 calc R . . H40C H 0.9625 0.8349 -0.0624 0.266 Uiso 1 1 calc R . . C41 C 0.2415(18) 0.292(2) -0.0810(14) 0.233(18) Uani 1 1 d D . . H41A H 0.2558 0.3612 -0.0985 0.279 Uiso 1 1 calc R . . H41B H 0.1875 0.3016 -0.0500 0.279 Uiso 1 1 calc R . . C42 C 0.193(3) 0.218(4) -0.1236(15) 0.32(3) Uani 1 1 d D . . H42A H 0.1206 0.2461 -0.1383 0.481 Uiso 1 1 calc R . . H42B H 0.1807 0.1492 -0.1061 0.481 Uiso 1 1 calc R . . H42C H 0.2459 0.2106 -0.1548 0.481 Uiso 1 1 calc R . . C43 C 0.726(3) 0.0644(18) 0.1774(11) 0.30(3) Uani 1 1 d D . . H43A H 0.8063 0.0733 0.1903 0.365 Uiso 1 1 calc R . . H43B H 0.7194 0.0742 0.1359 0.365 Uiso 1 1 calc R . . C44 C 0.673(3) -0.0426(17) 0.1977(14) 0.256(19) Uani 1 1 d D . . H44A H 0.7138 -0.1018 0.1808 0.384 Uiso 1 1 calc R . . H44B H 0.5928 -0.0455 0.1859 0.384 Uiso 1 1 calc R . . H44C H 0.6798 -0.0473 0.2390 0.384 Uiso 1 1 calc R . . C45 C 0.382(3) 0.744(3) 0.4560(14) 0.26(2) Uani 1 1 d D . . H45A H 0.4433 0.7151 0.4328 0.306 Uiso 1 1 calc R . . H45B H 0.3363 0.6851 0.4703 0.306 Uiso 1 1 calc R . . C46 C 0.434(3) 0.807(4) 0.5058(13) 0.34(3) Uani 1 1 d D . . H46A H 0.4809 0.7606 0.5295 0.513 Uiso 1 1 calc R . . H46B H 0.3724 0.8367 0.5284 0.513 Uiso 1 1 calc R . . H46C H 0.4802 0.8649 0.4913 0.513 Uiso 1 1 calc R . . C47 C 0.886(2) 0.348(2) 0.1678(16) 0.27(2) Uani 1 1 d D . . H47A H 0.8665 0.4216 0.1769 0.321 Uiso 1 1 calc R . . H47B H 0.9402 0.3490 0.1365 0.321 Uiso 1 1 calc R . . C48 C 0.942(2) 0.299(3) 0.2178(12) 0.217(15) Uani 1 1 d D . . H48A H 1.0057 0.3432 0.2306 0.326 Uiso 1 1 calc R . . H48B H 0.9701 0.2287 0.2078 0.326 Uiso 1 1 calc R . . H48C H 0.8873 0.2925 0.2482 0.326 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0635(11) 0.0562(9) 0.0398(8) -0.0039(7) 0.0019(7) 0.0026(8) Mn2 0.0559(10) 0.0647(9) 0.0359(7) 0.0014(7) -0.0004(7) 0.0013(8) Mn3 0.0563(10) 0.0604(9) 0.0377(8) -0.0045(7) 0.0031(7) -0.0038(8) Mn4 0.0593(10) 0.0434(7) 0.0363(7) -0.0007(6) 0.0002(6) -0.0031(7) O1 0.072(5) 0.074(5) 0.048(4) -0.009(4) 0.000(4) 0.009(4) O2 0.149(9) 0.116(8) 0.051(5) -0.014(5) 0.023(5) 0.032(7) O3 0.065(6) 0.085(6) 0.064(5) -0.016(4) 0.003(4) -0.010(5) O4 0.070(6) 0.086(5) 0.042(4) -0.002(4) -0.011(4) 0.005(4) O5 0.093(6) 0.054(4) 0.057(5) -0.004(3) 0.006(4) -0.002(4) O6 0.089(6) 0.059(4) 0.056(4) -0.006(4) -0.007(4) 0.015(4) O7 0.067(5) 0.074(5) 0.056(5) -0.015(4) 0.007(4) -0.004(4) O8 0.055(5) 0.079(5) 0.058(4) -0.011(4) 0.010(4) -0.013(4) O9 0.100(7) 0.064(5) 0.048(4) 0.005(4) -0.008(4) -0.023(4) O10 0.107(6) 0.049(4) 0.044(4) -0.003(3) -0.003(4) -0.004(4) O11 0.059(5) 0.102(6) 0.049(4) 0.004(4) 0.007(4) 0.003(4) O12 0.045(4) 0.108(6) 0.044(4) 0.003(4) -0.002(3) 0.003(4) O13 0.062(5) 0.085(5) 0.042(4) -0.009(4) -0.006(3) -0.010(4) O14 0.053(5) 0.074(5) 0.058(4) 0.001(4) -0.005(4) 0.008(4) O15 0.073(6) 0.067(5) 0.059(4) 0.006(4) -0.003(4) 0.004(4) O16 0.068(6) 0.060(4) 0.057(4) 0.000(4) 0.010(4) 0.000(4) O17 0.053(5) 0.058(4) 0.038(3) -0.005(3) 0.004(3) -0.006(3) O18 0.043(4) 0.056(4) 0.038(3) -0.001(3) -0.005(3) -0.009(3) O19 0.071(5) 0.050(4) 0.039(3) -0.002(3) 0.004(3) -0.011(3) O20 0.111(7) 0.082(6) 0.041(4) 0.006(4) 0.011(4) -0.012(5) O21 0.171(16) 0.197(16) 0.185(15) -0.047(13) 0.034(12) -0.043(13) O22 0.199(18) 0.171(17) 0.31(3) -0.003(17) 0.006(17) 0.004(14) O23 0.24(3) 0.24(2) 0.21(2) -0.015(18) 0.071(19) 0.054(19) O24 0.26(3) 0.144(14) 0.31(3) 0.110(16) -0.10(2) -0.023(15) N1 0.055(5) 0.062(5) 0.042(4) 0.004(4) 0.003(4) 0.006(4) N2 0.080(8) 0.105(9) 0.058(6) 0.024(6) -0.001(5) 0.003(7) N3 0.065(6) 0.051(5) 0.042(4) -0.005(4) -0.001(4) 0.005(4) N4 0.108(8) 0.056(6) 0.061(6) -0.016(5) 0.011(5) -0.001(6) N5 0.069(6) 0.056(5) 0.073(6) 0.000(5) 0.009(5) -0.012(5) C1 0.068(8) 0.078(8) 0.047(6) 0.005(6) -0.003(5) 0.001(6) C2 0.064(8) 0.070(7) 0.083(9) 0.008(7) -0.004(7) 0.002(6) C3 0.078(9) 0.097(10) 0.058(7) 0.015(7) 0.000(6) 0.014(8) C4 0.067(8) 0.080(8) 0.040(5) -0.001(5) -0.002(5) -0.003(6) C5 0.060(7) 0.086(8) 0.046(6) -0.001(6) 0.005(5) 0.004(6) C6 0.074(9) 0.086(9) 0.041(6) 0.002(6) 0.006(6) -0.015(7) C7 0.085(11) 0.159(15) 0.064(8) -0.026(9) -0.027(7) 0.006(10) C8 0.076(8) 0.060(7) 0.050(6) 0.001(5) 0.010(6) 0.009(6) C9 0.155(15) 0.072(9) 0.075(9) 0.005(7) 0.017(9) 0.031(9) C10 0.054(7) 0.076(7) 0.038(5) 0.007(5) 0.002(5) 0.009(5) C11 0.070(8) 0.116(11) 0.055(7) 0.004(7) 0.002(6) -0.016(8) C12 0.063(7) 0.057(6) 0.068(7) -0.003(6) 0.010(6) -0.003(5) C13 0.170(17) 0.061(8) 0.088(10) -0.016(7) -0.010(10) -0.022(9) C14 0.059(8) 0.085(8) 0.046(6) -0.007(5) 0.004(5) 0.003(6) C15 0.082(10) 0.173(16) 0.054(7) 0.003(9) 0.002(7) 0.011(10) C16 0.046(7) 0.106(9) 0.048(6) -0.009(7) -0.017(5) 0.021(7) C17 0.060(9) 0.25(2) 0.087(10) 0.056(13) -0.020(8) -0.011(12) C18 0.071(9) 0.063(7) 0.057(7) 0.006(6) 0.018(6) 0.001(6) C19 0.114(14) 0.059(8) 0.125(11) -0.010(8) 0.035(10) 0.009(7) C20 0.088(8) 0.048(6) 0.049(6) -0.002(5) 0.008(5) -0.001(6) C21 0.097(9) 0.059(7) 0.070(8) -0.009(6) 0.017(7) -0.016(6) C22 0.069(8) 0.071(7) 0.042(5) 0.000(5) 0.008(5) 0.009(6) C23 0.057(6) 0.051(5) 0.032(4) -0.003(4) -0.004(4) 0.010(5) C24 0.074(8) 0.057(6) 0.040(6) 0.002(5) -0.008(5) 0.005(6) C25 0.094(9) 0.050(6) 0.077(8) 0.009(6) 0.012(7) -0.001(6) C26 0.137(13) 0.068(8) 0.078(9) -0.012(7) 0.024(9) 0.011(8) C27 0.127(14) 0.088(10) 0.091(10) 0.002(8) 0.031(10) 0.010(10) C28 0.16(2) 0.23(3) 0.16(2) -0.06(2) 0.044(18) -0.01(2) C29 0.086(9) 0.061(7) 0.075(8) -0.011(6) 0.016(7) -0.002(6) C30 0.103(12) 0.114(12) 0.100(11) -0.003(9) 0.034(9) 0.005(10) C31 0.133(16) 0.128(15) 0.108(14) -0.013(11) 0.044(12) 0.024(13) C32 0.19(2) 0.140(17) 0.105(14) -0.016(13) 0.022(15) -0.008(16) C33 0.085(10) 0.059(7) 0.085(9) 0.004(6) 0.002(7) -0.005(6) C34 0.088(10) 0.077(9) 0.114(12) 0.010(8) -0.014(9) -0.013(8) C35 0.116(13) 0.086(10) 0.094(11) 0.018(8) -0.005(9) -0.003(9) C36 0.20(2) 0.152(18) 0.113(14) 0.031(13) -0.042(14) -0.024(16) C37 0.094(11) 0.074(8) 0.077(8) 0.000(6) -0.007(7) -0.021(7) C38 0.086(10) 0.101(11) 0.083(9) 0.004(8) 0.000(8) 0.008(8) C39 0.111(14) 0.138(15) 0.110(13) 0.013(11) -0.025(11) -0.004(11) C40 0.19(3) 0.20(3) 0.133(19) -0.013(17) -0.050(18) 0.07(2) C41 0.065(14) 0.39(5) 0.24(3) -0.11(3) -0.015(17) -0.03(2) C42 0.18(3) 0.57(8) 0.20(3) -0.05(4) -0.05(3) -0.04(4) C43 0.50(6) 0.12(2) 0.27(4) -0.11(2) -0.25(4) 0.15(3) C44 0.33(5) 0.12(2) 0.31(5) -0.08(2) -0.06(4) 0.02(2) C45 0.16(3) 0.37(5) 0.24(4) 0.14(4) 0.01(3) 0.04(3) C46 0.15(3) 0.71(11) 0.16(3) -0.01(4) -0.01(2) 0.13(4) C47 0.15(3) 0.17(3) 0.48(7) 0.11(3) -0.13(3) -0.03(2) C48 0.13(2) 0.27(4) 0.25(3) 0.09(3) -0.04(2) -0.02(2) _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 O17 1.845(7) . ? Mn1 O1 1.944(7) . ? Mn1 O5 1.946(8) . ? Mn1 N1 2.110(8) . ? Mn1 O3 2.159(9) . ? Mn1 O7 2.176(8) . ? Mn2 O18 1.894(7) . ? Mn2 O17 1.920(7) . ? Mn2 O4 1.948(7) . ? Mn2 O11 1.961(8) . ? Mn2 O9 2.193(8) . ? Mn2 O15 2.268(8) . ? Mn2 Mn3 2.8563(19) . ? Mn3 O18 1.911(7) . ? Mn3 O17 1.913(7) . ? Mn3 O13 1.948(7) . ? Mn3 O8 1.964(8) . ? Mn3 O6 2.202(8) . ? Mn3 O16 2.246(8) . ? Mn4 O18 1.853(7) . ? Mn4 O19 1.948(7) . ? Mn4 O10 1.958(7) . ? Mn4 O12 2.123(8) . ? Mn4 N3 2.128(8) . ? Mn4 O14 2.135(8) . ? O1 C5 1.290(13) . ? O2 C5 1.227(13) . ? O3 C6 1.228(16) . ? O4 C6 1.294(14) . ? O5 C8 1.296(13) . ? O6 C8 1.219(13) . ? O7 C10 1.220(13) . ? O8 C10 1.278(13) . ? O9 C12 1.246(13) . ? O10 C12 1.277(13) . ? O11 C14 1.282(13) . ? O12 C14 1.235(13) . ? O13 C16 1.289(15) . ? O14 C16 1.253(15) . ? O15 C18 1.263(16) . ? O16 C18 1.253(16) . ? O19 C24 1.296(12) . ? O20 C24 1.231(13) . ? O21 C41 1.443(18) . ? O21 H21A 0.8200 . ? O22 C43 1.439(18) . ? O22 H22A 0.8200 . ? O23 C45 1.429(18) . ? O23 H23A 0.8200 . ? O24 C47 1.370(17) . ? O24 H24A 0.8200 . ? N1 C1 1.290(14) . ? N1 C4 1.360(13) . ? N2 C3 1.317(17) . ? N2 C2 1.331(17) . ? N3 C20 1.308(13) . ? N3 C23 1.349(12) . ? N4 C22 1.328(15) . ? N4 C21 1.337(15) . ? N5 C37 1.503(17) . ? N5 C29 1.514(14) . ? N5 C33 1.533(15) . ? N5 C25 1.559(14) . ? C1 C2 1.412(17) . ? C1 H1A 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.365(16) . ? C3 H3A 0.9300 . ? C4 C5 1.489(17) . ? C6 C7 1.550(18) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.511(16) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.495(17) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.507(16) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.505(18) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.472(17) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.526(16) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.384(15) . ? C20 H20A 0.9300 . ? C21 H21B 0.9300 . ? C22 C23 1.396(14) . ? C22 H22B 0.9300 . ? C23 C24 1.481(15) . ? C25 C26 1.483(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.50(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.46(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.515(18) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.55(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.46(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.516(18) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.502(19) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.52(2) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.525(19) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.48(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.48(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.446(19) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.542(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.50(2) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.445(18) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O17 Mn1 O1 171.9(3) . . ? O17 Mn1 O5 98.9(3) . . ? O1 Mn1 O5 89.2(3) . . ? O17 Mn1 N1 92.1(3) . . ? O1 Mn1 N1 79.8(3) . . ? O5 Mn1 N1 168.8(3) . . ? O17 Mn1 O3 91.1(3) . . ? O1 Mn1 O3 87.2(3) . . ? O5 Mn1 O3 99.2(3) . . ? N1 Mn1 O3 82.3(3) . . ? O17 Mn1 O7 93.0(3) . . ? O1 Mn1 O7 86.8(3) . . ? O5 Mn1 O7 94.2(3) . . ? N1 Mn1 O7 83.3(3) . . ? O3 Mn1 O7 165.2(3) . . ? O18 Mn2 O17 82.8(3) . . ? O18 Mn2 O4 176.3(4) . . ? O17 Mn2 O4 93.6(3) . . ? O18 Mn2 O11 98.7(3) . . ? O17 Mn2 O11 173.2(3) . . ? O4 Mn2 O11 84.9(3) . . ? O18 Mn2 O9 88.4(3) . . ? O17 Mn2 O9 97.9(3) . . ? O4 Mn2 O9 91.4(3) . . ? O11 Mn2 O9 88.8(4) . . ? O18 Mn2 O15 89.1(3) . . ? O17 Mn2 O15 85.5(3) . . ? O4 Mn2 O15 91.3(3) . . ? O11 Mn2 O15 87.8(3) . . ? O9 Mn2 O15 175.5(3) . . ? O18 Mn2 Mn3 41.6(2) . . ? O17 Mn2 Mn3 41.7(2) . . ? O4 Mn2 Mn3 134.9(3) . . ? O11 Mn2 Mn3 138.4(3) . . ? O9 Mn2 Mn3 99.4(3) . . ? O15 Mn2 Mn3 81.2(2) . . ? O18 Mn3 O17 82.5(3) . . ? O18 Mn3 O13 94.1(3) . . ? O17 Mn3 O13 173.8(3) . . ? O18 Mn3 O8 170.7(3) . . ? O17 Mn3 O8 96.8(3) . . ? O13 Mn3 O8 87.4(3) . . ? O18 Mn3 O6 98.2(3) . . ? O17 Mn3 O6 88.8(3) . . ? O13 Mn3 O6 86.5(3) . . ? O8 Mn3 O6 91.0(3) . . ? O18 Mn3 O16 84.9(3) . . ? O17 Mn3 O16 91.6(3) . . ? O13 Mn3 O16 93.3(3) . . ? O8 Mn3 O16 85.9(3) . . ? O6 Mn3 O16 176.9(3) . . ? O18 Mn3 Mn2 41.1(2) . . ? O17 Mn3 Mn2 41.9(2) . . ? O13 Mn3 Mn2 135.2(2) . . ? O8 Mn3 Mn2 136.2(2) . . ? O6 Mn3 Mn2 99.9(2) . . ? O16 Mn3 Mn2 82.5(2) . . ? O18 Mn4 O19 172.1(3) . . ? O18 Mn4 O10 96.8(3) . . ? O19 Mn4 O10 91.1(3) . . ? O18 Mn4 O12 92.1(3) . . ? O19 Mn4 O12 86.3(3) . . ? O10 Mn4 O12 94.0(4) . . ? O18 Mn4 N3 92.7(3) . . ? O19 Mn4 N3 79.4(3) . . ? O10 Mn4 N3 170.5(3) . . ? O12 Mn4 N3 85.9(3) . . ? O18 Mn4 O14 92.0(3) . . ? O19 Mn4 O14 88.3(3) . . ? O10 Mn4 O14 95.4(3) . . ? O12 Mn4 O14 169.2(3) . . ? N3 Mn4 O14 83.9(3) . . ? C5 O1 Mn1 119.4(7) . . ? C6 O3 Mn1 129.1(8) . . ? C6 O4 Mn2 125.8(8) . . ? C8 O5 Mn1 126.3(7) . . ? C8 O6 Mn3 134.8(7) . . ? C10 O7 Mn1 131.6(7) . . ? C10 O8 Mn3 130.5(8) . . ? C12 O9 Mn2 132.7(7) . . ? C12 O10 Mn4 129.4(7) . . ? C14 O11 Mn2 131.0(8) . . ? C14 O12 Mn4 134.1(7) . . ? C16 O13 Mn3 126.1(7) . . ? C16 O14 Mn4 129.6(7) . . ? C18 O15 Mn2 123.9(8) . . ? C18 O16 Mn3 124.7(8) . . ? Mn1 O17 Mn3 123.3(4) . . ? Mn1 O17 Mn2 130.2(4) . . ? Mn3 O17 Mn2 96.3(3) . . ? Mn4 O18 Mn2 124.8(4) . . ? Mn4 O18 Mn3 131.2(4) . . ? Mn2 O18 Mn3 97.3(3) . . ? C24 O19 Mn4 118.7(6) . . ? C41 O21 H21A 109.5 . . ? C43 O22 H22A 109.5 . . ? C45 O23 H23A 109.5 . . ? C47 O24 H24A 109.5 . . ? C1 N1 C4 118.1(9) . . ? C1 N1 Mn1 130.8(7) . . ? C4 N1 Mn1 111.1(7) . . ? C3 N2 C2 116.4(11) . . ? C20 N3 C23 118.6(8) . . ? C20 N3 Mn4 130.3(7) . . ? C23 N3 Mn4 111.0(7) . . ? C22 N4 C21 115.2(9) . . ? C37 N5 C29 112.2(10) . . ? C37 N5 C33 106.2(9) . . ? C29 N5 C33 111.7(9) . . ? C37 N5 C25 111.7(10) . . ? C29 N5 C25 104.5(8) . . ? C33 N5 C25 110.7(9) . . ? N1 C1 C2 121.6(11) . . ? N1 C1 H1A 119.2 . . ? C2 C1 H1A 119.2 . . ? N2 C2 C1 120.6(12) . . ? N2 C2 H2B 119.7 . . ? C1 C2 H2B 119.7 . . ? N2 C3 C4 123.9(12) . . ? N2 C3 H3A 118.1 . . ? C4 C3 H3A 118.1 . . ? N1 C4 C3 119.3(12) . . ? N1 C4 C5 114.7(9) . . ? C3 C4 C5 125.9(11) . . ? O2 C5 O1 123.9(12) . . ? O2 C5 C4 121.1(11) . . ? O1 C5 C4 114.9(9) . . ? O3 C6 O4 126.8(12) . . ? O3 C6 C7 119.3(12) . . ? O4 C6 C7 113.7(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O6 C8 O5 126.8(10) . . ? O6 C8 C9 119.3(11) . . ? O5 C8 C9 113.9(10) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C10 O8 126.5(11) . . ? O7 C10 C11 117.7(10) . . ? O8 C10 C11 115.8(11) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O10 127.0(10) . . ? O9 C12 C13 118.3(11) . . ? O10 C12 C13 114.6(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O12 C14 O11 124.7(11) . . ? O12 C14 C15 120.7(10) . . ? O11 C14 C15 114.6(10) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O14 C16 O13 124.9(10) . . ? O14 C16 C17 120.1(13) . . ? O13 C16 C17 115.0(13) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O16 C18 O15 125.3(11) . . ? O16 C18 C19 117.1(13) . . ? O15 C18 C19 117.6(13) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 120.8(10) . . ? N3 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? N4 C21 C20 122.9(11) . . ? N4 C21 H21B 118.6 . . ? C20 C21 H21B 118.6 . . ? N4 C22 C23 123.4(10) . . ? N4 C22 H22B 118.3 . . ? C23 C22 H22B 118.3 . . ? N3 C23 C22 119.0(9) . . ? N3 C23 C24 114.8(8) . . ? C22 C23 C24 126.1(9) . . ? O20 C24 O19 124.3(10) . . ? O20 C24 C23 120.1(9) . . ? O19 C24 C23 115.6(9) . . ? C26 C25 N5 116.3(10) . . ? C26 C25 H25A 108.2 . . ? N5 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? N5 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C27 112.0(12) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 114.7(16) . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 116.0(11) . . ? N5 C29 H29A 108.3 . . ? C30 C29 H29A 108.3 . . ? N5 C29 H29B 108.3 . . ? C30 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 109.6(13) . . ? C29 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? C29 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? C32 C31 C30 111.2(16) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N5 116.5(10) . . ? C34 C33 H33A 108.2 . . ? N5 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? N5 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? C35 C34 C33 110.5(12) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 113.2(14) . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C38 116.4(11) . . ? N5 C37 H37A 108.2 . . ? C38 C37 H37A 108.2 . . ? N5 C37 H37B 108.2 . . ? C38 C37 H37B 108.2 . . ? H37A C37 H37B 107.3 . . ? C39 C38 C37 111.5(13) . . ? C39 C38 H38A 109.3 . . ? C37 C38 H38A 109.3 . . ? C39 C38 H38B 109.3 . . ? C37 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C40 115.2(18) . . ? C38 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? C38 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O21 C41 C42 109(2) . . ? O21 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O21 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O22 C43 C44 95.2(17) . . ? O22 C43 H43A 112.7 . . ? C44 C43 H43A 112.7 . . ? O22 C43 H43B 112.7 . . ? C44 C43 H43B 112.7 . . ? H43A C43 H43B 110.2 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O23 C45 C46 109(2) . . ? O23 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? O23 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O24 C47 C48 114(2) . . ? O24 C47 H47A 108.7 . . ? C48 C47 H47A 108.7 . . ? O24 C47 H47B 108.7 . . ? C48 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 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 O21 H21A O16 0.82 2.17 2.979(18) 169.6 . O24 H24A O15 0.82 1.89 2.698(18) 170.4 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.502 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.066 #==END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 614092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4O2(AcO)7(pyz)2(CH3CN)K.2CH3CN]n' _chemical_formula_sum 'C30 H36 K Mn4 N7 O20' _chemical_formula_weight 1073.52 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' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.34030(10) _cell_length_b 14.87040(10) _cell_length_c 26.4903(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8800.32(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 25.07 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max .78 _exptl_crystal_size_mid .66 _exptl_crystal_size_min .42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352 _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7347 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 43703 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.07 _reflns_number_total 7783 _reflns_number_gt 5879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+17.0454P] 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 7783 _refine_ls_number_parameters 564 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.220 _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 0.10930(3) 0.87620(5) 0.39640(2) 0.03813(17) Uani 1 1 d . A . Mn2 Mn 0.10461(3) 0.73926(4) 0.29360(2) 0.03337(16) Uani 1 1 d . A . Mn3 Mn 0.10229(3) 0.92656(4) 0.27589(2) 0.03243(16) Uani 1 1 d . . . Mn4 Mn 0.19331(3) 0.80374(4) 0.20069(2) 0.03488(16) Uani 1 1 d . A . K1 K -0.00438(5) 0.56884(8) 0.29110(4) 0.0575(3) Uani 1 1 d . . . O1 O 0.11852(15) 0.9030(2) 0.46694(12) 0.0524(8) Uani 1 1 d . A . O2 O 0.0719(2) 0.9243(3) 0.54039(14) 0.0829(13) Uani 1 1 d . A . O3 O 0.12521(15) 0.7359(2) 0.41279(12) 0.0499(8) Uani 1 1 d . A . O4 O 0.08262(14) 0.6605(2) 0.34899(11) 0.0443(7) Uani 1 1 d . A . O5 O 0.07753(16) 1.0147(2) 0.38631(12) 0.0512(8) Uani 1 1 d . . . O6 O 0.05946(14) 1.0299(2) 0.30421(11) 0.0443(7) Uani 1 1 d . . . O7 O 0.19280(14) 0.9058(2) 0.38410(12) 0.0517(8) Uani 1 1 d . . . O8 O 0.18622(14) 0.9687(2) 0.30772(12) 0.0487(8) Uani 1 1 d . . . O9 O 0.17209(15) 0.6611(2) 0.19320(12) 0.0478(8) Uani 1 1 d . A . O10 O 0.10234(14) 0.62989(19) 0.25063(12) 0.0469(8) Uani 1 1 d . A . O11 O 0.20567(14) 0.9458(2) 0.19245(12) 0.0465(8) Uani 1 1 d . . . O12 O 0.11883(13) 1.00408(19) 0.21869(11) 0.0404(7) Uani 1 1 d . . . O13 O 0.25231(13) 0.7776(2) 0.25278(12) 0.0466(8) Uani 1 1 d . . . O14 O 0.19588(14) 0.7103(2) 0.31142(12) 0.0491(8) Uani 1 1 d . . . O15 O 0.00871(14) 0.7501(2) 0.27076(12) 0.0465(8) Uani 1 1 d . A . O16 O 0.01067(14) 0.8935(2) 0.24493(12) 0.0455(8) Uani 1 1 d . . . O17 O 0.09026(12) 0.84764(18) 0.33043(10) 0.0329(6) Uani 1 1 d . . . O18 O 0.12848(12) 0.81998(17) 0.24296(10) 0.0328(6) Uani 1 1 d . . . O19 O 0.25230(14) 0.7862(2) 0.14935(11) 0.0452(8) Uani 1 1 d . . . O20 O 0.26850(19) 0.7536(4) 0.06906(15) 0.0952(15) Uani 1 1 d . . . N1 N 0.02146(18) 0.8545(3) 0.42117(14) 0.0447(9) Uani 1 1 d . . . N2 N -0.0892(2) 0.8460(4) 0.4676(2) 0.0781(15) Uani 1 1 d . A . N3 N 0.13917(16) 0.8119(2) 0.13635(13) 0.0380(8) Uani 1 1 d . . . N4 N 0.0819(2) 0.8008(4) 0.04391(17) 0.0681(13) Uani 1 1 d . A . C1 C -0.0268(2) 0.8291(4) 0.39589(19) 0.0550(13) Uani 1 1 d . A . H1A H -0.0237 0.8139 0.3619 0.066 Uiso 1 1 calc R . . C2 C -0.0816(3) 0.8252(4) 0.4195(2) 0.0704(16) Uani 1 1 d . . . H2B H -0.1147 0.8071 0.4008 0.085 Uiso 1 1 calc R A . C3 C -0.0404(3) 0.8715(4) 0.4925(2) 0.0708(16) Uani 1 1 d . . . H3A H -0.0438 0.8872 0.5264 0.085 Uiso 1 1 calc R A . C4 C 0.0150(2) 0.8756(3) 0.46996(17) 0.0498(12) Uani 1 1 d . A . C5 C 0.0718(3) 0.9032(3) 0.49629(19) 0.0551(13) Uani 1 1 d . . . C6 C 0.1044(2) 0.6666(3) 0.39391(18) 0.0443(11) Uani 1 1 d . . . C7 C 0.1038(3) 0.5823(4) 0.4247(2) 0.0690(16) Uani 1 1 d . A . H7A H 0.1429 0.5723 0.4387 0.103 Uiso 1 1 calc R . . H7B H 0.0931 0.5323 0.4036 0.103 Uiso 1 1 calc R . . H7C H 0.0752 0.5880 0.4515 0.103 Uiso 1 1 calc R . . C8 C 0.0548(2) 1.0543(3) 0.35000(17) 0.0412(11) Uani 1 1 d . . . C9 C 0.0188(3) 1.1383(3) 0.3591(2) 0.0615(15) Uani 1 1 d . . . H9A H -0.0135 1.1252 0.3819 0.092 Uiso 1 1 calc R . . H9B H 0.0028 1.1596 0.3276 0.092 Uiso 1 1 calc R . . H9C H 0.0441 1.1837 0.3735 0.092 Uiso 1 1 calc R . . C10 C 0.2143(2) 0.9452(3) 0.3456(2) 0.0470(12) Uani 1 1 d . . . C11 C 0.2802(2) 0.9653(5) 0.3468(3) 0.081(2) Uani 1 1 d . . . H11A H 0.2993 0.9377 0.3183 0.122 Uiso 1 1 calc R . . H11B H 0.2972 0.9418 0.3774 0.122 Uiso 1 1 calc R . . H11C H 0.2862 1.0291 0.3456 0.122 Uiso 1 1 calc R . . C12 C 0.1343(2) 0.6109(3) 0.21250(17) 0.0438(11) Uani 1 1 d . . . C13 C 0.1247(3) 0.5197(4) 0.1894(3) 0.087(2) Uani 1 1 d . A . H13A H 0.1210 0.5256 0.1535 0.131 Uiso 1 1 calc R . . H13B H 0.0888 0.4936 0.2029 0.131 Uiso 1 1 calc R . . H13C H 0.1582 0.4817 0.1972 0.131 Uiso 1 1 calc R . . C14 C 0.1697(2) 1.0086(3) 0.19585(17) 0.0393(10) Uani 1 1 d . . . C15 C 0.1836(3) 1.0973(3) 0.1719(2) 0.0605(14) Uani 1 1 d . . . H15A H 0.2262 1.1055 0.1706 0.091 Uiso 1 1 calc R . . H15B H 0.1659 1.1447 0.1915 0.091 Uiso 1 1 calc R . . H15C H 0.1675 1.0986 0.1383 0.091 Uiso 1 1 calc R . . C16 C 0.2445(2) 0.7306(3) 0.29261(17) 0.0401(10) Uani 1 1 d . A . C17 C 0.3006(2) 0.6951(4) 0.3172(2) 0.0652(15) Uani 1 1 d . . . H17A H 0.2900 0.6583 0.3456 0.098 Uiso 1 1 calc R A . H17B H 0.3248 0.7445 0.3283 0.098 Uiso 1 1 calc R . . H17C H 0.3226 0.6597 0.2932 0.098 Uiso 1 1 calc R . . C18 C -0.0153(2) 0.8184(3) 0.25187(18) 0.0462(12) Uani 1 1 d . . . C19 C -0.0793(3) 0.8107(5) 0.2355(3) 0.095(2) Uani 1 1 d . A . H19A H -0.0844 0.7570 0.2159 0.142 Uiso 1 1 calc R . . H19B H -0.0898 0.8621 0.2155 0.142 Uiso 1 1 calc R . . H19C H -0.1046 0.8081 0.2647 0.142 Uiso 1 1 calc R . . C20 C 0.0811(2) 0.8285(3) 0.13240(18) 0.0462(11) Uani 1 1 d . A . H20A H 0.0591 0.8435 0.1610 0.055 Uiso 1 1 calc R . . C21 C 0.0534(2) 0.8237(4) 0.0861(2) 0.0570(13) Uani 1 1 d . . . H21A H 0.0128 0.8370 0.0842 0.068 Uiso 1 1 calc R A . C22 C 0.1404(3) 0.7847(4) 0.04857(19) 0.0670(16) Uani 1 1 d . . . H22A H 0.1623 0.7695 0.0199 0.080 Uiso 1 1 calc R A . C23 C 0.1696(2) 0.7899(3) 0.09437(17) 0.0474(12) Uani 1 1 d . A . C24 C 0.2356(2) 0.7743(3) 0.1034(2) 0.0541(13) Uani 1 1 d . A . C25 C -0.0558(6) 0.5745(8) 0.4292(3) 0.152(4) Uani 1 1 d D . . N5 N -0.0412(5) 0.5401(9) 0.3922(4) 0.071(3) Uiso 0.50 1 d PD A 1 C26 C -0.0923(12) 0.6058(19) 0.4751(9) 0.120(9) Uiso 0.35 1 d PD A 1 N5' N -0.0507(6) 0.5773(10) 0.3881(4) 0.080(4) Uiso 0.50 1 d PD A 2 C26' C -0.0541(11) 0.5912(15) 0.4855(6) 0.098(6) Uiso 0.40 1 d PD A 2 C26" C -0.0286(16) 0.633(2) 0.4760(12) 0.112(11) Uiso 0.25 1 d PD A 3 C27 C -0.3471(4) 0.2128(8) 0.5666(3) 0.125(3) Uani 1 1 d D . . N6 N -0.3901(6) 0.1817(11) 0.5828(6) 0.113(6) Uiso 0.70 1 d PD B 1 C28 C -0.2918(8) 0.2725(15) 0.5501(8) 0.112(6) Uiso 0.45 1 d PD B 1 N6' N -0.3933(11) 0.210(3) 0.5814(16) 0.134(17) Uiso 0.30 1 d PD B 2 C28' C -0.2848(7) 0.2173(13) 0.5457(6) 0.111(5) Uiso 0.55 1 d PD B 2 C30 C -0.2913(4) 0.5067(9) 0.4394(5) 0.155(4) Uani 1 1 d D . . N7 N -0.239(3) 0.500(5) 0.515(3) 0.21(3) Uiso 0.19 1 d PD C 1 C29 C -0.279(3) 0.476(4) 0.4934(12) 0.17(2) Uiso 0.20 1 d PD C 1 N7' N -0.1807(7) 0.4966(10) 0.4587(6) 0.206(6) Uiso 0.81 1 d PD C 2 C29' C -0.2321(6) 0.4982(10) 0.4623(6) 0.141(5) Uiso 0.80 1 d PD C 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 0.0429(4) 0.0419(4) 0.0296(3) -0.0005(3) -0.0032(3) -0.0029(3) Mn2 0.0376(3) 0.0288(3) 0.0337(3) 0.0001(3) 0.0050(3) -0.0045(3) Mn3 0.0375(3) 0.0294(3) 0.0304(3) 0.0005(3) 0.0012(3) 0.0021(3) Mn4 0.0345(3) 0.0344(3) 0.0357(3) 0.0032(3) 0.0069(3) 0.0020(3) K1 0.0613(7) 0.0537(7) 0.0574(7) -0.0098(5) 0.0045(5) -0.0257(6) O1 0.062(2) 0.063(2) 0.0322(17) -0.0032(15) -0.0060(16) -0.0076(17) O2 0.099(3) 0.111(4) 0.038(2) -0.016(2) 0.003(2) -0.015(3) O3 0.063(2) 0.0452(19) 0.0421(18) 0.0053(15) -0.0060(16) 0.0004(17) O4 0.0506(19) 0.0412(17) 0.0412(18) 0.0072(14) 0.0050(15) -0.0098(15) O5 0.075(2) 0.0395(18) 0.0390(18) -0.0047(15) -0.0055(17) 0.0075(17) O6 0.058(2) 0.0382(17) 0.0368(17) -0.0029(14) 0.0016(14) 0.0114(15) O7 0.0422(19) 0.062(2) 0.051(2) 0.0060(17) -0.0104(15) -0.0077(16) O8 0.0485(19) 0.0497(19) 0.0479(19) 0.0075(15) -0.0072(16) -0.0142(15) O9 0.055(2) 0.0362(17) 0.052(2) -0.0006(15) 0.0191(16) -0.0013(15) O10 0.056(2) 0.0369(16) 0.0482(18) -0.0065(14) 0.0175(15) -0.0106(15) O11 0.0435(18) 0.0362(17) 0.060(2) 0.0019(15) 0.0110(15) -0.0036(15) O12 0.0438(18) 0.0374(16) 0.0399(17) 0.0086(13) 0.0047(14) 0.0040(14) O13 0.0363(17) 0.0521(19) 0.0514(19) 0.0116(16) 0.0010(15) -0.0020(14) O14 0.0401(18) 0.054(2) 0.053(2) 0.0168(16) 0.0058(15) 0.0043(15) O15 0.0429(18) 0.0451(19) 0.0513(19) -0.0064(15) -0.0025(15) -0.0074(15) O16 0.0412(18) 0.0505(19) 0.0448(18) 0.0015(15) -0.0037(14) 0.0047(15) O17 0.0381(16) 0.0330(15) 0.0276(14) -0.0015(12) 0.0004(12) -0.0019(12) O18 0.0360(15) 0.0298(14) 0.0325(15) 0.0003(12) 0.0051(12) 0.0002(12) O19 0.0424(18) 0.0492(19) 0.0439(19) 0.0052(15) 0.0143(14) 0.0058(15) O20 0.073(3) 0.157(5) 0.056(2) -0.008(3) 0.027(2) 0.023(3) N1 0.052(2) 0.045(2) 0.037(2) 0.0004(17) 0.0036(18) -0.0010(19) N2 0.071(3) 0.101(4) 0.062(3) -0.007(3) 0.017(3) -0.009(3) N3 0.043(2) 0.037(2) 0.0341(19) 0.0033(15) 0.0065(16) -0.0026(16) N4 0.068(3) 0.089(4) 0.047(3) 0.004(2) -0.005(2) -0.006(3) C1 0.055(3) 0.068(4) 0.042(3) -0.001(2) 0.002(2) -0.003(3) C2 0.056(3) 0.085(4) 0.071(4) -0.008(3) 0.001(3) -0.007(3) C3 0.076(4) 0.090(4) 0.046(3) -0.005(3) 0.019(3) -0.002(4) C4 0.067(3) 0.048(3) 0.035(2) 0.002(2) 0.005(2) -0.002(2) C5 0.073(4) 0.053(3) 0.039(3) 0.000(2) 0.005(3) 0.000(3) C6 0.042(3) 0.045(3) 0.046(3) 0.005(2) 0.010(2) 0.004(2) C7 0.101(5) 0.048(3) 0.058(3) 0.015(3) 0.006(3) 0.004(3) C8 0.051(3) 0.031(2) 0.042(3) -0.002(2) 0.003(2) 0.000(2) C9 0.087(4) 0.046(3) 0.052(3) -0.005(2) 0.009(3) 0.019(3) C10 0.042(3) 0.038(3) 0.060(3) -0.003(2) -0.003(2) -0.008(2) C11 0.046(3) 0.093(5) 0.104(5) 0.027(4) -0.013(3) -0.017(3) C12 0.053(3) 0.035(2) 0.043(3) -0.005(2) 0.007(2) 0.002(2) C13 0.114(5) 0.053(4) 0.095(5) -0.027(3) 0.044(4) -0.019(4) C14 0.045(3) 0.033(2) 0.040(2) 0.0011(19) -0.004(2) -0.004(2) C15 0.067(4) 0.042(3) 0.072(4) 0.013(3) 0.008(3) -0.008(3) C16 0.041(3) 0.036(2) 0.043(3) -0.002(2) -0.002(2) 0.000(2) C17 0.049(3) 0.077(4) 0.070(4) 0.021(3) -0.008(3) 0.001(3) C18 0.036(3) 0.059(3) 0.043(3) -0.017(2) -0.004(2) -0.001(2) C19 0.045(3) 0.100(5) 0.139(7) -0.027(5) -0.027(4) -0.003(3) C20 0.047(3) 0.049(3) 0.043(3) 0.004(2) 0.005(2) 0.004(2) C21 0.055(3) 0.063(3) 0.053(3) 0.007(3) -0.005(3) -0.005(3) C22 0.069(4) 0.094(4) 0.038(3) -0.002(3) 0.009(3) -0.005(3) C23 0.059(3) 0.045(3) 0.038(3) 0.002(2) 0.008(2) -0.002(2) C24 0.055(3) 0.056(3) 0.051(3) 0.005(2) 0.019(3) 0.004(2) C25 0.228(13) 0.147(9) 0.082(6) 0.002(6) 0.024(7) -0.019(9) C27 0.117(7) 0.183(10) 0.074(5) -0.001(6) -0.020(5) 0.019(7) C30 0.093(7) 0.192(11) 0.180(11) -0.001(9) 0.012(7) 0.008(7) _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 O17 1.848(3) . ? Mn1 O1 1.922(3) . ? Mn1 O7 1.944(3) . ? Mn1 N1 2.094(4) . ? Mn1 O3 2.161(3) . ? Mn1 O5 2.194(3) . ? Mn2 O18 1.877(3) . ? Mn2 O17 1.911(3) . ? Mn2 O4 1.941(3) . ? Mn2 O10 1.986(3) . ? Mn2 O14 2.137(3) . ? Mn2 O15 2.232(3) . ? Mn2 Mn3 2.8249(8) . ? Mn2 K1 3.5150(12) . ? Mn3 O17 1.881(3) . ? Mn3 O18 1.901(3) . ? Mn3 O12 1.940(3) . ? Mn3 O6 1.959(3) . ? Mn3 O8 2.149(3) . ? Mn3 O16 2.259(3) . ? Mn3 K1 3.5228(12) 3 ? Mn4 O18 1.847(3) . ? Mn4 O19 1.912(3) . ? Mn4 O13 1.947(3) . ? Mn4 N3 2.093(4) . ? Mn4 O11 2.142(3) . ? Mn4 O9 2.182(3) . ? K1 O12 2.745(3) 3_545 ? K1 O15 2.764(3) . ? K1 O10 2.767(3) . ? K1 N5' 2.772(12) . ? K1 O16 2.780(3) 3_545 ? K1 O4 2.826(3) . ? K1 N5 2.834(12) . ? K1 O6 2.868(3) 3_545 ? K1 Mn3 3.5228(12) 3_545 ? O1 C5 1.302(6) . ? O2 C5 1.210(6) . ? O3 C6 1.236(6) . ? O4 C6 1.288(6) . ? O5 C8 1.238(5) . ? O6 C8 1.271(5) . ? O6 K1 2.868(3) 3 ? O7 C10 1.270(6) . ? O8 C10 1.234(6) . ? O9 C12 1.238(5) . ? O10 C12 1.268(5) . ? O11 C14 1.236(5) . ? O12 C14 1.289(5) . ? O12 K1 2.745(3) 3 ? O13 C16 1.278(5) . ? O14 C16 1.233(5) . ? O15 C18 1.254(6) . ? O16 C18 1.272(6) . ? O16 K1 2.780(3) 3 ? O19 C24 1.286(6) . ? O20 C24 1.209(6) . ? N1 C1 1.324(6) . ? N1 C4 1.338(6) . ? N2 C2 1.323(7) . ? N2 C3 1.330(8) . ? N3 C20 1.324(6) . ? N3 C23 1.344(6) . ? N4 C21 1.330(7) . ? N4 C22 1.334(7) . ? C1 C2 1.376(7) . ? C1 H1A 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.375(7) . ? C3 H3A 0.9300 . ? C4 C5 1.504(7) . ? C6 C7 1.495(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.504(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.503(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.503(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.495(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.507(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.497(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.376(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.379(7) . ? C22 H22A 0.9300 . ? C23 C24 1.512(7) . ? C25 N5' 1.095(12) . ? C25 N5 1.152(12) . ? C25 C26' 1.513(15) . ? C25 C26 1.538(17) . ? C25 C26" 1.630(18) . ? C27 N6' 1.106(19) . ? C27 N6 1.150(12) . ? C27 C28' 1.499(14) . ? C27 C28 1.583(16) . ? C30 C29' 1.459(13) . ? C30 C29 1.53(2) . ? N7 C29 1.13(2) . ? N7' C29' 1.154(13) . ? 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 O17 Mn1 O1 172.68(14) . . ? O17 Mn1 O7 96.56(13) . . ? O1 Mn1 O7 90.75(14) . . ? O17 Mn1 N1 92.59(14) . . ? O1 Mn1 N1 80.09(15) . . ? O7 Mn1 N1 170.58(15) . . ? O17 Mn1 O3 90.34(12) . . ? O1 Mn1 O3 89.28(14) . . ? O7 Mn1 O3 95.43(14) . . ? N1 Mn1 O3 86.70(14) . . ? O17 Mn1 O5 91.49(12) . . ? O1 Mn1 O5 87.62(13) . . ? O7 Mn1 O5 94.44(14) . . ? N1 Mn1 O5 83.09(14) . . ? O3 Mn1 O5 169.70(13) . . ? O18 Mn2 O17 82.71(11) . . ? O18 Mn2 O4 176.39(13) . . ? O17 Mn2 O4 94.62(12) . . ? O18 Mn2 O10 96.97(12) . . ? O17 Mn2 O10 168.25(13) . . ? O4 Mn2 O10 86.14(13) . . ? O18 Mn2 O14 90.89(12) . . ? O17 Mn2 O14 102.53(13) . . ? O4 Mn2 O14 87.31(13) . . ? O10 Mn2 O14 89.21(14) . . ? O18 Mn2 O15 91.88(12) . . ? O17 Mn2 O15 85.21(12) . . ? O4 Mn2 O15 90.31(13) . . ? O10 Mn2 O15 83.06(13) . . ? O14 Mn2 O15 172.05(13) . . ? O18 Mn2 Mn3 41.94(8) . . ? O17 Mn2 Mn3 41.43(8) . . ? O4 Mn2 Mn3 135.72(10) . . ? O10 Mn2 Mn3 135.38(10) . . ? O14 Mn2 Mn3 104.64(9) . . ? O15 Mn2 Mn3 82.32(9) . . ? O18 Mn2 K1 130.11(9) . . ? O17 Mn2 K1 120.10(9) . . ? O4 Mn2 K1 53.40(10) . . ? O10 Mn2 K1 51.76(9) . . ? O14 Mn2 K1 121.34(9) . . ? O15 Mn2 K1 51.83(9) . . ? Mn3 Mn2 K1 134.03(3) . . ? O17 Mn3 O18 82.89(11) . . ? O17 Mn3 O12 176.70(13) . . ? O18 Mn3 O12 94.49(12) . . ? O17 Mn3 O6 97.21(12) . . ? O18 Mn3 O6 168.41(13) . . ? O12 Mn3 O6 85.76(12) . . ? O17 Mn3 O8 90.29(12) . . ? O18 Mn3 O8 98.88(13) . . ? O12 Mn3 O8 88.11(12) . . ? O6 Mn3 O8 92.71(13) . . ? O17 Mn3 O16 90.80(12) . . ? O18 Mn3 O16 86.05(12) . . ? O12 Mn3 O16 91.04(12) . . ? O6 Mn3 O16 82.36(13) . . ? O8 Mn3 O16 175.05(12) . . ? O17 Mn3 Mn2 42.25(8) . . ? O18 Mn3 Mn2 41.30(8) . . ? O12 Mn3 Mn2 135.42(9) . . ? O6 Mn3 Mn2 135.94(10) . . ? O8 Mn3 Mn2 101.90(9) . . ? O16 Mn3 Mn2 82.10(8) . . ? O17 Mn3 K1 132.31(9) . 3 ? O18 Mn3 K1 117.42(9) . 3 ? O12 Mn3 K1 50.78(9) . 3 ? O6 Mn3 K1 54.46(9) . 3 ? O8 Mn3 K1 124.35(9) . 3 ? O16 Mn3 K1 52.06(8) . 3 ? Mn2 Mn3 K1 133.41(3) . 3 ? O18 Mn4 O19 171.87(14) . . ? O18 Mn4 O13 97.32(13) . . ? O19 Mn4 O13 90.58(13) . . ? O18 Mn4 N3 91.89(13) . . ? O19 Mn4 N3 80.03(14) . . ? O13 Mn4 N3 168.37(14) . . ? O18 Mn4 O11 91.94(12) . . ? O19 Mn4 O11 88.47(13) . . ? O13 Mn4 O11 100.47(13) . . ? N3 Mn4 O11 86.24(13) . . ? O18 Mn4 O9 90.68(12) . . ? O19 Mn4 O9 87.27(13) . . ? O13 Mn4 O9 91.02(13) . . ? N3 Mn4 O9 81.76(13) . . ? O11 Mn4 O9 167.79(13) . . ? O12 K1 O15 114.98(10) 3_545 . ? O12 K1 O10 151.78(10) 3_545 . ? O15 K1 O10 60.89(9) . . ? O12 K1 N5' 75.9(3) 3_545 . ? O15 K1 N5' 100.1(3) . . ? O10 K1 N5' 131.7(3) . . ? O12 K1 O16 65.88(9) 3_545 3_545 ? O15 K1 O16 148.53(10) . 3_545 ? O10 K1 O16 102.60(10) . 3_545 ? N5' K1 O16 110.0(3) . 3_545 ? O12 K1 O4 149.45(10) 3_545 . ? O15 K1 O4 64.07(9) . . ? O10 K1 O4 57.28(9) . . ? N5' K1 O4 74.5(3) . . ? O16 K1 O4 132.33(10) 3_545 . ? O12 K1 N5 76.4(2) 3_545 . ? O15 K1 N5 111.2(3) . . ? O10 K1 N5 131.8(3) . . ? N5' K1 N5 12.3(3) . . ? O16 K1 N5 99.7(3) 3_545 . ? O4 K1 N5 76.1(2) . . ? O12 K1 O6 56.37(9) 3_545 3_545 ? O15 K1 O6 94.05(9) . 3_545 ? O10 K1 O6 95.44(10) . 3_545 ? N5' K1 O6 131.7(3) . 3_545 ? O16 K1 O6 59.11(9) 3_545 3_545 ? O4 K1 O6 150.48(9) . 3_545 ? N5 K1 O6 132.6(2) . 3_545 ? O12 K1 Mn2 154.17(8) 3_545 . ? O15 K1 Mn2 39.41(7) . . ? O10 K1 Mn2 34.31(6) . . ? N5' K1 Mn2 102.0(3) . . ? O16 K1 Mn2 135.86(8) 3_545 . ? O4 K1 Mn2 33.46(6) . . ? N5 K1 Mn2 107.0(2) . . ? O6 K1 Mn2 117.35(7) 3_545 . ? O12 K1 Mn3 33.20(6) 3_545 3_545 ? O15 K1 Mn3 123.58(8) . 3_545 ? O10 K1 Mn3 122.46(7) . 3_545 ? N5' K1 Mn3 105.2(3) . 3_545 ? O16 K1 Mn3 39.86(7) 3_545 3_545 ? O4 K1 Mn3 171.90(8) . 3_545 ? N5 K1 Mn3 101.8(2) . 3_545 ? O6 K1 Mn3 33.78(6) 3_545 3_545 ? Mn2 K1 Mn3 150.76(4) . 3_545 ? C5 O1 Mn1 119.7(3) . . ? C6 O3 Mn1 131.4(3) . . ? C6 O4 Mn2 124.1(3) . . ? C6 O4 K1 142.6(3) . . ? Mn2 O4 K1 93.15(12) . . ? C8 O5 Mn1 132.4(3) . . ? C8 O6 Mn3 129.0(3) . . ? C8 O6 K1 138.4(3) . 3 ? Mn3 O6 K1 91.77(11) . 3 ? C10 O7 Mn1 127.0(3) . . ? C10 O8 Mn3 132.8(3) . . ? C12 O9 Mn4 134.2(3) . . ? C12 O10 Mn2 128.6(3) . . ? C12 O10 K1 136.1(3) . . ? Mn2 O10 K1 93.93(11) . . ? C14 O11 Mn4 130.9(3) . . ? C14 O12 Mn3 124.5(3) . . ? C14 O12 K1 139.3(3) . 3 ? Mn3 O12 K1 96.02(11) . 3 ? C16 O13 Mn4 127.0(3) . . ? C16 O14 Mn2 134.6(3) . . ? C18 O15 Mn2 125.3(3) . . ? C18 O15 K1 145.4(3) . . ? Mn2 O15 K1 88.76(11) . . ? C18 O16 Mn3 123.5(3) . . ? C18 O16 K1 148.2(3) . 3 ? Mn3 O16 K1 88.09(11) . 3 ? Mn1 O17 Mn3 123.38(14) . . ? Mn1 O17 Mn2 129.64(15) . . ? Mn3 O17 Mn2 96.32(12) . . ? Mn4 O18 Mn2 124.91(15) . . ? Mn4 O18 Mn3 128.95(15) . . ? Mn2 O18 Mn3 96.76(12) . . ? C24 O19 Mn4 119.5(3) . . ? C1 N1 C4 117.9(4) . . ? C1 N1 Mn1 130.4(3) . . ? C4 N1 Mn1 111.6(3) . . ? C2 N2 C3 116.0(5) . . ? C20 N3 C23 118.4(4) . . ? C20 N3 Mn4 129.9(3) . . ? C23 N3 Mn4 111.6(3) . . ? C21 N4 C22 115.9(5) . . ? N1 C1 C2 120.4(5) . . ? N1 C1 H1A 119.8 . . ? C2 C1 H1A 119.8 . . ? N2 C2 C1 122.9(6) . . ? N2 C2 H2B 118.5 . . ? C1 C2 H2B 118.5 . . ? N2 C3 C4 122.4(5) . . ? N2 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? N1 C4 C3 120.4(5) . . ? N1 C4 C5 114.9(4) . . ? C3 C4 C5 124.7(5) . . ? O2 C5 O1 125.1(5) . . ? O2 C5 C4 121.4(5) . . ? O1 C5 C4 113.5(4) . . ? O3 C6 O4 125.0(4) . . ? O3 C6 C7 118.8(5) . . ? O4 C6 C7 116.2(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 O6 124.9(4) . . ? O5 C8 C9 119.4(4) . . ? O6 C8 C9 115.7(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O8 C10 O7 126.2(4) . . ? O8 C10 C11 117.4(5) . . ? O7 C10 C11 116.4(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O10 125.3(4) . . ? O9 C12 C13 118.3(4) . . ? O10 C12 C13 116.4(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O11 C14 O12 124.6(4) . . ? O11 C14 C15 120.0(4) . . ? O12 C14 C15 115.3(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O14 C16 O13 126.0(4) . . ? O14 C16 C17 118.2(4) . . ? O13 C16 C17 115.8(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O15 C18 O16 125.0(4) . . ? O15 C18 C19 117.5(5) . . ? O16 C18 C19 117.5(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 120.1(5) . . ? N3 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? N4 C21 C20 123.2(5) . . ? N4 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? N4 C22 C23 122.3(5) . . ? N4 C22 H22A 118.9 . . ? C23 C22 H22A 118.9 . . ? N3 C23 C22 120.2(5) . . ? N3 C23 C24 113.6(4) . . ? C22 C23 C24 126.2(5) . . ? O20 C24 O19 124.8(5) . . ? O20 C24 C23 120.9(5) . . ? O19 C24 C23 114.3(4) . . ? N5' C25 N5 30.9(9) . . ? N5' C25 C26' 166.2(17) . . ? N5 C25 C26' 154.7(17) . . ? N5' C25 C26 146.2(19) . . ? N5 C25 C26 163.3(17) . . ? C26' C25 C26 35.2(11) . . ? N5' C25 C26" 134(2) . . ? N5 C25 C26" 141.1(19) . . ? C26' C25 C26" 32.1(14) . . ? C26 C25 C26" 55.5(17) . . ? C25 N5 K1 144.9(11) . . ? C25 N5' K1 163.3(13) . . ? N6' C27 N6 21(3) . . ? N6' C27 C28' 179(3) . . ? N6 C27 C28' 158.8(16) . . ? N6' C27 C28 148(3) . . ? N6 C27 C28 168.8(16) . . ? C28' C27 C28 31.6(9) . . ? C29' C30 C29 55(3) . . ? N7 C29 C30 121(6) . . ? N7' C29' C30 150.4(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.561 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.073 #==END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 614093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4O2(AcO)7(pyz)2]2 K(CH3CN)(Et4N)' _chemical_formula_sum 'C58 H77 Cl0 K Mn8 N10 O40' _chemical_formula_weight 2032.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3702(2) _cell_length_b 25.8446(5) _cell_length_c 16.3161(2) _cell_angle_alpha 90.00 _cell_angle_beta 123.9790(10) _cell_angle_gamma 90.00 _cell_volume 8172.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8001 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4136 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7717 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13923 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7190 _reflns_number_gt 5797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+31.9100P] 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 7190 _refine_ls_number_parameters 545 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.69804(3) 0.07690(2) 0.66503(4) 0.03421(16) Uani 1 1 d . . . Mn2 Mn 0.60700(3) 0.17628(2) 0.67176(4) 0.03244(15) Uani 1 1 d . . . Mn3 Mn 0.75261(3) 0.18641(2) 0.78919(4) 0.03070(15) Uani 1 1 d . . . Mn4 Mn 0.65818(3) 0.28824(2) 0.64171(4) 0.03313(15) Uani 1 1 d . . . K1 K 0.5000 0.13936(7) 0.7500 0.0705(5) Uani 1 2 d S . . O1 O 0.70639(16) 0.01243(11) 0.6131(2) 0.0450(7) Uani 1 1 d . . . O2 O 0.7110(2) -0.07344(12) 0.6277(3) 0.0665(10) Uani 1 1 d . . . O3 O 0.58500(16) 0.06649(11) 0.5650(2) 0.0525(8) Uani 1 1 d . . . O4 O 0.54154(15) 0.11952(11) 0.6250(2) 0.0478(7) Uani 1 1 d . . . O5 O 0.80946(15) 0.07247(11) 0.7823(2) 0.0464(7) Uani 1 1 d . . . O6 O 0.82829(15) 0.14019(11) 0.8791(2) 0.0436(7) Uani 1 1 d . . . O7 O 0.71282(15) 0.11463(11) 0.5775(2) 0.0430(7) Uani 1 1 d . . . O8 O 0.77765(15) 0.17996(11) 0.6776(2) 0.0426(7) Uani 1 1 d . . . O9 O 0.54733(15) 0.28944(11) 0.5816(2) 0.0469(7) Uani 1 1 d . . . O10 O 0.52898(15) 0.21981(11) 0.6443(2) 0.0460(7) Uani 1 1 d . . . O11 O 0.76676(15) 0.30086(11) 0.7174(2) 0.0437(7) Uani 1 1 d . . . O12 O 0.81781(14) 0.24308(10) 0.8417(2) 0.0391(6) Uani 1 1 d . . . O13 O 0.63888(15) 0.25252(11) 0.5230(2) 0.0435(7) Uani 1 1 d . . . O14 O 0.57863(15) 0.18470(11) 0.5207(2) 0.0452(7) Uani 1 1 d . . . O15 O 0.62286(16) 0.16883(12) 0.8152(2) 0.0467(7) Uani 1 1 d . . . O16 O 0.73405(15) 0.19092(11) 0.9100(2) 0.0423(7) Uani 1 1 d . . . O17 O 0.68672(13) 0.13335(9) 0.72370(18) 0.0316(6) Uani 1 1 d . . . O18 O 0.67278(13) 0.22978(9) 0.71570(18) 0.0305(6) Uani 1 1 d . . . O19 O 0.64133(16) 0.35349(10) 0.5756(2) 0.0440(7) Uani 1 1 d . . . O20 O 0.6071(3) 0.43450(14) 0.5669(3) 0.0892(14) Uani 1 1 d . . . N1 N 0.69391(18) 0.02534(13) 0.7597(3) 0.0405(8) Uani 1 1 d . . . N2 N 0.7035(4) -0.0543(2) 0.8788(5) 0.106(2) Uani 1 1 d . . . N3 N 0.65723(17) 0.33767(12) 0.7443(2) 0.0364(7) Uani 1 1 d . . . N4 N 0.6361(3) 0.41308(17) 0.8451(3) 0.0673(12) Uani 1 1 d . . . C1 C 0.6911(3) 0.0350(2) 0.8376(4) 0.0600(13) Uani 1 1 d . . . H1A H 0.6860 0.0688 0.8522 0.072 Uiso 1 1 calc R . . C2 C 0.6958(4) -0.0053(2) 0.8961(5) 0.096(2) Uani 1 1 d . . . H2B H 0.6935 0.0020 0.9500 0.115 Uiso 1 1 calc R . . C3 C 0.7070(3) -0.0627(2) 0.8018(5) 0.0727(16) Uani 1 1 d . . . H3A H 0.7125 -0.0965 0.7877 0.087 Uiso 1 1 calc R . . C4 C 0.7027(2) -0.02353(15) 0.7418(3) 0.0420(10) Uani 1 1 d . . . C5 C 0.7071(2) -0.03049(16) 0.6544(3) 0.0425(10) Uani 1 1 d . . . C6 C 0.5366(2) 0.08343(17) 0.5680(4) 0.0505(12) Uani 1 1 d . . . C7 C 0.4647(3) 0.0619(2) 0.5000(6) 0.096(2) Uani 1 1 d . . . H7A H 0.4587 0.0503 0.4398 0.144 Uiso 1 1 calc R . . H7B H 0.4315 0.0885 0.4853 0.144 Uiso 1 1 calc R . . H7C H 0.4581 0.0334 0.5316 0.144 Uiso 1 1 calc R . . C8 C 0.8432(2) 0.09556(16) 0.8629(3) 0.0408(10) Uani 1 1 d . . . C9 C 0.9061(3) 0.0706(2) 0.9498(4) 0.0674(15) Uani 1 1 d . . . H9A H 0.8949 0.0565 0.9936 0.101 Uiso 1 1 calc R . . H9B H 0.9420 0.0959 0.9843 0.101 Uiso 1 1 calc R . . H9C H 0.9217 0.0433 0.9269 0.101 Uiso 1 1 calc R . . C10 C 0.7522(2) 0.15429(16) 0.6004(3) 0.0384(9) Uani 1 1 d . . . C11 C 0.7669(3) 0.1693(2) 0.5250(4) 0.0604(14) Uani 1 1 d . . . H11A H 0.7248 0.1684 0.4602 0.091 Uiso 1 1 calc R . . H11B H 0.7994 0.1454 0.5277 0.091 Uiso 1 1 calc R . . H11C H 0.7859 0.2036 0.5388 0.091 Uiso 1 1 calc R . . C12 C 0.5146(2) 0.26519(17) 0.6081(3) 0.0407(10) Uani 1 1 d . . . C13 C 0.4528(3) 0.2903(2) 0.5970(4) 0.0628(14) Uani 1 1 d . . . H13A H 0.4637 0.3255 0.6194 0.094 Uiso 1 1 calc R . . H13B H 0.4403 0.2719 0.6358 0.094 Uiso 1 1 calc R . . H13C H 0.4150 0.2897 0.5288 0.094 Uiso 1 1 calc R . . C14 C 0.8176(2) 0.28290(15) 0.7951(3) 0.0382(9) Uani 1 1 d . . . C15 C 0.8858(3) 0.3102(2) 0.8418(4) 0.0619(14) Uani 1 1 d . . . H15A H 0.8974 0.3136 0.7942 0.093 Uiso 1 1 calc R . . H15B H 0.9209 0.2904 0.8973 0.093 Uiso 1 1 calc R . . H15C H 0.8827 0.3439 0.8637 0.093 Uiso 1 1 calc R . . C16 C 0.6013(2) 0.21273(17) 0.4838(3) 0.0412(10) Uani 1 1 d . . . C17 C 0.5836(3) 0.1986(2) 0.3824(4) 0.0717(16) Uani 1 1 d . . . H17A H 0.5968 0.1634 0.3827 0.108 Uiso 1 1 calc R . . H17B H 0.6079 0.2211 0.3650 0.108 Uiso 1 1 calc R . . H17C H 0.5348 0.2024 0.3350 0.108 Uiso 1 1 calc R . . C18 C 0.6770(2) 0.18077(15) 0.8968(3) 0.0386(9) Uani 1 1 d . . . C19 C 0.6709(3) 0.1819(2) 0.9841(4) 0.0598(13) Uani 1 1 d . . . H19A H 0.6917 0.1514 1.0234 0.090 Uiso 1 1 calc R . . H19B H 0.6231 0.1832 0.9610 0.090 Uiso 1 1 calc R . . H19C H 0.6941 0.2120 1.0236 0.090 Uiso 1 1 calc R . . C20 C 0.6662(2) 0.32785(16) 0.8303(3) 0.0427(10) Uani 1 1 d . . . H20A H 0.6793 0.2948 0.8573 0.051 Uiso 1 1 calc R . . C21 C 0.6564(2) 0.36598(19) 0.8808(4) 0.0524(12) Uani 1 1 d . . . H21A H 0.6645 0.3581 0.9421 0.063 Uiso 1 1 calc R . . C22 C 0.6267(3) 0.4225(2) 0.7577(4) 0.0667(15) Uani 1 1 d . . . H22A H 0.6123 0.4553 0.7301 0.080 Uiso 1 1 calc R . . C23 C 0.6373(2) 0.38550(16) 0.7074(3) 0.0437(10) Uani 1 1 d . . . C24 C 0.6270(3) 0.39358(17) 0.6091(4) 0.0519(12) Uani 1 1 d . . . C25 C 0.5213(13) -0.0123(6) 0.7953(15) 0.137(8) Uani 0.50 1 d PD . . N5 N 0.5000 0.0259(9) 0.7500 0.124(10) Uiso 0.50 2 d SPD . 1 C26 C 0.5592(15) -0.0632(9) 0.854(2) 0.090(8) Uiso 0.25 1 d PD . 1 N5' N 0.527(2) 0.0313(9) 0.792(3) 0.132(12) Uiso 0.25 1 d PD . 2 C26' C 0.5199(16) -0.0696(8) 0.804(2) 0.087(8) Uiso 0.25 1 d PD . 2 N6 N 0.5000 0.3924(3) 0.2500 0.086(2) Uani 1 2 d SD . . C27 C 0.4399(7) 0.4248(5) 0.2302(8) 0.240(8) Uani 1 1 d D . . H27A H 0.4540 0.4437 0.2900 0.288 Uiso 1 1 calc R . . H27B H 0.4029 0.4017 0.2166 0.288 Uiso 1 1 calc R . . C28 C 0.4116(11) 0.4631(5) 0.1458(9) 0.378(16) Uani 1 1 d D . . H28A H 0.3728 0.4809 0.1381 0.567 Uiso 1 1 calc R . . H28B H 0.3972 0.4450 0.0858 0.567 Uiso 1 1 calc R . . H28C H 0.4467 0.4878 0.1600 0.567 Uiso 1 1 calc R . . C29 C 0.5224(4) 0.3616(3) 0.3399(5) 0.100(2) Uani 1 1 d D . . H29A H 0.5338 0.3852 0.3931 0.120 Uiso 1 1 calc R . . H29B H 0.5643 0.3432 0.3589 0.120 Uiso 1 1 calc R . . C30 C 0.4709(3) 0.3230(3) 0.3302(5) 0.0870(19) Uani 1 1 d D . . H30A H 0.4902 0.3048 0.3915 0.131 Uiso 1 1 calc R . . H30B H 0.4598 0.2988 0.2787 0.131 Uiso 1 1 calc R . . H30C H 0.4298 0.3407 0.3142 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0476(4) 0.0263(3) 0.0355(3) -0.0043(2) 0.0274(3) -0.0042(3) Mn2 0.0339(3) 0.0288(3) 0.0366(3) -0.0012(2) 0.0209(3) -0.0029(2) Mn3 0.0337(3) 0.0260(3) 0.0305(3) -0.0023(2) 0.0168(3) -0.0022(2) Mn4 0.0424(3) 0.0273(3) 0.0329(3) 0.0012(2) 0.0229(3) -0.0008(3) K1 0.0562(10) 0.0771(11) 0.1004(14) 0.000 0.0574(10) 0.000 O1 0.064(2) 0.0334(16) 0.0469(17) -0.0088(13) 0.0365(16) -0.0033(14) O2 0.090(3) 0.0356(18) 0.078(2) -0.0157(17) 0.050(2) 0.0035(17) O3 0.0468(18) 0.0406(17) 0.057(2) -0.0127(15) 0.0207(16) -0.0075(14) O4 0.0457(17) 0.0404(17) 0.0601(19) -0.0089(15) 0.0313(16) -0.0140(14) O5 0.0473(18) 0.0415(17) 0.0450(17) -0.0066(14) 0.0224(15) 0.0036(14) O6 0.0429(16) 0.0378(16) 0.0408(16) -0.0003(13) 0.0177(14) 0.0027(13) O7 0.0592(18) 0.0405(16) 0.0383(16) -0.0064(13) 0.0328(15) -0.0124(14) O8 0.0518(18) 0.0399(16) 0.0468(17) -0.0070(14) 0.0341(15) -0.0100(13) O9 0.0417(16) 0.0447(17) 0.0515(18) 0.0068(14) 0.0243(15) 0.0023(14) O10 0.0419(17) 0.0434(17) 0.0584(19) 0.0070(15) 0.0317(15) 0.0061(13) O11 0.0451(17) 0.0400(16) 0.0499(18) 0.0040(14) 0.0290(16) -0.0041(13) O12 0.0418(16) 0.0342(15) 0.0372(15) -0.0045(12) 0.0196(13) -0.0098(12) O13 0.0531(18) 0.0453(17) 0.0377(16) -0.0034(13) 0.0289(15) -0.0048(14) O14 0.0505(18) 0.0434(17) 0.0345(15) -0.0030(13) 0.0194(14) -0.0075(14) O15 0.0473(18) 0.0607(19) 0.0394(17) -0.0025(14) 0.0287(15) -0.0053(15) O16 0.0481(17) 0.0471(17) 0.0340(15) -0.0028(13) 0.0243(14) -0.0030(14) O17 0.0385(14) 0.0252(13) 0.0331(14) -0.0040(11) 0.0211(12) -0.0014(11) O18 0.0348(14) 0.0256(13) 0.0326(14) 0.0001(11) 0.0199(12) -0.0003(11) O19 0.0628(19) 0.0334(15) 0.0434(17) 0.0063(13) 0.0345(16) 0.0023(14) O20 0.162(4) 0.044(2) 0.076(3) 0.028(2) 0.075(3) 0.033(2) N1 0.050(2) 0.0343(18) 0.045(2) 0.0027(16) 0.0307(18) 0.0026(15) N2 0.186(7) 0.069(3) 0.117(5) 0.043(3) 0.117(5) 0.036(4) N3 0.0381(18) 0.0305(17) 0.0393(19) 0.0034(14) 0.0208(16) 0.0000(14) N4 0.094(3) 0.056(3) 0.065(3) -0.001(2) 0.052(3) 0.015(2) C1 0.093(4) 0.049(3) 0.061(3) 0.005(2) 0.057(3) 0.007(3) C2 0.173(7) 0.074(4) 0.086(5) 0.032(4) 0.101(5) 0.035(4) C3 0.111(5) 0.045(3) 0.083(4) 0.018(3) 0.066(4) 0.019(3) C4 0.048(2) 0.026(2) 0.051(3) 0.0017(18) 0.028(2) 0.0028(18) C5 0.039(2) 0.036(2) 0.049(3) -0.007(2) 0.022(2) 0.0001(18) C6 0.046(3) 0.032(2) 0.054(3) 0.002(2) 0.016(2) -0.007(2) C7 0.045(3) 0.064(4) 0.133(6) -0.036(4) 0.021(4) -0.011(3) C8 0.044(2) 0.036(2) 0.046(3) 0.0044(19) 0.027(2) 0.0038(19) C9 0.070(4) 0.055(3) 0.053(3) 0.007(2) 0.019(3) 0.020(3) C10 0.044(2) 0.037(2) 0.040(2) 0.0029(19) 0.027(2) 0.0041(19) C11 0.081(4) 0.061(3) 0.061(3) -0.004(3) 0.053(3) -0.017(3) C12 0.034(2) 0.041(2) 0.039(2) -0.0045(19) 0.0153(19) 0.0022(18) C13 0.049(3) 0.062(3) 0.076(4) 0.004(3) 0.034(3) 0.016(2) C14 0.044(2) 0.033(2) 0.047(2) -0.0141(19) 0.031(2) -0.0095(18) C15 0.051(3) 0.059(3) 0.070(3) -0.002(3) 0.031(3) -0.019(2) C16 0.049(2) 0.041(2) 0.033(2) 0.0006(19) 0.023(2) 0.007(2) C17 0.093(4) 0.077(4) 0.039(3) -0.011(3) 0.034(3) -0.008(3) C18 0.058(3) 0.029(2) 0.040(2) 0.0049(18) 0.034(2) 0.0087(19) C19 0.062(3) 0.083(4) 0.047(3) 0.002(3) 0.039(3) 0.004(3) C20 0.047(2) 0.039(2) 0.041(2) 0.0039(19) 0.023(2) -0.0012(19) C21 0.059(3) 0.059(3) 0.046(3) -0.002(2) 0.035(2) -0.001(2) C22 0.098(4) 0.046(3) 0.065(3) 0.008(3) 0.051(3) 0.021(3) C23 0.053(3) 0.032(2) 0.048(3) 0.0013(19) 0.029(2) 0.0039(19) C24 0.070(3) 0.036(2) 0.052(3) 0.008(2) 0.035(3) 0.003(2) C25 0.16(2) 0.122(14) 0.16(2) 0.021(12) 0.11(2) 0.030(14) N6 0.158(8) 0.054(4) 0.043(4) 0.000 0.055(4) 0.000 C27 0.42(2) 0.197(12) 0.137(10) 0.053(9) 0.177(14) 0.178(13) C28 0.79(4) 0.226(13) 0.176(11) 0.148(11) 0.31(2) 0.36(2) C29 0.110(6) 0.111(6) 0.068(4) 0.006(4) 0.042(4) -0.008(5) C30 0.083(4) 0.095(5) 0.091(5) -0.004(4) 0.053(4) -0.017(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 O17 1.843(2) . ? Mn1 O7 1.913(3) . ? Mn1 O1 1.928(3) . ? Mn1 N1 2.082(3) . ? Mn1 O5 2.210(3) . ? Mn1 O3 2.213(3) . ? Mn2 O18 1.886(2) . ? Mn2 O17 1.912(3) . ? Mn2 O4 1.942(3) . ? Mn2 O10 1.969(3) . ? Mn2 O15 2.163(3) . ? Mn2 O14 2.176(3) . ? Mn2 Mn3 2.8340(8) . ? Mn2 K1 3.5158(8) . ? Mn3 O17 1.885(2) . ? Mn3 O18 1.917(2) . ? Mn3 O12 1.934(3) . ? Mn3 O6 1.951(3) . ? Mn3 O8 2.209(3) . ? Mn3 O16 2.246(3) . ? Mn4 O18 1.843(2) . ? Mn4 O19 1.920(3) . ? Mn4 O13 1.957(3) . ? Mn4 N3 2.116(3) . ? Mn4 O11 2.137(3) . ? Mn4 O9 2.199(3) . ? K1 O15 2.558(3) 2_656 ? K1 O15 2.558(3) . ? K1 O4 2.754(3) 2_656 ? K1 O4 2.754(3) . ? K1 N5' 2.86(2) 2_656 ? K1 N5' 2.86(2) . ? K1 N5 2.93(2) . ? K1 O10 3.010(3) 2_656 ? K1 O10 3.010(3) . ? K1 Mn2 3.5158(8) 2_656 ? O1 C5 1.293(5) . ? O2 C5 1.214(5) . ? O3 C6 1.239(6) . ? O4 C6 1.275(5) . ? O5 C8 1.245(5) . ? O6 C8 1.274(5) . ? O7 C10 1.285(5) . ? O8 C10 1.241(5) . ? O9 C12 1.239(5) . ? O10 C12 1.271(5) . ? O11 C14 1.246(5) . ? O12 C14 1.278(5) . ? O13 C16 1.269(5) . ? O14 C16 1.235(5) . ? O15 C18 1.260(5) . ? O16 C18 1.253(5) . ? O19 C24 1.300(5) . ? O20 C24 1.204(5) . ? N1 C1 1.332(6) . ? N1 C4 1.337(5) . ? N2 C3 1.321(7) . ? N2 C2 1.333(8) . ? N3 C20 1.323(5) . ? N3 C23 1.340(5) . ? N4 C21 1.318(6) . ? N4 C22 1.336(6) . ? C1 C2 1.376(7) . ? C1 H1A 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.372(6) . ? C3 H3A 0.9300 . ? C4 C5 1.498(6) . ? C6 C7 1.510(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.504(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.502(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.499(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.504(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.508(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.509(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.383(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.370(6) . ? C22 H22A 0.9300 . ? C23 C24 1.498(6) . ? C25 N5' 1.140(19) . ? C25 N5 1.165(17) . ? C25 C25 1.24(4) 2_656 ? C25 C26' 1.490(17) . ? C25 C26 1.577(18) . ? C25 N5' 1.67(3) 2_656 ? C25 C26' 2.00(3) 2_656 ? N5 C25 1.165(17) 2_656 ? N5' N5' 1.24(9) 2_656 ? N5' C25 1.67(3) 2_656 ? C26' C26' 1.47(6) 2_656 ? C26' C25 2.00(3) 2_656 ? N6 C29 1.484(7) . ? N6 C29 1.484(7) 2_655 ? N6 C27 1.506(10) . ? N6 C27 1.506(10) 2_655 ? C27 C28 1.517(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.503(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O17 Mn1 O7 97.02(12) . . ? O17 Mn1 O1 172.48(12) . . ? O7 Mn1 O1 90.45(12) . . ? O17 Mn1 N1 92.39(12) . . ? O7 Mn1 N1 169.17(13) . . ? O1 Mn1 N1 80.27(13) . . ? O17 Mn1 O5 91.90(11) . . ? O7 Mn1 O5 93.18(12) . . ? O1 Mn1 O5 88.62(12) . . ? N1 Mn1 O5 81.12(13) . . ? O17 Mn1 O3 91.17(12) . . ? O7 Mn1 O3 98.67(13) . . ? O1 Mn1 O3 86.75(12) . . ? N1 Mn1 O3 86.45(13) . . ? O5 Mn1 O3 167.30(12) . . ? O18 Mn2 O17 82.62(11) . . ? O18 Mn2 O4 177.55(12) . . ? O17 Mn2 O4 95.41(12) . . ? O18 Mn2 O10 97.02(12) . . ? O17 Mn2 O10 168.93(12) . . ? O4 Mn2 O10 85.20(13) . . ? O18 Mn2 O15 92.50(11) . . ? O17 Mn2 O15 86.19(11) . . ? O4 Mn2 O15 88.81(13) . . ? O10 Mn2 O15 82.78(12) . . ? O18 Mn2 O14 91.43(11) . . ? O17 Mn2 O14 99.47(11) . . ? O4 Mn2 O14 87.46(12) . . ? O10 Mn2 O14 91.60(12) . . ? O15 Mn2 O14 173.49(12) . . ? O18 Mn2 Mn3 42.24(8) . . ? O17 Mn2 Mn3 41.37(7) . . ? O4 Mn2 Mn3 136.06(10) . . ? O10 Mn2 Mn3 135.27(9) . . ? O15 Mn2 Mn3 82.06(8) . . ? O14 Mn2 Mn3 104.30(8) . . ? O18 Mn2 K1 130.92(8) . . ? O17 Mn2 K1 113.34(8) . . ? O4 Mn2 K1 51.23(9) . . ? O10 Mn2 K1 58.78(9) . . ? O15 Mn2 K1 46.35(8) . . ? O14 Mn2 K1 127.60(8) . . ? Mn3 Mn2 K1 127.49(2) . . ? O17 Mn3 O18 82.51(11) . . ? O17 Mn3 O12 173.47(11) . . ? O18 Mn3 O12 94.86(11) . . ? O17 Mn3 O6 95.21(11) . . ? O18 Mn3 O6 169.96(12) . . ? O12 Mn3 O6 88.38(12) . . ? O17 Mn3 O8 89.24(11) . . ? O18 Mn3 O8 98.18(11) . . ? O12 Mn3 O8 85.21(11) . . ? O6 Mn3 O8 91.56(12) . . ? O17 Mn3 O16 92.18(11) . . ? O18 Mn3 O16 85.46(11) . . ? O12 Mn3 O16 93.58(11) . . ? O6 Mn3 O16 84.85(12) . . ? O8 Mn3 O16 176.25(11) . . ? O17 Mn3 Mn2 42.09(8) . . ? O18 Mn3 Mn2 41.41(7) . . ? O12 Mn3 Mn2 136.09(9) . . ? O6 Mn3 Mn2 133.88(9) . . ? O8 Mn3 Mn2 101.95(8) . . ? O16 Mn3 Mn2 81.39(8) . . ? O18 Mn4 O19 173.08(12) . . ? O18 Mn4 O13 96.74(12) . . ? O19 Mn4 O13 89.82(12) . . ? O18 Mn4 N3 93.24(12) . . ? O19 Mn4 N3 79.92(12) . . ? O13 Mn4 N3 165.77(13) . . ? O18 Mn4 O11 91.23(11) . . ? O19 Mn4 O11 89.71(12) . . ? O13 Mn4 O11 100.72(12) . . ? N3 Mn4 O11 89.15(12) . . ? O18 Mn4 O9 92.53(11) . . ? O19 Mn4 O9 85.22(12) . . ? O13 Mn4 O9 90.17(12) . . ? N3 Mn4 O9 79.26(12) . . ? O11 Mn4 O9 167.99(12) . . ? O15 K1 O15 145.36(16) 2_656 . ? O15 K1 O4 65.47(9) 2_656 2_656 ? O15 K1 O4 121.74(9) . 2_656 ? O15 K1 O4 121.74(9) 2_656 . ? O15 K1 O4 65.47(9) . . ? O4 K1 O4 158.53(14) 2_656 . ? O15 K1 N5' 98.3(8) 2_656 2_656 ? O15 K1 N5' 115.9(8) . 2_656 ? O4 K1 N5' 82.7(7) 2_656 2_656 ? O4 K1 N5' 76.3(7) . 2_656 ? O15 K1 N5' 115.9(8) 2_656 . ? O15 K1 N5' 98.3(8) . . ? O4 K1 N5' 76.3(7) 2_656 . ? O4 K1 N5' 82.7(7) . . ? N5' K1 N5' 25.1(17) 2_656 . ? O15 K1 N5 107.32(8) 2_656 . ? O15 K1 N5 107.32(8) . . ? O4 K1 N5 79.26(7) 2_656 . ? O4 K1 N5 79.26(7) . . ? N5' K1 N5 12.5(9) 2_656 . ? N5' K1 N5 12.5(9) . . ? O15 K1 O10 58.19(9) 2_656 2_656 ? O15 K1 O10 96.65(10) . 2_656 ? O4 K1 O10 54.46(8) 2_656 2_656 ? O4 K1 O10 146.99(10) . 2_656 ? N5' K1 O10 136.1(7) 2_656 2_656 ? N5' K1 O10 128.9(8) . 2_656 ? N5 K1 O10 133.68(6) . 2_656 ? O15 K1 O10 96.65(10) 2_656 . ? O15 K1 O10 58.19(9) . . ? O4 K1 O10 146.99(10) 2_656 . ? O4 K1 O10 54.46(8) . . ? N5' K1 O10 128.9(8) 2_656 . ? N5' K1 O10 136.1(7) . . ? N5 K1 O10 133.68(6) . . ? O10 K1 O10 92.64(12) 2_656 . ? O15 K1 Mn2 37.74(7) 2_656 2_656 ? O15 K1 Mn2 128.99(8) . 2_656 ? O4 K1 Mn2 33.35(6) 2_656 2_656 ? O4 K1 Mn2 159.46(7) . 2_656 ? N5' K1 Mn2 104.2(7) 2_656 2_656 ? N5' K1 Mn2 106.6(7) . 2_656 ? N5 K1 Mn2 105.75(3) . 2_656 ? O10 K1 Mn2 34.01(5) 2_656 2_656 ? O10 K1 Mn2 117.00(7) . 2_656 ? O15 K1 Mn2 128.99(8) 2_656 . ? O15 K1 Mn2 37.74(7) . . ? O4 K1 Mn2 159.46(7) 2_656 . ? O4 K1 Mn2 33.35(6) . . ? N5' K1 Mn2 106.6(7) 2_656 . ? N5' K1 Mn2 104.2(7) . . ? N5 K1 Mn2 105.75(3) . . ? O10 K1 Mn2 117.00(7) 2_656 . ? O10 K1 Mn2 34.01(5) . . ? Mn2 K1 Mn2 148.50(6) 2_656 . ? C5 O1 Mn1 119.2(3) . . ? C6 O3 Mn1 131.9(3) . . ? C6 O4 Mn2 124.7(3) . . ? C6 O4 K1 138.6(3) . . ? Mn2 O4 K1 95.41(12) . . ? C8 O5 Mn1 129.3(3) . . ? C8 O6 Mn3 129.5(3) . . ? C10 O7 Mn1 126.0(3) . . ? C10 O8 Mn3 132.7(3) . . ? C12 O9 Mn4 129.8(3) . . ? C12 O10 Mn2 127.1(3) . . ? C12 O10 K1 144.9(3) . . ? Mn2 O10 K1 87.20(10) . . ? C14 O11 Mn4 132.8(3) . . ? C14 O12 Mn3 127.3(3) . . ? C16 O13 Mn4 126.4(3) . . ? C16 O14 Mn2 132.0(3) . . ? C18 O15 Mn2 125.8(3) . . ? C18 O15 K1 138.0(3) . . ? Mn2 O15 K1 95.90(11) . . ? C18 O16 Mn3 123.2(3) . . ? Mn1 O17 Mn3 124.14(14) . . ? Mn1 O17 Mn2 128.04(14) . . ? Mn3 O17 Mn2 96.54(11) . . ? Mn4 O18 Mn2 122.61(13) . . ? Mn4 O18 Mn3 130.41(14) . . ? Mn2 O18 Mn3 96.36(11) . . ? C24 O19 Mn4 118.9(3) . . ? C1 N1 C4 118.7(4) . . ? C1 N1 Mn1 129.4(3) . . ? C4 N1 Mn1 111.5(3) . . ? C3 N2 C2 116.4(5) . . ? C20 N3 C23 117.6(4) . . ? C20 N3 Mn4 131.2(3) . . ? C23 N3 Mn4 110.9(3) . . ? C21 N4 C22 116.3(4) . . ? N1 C1 C2 119.5(5) . . ? N1 C1 H1A 120.2 . . ? C2 C1 H1A 120.2 . . ? N2 C2 C1 122.7(5) . . ? N2 C2 H2B 118.7 . . ? C1 C2 H2B 118.7 . . ? N2 C3 C4 122.6(5) . . ? N2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? N1 C4 C3 120.0(4) . . ? N1 C4 C5 114.9(4) . . ? C3 C4 C5 125.0(4) . . ? O2 C5 O1 125.4(4) . . ? O2 C5 C4 120.7(4) . . ? O1 C5 C4 113.9(3) . . ? O3 C6 O4 125.0(4) . . ? O3 C6 C7 120.4(5) . . ? O4 C6 C7 114.5(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 O6 124.6(4) . . ? O5 C8 C9 119.9(4) . . ? O6 C8 C9 115.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O8 C10 O7 125.5(4) . . ? O8 C10 C11 119.6(4) . . ? O7 C10 C11 115.0(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O10 125.1(4) . . ? O9 C12 C13 118.6(4) . . ? O10 C12 C13 116.3(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O11 C14 O12 126.2(4) . . ? O11 C14 C15 118.6(4) . . ? O12 C14 C15 115.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O14 C16 O13 126.4(4) . . ? O14 C16 C17 117.6(4) . . ? O13 C16 C17 115.9(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O16 C18 O15 125.2(4) . . ? O16 C18 C19 119.1(4) . . ? O15 C18 C19 115.7(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 120.9(4) . . ? N3 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? N4 C21 C20 122.2(4) . . ? N4 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? N4 C22 C23 122.4(5) . . ? N4 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? N3 C23 C22 120.5(4) . . ? N3 C23 C24 114.7(4) . . ? C22 C23 C24 124.8(4) . . ? O20 C24 O19 124.6(4) . . ? O20 C24 C23 120.9(4) . . ? O19 C24 C23 114.5(4) . . ? N5' C25 N5 32(2) . . ? N5' C25 C25 89(3) . 2_656 ? N5 C25 C25 57.9(14) . 2_656 ? N5' C25 C26' 175(4) . . ? N5 C25 C26' 152(3) . . ? C25 C25 C26' 94.1(15) 2_656 . ? N5' C25 C26 144(4) . . ? N5 C25 C26 171(2) . . ? C25 C25 C26 122.0(15) 2_656 . ? C26' C25 C26 31.4(13) . . ? N5' C25 N5' 48(4) . 2_656 ? N5 C25 N5' 16.2(18) . 2_656 ? C25 C25 N5' 43.1(11) 2_656 2_656 ? C26' C25 N5' 135.6(19) . 2_656 ? C26 C25 N5' 165.0(18) . 2_656 ? N5' C25 C26' 135(3) . 2_656 ? N5 C25 C26' 105.7(19) . 2_656 ? C25 C25 C26' 47.9(8) 2_656 2_656 ? C26' C25 C26' 47.1(18) . 2_656 ? C26 C25 C26' 74.2(16) . 2_656 ? N5' C25 C26' 91.0(13) 2_656 2_656 ? C25 N5 C25 64(3) 2_656 . ? C25 N5 K1 147.9(14) 2_656 . ? C25 N5 K1 147.9(14) . . ? C25 N5' N5' 89(3) . 2_656 ? C25 N5' C25 48(2) . 2_656 ? N5' N5' C25 43.1(11) 2_656 2_656 ? C25 N5' K1 164(4) . . ? N5' N5' K1 77.5(9) 2_656 . ? C25 N5' K1 120.1(18) 2_656 . ? C26' C26' C25 85.1(14) 2_656 . ? C26' C26' C25 47.8(8) 2_656 2_656 ? C25 C26' C25 38.0(14) . 2_656 ? C29 N6 C29 115.0(7) . 2_655 ? C29 N6 C27 106.4(5) . . ? C29 N6 C27 108.3(6) 2_655 . ? C29 N6 C27 108.3(6) . 2_655 ? C29 N6 C27 106.4(5) 2_655 2_655 ? C27 N6 C27 112.6(13) . 2_655 ? N6 C27 C28 116.1(10) . . ? N6 C27 H27A 108.3 . . ? C28 C27 H27A 108.3 . . ? N6 C27 H27B 108.3 . . ? C28 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 C30 115.7(6) . . ? N6 C29 H29A 108.4 . . ? C30 C29 H29A 108.4 . . ? N6 C29 H29B 108.4 . . ? C30 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.950 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.081 #==END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 614094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn4O2(AcO)7(pyz)2]2(CH3CN)Na(Et4N)' _chemical_formula_sum 'C58 H77 Mn8 N10 Na O40' _chemical_formula_weight 2016.81 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.861(5) _cell_length_b 25.778(5) _cell_length_c 16.294(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.94(3) _cell_angle_gamma 90.00 _cell_volume 8058(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28237 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7923 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Weissenberg IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16656 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9123 _reflns_number_gt 6299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^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 9123 _refine_ls_number_parameters 545 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.943 _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 0.69500(2) 0.076232(15) 0.66841(3) 0.03247(11) Uani 1 1 d . . . Mn2 Mn 0.60244(2) 0.176749(15) 0.67302(3) 0.03045(10) Uani 1 1 d . . . Mn3 Mn 0.74946(2) 0.186394(15) 0.78905(3) 0.02949(10) Uani 1 1 d . . . Mn4 Mn 0.65623(2) 0.287757(16) 0.64023(3) 0.03236(11) Uani 1 1 d . . . Na1 Na 0.5000 0.14500(9) 0.7500 0.0646(6) Uani 1 2 d S . . O1 O 0.70423(11) 0.01126(8) 0.61802(14) 0.0423(5) Uani 1 1 d . . . O2 O 0.71141(14) -0.07478(9) 0.63657(19) 0.0619(7) Uani 1 1 d . . . O3 O 0.58082(11) 0.06583(8) 0.57303(16) 0.0496(5) Uani 1 1 d . . . O4 O 0.53506(10) 0.12089(8) 0.62922(16) 0.0439(5) Uani 1 1 d . . . O5 O 0.80796(11) 0.07218(8) 0.78397(15) 0.0447(5) Uani 1 1 d . . . O6 O 0.82504(10) 0.14041(8) 0.87912(13) 0.0396(5) Uani 1 1 d . . . O7 O 0.71085(11) 0.11347(8) 0.58064(14) 0.0415(5) Uani 1 1 d . . . O8 O 0.77714(11) 0.17844(8) 0.67939(15) 0.0409(5) Uani 1 1 d . . . O9 O 0.54459(11) 0.29050(8) 0.58356(15) 0.0451(5) Uani 1 1 d . . . O10 O 0.52400(10) 0.22116(8) 0.64629(15) 0.0425(5) Uani 1 1 d . . . O11 O 0.76638(11) 0.29920(8) 0.71345(15) 0.0426(5) Uani 1 1 d . . . O12 O 0.81524(10) 0.24336(8) 0.83987(13) 0.0382(4) Uani 1 1 d . . . O13 O 0.63696(11) 0.25105(8) 0.52293(14) 0.0428(5) Uani 1 1 d . . . O14 O 0.57492(11) 0.18391(8) 0.52313(14) 0.0433(5) Uani 1 1 d . . . O15 O 0.61384(10) 0.16909(8) 0.81418(14) 0.0420(5) Uani 1 1 d . . . O16 O 0.72608(11) 0.19064(8) 0.90668(13) 0.0392(5) Uani 1 1 d . . . O17 O 0.68272(9) 0.13326(7) 0.72581(12) 0.0298(4) Uani 1 1 d . . . O18 O 0.66953(9) 0.22993(7) 0.71502(12) 0.0302(4) Uani 1 1 d . . . O19 O 0.63993(11) 0.35278(8) 0.57388(14) 0.0429(5) Uani 1 1 d . . . O20 O 0.60296(19) 0.43396(10) 0.5638(2) 0.0832(10) Uani 1 1 d . . . N1 N 0.69166(13) 0.02557(9) 0.76512(17) 0.0388(6) Uani 1 1 d . . . N2 N 0.7045(3) -0.05292(15) 0.8886(3) 0.1021(15) Uani 1 1 d . . . N3 N 0.65788(12) 0.33801(9) 0.74317(17) 0.0363(5) Uani 1 1 d . . . N4 N 0.63962(18) 0.41457(12) 0.8468(2) 0.0631(8) Uani 1 1 d . . . C1 C 0.6891(2) 0.03589(14) 0.8431(3) 0.0576(9) Uani 1 1 d . . . H1A H 0.6833 0.0698 0.8569 0.069 Uiso 1 1 calc R . . C2 C 0.6952(3) -0.00400(18) 0.9032(3) 0.0891(16) Uani 1 1 d . . . H2B H 0.6925 0.0038 0.9569 0.107 Uiso 1 1 calc R . . C3 C 0.7081(2) -0.06249(14) 0.8112(3) 0.0707(11) Uani 1 1 d . . . H3A H 0.7153 -0.0964 0.7991 0.085 Uiso 1 1 calc R . . C4 C 0.70155(16) -0.02381(11) 0.7485(2) 0.0416(7) Uani 1 1 d . . . C5 C 0.70610(15) -0.03139(11) 0.6614(2) 0.0414(7) Uani 1 1 d . . . C6 C 0.53133(17) 0.08322(12) 0.5762(3) 0.0495(8) Uani 1 1 d . . . C7 C 0.4598(2) 0.06064(18) 0.5102(4) 0.105(2) Uani 1 1 d . . . H7A H 0.4520 0.0540 0.4470 0.157 Uiso 1 1 calc R . . H7B H 0.4256 0.0847 0.5038 0.157 Uiso 1 1 calc R . . H7C H 0.4563 0.0288 0.5376 0.157 Uiso 1 1 calc R . . C8 C 0.84058(15) 0.09566(12) 0.8633(2) 0.0387(6) Uani 1 1 d . . . C9 C 0.9039(2) 0.07056(15) 0.9486(3) 0.0639(10) Uani 1 1 d . . . H9A H 0.8933 0.0590 0.9950 0.096 Uiso 1 1 calc R . . H9B H 0.9414 0.0952 0.9791 0.096 Uiso 1 1 calc R . . H9C H 0.9176 0.0414 0.9260 0.096 Uiso 1 1 calc R . . C10 C 0.75117(15) 0.15340(11) 0.6025(2) 0.0365(6) Uani 1 1 d . . . C11 C 0.7669(2) 0.16825(14) 0.5276(3) 0.0560(9) Uani 1 1 d . . . H11A H 0.7402 0.1468 0.4706 0.084 Uiso 1 1 calc R . . H11B H 0.8157 0.1635 0.5542 0.084 Uiso 1 1 calc R . . H11C H 0.7548 0.2040 0.5099 0.084 Uiso 1 1 calc R . . C12 C 0.51035(15) 0.26658(12) 0.6099(2) 0.0399(7) Uani 1 1 d . . . C13 C 0.44725(19) 0.29217(15) 0.5978(3) 0.0630(10) Uani 1 1 d . . . H13A H 0.4590 0.3267 0.6239 0.095 Uiso 1 1 calc R . . H13B H 0.4314 0.2726 0.6323 0.095 Uiso 1 1 calc R . . H13C H 0.4109 0.2936 0.5297 0.095 Uiso 1 1 calc R . . C14 C 0.81644(15) 0.28257(11) 0.7921(2) 0.0355(6) Uani 1 1 d . . . C15 C 0.88473(18) 0.31040(14) 0.8384(3) 0.0559(9) Uani 1 1 d . . . H15A H 0.8986 0.3127 0.7925 0.084 Uiso 1 1 calc R . . H15B H 0.9194 0.2917 0.8953 0.084 Uiso 1 1 calc R . . H15C H 0.8800 0.3447 0.8572 0.084 Uiso 1 1 calc R . . C16 C 0.59879(16) 0.21099(12) 0.4853(2) 0.0392(7) Uani 1 1 d . . . C17 C 0.5817(2) 0.19617(16) 0.3848(2) 0.0651(10) Uani 1 1 d . . . H17A H 0.5960 0.1610 0.3859 0.098 Uiso 1 1 calc R . . H17B H 0.6060 0.2189 0.3663 0.098 Uiso 1 1 calc R . . H17C H 0.5324 0.1992 0.3384 0.098 Uiso 1 1 calc R . . C18 C 0.66891(16) 0.17972(10) 0.8954(2) 0.0364(6) Uani 1 1 d . . . C19 C 0.66337(19) 0.17865(15) 0.9829(2) 0.0575(9) Uani 1 1 d . . . H19A H 0.6838 0.1472 1.0191 0.086 Uiso 1 1 calc R . . H19B H 0.6152 0.1801 0.9619 0.086 Uiso 1 1 calc R . . H19C H 0.6875 0.2080 1.0240 0.086 Uiso 1 1 calc R . . C20 C 0.67112(16) 0.32890(12) 0.8324(2) 0.0425(7) Uani 1 1 d . . . H20A H 0.6864 0.2963 0.8607 0.051 Uiso 1 1 calc R . . C21 C 0.66213(18) 0.36763(13) 0.8828(2) 0.0494(8) Uani 1 1 d . . . H21A H 0.6724 0.3604 0.9452 0.059 Uiso 1 1 calc R . . C22 C 0.6276(2) 0.42322(13) 0.7579(3) 0.0614(10) Uani 1 1 d . . . H22A H 0.6125 0.4559 0.7301 0.074 Uiso 1 1 calc R . . C23 C 0.63678(17) 0.38572(11) 0.7059(2) 0.0427(7) Uani 1 1 d . . . C24 C 0.62452(19) 0.39309(12) 0.6061(2) 0.0502(8) Uani 1 1 d . . . C25 C 0.5191(9) -0.0007(4) 0.7947(10) 0.120(5) Uani 0.50 1 d PD . . N5 N 0.5000 0.0385(7) 0.7500 0.111(8) Uiso 0.50 2 d SPD . 1 C26 C 0.5475(13) -0.0548(8) 0.8531(18) 0.104(7) Uiso 0.25 1 d PD . 1 N5' N 0.5236(13) 0.0436(7) 0.7844(18) 0.101(7) Uiso 0.25 1 d PD . 2 C26' C 0.5160(14) -0.0579(7) 0.8057(18) 0.102(7) Uiso 0.25 1 d PD . 2 N6 N 0.5000 0.39050(18) 0.2500 0.0723(14) Uani 1 2 d SD . . C27 C 0.4379(4) 0.4218(3) 0.2297(5) 0.182(4) Uani 1 1 d D . . H27A H 0.4498 0.4393 0.2895 0.218 Uiso 1 1 calc R . . H27B H 0.4001 0.3979 0.2130 0.218 Uiso 1 1 calc R . . C28 C 0.4111(6) 0.4622(3) 0.1483(5) 0.287(8) Uani 1 1 d D . . H28A H 0.3717 0.4799 0.1415 0.430 Uiso 1 1 calc R . . H28B H 0.3973 0.4454 0.0879 0.430 Uiso 1 1 calc R . . H28C H 0.4474 0.4868 0.1645 0.430 Uiso 1 1 calc R . . C29 C 0.5222(3) 0.3586(2) 0.3388(3) 0.0888(14) Uani 1 1 d D . . H29A H 0.5343 0.3820 0.3926 0.107 Uiso 1 1 calc R . . H29B H 0.5641 0.3398 0.3558 0.107 Uiso 1 1 calc R . . C30 C 0.4698(2) 0.32048(18) 0.3303(4) 0.0836(13) Uani 1 1 d D . . H30A H 0.4888 0.3024 0.3911 0.125 Uiso 1 1 calc R . . H30B H 0.4587 0.2961 0.2792 0.125 Uiso 1 1 calc R . . H30C H 0.4283 0.3385 0.3149 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0436(2) 0.0252(2) 0.0325(2) -0.00376(17) 0.02325(19) -0.00277(18) Mn2 0.0319(2) 0.0275(2) 0.0323(2) -0.00095(17) 0.01769(17) -0.00193(17) Mn3 0.0319(2) 0.0253(2) 0.0281(2) -0.00255(16) 0.01432(17) -0.00195(16) Mn4 0.0412(2) 0.0270(2) 0.0299(2) 0.00130(17) 0.01999(19) -0.00109(18) Na1 0.0426(10) 0.0906(16) 0.0701(13) 0.000 0.0369(10) 0.000 O1 0.0579(13) 0.0334(11) 0.0415(11) -0.0089(9) 0.0308(10) -0.0031(10) O2 0.0799(18) 0.0348(12) 0.0683(16) -0.0111(12) 0.0385(14) 0.0082(12) O3 0.0451(13) 0.0387(12) 0.0526(13) -0.0127(10) 0.0186(11) -0.0069(10) O4 0.0399(11) 0.0371(11) 0.0536(12) -0.0075(10) 0.0247(10) -0.0093(9) O5 0.0437(12) 0.0409(12) 0.0440(12) -0.0068(10) 0.0203(10) 0.0018(10) O6 0.0398(11) 0.0349(11) 0.0345(10) -0.0011(9) 0.0140(9) 0.0048(9) O7 0.0572(13) 0.0391(11) 0.0344(10) -0.0049(9) 0.0289(10) -0.0094(10) O8 0.0486(12) 0.0405(11) 0.0408(11) -0.0079(9) 0.0290(10) -0.0079(9) O9 0.0414(12) 0.0407(12) 0.0493(12) 0.0078(10) 0.0222(10) 0.0030(10) O10 0.0369(11) 0.0398(12) 0.0534(12) 0.0056(10) 0.0262(10) 0.0057(9) O11 0.0450(12) 0.0389(11) 0.0454(12) 0.0043(10) 0.0256(10) -0.0037(9) O12 0.0409(11) 0.0345(11) 0.0341(10) -0.0046(9) 0.0172(9) -0.0068(9) O13 0.0552(13) 0.0432(12) 0.0362(11) -0.0037(9) 0.0288(10) -0.0065(10) O14 0.0497(12) 0.0411(12) 0.0321(10) -0.0039(9) 0.0177(10) -0.0080(10) O15 0.0406(11) 0.0545(13) 0.0341(10) -0.0037(10) 0.0223(9) -0.0035(10) O16 0.0446(11) 0.0438(12) 0.0309(10) -0.0023(9) 0.0216(9) -0.0033(9) O17 0.0334(10) 0.0255(9) 0.0300(9) -0.0030(7) 0.0169(8) -0.0045(7) O18 0.0352(10) 0.0263(9) 0.0297(9) -0.0004(8) 0.0179(8) -0.0012(8) O19 0.0599(13) 0.0334(11) 0.0394(11) 0.0074(9) 0.0296(10) 0.0005(10) O20 0.147(3) 0.0411(14) 0.0652(17) 0.0237(13) 0.0598(19) 0.0300(16) N1 0.0462(14) 0.0319(12) 0.0409(13) 0.0004(11) 0.0254(11) 0.0014(11) N2 0.187(5) 0.066(2) 0.100(3) 0.041(2) 0.108(3) 0.037(3) N3 0.0414(13) 0.0303(12) 0.0362(12) 0.0021(10) 0.0204(11) -0.0004(10) N4 0.088(2) 0.0490(17) 0.0597(19) -0.0032(15) 0.0454(18) 0.0096(16) C1 0.089(3) 0.049(2) 0.055(2) 0.0029(17) 0.053(2) 0.0099(19) C2 0.155(5) 0.073(3) 0.075(3) 0.028(2) 0.086(3) 0.032(3) C3 0.102(3) 0.041(2) 0.083(3) 0.018(2) 0.059(3) 0.017(2) C4 0.0484(17) 0.0306(15) 0.0443(16) 0.0037(13) 0.0241(14) 0.0045(13) C5 0.0376(15) 0.0340(15) 0.0445(16) -0.0073(13) 0.0171(13) 0.0011(13) C6 0.0384(17) 0.0332(16) 0.062(2) -0.0044(15) 0.0177(16) -0.0058(14) C7 0.045(2) 0.074(3) 0.147(5) -0.056(3) 0.021(3) -0.016(2) C8 0.0383(15) 0.0370(15) 0.0394(15) 0.0047(13) 0.0201(13) 0.0018(13) C9 0.065(2) 0.054(2) 0.0468(19) 0.0042(17) 0.0141(17) 0.0229(18) C10 0.0399(15) 0.0361(15) 0.0391(15) 0.0004(13) 0.0253(13) -0.0006(13) C11 0.075(2) 0.060(2) 0.0531(19) -0.0050(17) 0.0472(19) -0.0148(19) C12 0.0361(15) 0.0408(16) 0.0349(15) -0.0037(13) 0.0141(13) 0.0044(13) C13 0.057(2) 0.056(2) 0.081(3) 0.011(2) 0.040(2) 0.0179(18) C14 0.0423(16) 0.0315(14) 0.0390(15) -0.0086(13) 0.0262(14) -0.0052(12) C15 0.0496(19) 0.056(2) 0.062(2) -0.0017(18) 0.0297(17) -0.0159(17) C16 0.0434(16) 0.0418(16) 0.0283(13) 0.0001(13) 0.0168(13) 0.0039(14) C17 0.084(3) 0.072(3) 0.0375(17) -0.0125(18) 0.0321(19) -0.010(2) C18 0.0483(17) 0.0307(14) 0.0361(14) 0.0049(12) 0.0267(14) 0.0060(13) C19 0.057(2) 0.084(3) 0.0375(16) 0.0037(17) 0.0302(16) 0.0070(19) C20 0.0466(17) 0.0405(16) 0.0387(16) 0.0033(13) 0.0220(14) -0.0018(14) C21 0.057(2) 0.053(2) 0.0406(17) -0.0021(15) 0.0278(15) -0.0026(16) C22 0.087(3) 0.0394(18) 0.059(2) 0.0070(17) 0.040(2) 0.0201(19) C23 0.0526(18) 0.0320(15) 0.0423(16) 0.0039(13) 0.0251(14) 0.0066(14) C24 0.069(2) 0.0336(16) 0.0461(18) 0.0051(14) 0.0305(17) 0.0017(16) C25 0.161(15) 0.086(7) 0.156(13) 0.013(7) 0.114(14) 0.022(8) N6 0.122(4) 0.051(3) 0.042(2) 0.000 0.043(3) 0.000 C27 0.280(10) 0.171(7) 0.094(4) 0.025(5) 0.102(6) 0.118(7) C28 0.59(2) 0.182(8) 0.135(6) 0.109(6) 0.225(10) 0.270(11) C29 0.094(3) 0.095(4) 0.063(3) 0.011(3) 0.033(2) 0.001(3) C30 0.077(3) 0.090(3) 0.091(3) -0.005(3) 0.050(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O17 1.8439(18) . ? Mn1 O7 1.9134(19) . ? Mn1 O1 1.927(2) . ? Mn1 N1 2.080(2) . ? Mn1 O3 2.211(2) . ? Mn1 O5 2.222(2) . ? Mn2 O18 1.8864(18) . ? Mn2 O17 1.9100(19) . ? Mn2 O4 1.939(2) . ? Mn2 O10 1.966(2) . ? Mn2 O14 2.173(2) . ? Mn2 O15 2.178(2) . ? Mn2 Mn3 2.8322(13) . ? Mn2 Na1 3.3048(10) . ? Mn3 O17 1.8856(18) . ? Mn3 O18 1.9119(19) . ? Mn3 O12 1.936(2) . ? Mn3 O6 1.946(2) . ? Mn3 O8 2.206(2) . ? Mn3 O16 2.255(2) . ? Mn4 O18 1.8430(18) . ? Mn4 O19 1.918(2) . ? Mn4 O13 1.956(2) . ? Mn4 N3 2.103(2) . ? Mn4 O11 2.141(2) . ? Mn4 O9 2.193(2) . ? Na1 O15 2.300(2) 2_656 ? Na1 O15 2.300(2) . ? Na1 O4 2.572(2) . ? Na1 O4 2.572(2) 2_656 ? Na1 N5' 2.665(18) 2_656 ? Na1 N5' 2.665(18) . ? Na1 N5 2.744(18) . ? Na1 O10 2.832(3) 2_656 ? Na1 O10 2.832(3) . ? Na1 Mn2 3.3048(10) 2_656 ? O1 C5 1.296(4) . ? O2 C5 1.218(3) . ? O3 C6 1.244(4) . ? O4 C6 1.271(4) . ? O5 C8 1.243(3) . ? O6 C8 1.274(3) . ? O7 C10 1.296(3) . ? O8 C10 1.237(3) . ? O9 C12 1.241(4) . ? O10 C12 1.273(4) . ? O11 C14 1.242(3) . ? O12 C14 1.285(3) . ? O13 C16 1.273(4) . ? O14 C16 1.237(4) . ? O15 C18 1.264(4) . ? O16 C18 1.249(4) . ? O19 C24 1.297(4) . ? O20 C24 1.208(4) . ? N1 C1 1.330(4) . ? N1 C4 1.346(4) . ? N2 C2 1.322(5) . ? N2 C3 1.332(5) . ? N3 C20 1.336(4) . ? N3 C23 1.340(4) . ? N4 C21 1.321(4) . ? N4 C22 1.339(4) . ? C1 C2 1.374(5) . ? C1 H1A 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.376(5) . ? C3 H3A 0.9300 . ? C4 C5 1.491(4) . ? C6 C7 1.502(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.502(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.497(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.499(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.497(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.511(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.500(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.377(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.373(4) . ? C22 H22A 0.9300 . ? C23 C24 1.504(4) . ? C25 N5' 1.167(16) . ? C25 N5 1.182(15) . ? C25 C25 1.22(3) 2_656 ? C25 C26' 1.492(16) . ? C25 N5' 1.60(2) 2_656 ? C25 C26 1.613(16) . ? C25 C26' 2.02(2) 2_656 ? N5 C25 1.182(15) 2_656 ? N5' N5' 1.05(5) 2_656 ? N5' C25 1.60(2) 2_656 ? C26' C26' 1.54(5) 2_656 ? C26' C25 2.02(2) 2_656 ? N6 C29 1.493(5) 2_655 ? N6 C29 1.493(5) . ? N6 C27 1.505(7) 2_655 ? N6 C27 1.505(7) . ? C27 C28 1.529(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.496(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O17 Mn1 O7 97.01(8) . . ? O17 Mn1 O1 172.45(8) . . ? O7 Mn1 O1 90.49(9) . . ? O17 Mn1 N1 92.17(9) . . ? O7 Mn1 N1 168.87(9) . . ? O1 Mn1 N1 80.49(9) . . ? O17 Mn1 O3 90.34(8) . . ? O7 Mn1 O3 99.59(9) . . ? O1 Mn1 O3 87.49(9) . . ? N1 Mn1 O3 86.60(10) . . ? O17 Mn1 O5 92.01(8) . . ? O7 Mn1 O5 92.97(9) . . ? O1 Mn1 O5 88.51(8) . . ? N1 Mn1 O5 80.38(9) . . ? O3 Mn1 O5 166.85(9) . . ? O18 Mn2 O17 82.56(8) . . ? O18 Mn2 O4 178.44(9) . . ? O17 Mn2 O4 96.10(8) . . ? O18 Mn2 O10 96.94(8) . . ? O17 Mn2 O10 168.16(8) . . ? O4 Mn2 O10 84.53(9) . . ? O18 Mn2 O14 91.56(8) . . ? O17 Mn2 O14 100.13(8) . . ? O4 Mn2 O14 87.88(9) . . ? O10 Mn2 O14 91.71(9) . . ? O18 Mn2 O15 94.36(8) . . ? O17 Mn2 O15 86.41(8) . . ? O4 Mn2 O15 86.34(9) . . ? O10 Mn2 O15 81.82(9) . . ? O14 Mn2 O15 171.70(8) . . ? O18 Mn2 Mn3 42.13(6) . . ? O17 Mn2 Mn3 41.41(5) . . ? O4 Mn2 Mn3 136.69(7) . . ? O10 Mn2 Mn3 134.82(6) . . ? O14 Mn2 Mn3 104.82(7) . . ? O15 Mn2 Mn3 83.45(6) . . ? O18 Mn2 Na1 130.28(6) . . ? O17 Mn2 Na1 112.92(6) . . ? O4 Mn2 Na1 51.00(7) . . ? O10 Mn2 Na1 58.62(7) . . ? O14 Mn2 Na1 128.00(6) . . ? O15 Mn2 Na1 43.90(6) . . ? Mn3 Mn2 Na1 126.66(2) . . ? O17 Mn3 O18 82.53(8) . . ? O17 Mn3 O12 173.72(8) . . ? O18 Mn3 O12 94.48(9) . . ? O17 Mn3 O6 95.30(9) . . ? O18 Mn3 O6 170.17(8) . . ? O12 Mn3 O6 88.56(9) . . ? O17 Mn3 O8 89.60(8) . . ? O18 Mn3 O8 98.06(8) . . ? O12 Mn3 O8 85.33(8) . . ? O6 Mn3 O8 91.49(8) . . ? O17 Mn3 O16 90.26(8) . . ? O18 Mn3 O16 85.46(8) . . ? O12 Mn3 O16 95.03(8) . . ? O6 Mn3 O16 84.96(8) . . ? O8 Mn3 O16 176.42(8) . . ? O17 Mn3 Mn2 42.07(6) . . ? O18 Mn3 Mn2 41.44(6) . . ? O12 Mn3 Mn2 135.71(6) . . ? O6 Mn3 Mn2 134.00(7) . . ? O8 Mn3 Mn2 102.14(6) . . ? O16 Mn3 Mn2 80.09(6) . . ? O18 Mn4 O19 172.37(9) . . ? O18 Mn4 O13 97.08(8) . . ? O19 Mn4 O13 90.03(9) . . ? O18 Mn4 N3 92.63(8) . . ? O19 Mn4 N3 79.92(9) . . ? O13 Mn4 N3 166.88(9) . . ? O18 Mn4 O11 91.25(8) . . ? O19 Mn4 O11 90.16(9) . . ? O13 Mn4 O11 100.53(9) . . ? N3 Mn4 O11 88.01(9) . . ? O18 Mn4 O9 92.31(8) . . ? O19 Mn4 O9 84.81(9) . . ? O13 Mn4 O9 90.69(9) . . ? N3 Mn4 O9 80.09(9) . . ? O11 Mn4 O9 167.71(8) . . ? O15 Na1 O15 148.67(16) 2_656 . ? O15 Na1 O4 117.62(7) 2_656 . ? O15 Na1 O4 70.54(7) . . ? O15 Na1 O4 70.54(7) 2_656 2_656 ? O15 Na1 O4 117.62(7) . 2_656 ? O4 Na1 O4 152.04(14) . 2_656 ? O15 Na1 N5' 96.9(5) 2_656 2_656 ? O15 Na1 N5' 114.2(5) . 2_656 ? O4 Na1 N5' 73.4(4) . 2_656 ? O4 Na1 N5' 79.2(5) 2_656 2_656 ? O15 Na1 N5' 114.2(5) 2_656 . ? O15 Na1 N5' 96.9(5) . . ? O4 Na1 N5' 79.2(5) . . ? O4 Na1 N5' 73.4(4) 2_656 . ? N5' Na1 N5' 22.7(11) 2_656 . ? O15 Na1 N5 105.66(8) 2_656 . ? O15 Na1 N5 105.66(8) . . ? O4 Na1 N5 76.02(7) . . ? O4 Na1 N5 76.02(7) 2_656 . ? N5' Na1 N5 11.4(6) 2_656 . ? N5' Na1 N5 11.4(6) . . ? O15 Na1 O10 62.98(8) 2_656 2_656 ? O15 Na1 O10 94.59(9) . 2_656 ? O4 Na1 O10 150.01(11) . 2_656 ? O4 Na1 O10 57.92(6) 2_656 2_656 ? N5' Na1 O10 136.2(4) 2_656 2_656 ? N5' Na1 O10 129.6(5) . 2_656 ? N5 Na1 O10 133.89(6) . 2_656 ? O15 Na1 O10 94.59(9) 2_656 . ? O15 Na1 O10 62.98(8) . . ? O4 Na1 O10 57.92(6) . . ? O4 Na1 O10 150.01(11) 2_656 . ? N5' Na1 O10 129.6(5) 2_656 . ? N5' Na1 O10 136.2(4) . . ? N5 Na1 O10 133.89(6) . . ? O10 Na1 O10 92.21(11) 2_656 . ? O15 Na1 Mn2 41.04(5) 2_656 2_656 ? O15 Na1 Mn2 128.35(7) . 2_656 ? O4 Na1 Mn2 158.45(5) . 2_656 ? O4 Na1 Mn2 35.86(5) 2_656 2_656 ? N5' Na1 Mn2 102.6(4) 2_656 2_656 ? N5' Na1 Mn2 105.5(4) . 2_656 ? N5 Na1 Mn2 104.34(4) . 2_656 ? O10 Na1 Mn2 36.35(4) 2_656 2_656 ? O10 Na1 Mn2 117.51(8) . 2_656 ? O15 Na1 Mn2 128.35(7) 2_656 . ? O15 Na1 Mn2 41.04(5) . . ? O4 Na1 Mn2 35.86(5) . . ? O4 Na1 Mn2 158.45(5) 2_656 . ? N5' Na1 Mn2 105.5(4) 2_656 . ? N5' Na1 Mn2 102.6(4) . . ? N5 Na1 Mn2 104.34(4) . . ? O10 Na1 Mn2 117.51(8) 2_656 . ? O10 Na1 Mn2 36.35(4) . . ? Mn2 Na1 Mn2 151.32(8) 2_656 . ? C5 O1 Mn1 118.93(18) . . ? C6 O3 Mn1 132.8(2) . . ? C6 O4 Mn2 124.3(2) . . ? C6 O4 Na1 140.4(2) . . ? Mn2 O4 Na1 93.13(9) . . ? C8 O5 Mn1 128.45(19) . . ? C8 O6 Mn3 129.04(18) . . ? C10 O7 Mn1 126.09(18) . . ? C10 O8 Mn3 132.70(19) . . ? C12 O9 Mn4 130.29(19) . . ? C12 O10 Mn2 127.0(2) . . ? C12 O10 Na1 146.97(19) . . ? Mn2 O10 Na1 85.03(8) . . ? C14 O11 Mn4 132.23(19) . . ? C14 O12 Mn3 127.24(18) . . ? C16 O13 Mn4 126.45(19) . . ? C16 O14 Mn2 132.17(19) . . ? C18 O15 Mn2 124.35(19) . . ? C18 O15 Na1 140.43(19) . . ? Mn2 O15 Na1 95.06(8) . . ? C18 O16 Mn3 125.19(18) . . ? Mn1 O17 Mn3 123.72(10) . . ? Mn1 O17 Mn2 127.85(10) . . ? Mn3 O17 Mn2 96.52(8) . . ? Mn4 O18 Mn2 122.59(10) . . ? Mn4 O18 Mn3 130.49(10) . . ? Mn2 O18 Mn3 96.42(8) . . ? C24 O19 Mn4 118.96(19) . . ? C1 N1 C4 118.7(3) . . ? C1 N1 Mn1 129.6(2) . . ? C4 N1 Mn1 111.23(19) . . ? C2 N2 C3 116.5(3) . . ? C20 N3 C23 117.8(3) . . ? C20 N3 Mn4 131.0(2) . . ? C23 N3 Mn4 111.00(19) . . ? C21 N4 C22 115.8(3) . . ? N1 C1 C2 119.5(3) . . ? N1 C1 H1A 120.3 . . ? C2 C1 H1A 120.3 . . ? N2 C2 C1 123.3(4) . . ? N2 C2 H2B 118.4 . . ? C1 C2 H2B 118.4 . . ? N2 C3 C4 122.1(3) . . ? N2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? N1 C4 C3 119.9(3) . . ? N1 C4 C5 114.9(3) . . ? C3 C4 C5 125.1(3) . . ? O2 C5 O1 125.3(3) . . ? O2 C5 C4 120.5(3) . . ? O1 C5 C4 114.2(2) . . ? O3 C6 O4 125.2(3) . . ? O3 C6 C7 119.4(3) . . ? O4 C6 C7 115.3(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 O6 125.2(3) . . ? O5 C8 C9 118.9(3) . . ? O6 C8 C9 115.9(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O8 C10 O7 124.8(3) . . ? O8 C10 C11 119.8(3) . . ? O7 C10 C11 115.5(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O10 125.3(3) . . ? O9 C12 C13 118.6(3) . . ? O10 C12 C13 116.1(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O11 C14 O12 125.9(3) . . ? O11 C14 C15 118.6(3) . . ? O12 C14 C15 115.6(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O14 C16 O13 126.1(3) . . ? O14 C16 C17 118.3(3) . . ? O13 C16 C17 115.6(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O16 C18 O15 124.8(3) . . ? O16 C18 C19 119.1(3) . . ? O15 C18 C19 116.1(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 120.2(3) . . ? N3 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? N4 C21 C20 123.2(3) . . ? N4 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? N4 C22 C23 122.6(3) . . ? N4 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? N3 C23 C22 120.3(3) . . ? N3 C23 C24 114.5(3) . . ? C22 C23 C24 125.1(3) . . ? O20 C24 O19 125.7(3) . . ? O20 C24 C23 120.4(3) . . ? O19 C24 C23 113.9(3) . . ? N5' C25 N5 26.7(13) . . ? N5' C25 C25 83.7(16) . 2_656 ? N5 C25 C25 58.8(9) . 2_656 ? N5' C25 C26' 177(2) . . ? N5 C25 C26' 153.3(18) . . ? C25 C25 C26' 95.3(12) 2_656 . ? N5' C25 N5' 41(2) . 2_656 ? N5 C25 N5' 14.6(12) . 2_656 ? C25 C25 N5' 46.6(7) 2_656 2_656 ? C26' C25 N5' 139.1(15) . 2_656 ? N5' C25 C26 153(2) . . ? N5 C25 C26 177.1(15) . . ? C25 C25 C26 120.0(11) 2_656 . ? C26' C25 C26 26.4(12) . . ? N5' C25 C26 165.5(15) 2_656 . ? N5' C25 C26' 128.8(17) . 2_656 ? N5 C25 C26' 106.0(12) . 2_656 ? C25 C25 C26' 47.5(7) 2_656 2_656 ? C26' C25 C26' 49.5(15) . 2_656 ? N5' C25 C26' 94.0(10) 2_656 2_656 ? C26 C25 C26' 72.6(13) . 2_656 ? C25 N5 C25 62.4(18) 2_656 . ? C25 N5 Na1 148.8(9) 2_656 . ? C25 N5 Na1 148.8(9) . . ? N5' N5' C25 91.9(18) 2_656 . ? N5' N5' C25 46.9(8) 2_656 2_656 ? C25 N5' C25 49.7(14) . 2_656 ? N5' N5' Na1 78.6(6) 2_656 . ? C25 N5' Na1 165(2) . . ? C25 N5' Na1 124.5(12) 2_656 . ? C25 C26' C26' 83.2(11) . 2_656 ? C25 C26' C25 37.2(10) . 2_656 ? C26' C26' C25 47.3(7) 2_656 2_656 ? C29 N6 C29 113.3(5) 2_655 . ? C29 N6 C27 106.9(3) 2_655 2_655 ? C29 N6 C27 107.4(3) . 2_655 ? C29 N6 C27 107.4(3) 2_655 . ? C29 N6 C27 106.9(3) . . ? C27 N6 C27 115.3(8) 2_655 . ? N6 C27 C28 116.2(7) . . ? N6 C27 H27A 108.2 . . ? C28 C27 H27A 108.2 . . ? N6 C27 H27B 108.2 . . ? C28 C27 H27B 108.2 . . ? H27A C27 H27B 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 C30 116.0(4) . . ? N6 C29 H29A 108.3 . . ? C30 C29 H29A 108.3 . . ? N6 C29 H29B 108.3 . . ? C30 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.879 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.070 #==END