# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Reedijk, Jan' _publ_contact_author_email reedijk@chem.leidenuniv.nl _publ_section_title ; Trigonal Propeller-shaped MnIII3MIINa Complexes (M = Mn, Ca): Structural and Functional Models for the Dioxygen Evolving Centre of PSII ; loop_ _publ_author_name J.Reedijk H.Nayek S.Dehnen A.Powell S.Nayak data_NS174 _database_code_depnum_ccdc_archive 'CCDC 793192' #TrackingRef '2417_web_deposit_cif_file_0_JanReedijk_1284191254.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.44 H29 Cl3.50 Mn4 N4.50 Na O12.44' _chemical_formula_weight 1047.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7691(5) _cell_length_b 12.7467(5) _cell_length_c 19.0201(8) _cell_angle_alpha 108.120(3) _cell_angle_beta 91.029(4) _cell_angle_gamma 101.741(3) _cell_volume 2195.48(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8 _cell_measurement_theta_min 0 _cell_measurement_theta_max 180 _exptl_crystal_description block-shaped _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8493 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details 'SADABS-2008/1, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21131 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.73 _reflns_number_total 9305 _reflns_number_gt 6594 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9305 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1957 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 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 0.41012(5) 0.36729(4) 0.21587(3) 0.04794(12) Uani 1 1 d . B . Mn2 Mn 0.62407(5) 0.34179(4) 0.34011(2) 0.04406(12) Uani 1 1 d . . . Mn4 Mn 0.31746(6) 0.11766(4) 0.26725(3) 0.05115(13) Uani 1 1 d . . . Mn3 Mn 0.60832(5) 0.18637(4) 0.16715(2) 0.04556(12) Uani 1 1 d . . . Cl2 Cl 0.41829(10) 0.21593(7) 0.08353(4) 0.0568(2) Uani 1 1 d . B . Cl3 Cl 0.94332(10) 0.61903(9) 0.18960(6) 0.0688(3) Uani 1 1 d . . . Cl4 Cl 0.45932(11) 0.49123(8) 0.35478(5) 0.0644(2) Uani 1 1 d . B . O11 O 0.7564(2) 0.27781(17) 0.13368(11) 0.0465(5) Uani 1 1 d . B . O12 O 0.5229(2) 0.48239(17) 0.18508(12) 0.0482(5) Uani 1 1 d . . . O1 O 0.5697(2) 0.31608(16) 0.23848(11) 0.0429(5) Uani 1 1 d . B . O22 O 0.4744(3) 0.08038(17) 0.19440(12) 0.0517(6) Uani 1 1 d . C . O2 O 0.4749(2) 0.23009(18) 0.35121(11) 0.0512(6) Uani 1 1 d . C . O3 O 0.7816(2) 0.45949(18) 0.34186(11) 0.0490(6) Uani 1 1 d . B . O4 O 0.2783(3) 0.2571(2) 0.24161(17) 0.0751(8) Uani 1 1 d . B . N2 N 0.6589(3) 0.3742(2) 0.44818(14) 0.0544(8) Uani 1 1 d . C . N7 N 0.6573(3) 0.0474(2) 0.10049(15) 0.0565(8) Uani 1 1 d . C . O5 O 0.2221(3) 0.1214(2) 0.37252(14) 0.0711(8) Uani 1 1 d . C . O6 O 0.3079(3) -0.0639(2) 0.24601(17) 0.0784(9) Uani 1 1 d . C . C355 C 0.9069(3) 0.3320(3) 0.05141(17) 0.0492(8) Uani 1 1 d . C . H355 H 0.9057 0.4088 0.0767 0.059 Uiso 1 1 calc R . . N8 N 0.2390(3) 0.4151(2) 0.19336(16) 0.0545(7) Uani 1 1 d . . . C45 C 0.7440(4) 0.0406(3) 0.04995(17) 0.0508(8) Uani 1 1 d . . . O9 O 0.1029(3) 0.0599(3) 0.2091(2) 0.0930(11) Uani 1 1 d . B . C6 C 0.3429(3) 0.5339(3) 0.12342(17) 0.0472(8) Uani 1 1 d . . . C7 C 0.7441(4) 0.4590(3) 0.49381(17) 0.0539(9) Uani 1 1 d . . . C8 C 0.8253(4) 0.1331(3) 0.03377(17) 0.0501(8) Uani 1 1 d . C . C9 C 0.2285(4) 0.4798(3) 0.15435(18) 0.0518(8) Uani 1 1 d . C . C10 C 0.4321(5) 0.2547(4) 0.4246(2) 0.0712(12) Uani 1 1 d . . . H10 H 0.3861 0.3205 0.4341 0.085 Uiso 1 1 calc R C . C11 C 0.9253(4) 0.6302(3) 0.5326(2) 0.0616(10) Uani 1 1 d . . . H11 H 0.9132 0.6324 0.5824 0.074 Uiso 1 1 calc R C . C12 C 0.5874(4) 0.5895(2) 0.10560(17) 0.0473(8) Uani 1 1 d . . . H12 H 0.6834 0.5915 0.1165 0.057 Uiso 1 1 calc R C . C13 C 0.8576(4) 0.5387(3) 0.39970(18) 0.0498(8) Uani 1 1 d . . . C14 C 0.9891(5) 0.1962(4) -0.0471(2) 0.0727(12) Uani 1 1 d . C . H14 H 1.0444 0.1792 -0.0880 0.087 Uiso 1 1 calc R . . C16 C 0.8411(4) 0.5423(3) 0.47418(18) 0.0513(8) Uani 1 1 d . C . C18 C 0.9093(4) 0.1115(3) -0.0271(2) 0.0630(11) Uani 1 1 d . . . H18 H 0.9095 0.0353 -0.0548 0.076 Uiso 1 1 calc R C . C19 C 0.9893(4) 0.3078(3) -0.00719(19) 0.0588(10) Uani 1 1 d . . . H19 H 1.0463 0.3676 -0.0202 0.071 Uiso 1 1 calc R C . C20 C 0.9624(5) 0.6196(3) 0.3871(2) 0.0662(11) Uani 1 1 d . C . H20 H 0.9788 0.6162 0.3374 0.079 Uiso 1 1 calc R . . C21 C 1.0244(5) 0.7126(3) 0.5188(2) 0.0711(12) Uani 1 1 d . C . H21 H 1.0781 0.7730 0.5587 0.085 Uiso 1 1 calc R . . C22 C 1.0453(5) 0.7067(4) 0.4458(2) 0.0776(13) Uani 1 1 d . . . H22 H 1.1160 0.7619 0.4356 0.093 Uiso 1 1 calc R C . C23 C 0.3290(5) 0.1594(4) 0.4331(2) 0.0776(13) Uani 1 1 d . C . H23A H 0.3753 0.0971 0.4330 0.093 Uiso 1 1 calc R . . H23B H 0.2868 0.1834 0.4808 0.093 Uiso 1 1 calc R . . C26 C 0.5801(6) -0.0557(3) 0.1130(3) 0.0916(15) Uani 1 1 d . . . H26A H 0.5343 -0.1106 0.0651 0.110 Uiso 1 1 calc R C . H26B H 0.6466 -0.0906 0.1330 0.110 Uiso 1 1 calc R . . C27 C 0.5647(5) 0.2924(4) 0.4758(2) 0.0723(12) Uani 1 1 d . C . H27A H 0.5454 0.3286 0.5276 0.087 Uiso 1 1 calc R . . H27B H 0.6069 0.2273 0.4738 0.087 Uiso 1 1 calc R . . C28 C 0.4786(5) -0.0318(3) 0.1627(3) 0.0949(16) Uani 1 1 d . C . C29 C 0.3971(6) -0.1087(3) 0.1927(3) 0.0979(17) Uani 1 1 d . . . H29A H 0.4611 -0.1421 0.2158 0.117 Uiso 1 1 calc R C . H29B H 0.3388 -0.1709 0.1515 0.117 Uiso 1 1 calc R . . C35 C 0.8267(3) 0.2493(3) 0.07445(16) 0.0451(7) Uani 1 1 d . . . Na5 Na 0.74652(13) 0.46187(10) 0.21774(7) 0.0480(3) Uani 1 1 d . B . C121 C 0.4850(3) 0.5332(2) 0.13868(17) 0.0450(7) Uani 1 1 d . C . C122 C 0.5517(4) 0.6431(3) 0.05674(18) 0.0521(9) Uani 1 1 d . C . H122 H 0.6235 0.6804 0.0342 0.062 Uiso 1 1 calc R . . C124 C 0.3098(4) 0.5912(3) 0.07459(18) 0.0525(9) Uani 1 1 d . C . H124 H 0.2149 0.5938 0.0654 0.063 Uiso 1 1 calc R . . C123 C 0.4119(4) 0.6429(3) 0.04044(18) 0.0533(9) Uani 1 1 d . . . H123 H 0.3879 0.6781 0.0061 0.064 Uiso 1 1 calc R C . C111 C 0.1151(4) 0.3596(4) 0.2210(3) 0.0785(11) Uani 1 1 d . B . H11A H 0.0267 0.3621 0.1959 0.094 Uiso 1 1 calc R A 1 H11B H 0.1140 0.3929 0.2754 0.094 Uiso 1 1 calc R A 1 OW1 O 1.1938(4) 0.7742(3) 0.29880(19) 0.0677(10) Uani 0.814(4) 1 d P . . OW3 O 0.9022(6) 0.8829(4) 0.2231(3) 0.125(2) Uani 0.814(4) 1 d P . . OW2 O 1.0546(6) 0.9446(4) 0.3881(3) 0.127(2) Uani 0.814(4) 1 d P . . CW2 C 0.912(3) 0.9289(13) 0.4194(9) 0.366(10) Uani 0.814(4) 1 d P . . CW1 C 0.360(2) 0.7157(6) 0.3249(4) 0.286(9) Uani 0.814(4) 1 d P . . CW3 C 0.8662(15) 0.9700(10) 0.2152(13) 0.257(9) Uani 0.814(4) 1 d P . . C234 C 0.1428(6) 0.2315(5) 0.1976(3) 0.0410(14) Uani 0.50 1 d P B 1 H234 H 0.1500 0.1989 0.1431 0.028(13) Uiso 0.50 1 calc PR B 1 C236 C 0.0397(7) 0.1507(5) 0.2282(3) 0.0433(13) Uiso 0.50 1 d P B 1 H23C H 0.0366 0.1822 0.2826 0.052 Uiso 0.50 1 calc PR B 1 H23D H -0.0563 0.1312 0.2033 0.052 Uiso 0.50 1 calc PR B 1 C235 C 0.1331(10) 0.2731(7) 0.2452(5) 0.075(2) Uiso 0.50 1 d P B 2 H235 H 0.0911 0.2722 0.2926 0.090 Uiso 0.50 1 calc PR B 2 C237 C 0.0740(11) 0.1745(7) 0.1804(5) 0.077(2) Uiso 0.50 1 d P B 2 H23E H 0.1235 0.1778 0.1359 0.092 Uiso 0.50 1 calc PR B 2 H23F H -0.0273 0.1684 0.1695 0.092 Uiso 0.50 1 calc PR B 2 Cl7 Cl 0.7660(2) 0.20342(16) 0.28575(11) 0.0671(6) Uani 0.50 1 d P C 1 N330 N 0.7536(8) 0.1745(6) 0.2946(4) 0.0517(16) Uiso 0.50 1 d P D 2 N332 N 0.7435(8) 0.0565(5) 0.3281(4) 0.0690(19) Uani 0.50 1 d P D 2 N331 N 0.7432(6) 0.1257(4) 0.3078(3) 0.0467(13) Uani 0.50 1 d P D 2 H9 H 0.131(4) 0.509(3) 0.152(2) 0.066(11) Uiso 1 1 d . . . H45 H 0.758(3) -0.027(3) 0.0212(18) 0.042(8) Uiso 1 1 d . . . H7 H 0.745(4) 0.472(3) 0.5436(19) 0.050(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0394(2) 0.0521(2) 0.0509(2) 0.01946(19) -0.00111(19) 0.00280(19) Mn2 0.0455(2) 0.0457(2) 0.03443(19) 0.00808(17) 0.00050(18) 0.00343(19) Mn4 0.0508(3) 0.0497(2) 0.0433(2) 0.01006(19) 0.0055(2) -0.0029(2) Mn3 0.0519(3) 0.0420(2) 0.0368(2) 0.00877(17) 0.00583(19) 0.00298(19) Cl2 0.0620(5) 0.0563(4) 0.0412(3) 0.0124(3) -0.0096(3) -0.0046(4) Cl3 0.0551(5) 0.0836(5) 0.0692(5) 0.0336(4) 0.0042(4) 0.0048(4) Cl4 0.0720(5) 0.0688(4) 0.0534(4) 0.0159(4) 0.0119(4) 0.0229(4) O11 0.0514(11) 0.0457(10) 0.0374(9) 0.0097(8) 0.0069(9) 0.0052(9) O12 0.0421(11) 0.0535(10) 0.0488(10) 0.0202(9) -0.0020(9) 0.0051(9) O1 0.0420(10) 0.0427(9) 0.0373(9) 0.0097(8) 0.0001(8) -0.0002(8) O22 0.0630(13) 0.0421(10) 0.0419(10) 0.0078(8) 0.0092(10) 0.0017(10) O2 0.0545(12) 0.0549(11) 0.0373(10) 0.0118(9) 0.0038(9) 0.0016(10) O3 0.0485(11) 0.0519(11) 0.0369(10) 0.0076(8) -0.0004(9) 0.0002(9) O4 0.0401(12) 0.0907(14) 0.1094(17) 0.0632(13) -0.0020(12) -0.0005(12) N2 0.0604(16) 0.0570(14) 0.0377(12) 0.0112(11) -0.0022(12) 0.0016(13) N7 0.0725(18) 0.0448(12) 0.0450(13) 0.0097(11) 0.0100(13) 0.0042(13) O5 0.0709(16) 0.0787(16) 0.0512(13) 0.0156(12) 0.0129(12) -0.0038(14) O6 0.0926(19) 0.0484(12) 0.0842(17) 0.0163(12) 0.0339(15) -0.0011(13) C355 0.0492(16) 0.0545(15) 0.0405(14) 0.0132(12) -0.0013(13) 0.0074(13) N8 0.0447(14) 0.0637(14) 0.0524(14) 0.0203(12) -0.0004(12) 0.0037(12) C45 0.0597(18) 0.0460(15) 0.0383(14) 0.0047(12) 0.0035(14) 0.0066(14) O9 0.0594(16) 0.0828(18) 0.095(2) -0.0243(17) -0.0153(16) 0.0083(15) C6 0.0469(15) 0.0439(13) 0.0447(14) 0.0072(12) -0.0038(13) 0.0080(12) C7 0.0585(19) 0.0597(17) 0.0351(14) 0.0062(13) -0.0004(14) 0.0086(15) C8 0.0508(17) 0.0572(16) 0.0352(13) 0.0075(12) 0.0002(13) 0.0077(14) C9 0.0460(16) 0.0549(16) 0.0488(16) 0.0114(13) -0.0040(14) 0.0074(14) C10 0.079(3) 0.077(2) 0.0425(16) 0.0130(16) 0.0053(17) -0.006(2) C11 0.062(2) 0.0602(18) 0.0477(17) 0.0040(15) -0.0094(16) 0.0034(17) C12 0.0516(16) 0.0434(13) 0.0428(14) 0.0102(12) 0.0000(13) 0.0077(13) C13 0.0459(16) 0.0515(15) 0.0452(15) 0.0096(13) -0.0040(13) 0.0055(13) C14 0.068(2) 0.085(3) 0.0521(18) 0.0109(18) 0.0224(17) 0.005(2) C16 0.0516(17) 0.0505(15) 0.0419(15) 0.0033(13) -0.0044(13) 0.0083(14) C18 0.063(2) 0.0586(19) 0.0517(18) 0.0012(15) 0.0131(16) 0.0035(17) C19 0.0552(19) 0.0691(19) 0.0470(16) 0.0176(15) 0.0071(15) 0.0038(16) C20 0.071(2) 0.0615(19) 0.0520(18) 0.0136(15) -0.0098(17) -0.0073(18) C21 0.073(2) 0.063(2) 0.058(2) 0.0042(17) -0.0158(19) -0.0023(19) C22 0.079(3) 0.067(2) 0.064(2) 0.0110(19) -0.016(2) -0.017(2) C23 0.081(3) 0.096(3) 0.0481(18) 0.0263(18) 0.0066(19) -0.003(2) C26 0.148(4) 0.0436(17) 0.077(2) 0.0144(16) 0.062(2) 0.011(2) C27 0.080(3) 0.082(2) 0.0421(16) 0.0208(16) -0.0021(17) -0.013(2) C28 0.103(3) 0.0437(18) 0.130(3) 0.017(2) 0.068(3) 0.0111(19) C29 0.163(4) 0.0423(17) 0.081(2) 0.0137(17) 0.063(3) 0.011(2) C35 0.0399(14) 0.0563(15) 0.0350(13) 0.0119(12) -0.0002(11) 0.0063(12) Na5 0.0430(6) 0.0507(6) 0.0466(6) 0.0158(5) 0.0007(5) 0.0023(5) C121 0.0481(16) 0.0416(13) 0.0401(13) 0.0079(11) -0.0025(12) 0.0068(12) C122 0.0629(19) 0.0408(14) 0.0453(15) 0.0075(12) 0.0009(14) 0.0056(14) C124 0.0587(18) 0.0450(14) 0.0468(15) 0.0077(12) -0.0102(14) 0.0080(14) C123 0.0645(19) 0.0448(14) 0.0468(16) 0.0100(12) -0.0048(15) 0.0123(14) C111 0.0380(17) 0.115(2) 0.103(3) 0.068(2) 0.0032(17) 0.0101(18) OW1 0.065(2) 0.0665(16) 0.0693(18) 0.0295(14) 0.0076(15) -0.0025(15) OW3 0.123(4) 0.110(3) 0.094(3) -0.003(3) 0.038(3) -0.026(3) OW2 0.156(4) 0.089(3) 0.107(3) 0.029(2) 0.041(3) -0.036(3) CW2 0.65(3) 0.303(11) 0.323(10) 0.247(8) 0.317(14) 0.247(15) CW1 0.72(3) 0.064(3) 0.080(4) 0.031(3) 0.139(8) 0.072(8) CW3 0.173(10) 0.138(7) 0.48(3) 0.109(11) 0.094(13) 0.068(7) C234 0.030(3) 0.042(3) 0.035(3) -0.001(2) 0.000(2) -0.006(2) Cl7 0.0821(13) 0.0576(9) 0.0544(9) 0.0160(8) 0.0105(9) 0.0022(9) N332 0.085(4) 0.044(2) 0.077(4) 0.028(3) -0.017(3) 0.000(3) N331 0.053(3) 0.036(2) 0.052(3) 0.022(2) -0.009(2) 0.000(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.893(3) . ? Mn1 O1 1.899(2) . ? Mn1 O12 1.900(2) . ? Mn1 N8 1.975(3) . ? Mn1 Cl4 2.5994(10) . ? Mn1 Cl2 2.6672(9) . ? Mn1 Mn3 3.2370(7) . ? Mn1 Na5 3.2575(13) . ? Mn2 O2 1.884(2) . ? Mn2 O1 1.904(2) . ? Mn2 O3 1.910(2) . ? Mn2 N2 1.975(3) . ? Mn2 Cl7 2.452(2) . ? Mn2 Cl4 2.6889(11) . ? Mn2 Na5 3.2805(14) . ? Mn4 O4 2.087(3) . ? Mn4 O22 2.112(2) . ? Mn4 O2 2.135(2) . ? Mn4 O6 2.204(3) . ? Mn4 O5 2.215(3) . ? Mn4 O9 2.223(3) . ? Mn3 O22 1.883(2) . ? Mn3 O1 1.896(2) . ? Mn3 O11 1.914(2) . ? Mn3 N7 1.986(3) . ? Mn3 Cl2 2.5824(11) . ? Mn3 Cl7 2.635(2) . ? Mn3 Na5 3.3170(12) . ? Cl3 Na5 2.6706(16) . ? O11 C35 1.322(4) . ? O11 Na5 2.416(2) . ? O12 C121 1.333(4) . ? O12 Na5 2.348(3) . ? O1 Na5 2.402(2) . ? O22 C28 1.377(4) . ? O2 C10 1.423(4) . ? O3 C13 1.325(3) . ? O3 Na5 2.390(3) . ? O4 C235 1.474(10) . ? O4 C234 1.475(6) . ? N2 C7 1.280(4) . ? N2 C27 1.476(5) . ? N7 C45 1.287(5) . ? N7 C26 1.466(5) . ? O5 C23 1.434(5) . ? O6 C29 1.410(6) . ? C355 C35 1.371(5) . ? C355 C19 1.381(5) . ? N8 C9 1.286(5) . ? N8 C111 1.465(5) . ? C45 C8 1.403(5) . ? O9 C236 1.374(7) . ? O9 C237 1.780(11) . ? C6 C121 1.415(5) . ? C6 C124 1.418(5) . ? C6 C9 1.426(5) . ? C7 C16 1.419(5) . ? C8 C18 1.421(5) . ? C8 C35 1.439(4) . ? C10 C23 1.465(6) . ? C10 C27 1.505(6) . ? C11 C21 1.370(6) . ? C11 C16 1.409(4) . ? C12 C121 1.387(5) . ? C12 C122 1.390(5) . ? C13 C20 1.379(5) . ? C13 C16 1.416(5) . ? C14 C18 1.356(6) . ? C14 C19 1.388(6) . ? C20 C22 1.403(5) . ? C21 C22 1.387(6) . ? C26 C28 1.396(7) . ? C28 C29 1.403(6) . ? C122 C123 1.394(5) . ? C124 C123 1.369(5) . ? C111 C235 1.360(11) . ? C111 C234 1.635(7) . ? OW3 CW3 1.281(16) . ? OW2 CW2 1.53(2) . ? C234 C236 1.544(8) . ? C235 C237 1.466(12) . ? N330 N331 0.731(8) . ? N330 N332 1.793(10) . ? N332 N331 1.067(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O1 95.14(11) . . ? O4 Mn1 O12 172.88(11) . . ? O1 Mn1 O12 91.88(10) . . ? O4 Mn1 N8 82.39(12) . . ? O1 Mn1 N8 177.53(11) . . ? O12 Mn1 N8 90.59(11) . . ? O4 Mn1 Cl4 90.25(9) . . ? O1 Mn1 Cl4 82.26(6) . . ? O12 Mn1 Cl4 91.89(7) . . ? N8 Mn1 Cl4 97.86(9) . . ? O4 Mn1 Cl2 89.70(9) . . ? O1 Mn1 Cl2 81.59(6) . . ? O12 Mn1 Cl2 90.14(7) . . ? N8 Mn1 Cl2 98.21(8) . . ? Cl4 Mn1 Cl2 163.78(4) . . ? O4 Mn1 Mn3 88.61(9) . . ? O1 Mn1 Mn3 31.43(6) . . ? O12 Mn1 Mn3 96.78(7) . . ? N8 Mn1 Mn3 147.87(8) . . ? Cl4 Mn1 Mn3 113.03(3) . . ? Cl2 Mn1 Mn3 50.76(2) . . ? O4 Mn1 Na5 141.83(9) . . ? O1 Mn1 Na5 46.92(7) . . ? O12 Mn1 Na5 45.28(7) . . ? N8 Mn1 Na5 135.55(9) . . ? Cl4 Mn1 Na5 81.58(3) . . ? Cl2 Mn1 Na5 88.48(3) . . ? Mn3 Mn1 Na5 61.43(3) . . ? O2 Mn2 O1 94.81(9) . . ? O2 Mn2 O3 172.80(9) . . ? O1 Mn2 O3 92.37(9) . . ? O2 Mn2 N2 82.19(11) . . ? O1 Mn2 N2 173.07(12) . . ? O3 Mn2 N2 90.62(11) . . ? O2 Mn2 Cl7 92.77(9) . . ? O1 Mn2 Cl7 82.45(8) . . ? O3 Mn2 Cl7 88.65(9) . . ? N2 Mn2 Cl7 103.88(11) . . ? O2 Mn2 Cl4 92.23(8) . . ? O1 Mn2 Cl4 79.75(7) . . ? O3 Mn2 Cl4 88.56(8) . . ? N2 Mn2 Cl4 94.09(10) . . ? Cl7 Mn2 Cl4 161.85(6) . . ? O2 Mn2 Na5 141.10(7) . . ? O1 Mn2 Na5 46.37(6) . . ? O3 Mn2 Na5 46.04(7) . . ? N2 Mn2 Na5 135.99(9) . . ? Cl7 Mn2 Na5 85.31(6) . . ? Cl4 Mn2 Na5 79.87(3) . . ? O4 Mn4 O22 98.46(11) . . ? O4 Mn4 O2 88.77(10) . . ? O22 Mn4 O2 89.82(9) . . ? O4 Mn4 O6 154.75(12) . . ? O22 Mn4 O6 75.31(10) . . ? O2 Mn4 O6 115.30(11) . . ? O4 Mn4 O5 106.20(12) . . ? O22 Mn4 O5 151.04(11) . . ? O2 Mn4 O5 75.99(9) . . ? O6 Mn4 O5 87.96(11) . . ? O4 Mn4 O9 74.91(12) . . ? O22 Mn4 O9 112.65(11) . . ? O2 Mn4 O9 153.64(11) . . ? O6 Mn4 O9 84.86(13) . . ? O5 Mn4 O9 88.65(12) . . ? O22 Mn3 O1 95.81(9) . . ? O22 Mn3 O11 172.36(10) . . ? O1 Mn3 O11 91.33(9) . . ? O22 Mn3 N7 82.48(11) . . ? O1 Mn3 N7 174.48(12) . . ? O11 Mn3 N7 90.16(11) . . ? O22 Mn3 Cl2 90.76(8) . . ? O1 Mn3 Cl2 83.99(7) . . ? O11 Mn3 Cl2 92.70(7) . . ? N7 Mn3 Cl2 101.25(10) . . ? O22 Mn3 Cl7 86.61(9) . . ? O1 Mn3 Cl7 77.72(8) . . ? O11 Mn3 Cl7 92.27(8) . . ? N7 Mn3 Cl7 96.92(11) . . ? Cl2 Mn3 Cl7 161.14(6) . . ? O22 Mn3 Mn1 89.66(8) . . ? O1 Mn3 Mn1 31.48(6) . . ? O11 Mn3 Mn1 97.87(7) . . ? N7 Mn3 Mn1 153.25(10) . . ? Cl2 Mn3 Mn1 53.12(2) . . ? Cl7 Mn3 Mn1 108.14(5) . . ? O22 Mn3 Na5 141.05(7) . . ? O1 Mn3 Na5 45.41(7) . . ? O11 Mn3 Na5 45.93(6) . . ? N7 Mn3 Na5 135.68(9) . . ? Cl2 Mn3 Na5 88.64(3) . . ? Cl7 Mn3 Na5 81.82(5) . . ? Mn1 Mn3 Na5 59.59(3) . . ? Mn3 Cl2 Mn1 76.12(3) . . ? Mn1 Cl4 Mn2 76.13(3) . . ? C35 O11 Mn3 129.35(18) . . ? C35 O11 Na5 130.51(19) . . ? Mn3 O11 Na5 99.36(9) . . ? C121 O12 Mn1 127.98(19) . . ? C121 O12 Na5 129.6(2) . . ? Mn1 O12 Na5 99.62(10) . . ? Mn3 O1 Mn1 117.10(10) . . ? Mn3 O1 Mn2 117.70(12) . . ? Mn1 O1 Mn2 118.11(11) . . ? Mn3 O1 Na5 100.38(9) . . ? Mn1 O1 Na5 97.81(10) . . ? Mn2 O1 Na5 98.61(8) . . ? C28 O22 Mn3 116.5(2) . . ? C28 O22 Mn4 117.4(2) . . ? Mn3 O22 Mn4 126.03(11) . . ? C10 O2 Mn2 113.4(2) . . ? C10 O2 Mn4 114.4(2) . . ? Mn2 O2 Mn4 127.07(11) . . ? C13 O3 Mn2 129.1(2) . . ? C13 O3 Na5 128.8(2) . . ? Mn2 O3 Na5 98.84(9) . . ? C235 O4 C234 36.1(4) . . ? C235 O4 Mn1 116.3(4) . . ? C234 O4 Mn1 110.3(3) . . ? C235 O4 Mn4 116.7(4) . . ? C234 O4 Mn4 112.6(3) . . ? Mn1 O4 Mn4 127.02(14) . . ? C7 N2 C27 120.1(3) . . ? C7 N2 Mn2 127.3(3) . . ? C27 N2 Mn2 112.5(2) . . ? C45 N7 C26 120.0(3) . . ? C45 N7 Mn3 127.5(2) . . ? C26 N7 Mn3 112.5(2) . . ? C23 O5 Mn4 110.3(2) . . ? C29 O6 Mn4 113.8(2) . . ? C35 C355 C19 122.5(3) . . ? C9 N8 C111 121.1(3) . . ? C9 N8 Mn1 126.5(3) . . ? C111 N8 Mn1 112.1(3) . . ? N7 C45 C8 125.1(3) . . ? C236 O9 C237 37.4(4) . . ? C236 O9 Mn4 107.6(3) . . ? C237 O9 Mn4 105.4(3) . . ? C121 C6 C124 119.1(3) . . ? C121 C6 C9 124.0(3) . . ? C124 C6 C9 116.9(3) . . ? N2 C7 C16 125.4(3) . . ? C45 C8 C18 118.4(3) . . ? C45 C8 C35 123.8(3) . . ? C18 C8 C35 117.7(3) . . ? N8 C9 C6 124.6(3) . . ? O2 C10 C23 111.5(3) . . ? O2 C10 C27 106.2(3) . . ? C23 C10 C27 115.7(4) . . ? C21 C11 C16 121.1(4) . . ? C121 C12 C122 121.0(3) . . ? O3 C13 C20 118.7(3) . . ? O3 C13 C16 123.4(3) . . ? C20 C13 C16 117.9(3) . . ? C18 C14 C19 119.5(4) . . ? C11 C16 C13 119.9(3) . . ? C11 C16 C7 117.1(3) . . ? C13 C16 C7 123.0(3) . . ? C14 C18 C8 122.0(3) . . ? C355 C19 C14 120.0(4) . . ? C13 C20 C22 121.5(4) . . ? C11 C21 C22 119.2(3) . . ? C21 C22 C20 120.3(4) . . ? O5 C23 C10 108.6(4) . . ? C28 C26 N7 111.0(3) . . ? N2 C27 C10 105.0(3) . . ? O22 C28 C26 117.0(4) . . ? O22 C28 C29 116.5(4) . . ? C26 C28 C29 125.6(4) . . ? C28 C29 O6 115.9(4) . . ? O11 C35 C355 119.8(3) . . ? O11 C35 C8 122.1(3) . . ? C355 C35 C8 118.1(3) . . ? O12 Na5 O3 114.83(9) . . ? O12 Na5 O1 70.15(8) . . ? O3 Na5 O1 70.10(8) . . ? O12 Na5 O11 102.87(8) . . ? O3 Na5 O11 108.10(9) . . ? O1 Na5 O11 68.90(8) . . ? O12 Na5 Cl3 109.81(8) . . ? O3 Na5 Cl3 111.58(7) . . ? O1 Na5 Cl3 177.90(7) . . ? O11 Na5 Cl3 109.18(7) . . ? O12 Na5 Mn1 35.10(6) . . ? O3 Na5 Mn1 90.63(7) . . ? O1 Na5 Mn1 35.27(6) . . ? O11 Na5 Mn1 87.78(6) . . ? Cl3 Na5 Mn1 144.84(6) . . ? O12 Na5 Mn2 91.91(7) . . ? O3 Na5 Mn2 35.12(5) . . ? O1 Na5 Mn2 35.02(5) . . ? O11 Na5 Mn2 89.19(6) . . ? Cl3 Na5 Mn2 146.70(5) . . ? Mn1 Na5 Mn2 59.84(3) . . ? O12 Na5 Mn3 86.42(6) . . ? O3 Na5 Mn3 88.26(6) . . ? O1 Na5 Mn3 34.21(5) . . ? O11 Na5 Mn3 34.71(6) . . ? Cl3 Na5 Mn3 143.88(5) . . ? Mn1 Na5 Mn3 58.98(2) . . ? Mn2 Na5 Mn3 59.06(2) . . ? O12 C121 C12 119.4(3) . . ? O12 C121 C6 121.9(3) . . ? C12 C121 C6 118.7(3) . . ? C12 C122 C123 120.8(3) . . ? C123 C124 C6 121.3(3) . . ? C124 C123 C122 119.1(3) . . ? C235 C111 N8 115.3(5) . . ? C235 C111 C234 34.0(4) . . ? N8 C111 C234 99.3(3) . . ? O4 C234 C236 106.0(5) . . ? O4 C234 C111 98.4(3) . . ? C236 C234 C111 113.7(4) . . ? O9 C236 C234 99.0(5) . . ? C111 C235 C237 101.6(8) . . ? C111 C235 O4 112.4(7) . . ? C237 C235 O4 95.7(7) . . ? C235 C237 O9 102.5(7) . . ? Mn2 Cl7 Mn3 79.38(7) . . ? N331 N330 N332 4.7(6) . . ? N331 N332 N330 3.2(4) . . ? N330 N331 N332 172.0(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.443 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.122 # Attachment '2418_web_deposit_cif_file_1_JanReedijk_1284191254.cif' data_NS565 _database_code_depnum_ccdc_archive 'CCDC 793193' #TrackingRef '2418_web_deposit_cif_file_1_JanReedijk_1284191254.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H44 Ca Cl Mn3 N12 Na O16' _chemical_formula_weight 1152.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 43.964(6) _cell_length_b 43.964(6) _cell_length_c 11.235(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21715(6) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle shaped' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9424 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8758 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53165 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9411 _reflns_number_gt 6986 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1487P)^2^+50.8524P] 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 9411 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2306 _refine_ls_wR_factor_gt 0.2130 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.27860(2) 0.67097(2) 0.10671(6) 0.0433(3) Uani 1 1 d . A . Mn2 Mn 0.32162(2) 0.61197(2) -0.03545(6) 0.0402(2) Uani 1 1 d . A . Mn3 Mn 0.32739(2) 0.68085(2) -0.09025(6) 0.0428(3) Uani 1 1 d . A . Ca4 Ca 0.35884(3) 0.65877(3) 0.20895(9) 0.0519(3) Uani 1 1 d . . . Na1 Na 0.26112(5) 0.64544(5) -0.17888(17) 0.0441(5) Uani 1 1 d . . . Cl1 Cl 0.44556(4) 0.62314(5) 0.44029(15) 0.0674(5) Uani 1 1 d . . . O1 O 0.20648(10) 0.63727(10) -0.1354(3) 0.0502(10) Uani 1 1 d . A . O2 O 0.24456(10) 0.66509(10) 0.0052(3) 0.0475(10) Uani 1 1 d . A . O3 O 0.30907(10) 0.67705(10) 0.2218(3) 0.0507(10) Uani 1 1 d . A . O4 O 0.35239(15) 0.69091(16) 0.3806(5) 0.0899(19) Uani 1 1 d . A . O5 O 0.25725(10) 0.60933(9) -0.3454(3) 0.0459(9) Uani 1 1 d . A . O6 O 0.29443(9) 0.60406(9) -0.1641(3) 0.0438(9) Uani 1 1 d . A . O7 O 0.35062(9) 0.61569(9) 0.0873(3) 0.0444(9) Uani 1 1 d . A . O8 O 0.40240(16) 0.62426(16) 0.2166(6) 0.101(2) Uani 1 1 d . A . O9 O 0.24290(10) 0.68584(9) -0.3068(3) 0.0468(10) Uani 1 1 d . A . O10 O 0.29830(9) 0.68227(9) -0.2169(3) 0.0441(9) Uani 1 1 d . A . O11 O 0.35822(10) 0.68469(10) 0.0256(3) 0.0497(10) Uani 1 1 d . A . O12 O 0.40383(18) 0.6908(2) 0.1882(5) 0.082(2) Uani 0.80 1 d P A 1 O12A O 0.4087(6) 0.6690(10) 0.127(4) 0.104(12) Uani 0.20 1 d P A 2 O20 O 0.30458(9) 0.65076(9) -0.0029(3) 0.0427(9) Uani 1 1 d . A . O21 O 0.30629(12) 0.52656(12) 0.1120(4) 0.0663(13) Uani 1 1 d . . . O22 O 0.34477(18) 0.62375(15) 0.3708(4) 0.0895(18) Uani 1 1 d . A . O23 O 0.3894(3) 0.7102(4) 0.5505(9) 0.097(4) Uani 0.50 1 d P . . O24 O 0.4684(3) 0.6838(4) 0.2890(13) 0.105(4) Uani 0.50 1 d P . . N1 N 0.25302(13) 0.69470(12) 0.2184(4) 0.0504(12) Uani 1 1 d . . . N2 N 0.34188(12) 0.57225(12) -0.0621(4) 0.0452(11) Uani 1 1 d . . . N3 N 0.35219(13) 0.71180(13) -0.1730(4) 0.0540(13) Uani 1 1 d . . . N11 N 0.26237(14) 0.62593(14) 0.2021(4) 0.0575(14) Uani 1 1 d . . . N12 N 0.27467(12) 0.60648(11) 0.1493(4) 0.0453(11) Uani 1 1 d . A . N13 N 0.28657(13) 0.58766(13) 0.0890(4) 0.0518(13) Uani 1 1 d . . . N14 N 0.35057(12) 0.63971(12) -0.1715(4) 0.0478(12) Uani 1 1 d . . . N15 N 0.34803(13) 0.63730(12) -0.2774(4) 0.0502(12) Uani 1 1 d . A . N16 N 0.34525(19) 0.63517(15) -0.3779(4) 0.076(2) Uani 1 1 d . . . N17 N 0.29577(12) 0.71419(12) 0.0083(4) 0.0488(12) Uani 1 1 d . . . N18 N 0.30636(13) 0.73634(13) 0.0538(4) 0.0506(13) Uani 1 1 d . A . N19 N 0.31645(15) 0.75858(14) 0.0971(6) 0.0696(16) Uani 1 1 d . . . C1 C 0.21520(14) 0.66911(14) 0.0290(5) 0.0461(13) Uani 1 1 d . . . C2 C 0.19388(15) 0.65562(14) -0.0479(5) 0.0479(14) Uani 1 1 d . A . C3 C 0.16342(17) 0.65999(16) -0.0336(6) 0.0584(16) Uani 1 1 d . . . H3 H 0.1494 0.6503 -0.0856 0.070 Uiso 1 1 calc R A . C4 C 0.15288(17) 0.67906(17) 0.0593(6) 0.0608(17) Uani 1 1 d . A . H4 H 0.1317 0.6830 0.0674 0.073 Uiso 1 1 calc R . . C5 C 0.17290(16) 0.69161(16) 0.1364(6) 0.0554(16) Uani 1 1 d . . . H5 H 0.1656 0.7041 0.1993 0.066 Uiso 1 1 calc R A . C6 C 0.20444(15) 0.68645(14) 0.1249(5) 0.0475(14) Uani 1 1 d . A . C7 C 0.22439(15) 0.69886(15) 0.2134(5) 0.0496(14) Uani 1 1 d . A . H7 H 0.2155 0.7112 0.2734 0.060 Uiso 1 1 calc R . . C8 C 0.27183(18) 0.7088(2) 0.3127(7) 0.076(2) Uani 1 1 d . A . H8A H 0.2763 0.7302 0.2914 0.091 Uiso 1 1 calc R . . H8B H 0.2605 0.7087 0.3889 0.091 Uiso 1 1 calc R . . C9 C 0.3000(2) 0.6922(2) 0.3266(6) 0.080(2) Uani 1 1 d . . . H9 H 0.2952 0.6756 0.3847 0.095 Uiso 1 1 calc R A 1 C10A C 0.3290(7) 0.7087(12) 0.379(3) 0.081(6) Uani 0.50 1 d P A 1 H10A H 0.3337 0.7269 0.3304 0.097 Uiso 0.50 1 calc PR A 1 H10B H 0.3247 0.7156 0.4612 0.097 Uiso 0.50 1 calc PR A 1 C29 C 0.3818(2) 0.7047(3) 0.0005(7) 0.088(3) Uani 1 1 d . A 1 H29 H 0.3741 0.7241 0.0364 0.106 Uiso 1 1 calc R A 1 C30A C 0.4083(3) 0.6993(3) 0.0680(10) 0.055(4) Uani 0.50 1 d P A 1 H30A H 0.4209 0.7180 0.0666 0.066 Uiso 0.50 1 calc PR A 1 H30B H 0.4201 0.6830 0.0282 0.066 Uiso 0.50 1 calc PR A 1 C10B C 0.3202(7) 0.7027(12) 0.398(3) 0.081(6) Uani 0.50 1 d P A 2 H10C H 0.3139 0.6980 0.4803 0.097 Uiso 0.50 1 calc PR A 2 H10D H 0.3206 0.7251 0.3896 0.097 Uiso 0.50 1 calc PR A 2 C11 C 0.29378(14) 0.58101(13) -0.2395(4) 0.0422(13) Uani 1 1 d . . . C12 C 0.27318(14) 0.58259(13) -0.3374(4) 0.0431(13) Uani 1 1 d . A . C13 C 0.27019(15) 0.55864(14) -0.4165(5) 0.0482(14) Uani 1 1 d . . . H13 H 0.2561 0.5599 -0.4804 0.058 Uiso 1 1 calc R A . C14 C 0.28795(15) 0.53263(15) -0.4021(5) 0.0499(14) Uani 1 1 d . A . H14 H 0.2858 0.5162 -0.4563 0.060 Uiso 1 1 calc R . . C15 C 0.30854(15) 0.53045(14) -0.3108(5) 0.0472(14) Uani 1 1 d . . . H15 H 0.3207 0.5127 -0.3027 0.057 Uiso 1 1 calc R A . C16 C 0.31177(14) 0.55455(14) -0.2287(4) 0.0441(13) Uani 1 1 d . A . C17 C 0.33490(14) 0.55187(14) -0.1402(5) 0.0457(13) Uani 1 1 d . A . H17 H 0.3462 0.5334 -0.1386 0.055 Uiso 1 1 calc R . . C18 C 0.36616(15) 0.56642(17) 0.0252(6) 0.0571(16) Uani 1 1 d . A . H18A H 0.3583 0.5540 0.0920 0.069 Uiso 1 1 calc R . . H18B H 0.3832 0.5553 -0.0127 0.069 Uiso 1 1 calc R . . C19 C 0.3765(2) 0.5963(2) 0.0683(7) 0.078(2) Uani 1 1 d . . . H19 H 0.3893 0.6057 0.0047 0.093 Uiso 1 1 calc R A . C20 C 0.39508(17) 0.59500(17) 0.1806(6) 0.0599(17) Uani 1 1 d . A . H20A H 0.3834 0.5846 0.2440 0.072 Uiso 1 1 calc R . . H20B H 0.4139 0.5832 0.1661 0.072 Uiso 1 1 calc R . . C21 C 0.29170(15) 0.70703(13) -0.2792(4) 0.0456(14) Uani 1 1 d . . . C22 C 0.26174(15) 0.70957(13) -0.3282(4) 0.0441(14) Uani 1 1 d . A . C23 C 0.25374(16) 0.73515(14) -0.3922(4) 0.0490(15) Uani 1 1 d . . . H23 H 0.2337 0.7368 -0.4228 0.059 Uiso 1 1 calc R A . C24 C 0.27445(17) 0.75859(14) -0.4130(5) 0.0528(16) Uani 1 1 d . A . H24 H 0.2685 0.7759 -0.4577 0.063 Uiso 1 1 calc R . . C25 C 0.30323(18) 0.75660(15) -0.3691(5) 0.0558(16) Uani 1 1 d . . . H25 H 0.3175 0.7724 -0.3845 0.067 Uiso 1 1 calc R A . C26 C 0.31204(15) 0.73107(15) -0.3004(4) 0.0498(15) Uani 1 1 d . A . C27 C 0.34244(17) 0.73069(15) -0.2526(5) 0.0554(16) Uani 1 1 d . A . H27 H 0.3564 0.7454 -0.2817 0.066 Uiso 1 1 calc R . . C28 C 0.38345(19) 0.7129(2) -0.1300(7) 0.080(2) Uani 1 1 d . A . H28A H 0.3921 0.7336 -0.1405 0.097 Uiso 1 1 calc R B 1 H28B H 0.3963 0.6982 -0.1736 0.097 Uiso 1 1 calc R B 1 C31 C 0.18607(16) 0.61945(17) -0.2032(5) 0.0562(16) Uani 1 1 d . . . H31A H 0.1740 0.6066 -0.1498 0.084 Uiso 1 1 calc R A . H31B H 0.1976 0.6066 -0.2585 0.084 Uiso 1 1 calc R . . H31C H 0.1725 0.6328 -0.2482 0.084 Uiso 1 1 calc R . . C32 C 0.24083(18) 0.61426(17) -0.4541(5) 0.0618(18) Uani 1 1 d . . . H32A H 0.2547 0.6123 -0.5218 0.093 Uiso 1 1 calc R A . H32B H 0.2320 0.6347 -0.4536 0.093 Uiso 1 1 calc R . . H32C H 0.2246 0.5991 -0.4611 0.093 Uiso 1 1 calc R . . C33 C 0.21268(16) 0.68850(16) -0.3521(5) 0.0554(16) Uani 1 1 d . . . H33A H 0.2028 0.7064 -0.3171 0.083 Uiso 1 1 calc R A . H33B H 0.2011 0.6702 -0.3314 0.083 Uiso 1 1 calc R . . H33C H 0.2134 0.6907 -0.4389 0.083 Uiso 1 1 calc R . . C34 C 0.28914(18) 0.50620(17) 0.0409(5) 0.0609(17) Uani 1 1 d . . . H34A H 0.2679 0.5064 0.0672 0.091 Uiso 1 1 calc R . . H34B H 0.2974 0.4856 0.0491 0.091 Uiso 1 1 calc R . . H34C H 0.2903 0.5125 -0.0426 0.091 Uiso 1 1 calc R . . C35 C 0.3207(2) 0.6041(3) 0.3727(8) 0.089(3) Uani 1 1 d . . . H35A H 0.3017 0.6157 0.3802 0.134 Uiso 1 1 calc R A . H35B H 0.3227 0.5903 0.4406 0.134 Uiso 1 1 calc R . . H35C H 0.3203 0.5924 0.2987 0.134 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 0.0584(5) 0.0532(5) 0.0184(4) -0.0043(3) 0.0021(3) 0.0014(4) Mn2 0.0534(5) 0.0513(5) 0.0159(4) -0.0010(3) -0.0015(3) 0.0026(4) Mn3 0.0596(6) 0.0513(5) 0.0176(4) 0.0000(3) 0.0005(3) -0.0027(4) Ca4 0.0659(8) 0.0684(8) 0.0214(5) -0.0044(5) -0.0048(5) 0.0025(6) Na1 0.0578(13) 0.0516(13) 0.0229(9) -0.0008(8) -0.0022(9) 0.0024(10) Cl1 0.0680(11) 0.0858(12) 0.0485(8) 0.0145(8) -0.0273(8) -0.0035(9) O1 0.060(3) 0.060(3) 0.0311(19) -0.0029(18) -0.0035(18) -0.002(2) O2 0.060(3) 0.057(2) 0.0256(17) 0.0000(16) 0.0032(17) 0.003(2) O3 0.067(3) 0.065(3) 0.0206(17) -0.0095(17) -0.0004(17) 0.002(2) O4 0.096(4) 0.123(5) 0.051(3) -0.038(3) -0.020(3) 0.019(4) O5 0.062(2) 0.053(2) 0.0228(17) -0.0037(16) -0.0079(16) 0.0057(19) O6 0.061(2) 0.050(2) 0.0202(16) -0.0042(15) -0.0041(16) 0.0030(18) O7 0.054(2) 0.058(2) 0.0218(16) 0.0008(16) -0.0035(15) 0.0067(19) O8 0.102(5) 0.105(5) 0.095(4) -0.039(4) -0.047(4) 0.018(4) O9 0.066(3) 0.052(2) 0.0222(17) 0.0007(15) -0.0016(17) 0.000(2) O10 0.059(2) 0.051(2) 0.0218(16) -0.0001(16) 0.0003(16) 0.0011(19) O11 0.065(3) 0.056(2) 0.0274(18) -0.0021(17) -0.0005(17) -0.009(2) O12 0.092(5) 0.120(6) 0.033(3) 0.020(4) -0.021(3) -0.033(5) O12A 0.046(15) 0.15(3) 0.12(3) -0.03(3) -0.042(17) 0.002(18) O20 0.056(2) 0.056(2) 0.0160(15) 0.0012(15) 0.0003(15) -0.0004(18) O21 0.080(3) 0.076(3) 0.042(2) 0.008(2) -0.009(2) -0.001(3) O22 0.137(6) 0.094(4) 0.038(3) 0.005(3) 0.007(3) -0.006(4) O23 0.096(8) 0.154(12) 0.040(5) -0.042(6) -0.019(5) 0.016(8) O24 0.099(9) 0.115(10) 0.101(10) 0.031(8) -0.004(8) 0.041(8) N1 0.071(4) 0.055(3) 0.026(2) -0.008(2) 0.004(2) 0.002(3) N2 0.056(3) 0.058(3) 0.022(2) -0.001(2) 0.0008(19) 0.004(2) N3 0.066(3) 0.068(3) 0.029(2) 0.006(2) -0.001(2) -0.006(3) N11 0.073(4) 0.068(4) 0.032(2) -0.004(2) 0.013(2) -0.003(3) N12 0.053(3) 0.047(3) 0.035(2) 0.005(2) 0.006(2) -0.003(2) N13 0.062(3) 0.061(3) 0.032(2) 0.002(2) 0.004(2) -0.004(3) N14 0.062(3) 0.059(3) 0.022(2) -0.002(2) 0.004(2) 0.002(2) N15 0.072(3) 0.053(3) 0.025(2) -0.001(2) 0.008(2) 0.004(3) N16 0.136(6) 0.074(4) 0.018(2) -0.004(2) 0.002(3) 0.014(4) N17 0.067(3) 0.053(3) 0.026(2) -0.001(2) -0.001(2) -0.002(3) N18 0.067(3) 0.058(3) 0.028(2) -0.005(2) 0.005(2) 0.007(3) N19 0.081(4) 0.063(4) 0.065(4) -0.026(3) 0.004(3) -0.007(3) C1 0.057(4) 0.054(3) 0.028(3) 0.006(2) 0.008(2) 0.005(3) C2 0.065(4) 0.048(3) 0.031(3) 0.004(2) 0.004(3) 0.002(3) C3 0.063(4) 0.066(4) 0.047(3) 0.003(3) 0.002(3) 0.003(3) C4 0.057(4) 0.074(5) 0.052(4) 0.009(3) 0.004(3) 0.009(3) C5 0.060(4) 0.066(4) 0.040(3) 0.002(3) 0.011(3) 0.007(3) C6 0.059(4) 0.058(4) 0.026(2) 0.005(2) 0.005(2) 0.002(3) C7 0.061(4) 0.057(4) 0.030(3) -0.001(2) 0.008(3) 0.001(3) C8 0.070(5) 0.104(6) 0.054(4) -0.039(4) -0.001(3) 0.005(4) C9 0.093(6) 0.115(7) 0.031(3) -0.028(4) -0.005(3) 0.022(5) C10A 0.040(17) 0.15(2) 0.052(11) -0.044(11) 0.015(9) -0.021(13) C29 0.085(6) 0.130(8) 0.049(4) 0.022(5) -0.014(4) -0.026(6) C30A 0.043(6) 0.087(9) 0.036(6) 0.037(6) -0.019(5) -0.029(6) C10B 0.040(17) 0.15(2) 0.052(11) -0.044(11) 0.015(9) -0.021(13) C11 0.056(3) 0.047(3) 0.023(2) 0.000(2) 0.003(2) 0.002(3) C12 0.059(3) 0.050(3) 0.020(2) -0.002(2) 0.001(2) -0.001(3) C13 0.060(4) 0.056(4) 0.028(3) -0.004(2) 0.004(2) -0.001(3) C14 0.065(4) 0.055(4) 0.030(3) -0.015(2) 0.003(3) -0.002(3) C15 0.063(4) 0.048(3) 0.031(3) -0.002(2) 0.002(2) 0.005(3) C16 0.056(3) 0.052(3) 0.025(2) 0.000(2) 0.005(2) -0.004(3) C17 0.055(3) 0.049(3) 0.033(3) -0.001(2) 0.003(2) 0.007(3) C18 0.056(4) 0.078(5) 0.037(3) -0.002(3) -0.008(3) 0.014(3) C19 0.094(6) 0.083(5) 0.057(4) -0.006(4) -0.021(4) 0.008(5) C20 0.068(4) 0.068(4) 0.044(3) -0.004(3) -0.016(3) 0.012(3) C21 0.069(4) 0.048(3) 0.020(2) 0.001(2) 0.006(2) -0.002(3) C22 0.073(4) 0.047(3) 0.012(2) -0.006(2) 0.000(2) 0.000(3) C23 0.076(4) 0.052(3) 0.019(2) 0.001(2) 0.002(2) 0.003(3) C24 0.090(5) 0.050(3) 0.019(2) 0.005(2) 0.004(3) 0.009(3) C25 0.091(5) 0.050(4) 0.027(3) 0.001(2) 0.009(3) -0.002(3) C26 0.071(4) 0.060(4) 0.018(2) 0.002(2) 0.002(2) 0.006(3) C27 0.080(5) 0.057(4) 0.029(3) 0.005(3) 0.012(3) -0.005(3) C28 0.072(5) 0.108(7) 0.062(4) 0.036(5) -0.009(4) -0.016(5) C31 0.060(4) 0.073(4) 0.035(3) 0.001(3) -0.007(3) -0.005(3) C32 0.086(5) 0.071(4) 0.029(3) -0.009(3) -0.019(3) 0.011(4) C33 0.067(4) 0.062(4) 0.037(3) 0.008(3) -0.013(3) 0.005(3) C34 0.075(5) 0.071(4) 0.037(3) 0.003(3) 0.004(3) 0.002(4) C35 0.087(6) 0.124(8) 0.057(5) 0.002(5) -0.002(4) 0.011(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 1.881(4) . ? Mn1 O2 1.899(4) . ? Mn1 O20 1.900(4) . ? Mn1 N1 1.982(5) . ? Mn1 N17 2.324(5) . ? Mn1 N11 2.362(6) . ? Mn1 Mn3 3.1122(12) . ? Mn1 Na1 3.485(2) . ? Mn1 Ca4 3.7486(17) . ? Mn2 O7 1.885(4) . ? Mn2 O20 1.898(4) . ? Mn2 O6 1.908(4) . ? Mn2 N2 1.983(5) . ? Mn2 N14 2.333(5) . ? Mn2 N13 2.339(5) . ? Mn2 Mn3 3.1007(13) . ? Mn2 Na1 3.441(2) . ? Mn2 Ca4 3.8015(15) . ? Mn3 O11 1.887(4) . ? Mn3 O10 1.914(4) . ? Mn3 O20 1.928(4) . ? Mn3 N3 1.976(5) . ? Mn3 N14 2.268(5) . ? Mn3 N17 2.304(5) . ? Mn3 Na1 3.450(2) . ? Mn3 Ca4 3.7622(15) . ? Ca4 O3 2.335(5) . ? Ca4 O11 2.354(4) . ? Ca4 O7 2.363(4) . ? Ca4 O4 2.407(5) . ? Ca4 O12A 2.42(4) . ? Ca4 O12 2.439(7) . ? Ca4 O8 2.445(7) . ? Ca4 O22 2.462(6) . ? Ca4 C10B 3.33(4) . ? Ca4 C30A 3.228(11) . ? Na1 O10 2.340(5) . ? Na1 O6 2.342(5) . ? Na1 O2 2.356(4) . ? Na1 O9 2.421(4) . ? Na1 O5 2.459(4) . ? Na1 O1 2.477(5) . ? Na1 O20 2.759(4) . ? O1 C2 1.387(7) . ? O1 C31 1.414(8) . ? O2 C1 1.330(7) . ? O3 C9 1.412(7) . ? O4 C10B 1.52(4) . ? O4 C10A 1.29(5) . ? O5 C12 1.372(7) . ? O5 C32 1.435(7) . ? O6 C11 1.321(7) . ? O7 C19 1.436(10) . ? O8 C20 1.386(10) . ? O9 C22 1.353(7) . ? O9 C33 1.427(8) . ? O10 C21 1.327(7) . ? O11 C29 1.391(10) . ? O12 C30A 1.415(12) . ? O21 C34 1.417(9) . ? O22 C35 1.365(12) . ? N1 C7 1.273(8) . ? N1 C8 1.480(9) . ? N2 C17 1.291(8) . ? N2 C18 1.472(8) . ? N3 C27 1.293(8) . ? N3 C28 1.458(10) . ? N11 N12 1.173(7) . ? N12 N13 1.190(7) . ? N14 N15 1.200(6) . ? N15 N16 1.140(7) . ? N17 N18 1.194(7) . ? N18 N19 1.179(8) . ? C1 C6 1.402(8) . ? C1 C2 1.406(9) . ? C2 C3 1.362(10) . ? C3 C4 1.417(10) . ? C4 C5 1.353(10) . ? C5 C6 1.411(9) . ? C6 C7 1.434(9) . ? C8 C9 1.444(12) . ? C9 C10B 1.28(4) . ? C9 C10A 1.58(3) . ? C29 C30A 1.411(14) . ? C29 C28 1.511(11) . ? C11 C16 1.412(9) . ? C11 C12 1.426(8) . ? C12 C13 1.384(8) . ? C13 C14 1.394(9) . ? C14 C15 1.371(9) . ? C15 C16 1.412(8) . ? C16 C17 1.427(8) . ? C18 C19 1.472(11) . ? C19 C20 1.505(10) . ? C21 C26 1.405(9) . ? C21 C22 1.432(9) . ? C22 C23 1.380(8) . ? C23 C24 1.395(9) . ? C24 C25 1.361(10) . ? C25 C26 1.416(9) . ? C26 C27 1.441(10) . ? 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 O3 Mn1 O2 173.40(18) . . ? O3 Mn1 O20 94.80(17) . . ? O2 Mn1 O20 91.18(17) . . ? O3 Mn1 N1 83.9(2) . . ? O2 Mn1 N1 90.3(2) . . ? O20 Mn1 N1 176.0(2) . . ? O3 Mn1 N17 88.82(19) . . ? O2 Mn1 N17 94.68(18) . . ? O20 Mn1 N17 83.03(17) . . ? N1 Mn1 N17 93.2(2) . . ? O3 Mn1 N11 91.3(2) . . ? O2 Mn1 N11 85.43(19) . . ? O20 Mn1 N11 94.81(18) . . ? N1 Mn1 N11 89.0(2) . . ? N17 Mn1 N11 177.8(2) . . ? O3 Mn1 Mn3 88.74(13) . . ? O2 Mn1 Mn3 97.76(12) . . ? O20 Mn1 Mn3 35.92(12) . . ? N1 Mn1 Mn3 140.16(16) . . ? N17 Mn1 Mn3 47.46(13) . . ? N11 Mn1 Mn3 130.38(14) . . ? O3 Mn1 Na1 146.68(13) . . ? O2 Mn1 Na1 39.59(12) . . ? O20 Mn1 Na1 52.06(12) . . ? N1 Mn1 Na1 128.86(16) . . ? N17 Mn1 Na1 84.09(12) . . ? N11 Mn1 Na1 94.66(13) . . ? Mn3 Mn1 Na1 62.76(4) . . ? O3 Mn1 Ca4 30.61(13) . . ? O2 Mn1 Ca4 154.96(13) . . ? O20 Mn1 Ca4 64.28(12) . . ? N1 Mn1 Ca4 114.53(16) . . ? N17 Mn1 Ca4 87.54(14) . . ? N11 Mn1 Ca4 91.45(15) . . ? Mn3 Mn1 Ca4 65.75(3) . . ? Na1 Mn1 Ca4 116.33(5) . . ? O7 Mn2 O20 92.76(17) . . ? O7 Mn2 O6 173.64(18) . . ? O20 Mn2 O6 93.59(16) . . ? O7 Mn2 N2 83.30(18) . . ? O20 Mn2 N2 175.95(19) . . ? O6 Mn2 N2 90.35(18) . . ? O7 Mn2 N14 93.72(17) . . ? O20 Mn2 N14 82.63(17) . . ? O6 Mn2 N14 86.59(17) . . ? N2 Mn2 N14 96.68(19) . . ? O7 Mn2 N13 92.74(18) . . ? O20 Mn2 N13 92.03(18) . . ? O6 Mn2 N13 87.54(18) . . ? N2 Mn2 N13 89.1(2) . . ? N14 Mn2 N13 171.80(19) . . ? O7 Mn2 Mn3 90.29(13) . . ? O20 Mn2 Mn3 36.20(11) . . ? O6 Mn2 Mn3 94.52(12) . . ? N2 Mn2 Mn3 142.49(15) . . ? N14 Mn2 Mn3 46.75(13) . . ? N13 Mn2 Mn3 128.23(15) . . ? O7 Mn2 Na1 145.93(13) . . ? O20 Mn2 Na1 53.19(12) . . ? O6 Mn2 Na1 40.43(12) . . ? N2 Mn2 Na1 130.77(14) . . ? N14 Mn2 Na1 83.75(14) . . ? N13 Mn2 Na1 88.07(14) . . ? Mn3 Mn2 Na1 63.41(4) . . ? O7 Mn2 Ca4 29.95(13) . . ? O20 Mn2 Ca4 62.91(11) . . ? O6 Mn2 Ca4 156.32(13) . . ? N2 Mn2 Ca4 113.11(14) . . ? N14 Mn2 Ca4 87.45(12) . . ? N13 Mn2 Ca4 95.68(13) . . ? Mn3 Mn2 Ca4 65.14(3) . . ? Na1 Mn2 Ca4 116.08(5) . . ? O11 Mn3 O10 171.84(18) . . ? O11 Mn3 O20 94.81(17) . . ? O10 Mn3 O20 93.04(16) . . ? O11 Mn3 N3 82.34(19) . . ? O10 Mn3 N3 89.80(19) . . ? O20 Mn3 N3 177.15(19) . . ? O11 Mn3 N14 91.50(19) . . ? O10 Mn3 N14 91.54(17) . . ? O20 Mn3 N14 83.77(18) . . ? N3 Mn3 N14 96.4(2) . . ? O11 Mn3 N17 92.58(18) . . ? O10 Mn3 N17 86.18(17) . . ? O20 Mn3 N17 83.00(18) . . ? N3 Mn3 N17 97.0(2) . . ? N14 Mn3 N17 166.43(19) . . ? O11 Mn3 Mn2 90.52(13) . . ? O10 Mn3 Mn2 97.17(12) . . ? O20 Mn3 Mn2 35.55(12) . . ? N3 Mn3 Mn2 144.20(17) . . ? N14 Mn3 Mn2 48.54(13) . . ? N17 Mn3 Mn2 118.46(13) . . ? O11 Mn3 Mn1 90.98(13) . . ? O10 Mn3 Mn1 94.16(12) . . ? O20 Mn3 Mn1 35.32(12) . . ? N3 Mn3 Mn1 144.19(17) . . ? N14 Mn3 Mn1 118.99(13) . . ? N17 Mn3 Mn1 48.02(13) . . ? Mn2 Mn3 Mn1 70.50(3) . . ? O11 Mn3 Na1 147.79(13) . . ? O10 Mn3 Na1 40.17(12) . . ? O20 Mn3 Na1 53.00(11) . . ? N3 Mn3 Na1 129.85(15) . . ? N14 Mn3 Na1 84.46(14) . . ? N17 Mn3 Na1 85.20(14) . . ? Mn2 Mn3 Na1 63.10(4) . . ? Mn1 Mn3 Na1 63.91(4) . . ? O11 Mn3 Ca4 30.98(13) . . ? O10 Mn3 Ca4 156.65(12) . . ? O20 Mn3 Ca4 63.87(11) . . ? N3 Mn3 Ca4 113.28(15) . . ? N14 Mn3 Ca4 89.36(12) . . ? N17 Mn3 Ca4 87.50(12) . . ? Mn2 Mn3 Ca4 66.46(3) . . ? Mn1 Mn3 Ca4 65.29(3) . . ? Na1 Mn3 Ca4 116.86(5) . . ? O3 Ca4 O11 82.91(15) . . ? O3 Ca4 O7 99.67(15) . . ? O11 Ca4 O7 83.11(14) . . ? O3 Ca4 O4 68.80(18) . . ? O11 Ca4 O4 114.6(2) . . ? O7 Ca4 O4 156.3(2) . . ? O3 Ca4 O12A 144.0(10) . . ? O11 Ca4 O12A 65.7(9) . . ? O7 Ca4 O12A 93.9(10) . . ? O4 Ca4 O12A 107.6(10) . . ? O3 Ca4 O12 124.5(3) . . ? O11 Ca4 O12 69.29(17) . . ? O7 Ca4 O12 122.1(2) . . ? O4 Ca4 O12 80.4(3) . . ? O12A Ca4 O12 28.6(9) . . ? O3 Ca4 O8 160.9(2) . . ? O11 Ca4 O8 109.9(2) . . ? O7 Ca4 O8 69.07(17) . . ? O4 Ca4 O8 115.4(2) . . ? O12A Ca4 O8 54.4(10) . . ? O12 Ca4 O8 74.1(3) . . ? O3 Ca4 O22 86.2(2) . . ? O11 Ca4 O22 161.1(2) . . ? O7 Ca4 O22 83.54(17) . . ? O4 Ca4 O22 75.3(2) . . ? O12A Ca4 O22 128.6(9) . . ? O12 Ca4 O22 129.5(2) . . ? O8 Ca4 O22 77.4(3) . . ? O3 Ca4 C10B 44.3(7) . . ? O11 Ca4 C10B 105.7(9) . . ? O7 Ca4 C10B 139.0(5) . . ? O4 Ca4 C10B 24.5(6) . . ? O12A Ca4 C10B 126.6(11) . . ? O12 Ca4 C10B 98.0(6) . . ? O8 Ca4 C10B 137.4(8) . . ? O22 Ca4 C10B 76.4(8) . . ? O3 Ca4 C30A 118.2(3) . . ? O11 Ca4 C30A 46.5(2) . . ? O7 Ca4 C30A 105.2(3) . . ? O4 Ca4 C30A 98.5(3) . . ? O12A Ca4 C30A 25.9(10) . . ? O12 Ca4 C30A 24.2(2) . . ? O8 Ca4 C30A 80.3(3) . . ? O22 Ca4 C30A 151.3(3) . . ? C10B Ca4 C30A 109.6(7) . . ? O3 Ca4 Mn1 24.21(9) . . ? O11 Ca4 Mn1 69.61(11) . . ? O7 Ca4 Mn1 78.08(10) . . ? O4 Ca4 Mn1 92.91(15) . . ? O12A Ca4 Mn1 135.3(9) . . ? O12 Ca4 Mn1 130.63(19) . . ? O8 Ca4 Mn1 146.79(15) . . ? O22 Ca4 Mn1 94.55(19) . . ? C10B Ca4 Mn1 68.5(7) . . ? C30A Ca4 Mn1 113.9(2) . . ? O3 Ca4 Mn3 67.79(9) . . ? O11 Ca4 Mn3 24.36(11) . . ? O7 Ca4 Mn3 68.52(9) . . ? O4 Ca4 Mn3 121.41(16) . . ? O12A Ca4 Mn3 86.9(8) . . ? O12 Ca4 Mn3 93.65(14) . . ? O8 Ca4 Mn3 118.66(17) . . ? O22 Ca4 Mn3 136.81(18) . . ? C10B Ca4 Mn3 103.4(9) . . ? C30A Ca4 Mn3 70.55(18) . . ? Mn1 Ca4 Mn3 48.96(2) . . ? O10 Na1 O6 96.52(17) . . ? O10 Na1 O2 97.02(16) . . ? O6 Na1 O2 114.58(15) . . ? O10 Na1 O9 67.37(15) . . ? O6 Na1 O9 144.98(16) . . ? O2 Na1 O9 98.62(16) . . ? O10 Na1 O5 110.86(15) . . ? O6 Na1 O5 66.14(14) . . ? O2 Na1 O5 151.98(18) . . ? O9 Na1 O5 89.95(14) . . ? O10 Na1 O1 144.45(17) . . ? O6 Na1 O1 118.67(17) . . ? O2 Na1 O1 65.21(15) . . ? O9 Na1 O1 84.41(16) . . ? O5 Na1 O1 89.39(15) . . ? O10 Na1 O20 65.69(13) . . ? O6 Na1 O20 65.30(13) . . ? O2 Na1 O20 63.52(14) . . ? O9 Na1 O20 126.31(16) . . ? O5 Na1 O20 130.36(15) . . ? O1 Na1 O20 122.85(14) . . ? O10 Na1 Mn2 80.87(12) . . ? O6 Na1 Mn2 31.89(9) . . ? O2 Na1 Mn2 89.12(12) . . ? O9 Na1 Mn2 147.95(14) . . ? O5 Na1 Mn2 97.68(12) . . ? O1 Na1 Mn2 126.53(12) . . ? O20 Na1 Mn2 33.42(9) . . ? O10 Na1 Mn3 31.85(9) . . ? O6 Na1 Mn3 78.58(12) . . ? O2 Na1 Mn3 80.92(12) . . ? O9 Na1 Mn3 96.87(12) . . ? O5 Na1 Mn3 124.69(13) . . ? O1 Na1 Mn3 145.83(12) . . ? O20 Na1 Mn3 33.92(8) . . ? Mn2 Na1 Mn3 53.49(4) . . ? O10 Na1 Mn1 77.94(10) . . ? O6 Na1 Mn1 92.70(10) . . ? O2 Na1 Mn1 30.92(11) . . ? O9 Na1 Mn1 112.53(12) . . ? O5 Na1 Mn1 157.43(12) . . ? O1 Na1 Mn1 94.53(11) . . ? O20 Na1 Mn1 32.90(8) . . ? Mn2 Na1 Mn1 62.36(4) . . ? Mn3 Na1 Mn1 53.33(4) . . ? C2 O1 C31 116.8(5) . . ? C2 O1 Na1 116.3(4) . . ? C31 O1 Na1 126.1(4) . . ? C1 O2 Mn1 128.7(3) . . ? C1 O2 Na1 121.7(3) . . ? Mn1 O2 Na1 109.49(19) . . ? C9 O3 Mn1 116.0(4) . . ? C9 O3 Ca4 118.7(4) . . ? Mn1 O3 Ca4 125.18(18) . . ? C10B O4 C10A 19(3) . . ? C10B O4 Ca4 114.3(15) . . ? C10A O4 Ca4 116.1(18) . . ? C12 O5 C32 116.2(4) . . ? C12 O5 Na1 117.9(3) . . ? C32 O5 Na1 125.8(4) . . ? C11 O6 Mn2 129.7(4) . . ? C11 O6 Na1 122.5(3) . . ? Mn2 O6 Na1 107.68(17) . . ? C19 O7 Mn2 112.0(4) . . ? C19 O7 Ca4 116.1(4) . . ? Mn2 O7 Ca4 126.6(2) . . ? C20 O8 Ca4 112.6(5) . . ? C22 O9 C33 116.3(5) . . ? C22 O9 Na1 117.9(3) . . ? C33 O9 Na1 125.4(4) . . ? C21 O10 Mn3 124.4(4) . . ? C21 O10 Na1 120.7(4) . . ? Mn3 O10 Na1 107.98(17) . . ? C29 O11 Mn3 116.9(4) . . ? C29 O11 Ca4 118.4(4) . . ? Mn3 O11 Ca4 124.7(2) . . ? C30A O12 Ca4 110.9(6) . . ? Mn2 O20 Mn1 141.4(2) . . ? Mn2 O20 Mn3 108.25(19) . . ? Mn1 O20 Mn3 108.8(2) . . ? Mn2 O20 Na1 93.39(15) . . ? Mn1 O20 Na1 95.04(16) . . ? Mn3 O20 Na1 93.08(13) . . ? C35 O22 Ca4 126.9(5) . . ? C7 N1 C8 121.6(5) . . ? C7 N1 Mn1 127.5(4) . . ? C8 N1 Mn1 110.9(4) . . ? C17 N2 C18 120.3(5) . . ? C17 N2 Mn2 127.4(4) . . ? C18 N2 Mn2 112.2(4) . . ? C27 N3 C28 121.3(6) . . ? C27 N3 Mn3 125.8(5) . . ? C28 N3 Mn3 112.8(4) . . ? N12 N11 Mn1 104.0(4) . . ? N11 N12 N13 175.8(6) . . ? N12 N13 Mn2 108.2(4) . . ? N15 N14 Mn3 115.4(4) . . ? N15 N14 Mn2 123.6(4) . . ? Mn3 N14 Mn2 84.72(16) . . ? N16 N15 N14 179.1(8) . . ? N18 N17 Mn3 119.3(4) . . ? N18 N17 Mn1 126.1(4) . . ? Mn3 N17 Mn1 84.52(18) . . ? N19 N18 N17 178.6(7) . . ? O2 C1 C6 123.7(6) . . ? O2 C1 C2 117.8(5) . . ? C6 C1 C2 118.5(6) . . ? C3 C2 O1 123.9(6) . . ? C3 C2 C1 121.5(6) . . ? O1 C2 C1 114.5(5) . . ? C2 C3 C4 119.5(7) . . ? C5 C4 C3 120.0(7) . . ? C4 C5 C6 121.0(6) . . ? C1 C6 C5 119.3(6) . . ? C1 C6 C7 122.2(6) . . ? C5 C6 C7 118.5(5) . . ? N1 C7 C6 125.5(6) . . ? C9 C8 N1 110.2(6) . . ? C10B C9 O3 119.5(17) . . ? C10B C9 C8 119(2) . . ? O3 C9 C8 113.0(6) . . ? C10B C9 C10A 17(2) . . ? O3 C9 C10A 107.3(14) . . ? C8 C9 C10A 120(2) . . ? O4 C10A C9 112(3) . . ? O11 C29 C30A 113.6(8) . . ? O11 C29 C28 112.5(7) . . ? C30A C29 C28 121.5(9) . . ? C29 C30A O12 116.2(10) . . ? C29 C30A Ca4 78.5(6) . . ? O12 C30A Ca4 44.9(4) . . ? C9 C10B O4 116(3) . . ? C9 C10B Ca4 75.5(19) . . ? O4 C10B Ca4 41.2(12) . . ? O6 C11 C16 124.4(5) . . ? O6 C11 C12 118.1(5) . . ? C16 C11 C12 117.5(5) . . ? O5 C12 C13 124.2(5) . . ? O5 C12 C11 114.6(5) . . ? C13 C12 C11 121.2(6) . . ? C12 C13 C14 119.7(6) . . ? C15 C14 C13 120.9(5) . . ? C14 C15 C16 120.2(6) . . ? C15 C16 C11 120.4(5) . . ? C15 C16 C17 117.7(5) . . ? C11 C16 C17 121.8(5) . . ? N2 C17 C16 125.8(6) . . ? C19 C18 N2 106.7(6) . . ? O7 C19 C18 109.6(7) . . ? O7 C19 C20 109.2(6) . . ? C18 C19 C20 114.1(7) . . ? O8 C20 C19 109.6(6) . . ? O10 C21 C26 124.6(6) . . ? O10 C21 C22 117.9(5) . . ? C26 C21 C22 117.5(5) . . ? O9 C22 C23 124.4(6) . . ? O9 C22 C21 115.8(5) . . ? C23 C22 C21 119.8(6) . . ? C22 C23 C24 121.5(6) . . ? C25 C24 C23 119.9(6) . . ? C24 C25 C26 120.2(6) . . ? C21 C26 C25 121.0(6) . . ? C21 C26 C27 121.3(6) . . ? C25 C26 C27 117.8(6) . . ? N3 C27 C26 124.9(6) . . ? N3 C28 C29 105.6(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.430 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.113 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.250 0.377 778 -5 ' ' 2 0.000 0.750 0.614 778 -6 ' ' 3 0.500 0.250 0.613 778 -6 ' ' 4 0.500 0.750 0.379 778 -5 ' ' _platon_squeeze_details ; ;