# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email leigh.jones@nuigalway.ie _publ_contact_author_name 'Leigh Jones' _publ_author_name L.Jones.N.Berg # Attachment '- 3-picNa-Mnchain(4).cif' data_3-picNa-Mnchain(4) _database_code_depnum_ccdc_archive 'CCDC 778267' #TrackingRef '- 3-picNa-Mnchain(4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(biphen)2(3-pic)2][Na(EtOH)3(biphenH2)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 Mn N2 Na O9' _chemical_formula_weight 956.95 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.350(2) _cell_length_b 11.989(2) _cell_length_c 21.671(4) _cell_angle_alpha 86.90(3) _cell_angle_beta 78.51(3) _cell_angle_gamma 69.14(3) _cell_volume 2462.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.335 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.8721 _cell_measurement_reflns_used 6839 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.88946 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 20423 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.8721 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0477897000 _diffrn_orient_matrix_UB_12 -0.0575274000 _diffrn_orient_matrix_UB_13 -0.0107367000 _diffrn_orient_matrix_UB_21 0.0274789000 _diffrn_orient_matrix_UB_22 0.0253462000 _diffrn_orient_matrix_UB_23 -0.0275115000 _diffrn_orient_matrix_UB_31 0.0504671000 _diffrn_orient_matrix_UB_32 0.0075900000 _diffrn_orient_matrix_UB_33 0.0156116000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 48.00 90.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 150.0000 42 #__ type_ start__ end____ width___ exp.time_ 2 omega -40.00 50.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 -77.0000 30.0000 90 #__ type_ start__ end____ width___ exp.time_ 3 omega 6.00 83.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 -60.0000 77 #__ type_ start__ end____ width___ exp.time_ 4 omega -9.00 84.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 -150.0000 93 #__ type_ start__ end____ width___ exp.time_ 5 omega -48.00 46.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 -77.0000 90.0000 94 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 9016 _reflns_number_gt 6299 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0741P)^2^+0.0055P] 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 9016 _refine_ls_number_parameters 629 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.60346(5) 0.69255(4) 0.74082(2) 0.01962(15) Uani 1 1 d . . . Na1 Na 0.11514(13) 0.70194(13) 0.70159(6) 0.0317(4) Uani 1 1 d . . . N1 N 0.6255(3) 0.7224(3) 0.63090(13) 0.0252(7) Uani 1 1 d . . . N2 N 0.5764(3) 0.6552(2) 0.84884(12) 0.0220(6) Uani 1 1 d . . . O1 O 0.8005(2) 0.5930(2) 0.72900(10) 0.0238(5) Uani 1 1 d . . . O2 O 0.5535(2) 0.55782(19) 0.72692(10) 0.0210(5) Uani 1 1 d . . . O3 O 0.4091(2) 0.79760(19) 0.74995(10) 0.0227(5) Uani 1 1 d . . . O4 O 0.6577(2) 0.8258(2) 0.75103(10) 0.0221(5) Uani 1 1 d . . . O5 O -0.0219(2) 0.6375(2) 0.78316(11) 0.0273(6) Uani 1 1 d D . . O6 O 0.2027(2) 0.7249(2) 0.78804(11) 0.0308(6) Uani 1 1 d D . . O7 O 0.3441(2) 0.5442(2) 0.67286(12) 0.0331(6) Uani 1 1 d D . . O8 O 0.2178(3) 0.7087(3) 0.59576(13) 0.0509(8) Uani 1 1 d D . . O9 O -0.0958(2) 0.8460(2) 0.69069(12) 0.0353(7) Uani 1 1 d D . . C1 C 0.8631(3) 0.5127(3) 0.68098(15) 0.0226(8) Uani 1 1 d . . . C2 C 0.9530(3) 0.5377(3) 0.62896(16) 0.0281(8) Uani 1 1 d . . . H2 H 0.9668 0.6121 0.6270 0.034 Uiso 1 1 calc R . . C3 C 1.0214(4) 0.4549(4) 0.58091(17) 0.0342(9) Uani 1 1 d . . . H3 H 1.0831 0.4723 0.5463 0.041 Uiso 1 1 calc R . . C4 C 1.0016(4) 0.3471(4) 0.58220(17) 0.0353(9) Uani 1 1 d . . . H4 H 1.0483 0.2905 0.5486 0.042 Uiso 1 1 calc R . . C5 C 0.9119(3) 0.3226(3) 0.63370(16) 0.0297(8) Uani 1 1 d . . . H5 H 0.8983 0.2482 0.6349 0.036 Uiso 1 1 calc R . . C6 C 0.8419(3) 0.4033(3) 0.68308(15) 0.0223(7) Uani 1 1 d . . . C7 C 0.7464(3) 0.3752(3) 0.73774(15) 0.0233(8) Uani 1 1 d . . . C8 C 0.7926(4) 0.2684(3) 0.76931(17) 0.0327(9) Uani 1 1 d . . . H8 H 0.8879 0.2166 0.7579 0.039 Uiso 1 1 calc R . . C9 C 0.7024(4) 0.2360(3) 0.81708(17) 0.0392(10) Uani 1 1 d . . . H9 H 0.7356 0.1626 0.8380 0.047 Uiso 1 1 calc R . . C10 C 0.5650(4) 0.3107(3) 0.83384(17) 0.0369(10) Uani 1 1 d . . . H10 H 0.5025 0.2879 0.8659 0.044 Uiso 1 1 calc R . . C11 C 0.5164(4) 0.4188(3) 0.80456(15) 0.0270(8) Uani 1 1 d . . . H11 H 0.4215 0.4706 0.8173 0.032 Uiso 1 1 calc R . . C12 C 0.6059(3) 0.4518(3) 0.75648(15) 0.0213(7) Uani 1 1 d . . . C13 C 0.3643(3) 0.9107(3) 0.72864(15) 0.0224(8) Uani 1 1 d . . . C14 C 0.2874(3) 0.9359(3) 0.67987(16) 0.0279(8) Uani 1 1 d . . . H14 H 0.2759 0.8727 0.6596 0.034 Uiso 1 1 calc R . . C15 C 0.2283(4) 1.0524(3) 0.66111(17) 0.0336(9) Uani 1 1 d . . . H15 H 0.1753 1.0682 0.6285 0.040 Uiso 1 1 calc R . . C16 C 0.2449(4) 1.1452(3) 0.68883(17) 0.0332(9) Uani 1 1 d . . . H16 H 0.2029 1.2249 0.6760 0.040 Uiso 1 1 calc R . . C17 C 0.3245(3) 1.1208(3) 0.73613(17) 0.0300(9) Uani 1 1 d . . . H17 H 0.3391 1.1845 0.7545 0.036 Uiso 1 1 calc R . . C18 C 0.3838(3) 1.0037(3) 0.75711(16) 0.0242(8) Uani 1 1 d . . . C19 C 0.4636(3) 0.9842(3) 0.80928(15) 0.0212(7) Uani 1 1 d . . . C20 C 0.4067(4) 1.0535(3) 0.86420(16) 0.0291(8) Uani 1 1 d . . . H20 H 0.3140 1.1110 0.8693 0.035 Uiso 1 1 calc R . . C21 C 0.4834(4) 1.0402(3) 0.91203(17) 0.0343(9) Uani 1 1 d . . . H21 H 0.4431 1.0882 0.9493 0.041 Uiso 1 1 calc R . . C22 C 0.6172(4) 0.9573(3) 0.90487(17) 0.0314(9) Uani 1 1 d . . . H22 H 0.6701 0.9491 0.9371 0.038 Uiso 1 1 calc R . . C23 C 0.6761(3) 0.8856(3) 0.85132(16) 0.0272(8) Uani 1 1 d . . . H23 H 0.7693 0.8291 0.8469 0.033 Uiso 1 1 calc R . . C24 C 0.5989(3) 0.8959(3) 0.80341(15) 0.0208(7) Uani 1 1 d . . . C25 C 0.6232(3) 0.6414(3) 0.59155(17) 0.0305(9) Uani 1 1 d . . . H25 H 0.6165 0.5683 0.6082 0.037 Uiso 1 1 calc R . . C26 C 0.6303(4) 0.6595(4) 0.52746(17) 0.0381(10) Uani 1 1 d . . . H26 H 0.6249 0.6013 0.5010 0.046 Uiso 1 1 calc R . . C27 C 0.6452(4) 0.7636(4) 0.50281(18) 0.0401(11) Uani 1 1 d . . . H27 H 0.6522 0.7771 0.4589 0.048 Uiso 1 1 calc R . . C28 C 0.6499(4) 0.8484(4) 0.54235(17) 0.0348(9) Uani 1 1 d . . . C29 C 0.6683(5) 0.9649(4) 0.5188(2) 0.0536(13) Uani 1 1 d . . . H29A H 0.6052 1.0304 0.5477 0.080 Uiso 1 1 calc R . . H29B H 0.6454 0.9808 0.4767 0.080 Uiso 1 1 calc R . . H29C H 0.7661 0.9584 0.5169 0.080 Uiso 1 1 calc R . . C30 C 0.6379(3) 0.8237(3) 0.60615(17) 0.0307(9) Uani 1 1 d . . . H30 H 0.6386 0.8821 0.6339 0.037 Uiso 1 1 calc R . . C31 C 0.6813(4) 0.5720(3) 0.87163(16) 0.0291(9) Uani 1 1 d . . . H31 H 0.7618 0.5248 0.8427 0.035 Uiso 1 1 calc R . . C32 C 0.6773(4) 0.5523(4) 0.93499(17) 0.0422(11) Uani 1 1 d . . . H32 H 0.7542 0.4937 0.9495 0.051 Uiso 1 1 calc R . . C33 C 0.5599(4) 0.6190(4) 0.97701(18) 0.0448(11) Uani 1 1 d . . . H33 H 0.5552 0.6066 1.0209 0.054 Uiso 1 1 calc R . . C34 C 0.4492(4) 0.7039(3) 0.95556(16) 0.0329(9) Uani 1 1 d . . . C35 C 0.4634(3) 0.7182(3) 0.89074(16) 0.0267(8) Uani 1 1 d . . . H35 H 0.3878 0.7765 0.8752 0.032 Uiso 1 1 calc R . . C36 C 0.3168(4) 0.7803(4) 0.99922(19) 0.0520(12) Uani 1 1 d . . . H36A H 0.2937 0.7330 1.0352 0.078 Uiso 1 1 calc R . . H36B H 0.2386 0.8082 0.9764 0.078 Uiso 1 1 calc R . . H36C H 0.3323 0.8492 1.0144 0.078 Uiso 1 1 calc R . . C37 C 0.0364(3) 0.5507(3) 0.82397(16) 0.0291(9) Uani 1 1 d . . . C38 C 0.0501(3) 0.4339(3) 0.81605(18) 0.0344(9) Uani 1 1 d . . . H38 H 0.0203 0.4113 0.7815 0.041 Uiso 1 1 calc R . . C39 C 0.1077(4) 0.3487(4) 0.8586(2) 0.0473(12) Uani 1 1 d . . . H39 H 0.1147 0.2683 0.8541 0.057 Uiso 1 1 calc R . . C40 C 0.1550(4) 0.3819(5) 0.9078(2) 0.0539(14) Uani 1 1 d . . . H40 H 0.1969 0.3238 0.9364 0.065 Uiso 1 1 calc R . . C41 C 0.1412(4) 0.4996(4) 0.91522(18) 0.0456(12) Uani 1 1 d . . . H41 H 0.1729 0.5212 0.9494 0.055 Uiso 1 1 calc R . . C42 C 0.0817(3) 0.5878(4) 0.87377(16) 0.0318(9) Uani 1 1 d . . . C43 C 0.0574(3) 0.7146(4) 0.88560(16) 0.0317(9) Uani 1 1 d . . . C44 C -0.0266(4) 0.7712(4) 0.94196(18) 0.0445(11) Uani 1 1 d . . . H44 H -0.0671 0.7271 0.9724 0.053 Uiso 1 1 calc R . . C45 C -0.0520(4) 0.8891(5) 0.9544(2) 0.0529(13) Uani 1 1 d . . . H45 H -0.1090 0.9252 0.9932 0.064 Uiso 1 1 calc R . . C46 C 0.0051(4) 0.9551(4) 0.9108(2) 0.0508(12) Uani 1 1 d . . . H46 H -0.0138 1.0370 0.9190 0.061 Uiso 1 1 calc R . . C47 C 0.0902(4) 0.9010(4) 0.85479(19) 0.0399(10) Uani 1 1 d . . . H47 H 0.1301 0.9461 0.8247 0.048 Uiso 1 1 calc R . . C48 C 0.1176(3) 0.7819(4) 0.84235(17) 0.0312(9) Uani 1 1 d . . . C49 C 0.3561(4) 0.4227(4) 0.6712(2) 0.0400(10) Uani 1 1 d . . . H49A H 0.2771 0.4173 0.6537 0.048 Uiso 1 1 calc R . . H49B H 0.3474 0.3929 0.7148 0.048 Uiso 1 1 calc R . . C50 C 0.4920(4) 0.3440(4) 0.6327(2) 0.0516(12) Uani 1 1 d . . . H50A H 0.5009 0.3721 0.5893 0.077 Uiso 1 1 calc R . . H50B H 0.4934 0.2618 0.6330 0.077 Uiso 1 1 calc R . . H50C H 0.5708 0.3466 0.6505 0.077 Uiso 1 1 calc R . . C51 C 0.2195(5) 0.7410(4) 0.5314(2) 0.0601(14) Uani 1 1 d . . . H51A H 0.2227 0.6732 0.5062 0.072 Uiso 1 1 calc R . . H51B H 0.3038 0.7620 0.5141 0.072 Uiso 1 1 calc R . . C52 C 0.0908(5) 0.8440(4) 0.5283(2) 0.0605(14) Uani 1 1 d . . . H52A H 0.0081 0.8234 0.5471 0.091 Uiso 1 1 calc R . . H52B H 0.0874 0.8655 0.4842 0.091 Uiso 1 1 calc R . . H52C H 0.0911 0.9118 0.5515 0.091 Uiso 1 1 calc R . . C53 C -0.1219(4) 0.9689(3) 0.7028(2) 0.0415(10) Uani 1 1 d . . . H53A H -0.0354 0.9867 0.6856 0.050 Uiso 1 1 calc R . . H53B H -0.1446 0.9838 0.7489 0.050 Uiso 1 1 calc R . . C54 C -0.2413(4) 1.0512(3) 0.6739(2) 0.0438(11) Uani 1 1 d . . . H54A H -0.2221 1.0333 0.6287 0.066 Uiso 1 1 calc R . . H54B H -0.2504 1.1341 0.6803 0.066 Uiso 1 1 calc R . . H54C H -0.3292 1.0397 0.6939 0.066 Uiso 1 1 calc R . . H9A H -0.170(3) 0.837(4) 0.7161(17) 0.062(14) Uiso 1 1 d D . . H7A H 0.405(4) 0.554(4) 0.6937(19) 0.070(15) Uiso 1 1 d D . . H5A H -0.082(3) 0.617(3) 0.7659(17) 0.052(13) Uiso 1 1 d D . . H6A H 0.276(3) 0.747(4) 0.773(2) 0.087(18) Uiso 1 1 d D . . H8A H 0.283(5) 0.636(3) 0.593(3) 0.15(3) Uiso 1 1 d 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 0.0162(3) 0.0238(3) 0.0218(3) 0.0020(2) -0.00611(19) -0.0095(2) Na1 0.0237(7) 0.0407(9) 0.0310(8) 0.0029(7) -0.0066(6) -0.0112(7) N1 0.0240(15) 0.0306(17) 0.0251(16) 0.0040(13) -0.0085(12) -0.0131(13) N2 0.0207(14) 0.0273(16) 0.0210(14) 0.0000(12) -0.0060(11) -0.0108(13) O1 0.0189(11) 0.0298(14) 0.0252(12) -0.0039(10) -0.0074(9) -0.0092(10) O2 0.0225(11) 0.0213(12) 0.0245(12) 0.0030(10) -0.0091(9) -0.0119(10) O3 0.0175(11) 0.0227(13) 0.0299(13) 0.0053(10) -0.0080(10) -0.0083(10) O4 0.0190(11) 0.0271(13) 0.0238(12) -0.0029(10) -0.0029(9) -0.0125(10) O5 0.0264(13) 0.0348(15) 0.0292(13) 0.0056(11) -0.0150(11) -0.0163(12) O6 0.0236(13) 0.0410(16) 0.0328(14) -0.0063(12) -0.0011(11) -0.0188(12) O7 0.0275(13) 0.0367(16) 0.0411(16) 0.0025(12) -0.0172(12) -0.0130(12) O8 0.0420(17) 0.064(2) 0.0334(16) 0.0120(15) -0.0051(13) -0.0059(17) O9 0.0223(13) 0.0389(16) 0.0432(16) 0.0088(13) 0.0000(11) -0.0134(12) C1 0.0157(15) 0.028(2) 0.0214(17) 0.0000(15) -0.0084(13) -0.0019(15) C2 0.0230(17) 0.034(2) 0.031(2) 0.0056(17) -0.0096(15) -0.0132(16) C3 0.0229(18) 0.052(3) 0.025(2) -0.0009(18) -0.0033(15) -0.0108(18) C4 0.0275(19) 0.042(2) 0.033(2) -0.0081(18) -0.0036(16) -0.0079(18) C5 0.0273(18) 0.028(2) 0.033(2) -0.0029(16) -0.0065(16) -0.0076(16) C6 0.0194(16) 0.0234(19) 0.0254(18) 0.0008(15) -0.0105(14) -0.0059(15) C7 0.0285(18) 0.0229(18) 0.0217(18) 0.0007(14) -0.0084(14) -0.0112(15) C8 0.036(2) 0.028(2) 0.034(2) 0.0023(17) -0.0126(17) -0.0097(18) C9 0.058(3) 0.032(2) 0.028(2) 0.0089(17) -0.0115(19) -0.017(2) C10 0.049(2) 0.036(2) 0.027(2) 0.0013(17) -0.0009(17) -0.020(2) C11 0.0301(18) 0.030(2) 0.0244(19) 0.0001(15) -0.0053(15) -0.0143(17) C12 0.0264(17) 0.0212(18) 0.0206(17) -0.0011(14) -0.0094(14) -0.0106(15) C13 0.0153(15) 0.027(2) 0.0249(18) 0.0040(15) -0.0068(13) -0.0064(15) C14 0.0228(17) 0.033(2) 0.030(2) 0.0004(16) -0.0085(15) -0.0111(16) C15 0.0308(19) 0.042(2) 0.031(2) 0.0127(18) -0.0173(16) -0.0130(18) C16 0.0306(19) 0.031(2) 0.037(2) 0.0130(18) -0.0127(16) -0.0088(17) C17 0.0294(19) 0.027(2) 0.036(2) 0.0049(17) -0.0091(16) -0.0114(17) C18 0.0192(16) 0.028(2) 0.0257(18) 0.0024(15) -0.0042(14) -0.0084(15) C19 0.0221(16) 0.0205(18) 0.0251(18) 0.0037(14) -0.0068(14) -0.0116(15) C20 0.0296(18) 0.027(2) 0.028(2) -0.0020(16) -0.0043(15) -0.0074(16) C21 0.042(2) 0.037(2) 0.0244(19) -0.0051(16) -0.0053(16) -0.0145(19) C22 0.033(2) 0.038(2) 0.028(2) 0.0033(17) -0.0139(16) -0.0146(18) C23 0.0221(17) 0.034(2) 0.0295(19) 0.0019(16) -0.0094(14) -0.0123(16) C24 0.0212(16) 0.0215(18) 0.0235(18) 0.0026(14) -0.0043(13) -0.0126(15) C25 0.0270(18) 0.037(2) 0.030(2) -0.0009(17) -0.0053(15) -0.0138(17) C26 0.032(2) 0.052(3) 0.030(2) -0.0020(19) -0.0091(16) -0.0116(19) C27 0.038(2) 0.059(3) 0.023(2) 0.009(2) -0.0083(17) -0.017(2) C28 0.0305(19) 0.045(2) 0.031(2) 0.0084(19) -0.0072(16) -0.0157(18) C29 0.058(3) 0.066(3) 0.049(3) 0.024(2) -0.020(2) -0.035(3) C30 0.0293(19) 0.035(2) 0.031(2) 0.0031(17) -0.0078(15) -0.0142(17) C31 0.0247(18) 0.034(2) 0.027(2) 0.0006(16) -0.0089(15) -0.0068(16) C32 0.040(2) 0.048(3) 0.030(2) 0.0021(19) -0.0129(18) -0.003(2) C33 0.046(2) 0.062(3) 0.023(2) 0.005(2) -0.0117(18) -0.013(2) C34 0.035(2) 0.040(2) 0.0253(19) -0.0014(17) -0.0056(16) -0.0146(18) C35 0.0231(17) 0.029(2) 0.031(2) 0.0053(16) -0.0073(15) -0.0122(16) C36 0.052(3) 0.064(3) 0.031(2) -0.001(2) 0.0003(19) -0.013(2) C37 0.0149(16) 0.038(2) 0.032(2) 0.0089(17) -0.0052(14) -0.0077(16) C38 0.0234(18) 0.035(2) 0.042(2) 0.0060(18) -0.0070(16) -0.0077(17) C39 0.030(2) 0.040(3) 0.063(3) 0.014(2) -0.004(2) -0.006(2) C40 0.036(2) 0.069(4) 0.044(3) 0.030(3) -0.008(2) -0.008(2) C41 0.035(2) 0.071(3) 0.028(2) 0.013(2) -0.0095(17) -0.016(2) C42 0.0205(17) 0.052(3) 0.0236(19) 0.0074(18) -0.0061(14) -0.0134(18) C43 0.0192(17) 0.054(3) 0.0239(19) 0.0000(18) -0.0099(14) -0.0120(18) C44 0.030(2) 0.080(3) 0.026(2) -0.004(2) -0.0052(16) -0.021(2) C45 0.029(2) 0.085(4) 0.042(3) -0.027(3) -0.0096(19) -0.012(2) C46 0.030(2) 0.060(3) 0.064(3) -0.027(2) -0.013(2) -0.013(2) C47 0.0266(19) 0.051(3) 0.047(2) -0.011(2) -0.0076(17) -0.017(2) C48 0.0179(17) 0.047(2) 0.032(2) -0.0070(18) -0.0085(15) -0.0125(17) C49 0.039(2) 0.040(2) 0.051(3) 0.005(2) -0.0200(19) -0.020(2) C50 0.048(3) 0.043(3) 0.068(3) -0.019(2) -0.030(2) -0.009(2) C51 0.057(3) 0.071(4) 0.041(3) 0.008(2) -0.005(2) -0.013(3) C52 0.068(3) 0.062(3) 0.049(3) 0.016(2) -0.021(2) -0.017(3) C53 0.036(2) 0.041(3) 0.055(3) 0.010(2) -0.0157(19) -0.021(2) C54 0.049(2) 0.033(2) 0.057(3) 0.011(2) -0.020(2) -0.019(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 O4 1.908(2) . ? Mn1 O2 1.918(2) . ? Mn1 O3 1.933(2) . ? Mn1 O1 1.934(2) . ? Mn1 N2 2.339(3) . ? Mn1 N1 2.367(3) . ? Na1 O9 2.299(3) . ? Na1 O6 2.306(3) . ? Na1 O5 2.317(3) . ? Na1 O8 2.338(3) . ? Na1 O7 2.435(3) . ? Na1 H8A 2.60(6) . ? N1 C25 1.336(5) . ? N1 C30 1.338(4) . ? N2 C35 1.337(4) . ? N2 C31 1.344(4) . ? O1 C1 1.351(4) . ? O2 C12 1.371(4) . ? O3 C13 1.355(4) . ? O4 C24 1.353(4) . ? O5 C37 1.376(4) . ? O5 H5A 0.893(10) . ? O6 C48 1.369(4) . ? O6 H6A 0.891(10) . ? O7 C49 1.420(5) . ? O7 H7A 0.889(10) . ? O8 C51 1.426(5) . ? O8 H8A 0.889(10) . ? O9 C53 1.429(5) . ? O9 H9A 0.883(10) . ? C1 C6 1.402(5) . ? C1 C2 1.404(5) . ? C2 C3 1.374(5) . ? C2 H2 0.9500 . ? C3 C4 1.376(5) . ? C3 H3 0.9500 . ? C4 C5 1.393(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(5) . ? C5 H5 0.9500 . ? C6 C7 1.491(5) . ? C7 C8 1.392(4) . ? C7 C12 1.406(4) . ? C8 C9 1.387(5) . ? C8 H8 0.9500 . ? C9 C10 1.371(5) . ? C9 H9 0.9500 . ? C10 C11 1.382(5) . ? C10 H10 0.9500 . ? C11 C12 1.391(5) . ? C11 H11 0.9500 . ? C13 C18 1.396(5) . ? C13 C14 1.403(5) . ? C14 C15 1.386(5) . ? C14 H14 0.9500 . ? C15 C16 1.371(5) . ? C15 H15 0.9500 . ? C16 C17 1.396(5) . ? C16 H16 0.9500 . ? C17 C18 1.409(4) . ? C17 H17 0.9500 . ? C18 C19 1.490(5) . ? C19 C20 1.391(5) . ? C19 C24 1.409(4) . ? C20 C21 1.396(5) . ? C20 H20 0.9500 . ? C21 C22 1.372(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 C24 1.407(5) . ? C23 H23 0.9500 . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 C27 1.378(5) . ? C26 H26 0.9500 . ? C27 C28 1.384(6) . ? C27 H27 0.9500 . ? C28 C30 1.389(5) . ? C28 C29 1.523(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? C31 C32 1.376(5) . ? C31 H31 0.9500 . ? C32 C33 1.375(5) . ? C32 H32 0.9500 . ? C33 C34 1.377(5) . ? C33 H33 0.9500 . ? C34 C35 1.391(5) . ? C34 C36 1.515(5) . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.374(5) . ? C37 C42 1.408(5) . ? C38 C39 1.390(5) . ? C38 H38 0.9500 . ? C39 C40 1.388(7) . ? C39 H39 0.9500 . ? C40 C41 1.381(7) . ? C40 H40 0.9500 . ? C41 C42 1.399(5) . ? C41 H41 0.9500 . ? C42 C43 1.478(5) . ? C43 C44 1.398(5) . ? C43 C48 1.400(5) . ? C44 C45 1.374(6) . ? C44 H44 0.9500 . ? C45 C46 1.377(6) . ? C45 H45 0.9500 . ? C46 C47 1.386(6) . ? C46 H46 0.9500 . ? C47 C48 1.383(5) . ? C47 H47 0.9500 . ? C49 C50 1.496(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.470(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.505(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 177.53(9) . . ? O4 Mn1 O3 90.02(10) . . ? O2 Mn1 O3 91.02(10) . . ? O4 Mn1 O1 87.99(10) . . ? O2 Mn1 O1 90.89(10) . . ? O3 Mn1 O1 177.21(9) . . ? O4 Mn1 N2 92.02(10) . . ? O2 Mn1 N2 90.19(10) . . ? O3 Mn1 N2 91.75(10) . . ? O1 Mn1 N2 90.28(10) . . ? O4 Mn1 N1 91.05(10) . . ? O2 Mn1 N1 86.74(10) . . ? O3 Mn1 N1 87.85(10) . . ? O1 Mn1 N1 90.23(10) . . ? N2 Mn1 N1 176.90(10) . . ? O9 Na1 O6 115.57(12) . . ? O9 Na1 O5 84.12(9) . . ? O6 Na1 O5 77.42(9) . . ? O9 Na1 O8 93.36(11) . . ? O6 Na1 O8 126.73(11) . . ? O5 Na1 O8 153.14(13) . . ? O9 Na1 O7 159.48(11) . . ? O6 Na1 O7 83.31(10) . . ? O5 Na1 O7 109.07(10) . . ? O8 Na1 O7 67.67(10) . . ? O9 Na1 H8A 111.4(10) . . ? O6 Na1 H8A 120.4(15) . . ? O5 Na1 H8A 142.6(12) . . ? O8 Na1 H8A 19.8(7) . . ? O7 Na1 H8A 48.7(9) . . ? C25 N1 C30 117.5(3) . . ? C25 N1 Mn1 122.0(2) . . ? C30 N1 Mn1 120.4(2) . . ? C35 N2 C31 117.0(3) . . ? C35 N2 Mn1 123.0(2) . . ? C31 N2 Mn1 119.9(2) . . ? C1 O1 Mn1 122.04(19) . . ? C12 O2 Mn1 121.34(19) . . ? C13 O3 Mn1 125.48(18) . . ? C24 O4 Mn1 119.80(19) . . ? C37 O5 Na1 122.16(19) . . ? C37 O5 H5A 110(3) . . ? Na1 O5 H5A 106(3) . . ? C48 O6 Na1 122.57(19) . . ? C48 O6 H6A 116(3) . . ? Na1 O6 H6A 105(3) . . ? C49 O7 Na1 121.0(2) . . ? C49 O7 H7A 112(3) . . ? Na1 O7 H7A 110(3) . . ? C51 O8 Na1 155.8(3) . . ? C51 O8 H8A 103(5) . . ? Na1 O8 H8A 97(5) . . ? C53 O9 Na1 120.5(2) . . ? C53 O9 H9A 100(3) . . ? Na1 O9 H9A 114(3) . . ? O1 C1 C6 120.8(3) . . ? O1 C1 C2 119.7(3) . . ? C6 C1 C2 119.5(3) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 118.5(3) . . ? C5 C6 C7 121.2(3) . . ? C1 C6 C7 120.3(3) . . ? C8 C7 C12 118.4(3) . . ? C8 C7 C6 120.3(3) . . ? C12 C7 C6 121.3(3) . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? O2 C12 C11 118.9(3) . . ? O2 C12 C7 121.2(3) . . ? C11 C12 C7 119.9(3) . . ? O3 C13 C18 121.5(3) . . ? O3 C13 C14 118.9(3) . . ? C18 C13 C14 119.5(3) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 121.1(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.0(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 121.3(4) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 118.7(3) . . ? C13 C18 C19 122.6(3) . . ? C17 C18 C19 118.6(3) . . ? C20 C19 C24 118.9(3) . . ? C20 C19 C18 120.7(3) . . ? C24 C19 C18 120.4(3) . . ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.8(3) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? O4 C24 C23 119.9(3) . . ? O4 C24 C19 120.8(3) . . ? C23 C24 C19 119.2(3) . . ? N1 C25 C26 122.7(4) . . ? N1 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C27 C26 C25 118.8(4) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C30 117.3(4) . . ? C27 C28 C29 123.0(4) . . ? C30 C28 C29 119.7(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 C28 123.9(4) . . ? N1 C30 H30 118.0 . . ? C28 C30 H30 118.0 . . ? N2 C31 C32 122.9(3) . . ? N2 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C33 C32 C31 118.7(3) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 117.0(3) . . ? C33 C34 C36 122.9(3) . . ? C35 C34 C36 120.2(3) . . ? N2 C35 C34 124.2(3) . . ? N2 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 O5 121.4(3) . . ? C38 C37 C42 122.0(3) . . ? O5 C37 C42 116.7(3) . . ? C37 C38 C39 119.9(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 119.6(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 120.0(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 121.8(4) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C37 116.7(4) . . ? C41 C42 C43 120.8(4) . . ? C37 C42 C43 122.3(3) . . ? C44 C43 C48 117.5(4) . . ? C44 C43 C42 120.1(4) . . ? C48 C43 C42 122.4(3) . . ? C45 C44 C43 121.7(4) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 120.2(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 119.4(4) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C48 C47 C46 120.6(4) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? O6 C48 C47 122.3(3) . . ? O6 C48 C43 117.2(3) . . ? C47 C48 C43 120.5(4) . . ? O7 C49 C50 113.4(3) . . ? O7 C49 H49A 108.9 . . ? C50 C49 H49A 108.9 . . ? O7 C49 H49B 108.9 . . ? C50 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O8 C51 C52 108.0(4) . . ? O8 C51 H51A 110.1 . . ? C52 C51 H51A 110.1 . . ? O8 C51 H51B 110.1 . . ? C52 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O9 C53 C54 112.2(3) . . ? O9 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? O9 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.921 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.072 # Attachment '- 1.cif' data_! _database_code_depnum_ccdc_archive 'CCDC 778268' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Na2Mn2(biphen)4(py)3(EtOH)2)n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H59 Mn2 N3 Na2 O10' _chemical_formula_weight 1222.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.814(2) _cell_length_b 12.513(3) _cell_length_c 22.786(5) _cell_angle_alpha 96.06(3) _cell_angle_beta 98.11(3) _cell_angle_gamma 115.49(3) _cell_volume 2957.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.505 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9409 _cell_measurement_reflns_used 5803 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.99232 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 23081 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.9409 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0239606000 _diffrn_orient_matrix_UB_12 -0.0424771000 _diffrn_orient_matrix_UB_13 -0.0053608000 _diffrn_orient_matrix_UB_21 -0.0631644000 _diffrn_orient_matrix_UB_22 -0.0476428000 _diffrn_orient_matrix_UB_23 -0.0053932000 _diffrn_orient_matrix_UB_31 -0.0077219000 _diffrn_orient_matrix_UB_32 0.0033406000 _diffrn_orient_matrix_UB_33 -0.0310855000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 24.00 53.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -17.3903 77.0000 30.0000 29 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 39.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 -90.0000 48 #__ type_ start__ end____ width___ exp.time_ 3 omega -48.00 50.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -77.0000 30.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega -50.00 50.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 5 omega -6.00 86.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 150.0000 92 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 10822 _reflns_number_gt 6185 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0596P)^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 10822 _refine_ls_number_parameters 761 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 0.0000 0.5000 0.5000 0.0212(2) Uani 1 2 d S . . Mn2 Mn 0.00252(6) 0.22875(6) 0.25636(3) 0.02607(18) Uani 1 1 d . . . Mn3 Mn 0.0000 0.0000 0.0000 0.0252(2) Uani 1 2 d S . . Na1 Na 0.00749(15) 0.30721(13) 0.40173(6) 0.0240(4) Uani 1 1 d . . . Na2 Na -0.03411(18) 0.04105(16) 0.13347(7) 0.0403(5) Uani 1 1 d . . . N1 N 0.0571(4) 0.3973(3) 0.22178(15) 0.0358(10) Uani 1 1 d . . . N2 N 0.0822(4) 0.1707(3) 0.44695(16) 0.0388(10) Uani 1 1 d . . . N3 N -0.1703(5) -0.1517(6) 0.1646(2) 0.090(2) Uani 1 1 d . . . O1 O -0.1265(3) 0.1435(3) 0.18566(12) 0.0347(8) Uani 1 1 d . . . O2 O -0.1211(2) 0.2076(2) 0.30545(11) 0.0227(6) Uani 1 1 d . . . O3 O 0.1060(3) 0.1664(3) 0.22208(12) 0.0320(7) Uani 1 1 d . . . O4 O 0.1266(3) 0.3103(2) 0.32790(12) 0.0236(6) Uani 1 1 d . . . O5 O 0.1863(3) 0.4837(3) 0.48603(14) 0.0369(8) Uani 1 1 d D . . O6 O -0.0154(3) 0.4889(2) 0.41508(11) 0.0258(7) Uani 1 1 d . . . O7 O 0.0748(3) 0.6710(2) 0.51300(11) 0.0239(7) Uani 1 1 d . . . O8 O -0.0612(3) -0.1453(3) -0.05659(12) 0.0365(8) Uani 1 1 d . . . O9 O 0.0226(3) -0.0753(2) 0.06610(12) 0.0305(7) Uani 1 1 d . . . O10 O -0.1905(3) -0.0297(4) 0.03375(15) 0.0754(13) Uani 1 1 d D . . H10A H -0.1894 0.0490 0.0285 0.090 Uiso 1 1 calc RD . . C1 C -0.2165(4) 0.1807(4) 0.17105(18) 0.0335(11) Uani 1 1 d . . . C2 C -0.2130(5) 0.2420(5) 0.1233(2) 0.0462(13) Uani 1 1 d . . . H2 H -0.1448 0.2600 0.1024 0.055 Uiso 1 1 calc R . . C3 C -0.3062(5) 0.2769(5) 0.1058(2) 0.0553(15) Uani 1 1 d . . . H3 H -0.3016 0.3192 0.0733 0.066 Uiso 1 1 calc R . . C4 C -0.4058(5) 0.2509(5) 0.1353(2) 0.0540(15) Uani 1 1 d . . . H4 H -0.4699 0.2757 0.1237 0.065 Uiso 1 1 calc R . . C5 C -0.4118(5) 0.1878(4) 0.1823(2) 0.0408(12) Uani 1 1 d . . . H5 H -0.4809 0.1696 0.2027 0.049 Uiso 1 1 calc R . . C6 C -0.3204(4) 0.1509(4) 0.20021(18) 0.0302(10) Uani 1 1 d . . . C7 C -0.3332(4) 0.0755(4) 0.24727(19) 0.0294(10) Uani 1 1 d . . . C8 C -0.4472(5) -0.0288(4) 0.2424(2) 0.0444(13) Uani 1 1 d . . . H8 H -0.5164 -0.0495 0.2095 0.053 Uiso 1 1 calc R . . C9 C -0.4615(5) -0.1035(4) 0.2852(2) 0.0500(14) Uani 1 1 d . . . H9 H -0.5404 -0.1732 0.2819 0.060 Uiso 1 1 calc R . . C10 C -0.3607(4) -0.0754(4) 0.3319(2) 0.0443(13) Uani 1 1 d . . . H10 H -0.3689 -0.1278 0.3601 0.053 Uiso 1 1 calc R . . C11 C -0.2473(4) 0.0284(4) 0.33852(19) 0.0351(11) Uani 1 1 d . . . H11 H -0.1794 0.0480 0.3719 0.042 Uiso 1 1 calc R . . C12 C -0.2314(4) 0.1049(4) 0.29652(18) 0.0243(10) Uani 1 1 d . . . C13 C 0.1918(4) 0.1385(4) 0.25379(18) 0.0286(11) Uani 1 1 d . . . C14 C 0.1692(5) 0.0171(4) 0.24451(19) 0.0330(11) Uani 1 1 d . . . H14 H 0.0933 -0.0426 0.2179 0.040 Uiso 1 1 calc R . . C15 C 0.2563(5) -0.0155(4) 0.2737(2) 0.0407(12) Uani 1 1 d . . . H15 H 0.2399 -0.0976 0.2671 0.049 Uiso 1 1 calc R . . C16 C 0.3662(5) 0.0687(4) 0.3121(2) 0.0420(13) Uani 1 1 d . . . H16 H 0.4263 0.0459 0.3319 0.050 Uiso 1 1 calc R . . C17 C 0.3882(4) 0.1874(4) 0.3215(2) 0.0397(12) Uani 1 1 d . . . H17 H 0.4643 0.2457 0.3484 0.048 Uiso 1 1 calc R . . C18 C 0.3034(4) 0.2248(4) 0.2931(2) 0.0289(11) Uani 1 1 d . . . C19 C 0.3347(4) 0.3548(4) 0.3072(2) 0.0347(12) Uani 1 1 d . . . C20 C 0.4561(5) 0.4433(4) 0.3067(3) 0.0565(16) Uani 1 1 d . . . H20 H 0.5164 0.4196 0.2939 0.068 Uiso 1 1 calc R . . C21 C 0.4924(5) 0.5640(4) 0.3239(3) 0.0678(19) Uani 1 1 d . . . H21 H 0.5761 0.6227 0.3230 0.081 Uiso 1 1 calc R . . C22 C 0.4049(5) 0.5983(4) 0.3426(3) 0.0525(15) Uani 1 1 d . . . H22 H 0.4290 0.6813 0.3551 0.063 Uiso 1 1 calc R . . C23 C 0.2831(4) 0.5135(4) 0.3434(2) 0.0359(12) Uani 1 1 d . . . H23 H 0.2238 0.5385 0.3562 0.043 Uiso 1 1 calc R . . C24 C 0.2463(4) 0.3916(4) 0.32545(19) 0.0286(10) Uani 1 1 d . . . C25 C 0.0068(5) 0.4715(4) 0.2361(2) 0.0500(15) Uani 1 1 d . . . H25 H -0.0551 0.4489 0.2607 0.060 Uiso 1 1 calc R . . C26 C 0.0409(6) 0.5788(5) 0.2166(2) 0.0694(19) Uani 1 1 d . . . H26 H 0.0063 0.6313 0.2290 0.083 Uiso 1 1 calc R . . C27 C 0.1256(7) 0.6090(5) 0.1790(3) 0.080(2) Uani 1 1 d . . . H27 H 0.1477 0.6812 0.1634 0.096 Uiso 1 1 calc R . . C28 C 0.1782(6) 0.5345(5) 0.1640(3) 0.071(2) Uani 1 1 d . . . H28 H 0.2391 0.5551 0.1387 0.085 Uiso 1 1 calc R . . C29 C 0.1414(5) 0.4290(4) 0.1861(2) 0.0509(15) Uani 1 1 d . . . H29 H 0.1776 0.3769 0.1754 0.061 Uiso 1 1 calc R . . C30 C 0.1445(5) 0.1209(4) 0.4190(2) 0.0444(13) Uani 1 1 d . . . H30 H 0.1414 0.1212 0.3771 0.053 Uiso 1 1 calc R . . C31 C 0.2133(5) 0.0689(4) 0.4476(2) 0.0404(12) Uani 1 1 d . . . H31 H 0.2567 0.0350 0.4258 0.049 Uiso 1 1 calc R . . C32 C 0.2180(5) 0.0670(4) 0.5078(2) 0.0434(13) Uani 1 1 d . . . H32 H 0.2636 0.0309 0.5286 0.052 Uiso 1 1 calc R . . C33 C 0.1550(5) 0.1187(4) 0.5374(2) 0.0444(13) Uani 1 1 d . . . H33 H 0.1579 0.1204 0.5793 0.053 Uiso 1 1 calc R . . C34 C 0.0878(5) 0.1677(4) 0.5055(2) 0.0407(13) Uani 1 1 d . . . H34 H 0.0430 0.2013 0.5264 0.049 Uiso 1 1 calc R . . C35 C 0.2811(7) 0.4716(6) 0.5263(3) 0.0748(18) Uiso 1 1 d . . . C36A C 0.3911(13) 0.4787(13) 0.5050(7) 0.065(4) Uiso 0.40 1 d P . . H36A H 0.4232 0.5475 0.4843 0.097 Uiso 0.40 1 calc PR . . H36B H 0.3681 0.4043 0.4768 0.097 Uiso 0.40 1 calc PR . . H36C H 0.4578 0.4893 0.5391 0.097 Uiso 0.40 1 calc PR . . C36B C 0.3830(10) 0.5686(9) 0.5538(5) 0.081(3) Uiso 0.60 1 d P . . H36D H 0.4337 0.6053 0.5244 0.121 Uiso 0.60 1 calc PR . . H36E H 0.4345 0.5480 0.5839 0.121 Uiso 0.60 1 calc PR . . H36F H 0.3579 0.6257 0.5739 0.121 Uiso 0.60 1 calc PR . . H5A H 0.241(7) 0.537(7) 0.469(3) 0.16(4) Uiso 1 1 d D . . C37 C 0.1797(4) 0.7304(3) 0.49044(19) 0.0242(10) Uani 1 1 d . . . C38 C 0.1688(4) 0.7372(3) 0.42894(18) 0.0248(10) Uani 1 1 d . . . C39 C 0.2807(5) 0.7997(4) 0.4084(2) 0.0349(12) Uani 1 1 d . . . H40 H 0.2744 0.8049 0.3668 0.042 Uiso 1 1 calc R . . C40 C 0.3991(5) 0.8537(4) 0.4456(2) 0.0458(13) Uani 1 1 d . . . H41 H 0.4737 0.8957 0.4302 0.055 Uiso 1 1 calc R . . C41 C 0.4088(5) 0.8463(4) 0.5064(2) 0.0480(13) Uani 1 1 d . . . H42 H 0.4907 0.8826 0.5327 0.058 Uiso 1 1 calc R . . C42 C 0.2995(4) 0.7863(4) 0.5286(2) 0.0367(12) Uani 1 1 d . . . H43 H 0.3067 0.7834 0.5704 0.044 Uiso 1 1 calc R . . C43 C -0.0467(4) 0.5601(4) 0.38289(18) 0.0270(10) Uani 1 1 d . . . C44 C -0.1625(4) 0.5125(4) 0.34171(19) 0.0369(12) Uani 1 1 d . . . H44 H -0.2207 0.4297 0.3372 0.044 Uiso 1 1 calc R . . C45 C -0.1943(5) 0.5832(5) 0.3074(2) 0.0485(14) Uani 1 1 d . . . H45 H -0.2745 0.5486 0.2798 0.058 Uiso 1 1 calc R . . C46 C -0.1128(5) 0.7021(5) 0.3124(2) 0.0473(14) Uani 1 1 d . . . H46 H -0.1361 0.7505 0.2889 0.057 Uiso 1 1 calc R . . C47 C 0.0042(5) 0.7512(4) 0.35214(19) 0.0353(11) Uani 1 1 d . . . H47 H 0.0615 0.8339 0.3551 0.042 Uiso 1 1 calc R . . C48 C 0.0413(4) 0.6832(4) 0.38812(18) 0.0258(10) Uani 1 1 d . . . C49 C -0.1736(8) -0.2666(6) 0.1451(3) 0.088(2) Uani 1 1 d . . . H49 H -0.1056 -0.2649 0.1268 0.106 Uiso 1 1 calc R . . C50 C -0.2602(8) -0.3734(7) 0.1499(3) 0.097(3) Uani 1 1 d . . . H50 H -0.2536 -0.4437 0.1345 0.117 Uiso 1 1 calc R . . C51 C -0.3589(8) -0.3836(7) 0.1768(3) 0.090(2) Uani 1 1 d . . . H51 H -0.4215 -0.4590 0.1823 0.108 Uiso 1 1 calc R . . C52 C -0.3621(8) -0.2771(7) 0.1956(3) 0.096(2) Uani 1 1 d . . . H52 H -0.4280 -0.2748 0.2144 0.115 Uiso 1 1 calc R . . C53 C -0.2658(7) -0.1750(7) 0.1860(3) 0.082(2) Uani 1 1 d . . . H53 H -0.2750 -0.1049 0.1989 0.099 Uiso 1 1 calc R . . C54 C -0.1443(5) -0.2540(4) -0.0459(2) 0.0383(12) Uani 1 1 d . . . C55 C -0.2721(5) -0.3096(5) -0.0763(3) 0.0625(17) Uani 1 1 d . . . H55 H -0.3010 -0.2720 -0.1048 0.075 Uiso 1 1 calc R . . C56 C -0.3558(6) -0.4175(6) -0.0653(4) 0.088(2) Uani 1 1 d . . . H56 H -0.4427 -0.4546 -0.0862 0.106 Uiso 1 1 calc R . . C57 C -0.3154(6) -0.4727(5) -0.0243(4) 0.085(2) Uani 1 1 d . . . H57 H -0.3748 -0.5472 -0.0164 0.102 Uiso 1 1 calc R . . C58 C -0.1899(6) -0.4212(4) 0.0053(3) 0.0568(16) Uani 1 1 d . . . H58 H -0.1629 -0.4614 0.0331 0.068 Uiso 1 1 calc R . . C59 C -0.1009(5) -0.3108(4) -0.0045(2) 0.0375(12) Uani 1 1 d . . . C60 C 0.0338(4) -0.2551(4) 0.0275(2) 0.0317(11) Uani 1 1 d . . . C61 C 0.1079(5) -0.3159(4) 0.0238(2) 0.0373(12) Uani 1 1 d . . . H61 H 0.0711 -0.3944 -0.0001 0.045 Uiso 1 1 calc R . . C62 C 0.2345(5) -0.2642(5) 0.0544(2) 0.0474(14) Uani 1 1 d . . . H62 H 0.2846 -0.3061 0.0510 0.057 Uiso 1 1 calc R . . C63 C 0.2868(5) -0.1515(5) 0.0898(2) 0.0490(14) Uani 1 1 d . . . H63 H 0.3733 -0.1161 0.1113 0.059 Uiso 1 1 calc R . . C64 C 0.2157(5) -0.0890(4) 0.0946(2) 0.0386(12) Uani 1 1 d . . . H64 H 0.2530 -0.0118 0.1199 0.046 Uiso 1 1 calc R . . C65 C 0.0901(4) -0.1381(4) 0.06286(18) 0.0302(11) Uani 1 1 d . . . C66 C -0.3114(5) -0.0967(7) 0.0172(3) 0.106(3) Uani 1 1 d . . . H67 H -0.3229 -0.1805 0.0130 0.127 Uiso 1 1 calc R . . H66 H -0.3352 -0.0846 -0.0241 0.127 Uiso 1 1 calc R . . C67 C -0.4091(6) -0.0950(7) 0.0474(3) 0.095(2) Uani 1 1 d . . . H70 H -0.3802 -0.0852 0.0910 0.142 Uiso 1 1 calc R . . H68 H -0.4875 -0.1710 0.0330 0.142 Uiso 1 1 calc R . . H69 H -0.4264 -0.0277 0.0389 0.142 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 0.0244(5) 0.0186(5) 0.0179(5) 0.0001(4) 0.0075(4) 0.0072(4) Mn2 0.0357(4) 0.0363(4) 0.0154(3) 0.0050(3) 0.0097(3) 0.0233(3) Mn3 0.0284(6) 0.0314(5) 0.0169(5) -0.0029(4) 0.0035(4) 0.0164(5) Na1 0.0319(10) 0.0237(8) 0.0187(8) 0.0014(7) 0.0087(8) 0.0142(8) Na2 0.0569(13) 0.0569(12) 0.0207(9) 0.0004(9) 0.0093(9) 0.0392(11) N1 0.066(3) 0.042(2) 0.020(2) 0.0099(18) 0.016(2) 0.039(2) N2 0.057(3) 0.048(2) 0.028(2) 0.013(2) 0.015(2) 0.036(2) N3 0.048(3) 0.160(6) 0.042(3) 0.034(4) 0.020(3) 0.023(4) O1 0.049(2) 0.054(2) 0.0129(15) -0.0020(14) 0.0002(15) 0.0371(18) O2 0.0231(16) 0.0254(15) 0.0160(14) 0.0003(12) 0.0052(13) 0.0083(14) O3 0.046(2) 0.0462(19) 0.0218(16) 0.0087(15) 0.0122(15) 0.0356(17) O4 0.0237(17) 0.0277(15) 0.0212(15) 0.0036(13) 0.0070(13) 0.0128(14) O5 0.0313(19) 0.044(2) 0.041(2) 0.0055(17) 0.0044(17) 0.0236(17) O6 0.0391(18) 0.0192(15) 0.0182(15) 0.0022(13) 0.0096(14) 0.0115(14) O7 0.0315(17) 0.0188(14) 0.0205(15) 0.0013(12) 0.0111(14) 0.0095(14) O8 0.050(2) 0.0367(18) 0.0213(17) -0.0080(14) -0.0051(15) 0.0252(17) O9 0.0422(19) 0.0348(17) 0.0181(16) -0.0018(14) 0.0041(14) 0.0228(16) O10 0.034(2) 0.156(4) 0.031(2) 0.009(2) 0.0092(19) 0.040(3) C1 0.042(3) 0.051(3) 0.014(2) 0.001(2) -0.003(2) 0.031(3) C2 0.054(3) 0.070(4) 0.024(3) 0.015(3) 0.006(3) 0.037(3) C3 0.068(4) 0.071(4) 0.039(3) 0.030(3) 0.007(3) 0.040(3) C4 0.067(4) 0.063(4) 0.047(3) 0.014(3) -0.006(3) 0.049(3) C5 0.039(3) 0.053(3) 0.038(3) 0.006(3) 0.006(2) 0.029(3) C6 0.035(3) 0.038(3) 0.020(2) 0.000(2) -0.004(2) 0.022(2) C7 0.030(3) 0.030(2) 0.028(2) 0.002(2) 0.002(2) 0.015(2) C8 0.034(3) 0.049(3) 0.037(3) -0.002(3) -0.012(2) 0.014(3) C9 0.034(3) 0.039(3) 0.054(3) 0.010(3) -0.005(3) -0.001(2) C10 0.030(3) 0.042(3) 0.046(3) 0.019(3) -0.003(3) 0.004(2) C11 0.033(3) 0.037(3) 0.028(3) 0.010(2) -0.001(2) 0.011(2) C12 0.026(2) 0.026(2) 0.020(2) -0.0007(19) 0.002(2) 0.013(2) C13 0.041(3) 0.038(3) 0.022(2) 0.013(2) 0.020(2) 0.027(2) C14 0.048(3) 0.033(3) 0.026(2) 0.004(2) 0.010(2) 0.025(2) C15 0.058(4) 0.038(3) 0.041(3) 0.011(3) 0.016(3) 0.032(3) C16 0.046(3) 0.046(3) 0.052(3) 0.018(3) 0.014(3) 0.033(3) C17 0.033(3) 0.037(3) 0.056(3) 0.010(3) 0.011(3) 0.020(2) C18 0.026(3) 0.031(2) 0.041(3) 0.017(2) 0.023(2) 0.016(2) C19 0.033(3) 0.030(3) 0.050(3) 0.015(2) 0.022(3) 0.016(2) C20 0.039(3) 0.046(3) 0.103(5) 0.026(3) 0.041(3) 0.026(3) C21 0.043(4) 0.032(3) 0.140(6) 0.029(4) 0.050(4) 0.016(3) C22 0.049(3) 0.024(3) 0.092(4) 0.023(3) 0.032(3) 0.016(3) C23 0.039(3) 0.029(3) 0.048(3) 0.013(2) 0.019(3) 0.019(2) C24 0.028(3) 0.029(2) 0.031(3) 0.011(2) 0.014(2) 0.012(2) C25 0.085(4) 0.061(3) 0.037(3) 0.022(3) 0.029(3) 0.056(3) C26 0.137(6) 0.066(4) 0.048(4) 0.020(3) 0.033(4) 0.079(4) C27 0.153(7) 0.062(4) 0.061(4) 0.036(4) 0.051(5) 0.068(5) C28 0.125(6) 0.064(4) 0.068(4) 0.042(4) 0.064(4) 0.063(4) C29 0.081(4) 0.056(3) 0.044(3) 0.022(3) 0.040(3) 0.045(3) C30 0.063(4) 0.054(3) 0.035(3) 0.013(3) 0.021(3) 0.039(3) C31 0.046(3) 0.048(3) 0.043(3) 0.010(3) 0.015(3) 0.033(3) C32 0.050(3) 0.050(3) 0.040(3) 0.013(3) 0.007(3) 0.030(3) C33 0.067(4) 0.056(3) 0.027(3) 0.016(3) 0.012(3) 0.040(3) C34 0.062(4) 0.045(3) 0.034(3) 0.012(2) 0.019(3) 0.037(3) C37 0.029(3) 0.013(2) 0.030(2) 0.0022(19) 0.011(2) 0.008(2) C38 0.031(3) 0.015(2) 0.029(2) 0.0031(19) 0.011(2) 0.010(2) C39 0.042(3) 0.025(2) 0.042(3) 0.008(2) 0.024(3) 0.014(2) C40 0.031(3) 0.031(3) 0.061(4) 0.004(3) 0.020(3) -0.001(2) C41 0.029(3) 0.034(3) 0.059(4) -0.005(3) -0.001(3) 0.000(2) C42 0.039(3) 0.028(2) 0.032(3) 0.000(2) 0.005(2) 0.007(2) C43 0.029(3) 0.039(3) 0.018(2) 0.007(2) 0.013(2) 0.016(2) C44 0.026(3) 0.052(3) 0.027(3) 0.009(2) 0.011(2) 0.009(2) C45 0.028(3) 0.085(4) 0.036(3) 0.021(3) 0.009(2) 0.026(3) C46 0.056(4) 0.077(4) 0.035(3) 0.026(3) 0.015(3) 0.049(3) C47 0.048(3) 0.043(3) 0.027(3) 0.014(2) 0.017(2) 0.028(3) C48 0.035(3) 0.030(2) 0.021(2) 0.007(2) 0.014(2) 0.020(2) C49 0.150(8) 0.056(4) 0.078(5) 0.016(4) 0.044(5) 0.057(5) C50 0.128(7) 0.101(6) 0.057(5) 0.006(4) 0.038(5) 0.043(6) C51 0.115(7) 0.087(5) 0.063(5) 0.005(4) 0.010(5) 0.046(5) C52 0.109(6) 0.083(5) 0.099(6) -0.003(5) 0.003(5) 0.057(5) C53 0.086(5) 0.092(6) 0.084(5) 0.038(5) 0.022(5) 0.049(5) C54 0.039(3) 0.029(3) 0.041(3) -0.018(2) 0.003(3) 0.017(2) C55 0.040(3) 0.054(4) 0.080(5) -0.030(3) -0.011(3) 0.026(3) C56 0.030(4) 0.062(5) 0.139(7) -0.046(4) -0.003(4) 0.011(4) C57 0.049(4) 0.039(4) 0.150(8) -0.018(4) 0.047(5) 0.005(3) C58 0.055(4) 0.034(3) 0.081(4) -0.001(3) 0.036(4) 0.017(3) C59 0.038(3) 0.030(3) 0.049(3) 0.001(2) 0.017(3) 0.019(2) C60 0.040(3) 0.031(2) 0.033(3) 0.013(2) 0.018(2) 0.019(2) C61 0.051(3) 0.038(3) 0.036(3) 0.016(2) 0.022(3) 0.026(3) C62 0.058(4) 0.072(4) 0.040(3) 0.026(3) 0.020(3) 0.049(3) C63 0.044(3) 0.084(4) 0.030(3) 0.013(3) 0.004(3) 0.040(3) C64 0.045(3) 0.051(3) 0.023(3) 0.003(2) 0.003(2) 0.027(3) C65 0.040(3) 0.040(3) 0.020(2) 0.012(2) 0.014(2) 0.023(2) C66 0.029(4) 0.176(8) 0.053(4) -0.031(5) 0.009(3) 0.005(4) C67 0.045(4) 0.174(7) 0.061(4) 0.009(5) 0.016(4) 0.047(5) _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 O7 1.900(3) 2_566 ? Mn1 O7 1.900(3) . ? Mn1 O6 1.902(2) 2_566 ? Mn1 O6 1.902(2) . ? Mn1 O5 2.358(3) . ? Mn1 O5 2.358(3) 2_566 ? Mn1 Na1 3.1527(17) . ? Mn1 Na1 3.1527(17) 2_566 ? Mn2 O4 1.880(3) . ? Mn2 O1 1.898(3) . ? Mn2 O2 1.909(2) . ? Mn2 O3 1.917(3) . ? Mn2 N1 2.192(3) . ? Mn2 Na2 3.307(2) . ? Mn2 Na1 3.3390(17) . ? Mn3 O8 1.897(3) . ? Mn3 O8 1.897(3) 2 ? Mn3 O9 1.906(3) . ? Mn3 O9 1.906(3) 2 ? Mn3 O10 2.372(3) 2 ? Mn3 O10 2.372(3) . ? Mn3 Na2 3.1416(17) . ? Mn3 Na2 3.1416(17) 2 ? Na1 O7 2.333(3) 2_566 ? Na1 O4 2.334(3) . ? Na1 O2 2.351(3) . ? Na1 O6 2.396(3) . ? Na1 N2 2.484(4) . ? Na1 O5 2.641(4) . ? Na2 O3 2.330(4) . ? Na2 O1 2.345(3) . ? Na2 O9 2.363(3) . ? Na2 O8 2.411(3) 2 ? Na2 N3 2.501(6) . ? Na2 O10 2.519(4) . ? N1 C29 1.329(5) . ? N1 C25 1.337(5) . ? N2 C34 1.333(5) . ? N2 C30 1.334(5) . ? N3 C53 1.223(7) . ? N3 C49 1.441(8) . ? O1 C1 1.349(5) . ? O2 C12 1.349(5) . ? O3 C13 1.349(5) . ? O4 C24 1.354(5) . ? O5 C35 1.416(7) . ? O5 H5A 0.89(7) . ? O6 C43 1.347(5) . ? O7 C37 1.349(4) . ? O7 Na1 2.333(3) 2_566 ? O8 C54 1.364(5) . ? O8 Na2 2.411(3) 2 ? O9 C65 1.343(5) . ? O10 C66 1.279(6) . ? O10 H10A 1.0000 . ? C1 C2 1.390(6) . ? C1 C6 1.405(5) . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? C3 C4 1.371(6) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C4 H4 0.9500 . ? C5 C6 1.374(6) . ? C5 H5 0.9500 . ? C6 C7 1.483(5) . ? C7 C8 1.394(6) . ? C7 C12 1.412(6) . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C9 C10 1.370(6) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.399(5) . ? C11 H11 0.9500 . ? C13 C18 1.394(6) . ? C13 C14 1.412(5) . ? C14 C15 1.376(6) . ? C14 H14 0.9500 . ? C15 C16 1.366(6) . ? C15 H15 0.9500 . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C18 1.388(6) . ? C17 H17 0.9500 . ? C18 C19 1.492(6) . ? C19 C20 1.387(6) . ? C19 C24 1.403(5) . ? C20 C21 1.374(6) . ? C20 H20 0.9500 . ? C21 C22 1.379(6) . ? C21 H21 0.9500 . ? C22 C23 1.376(6) . ? C22 H22 0.9500 . ? C23 C24 1.389(6) . ? C23 H23 0.9500 . ? C25 C26 1.369(6) . ? C25 H25 0.9500 . ? C26 C27 1.364(7) . ? C26 H26 0.9500 . ? C27 C28 1.365(7) . ? C27 H27 0.9500 . ? C28 C29 1.376(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.379(6) . ? C30 H30 0.9500 . ? C31 C32 1.369(6) . ? C31 H31 0.9500 . ? C32 C33 1.374(6) . ? C32 H32 0.9500 . ? C33 C34 1.372(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36B 1.298(11) . ? C35 C36A 1.421(13) . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37 C42 1.386(6) . ? C37 C38 1.404(5) . ? C38 C39 1.393(5) . ? C38 C48 1.479(6) . ? C39 C40 1.364(7) . ? C39 H40 0.9500 . ? C40 C41 1.390(7) . ? C40 H41 0.9500 . ? C41 C42 1.385(6) . ? C41 H42 0.9500 . ? C42 H43 0.9500 . ? C43 C44 1.387(6) . ? C43 C48 1.419(6) . ? C44 C45 1.372(6) . ? C44 H44 0.9500 . ? C45 C46 1.361(7) . ? C45 H45 0.9500 . ? C46 C47 1.381(6) . ? C46 H46 0.9500 . ? C47 C48 1.398(6) . ? C47 H47 0.9500 . ? C49 C50 1.316(8) . ? C49 H49 0.9500 . ? C50 C51 1.358(8) . ? C50 H50 0.9500 . ? C51 C52 1.373(8) . ? C51 H51 0.9500 . ? C52 C53 1.362(9) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.393(7) . ? C54 C59 1.406(6) . ? C55 C56 1.362(8) . ? C55 H55 0.9500 . ? C56 C57 1.368(9) . ? C56 H56 0.9500 . ? C57 C58 1.368(8) . ? C57 H57 0.9500 . ? C58 C59 1.395(6) . ? C58 H58 0.9500 . ? C59 C60 1.469(6) . ? C60 C61 1.391(6) . ? C60 C65 1.413(6) . ? C61 C62 1.385(7) . ? C61 H61 0.9500 . ? C62 C63 1.375(7) . ? C62 H62 0.9500 . ? C63 C64 1.380(6) . ? C63 H63 0.9500 . ? C64 C65 1.386(6) . ? C64 H64 0.9500 . ? C66 C67 1.430(7) . ? C66 H67 0.9900 . ? C66 H66 0.9900 . ? C67 H70 0.9800 . ? C67 H68 0.9800 . ? C67 H69 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Mn1 O7 180.000(1) 2_566 . ? O7 Mn1 O6 91.89(11) 2_566 2_566 ? O7 Mn1 O6 88.11(11) . 2_566 ? O7 Mn1 O6 88.11(11) 2_566 . ? O7 Mn1 O6 91.89(11) . . ? O6 Mn1 O6 180.000(1) 2_566 . ? O7 Mn1 O5 83.47(12) 2_566 . ? O7 Mn1 O5 96.53(12) . . ? O6 Mn1 O5 101.64(12) 2_566 . ? O6 Mn1 O5 78.36(12) . . ? O7 Mn1 O5 96.53(12) 2_566 2_566 ? O7 Mn1 O5 83.47(12) . 2_566 ? O6 Mn1 O5 78.36(12) 2_566 2_566 ? O6 Mn1 O5 101.64(12) . 2_566 ? O5 Mn1 O5 180.00(15) . 2_566 ? O7 Mn1 Na1 47.42(8) 2_566 . ? O7 Mn1 Na1 132.58(8) . . ? O6 Mn1 Na1 130.66(8) 2_566 . ? O6 Mn1 Na1 49.34(8) . . ? O5 Mn1 Na1 55.01(9) . . ? O5 Mn1 Na1 124.99(9) 2_566 . ? O7 Mn1 Na1 132.58(8) 2_566 2_566 ? O7 Mn1 Na1 47.42(8) . 2_566 ? O6 Mn1 Na1 49.34(8) 2_566 2_566 ? O6 Mn1 Na1 130.66(8) . 2_566 ? O5 Mn1 Na1 124.99(9) . 2_566 ? O5 Mn1 Na1 55.01(9) 2_566 2_566 ? Na1 Mn1 Na1 180.0 . 2_566 ? O4 Mn2 O1 178.11(11) . . ? O4 Mn2 O2 85.98(11) . . ? O1 Mn2 O2 92.34(12) . . ? O4 Mn2 O3 93.55(12) . . ? O1 Mn2 O3 87.39(13) . . ? O2 Mn2 O3 147.49(11) . . ? O4 Mn2 N1 90.90(13) . . ? O1 Mn2 N1 90.52(14) . . ? O2 Mn2 N1 111.28(12) . . ? O3 Mn2 N1 101.23(12) . . ? O4 Mn2 Na2 136.89(9) . . ? O1 Mn2 Na2 43.92(9) . . ? O2 Mn2 Na2 126.02(9) . . ? O3 Mn2 Na2 43.60(10) . . ? N1 Mn2 Na2 100.70(10) . . ? O4 Mn2 Na1 42.63(8) . . ? O1 Mn2 Na1 135.71(9) . . ? O2 Mn2 Na1 43.37(9) . . ? O3 Mn2 Na1 128.55(10) . . ? N1 Mn2 Na1 104.06(10) . . ? Na2 Mn2 Na1 155.23(4) . . ? O8 Mn3 O8 180.0(2) . 2 ? O8 Mn3 O9 92.28(12) . . ? O8 Mn3 O9 87.72(12) 2 . ? O8 Mn3 O9 87.72(12) . 2 ? O8 Mn3 O9 92.28(12) 2 2 ? O9 Mn3 O9 180.0(2) . 2 ? O8 Mn3 O10 79.79(14) . 2 ? O8 Mn3 O10 100.21(14) 2 2 ? O9 Mn3 O10 97.93(13) . 2 ? O9 Mn3 O10 82.07(13) 2 2 ? O8 Mn3 O10 100.21(14) . . ? O8 Mn3 O10 79.79(14) 2 . ? O9 Mn3 O10 82.07(13) . . ? O9 Mn3 O10 97.93(13) 2 . ? O10 Mn3 O10 180.00(15) 2 . ? O8 Mn3 Na2 129.96(9) . . ? O8 Mn3 Na2 50.04(9) 2 . ? O9 Mn3 Na2 48.60(9) . . ? O9 Mn3 Na2 131.40(9) 2 . ? O10 Mn3 Na2 127.89(10) 2 . ? O10 Mn3 Na2 52.11(10) . . ? O8 Mn3 Na2 50.04(9) . 2 ? O8 Mn3 Na2 129.96(9) 2 2 ? O9 Mn3 Na2 131.40(9) . 2 ? O9 Mn3 Na2 48.60(9) 2 2 ? O10 Mn3 Na2 52.11(10) 2 2 ? O10 Mn3 Na2 127.89(10) . 2 ? Na2 Mn3 Na2 180.00(7) . 2 ? O7 Na1 O4 169.33(12) 2_566 . ? O7 Na1 O2 123.61(11) 2_566 . ? O4 Na1 O2 66.94(10) . . ? O7 Na1 O6 67.97(9) 2_566 . ? O4 Na1 O6 109.85(10) . . ? O2 Na1 O6 102.32(11) . . ? O7 Na1 N2 89.20(11) 2_566 . ? O4 Na1 N2 88.42(11) . . ? O2 Na1 N2 108.79(13) . . ? O6 Na1 N2 148.26(13) . . ? O7 Na1 O5 69.74(11) 2_566 . ? O4 Na1 O5 99.73(11) . . ? O2 Na1 O5 158.33(11) . . ? O6 Na1 O5 65.00(11) . . ? N2 Na1 O5 86.97(13) . . ? O7 Na1 Mn1 36.86(6) 2_566 . ? O4 Na1 Mn1 136.13(9) . . ? O2 Na1 Mn1 131.91(9) . . ? O6 Na1 Mn1 37.03(6) . . ? N2 Na1 Mn1 112.50(10) . . ? O5 Na1 Mn1 47.01(7) . . ? O7 Na1 Mn2 157.40(9) 2_566 . ? O4 Na1 Mn2 33.06(7) . . ? O2 Na1 Mn2 33.89(6) . . ? O6 Na1 Mn2 108.79(8) . . ? N2 Na1 Mn2 100.62(10) . . ? O5 Na1 Mn2 130.55(9) . . ? Mn1 Na1 Mn2 145.77(5) . . ? O3 Na2 O1 68.64(11) . . ? O3 Na2 O9 122.48(13) . . ? O1 Na2 O9 168.81(14) . . ? O3 Na2 O8 102.50(12) . 2 ? O1 Na2 O8 111.11(12) . 2 ? O9 Na2 O8 67.00(10) . 2 ? O3 Na2 N3 105.13(15) . . ? O1 Na2 N3 91.47(18) . . ? O9 Na2 N3 86.74(17) . . ? O8 Na2 N3 149.26(17) 2 . ? O3 Na2 O10 160.59(15) . . ? O1 Na2 O10 98.16(13) . . ? O9 Na2 O10 70.78(12) . . ? O8 Na2 O10 68.11(12) 2 . ? N3 Na2 O10 88.87(16) . . ? O3 Na2 Mn3 132.82(10) . . ? O1 Na2 Mn3 135.33(10) . . ? O9 Na2 Mn3 37.22(7) . . ? O8 Na2 Mn3 37.10(7) 2 . ? N3 Na2 Mn3 112.22(15) . . ? O10 Na2 Mn3 48.00(8) . . ? O3 Na2 Mn2 34.57(7) . . ? O1 Na2 Mn2 34.15(8) . . ? O9 Na2 Mn2 157.01(11) . . ? O8 Na2 Mn2 112.30(9) 2 . ? N3 Na2 Mn2 98.14(15) . . ? O10 Na2 Mn2 131.46(11) . . ? Mn3 Na2 Mn2 149.22(6) . . ? C29 N1 C25 117.9(4) . . ? C29 N1 Mn2 121.1(3) . . ? C25 N1 Mn2 121.0(3) . . ? C34 N2 C30 116.6(4) . . ? C34 N2 Na1 119.5(3) . . ? C30 N2 Na1 122.1(3) . . ? C53 N3 C49 105.3(6) . . ? C53 N3 Na2 127.4(6) . . ? C49 N3 Na2 125.2(4) . . ? C1 O1 Mn2 118.1(3) . . ? C1 O1 Na2 136.2(3) . . ? Mn2 O1 Na2 101.93(14) . . ? C12 O2 Mn2 122.1(2) . . ? C12 O2 Na1 122.8(2) . . ? Mn2 O2 Na1 102.74(12) . . ? C13 O3 Mn2 125.1(2) . . ? C13 O3 Na2 121.7(3) . . ? Mn2 O3 Na2 101.83(14) . . ? C24 O4 Mn2 120.0(2) . . ? C24 O4 Na1 129.5(2) . . ? Mn2 O4 Na1 104.31(12) . . ? C35 O5 Mn1 131.8(3) . . ? C35 O5 Na1 124.3(3) . . ? Mn1 O5 Na1 77.99(10) . . ? C35 O5 H5A 95(5) . . ? Mn1 O5 H5A 119(5) . . ? Na1 O5 H5A 109(5) . . ? C43 O6 Mn1 124.8(2) . . ? C43 O6 Na1 140.9(2) . . ? Mn1 O6 Na1 93.63(11) . . ? C37 O7 Mn1 118.3(2) . . ? C37 O7 Na1 139.2(2) . 2_566 ? Mn1 O7 Na1 95.72(10) . 2_566 ? C54 O8 Mn3 122.4(3) . . ? C54 O8 Na2 144.0(3) . 2 ? Mn3 O8 Na2 92.86(12) . 2 ? C65 O9 Mn3 118.1(2) . . ? C65 O9 Na2 143.8(3) . . ? Mn3 O9 Na2 94.18(12) . . ? C66 O10 Mn3 138.9(4) . . ? C66 O10 Na2 133.9(4) . . ? Mn3 O10 Na2 79.88(12) . . ? C66 O10 H10A 98.3 . . ? Mn3 O10 H10A 98.3 . . ? Na2 O10 H10A 98.3 . . ? O1 C1 C2 120.0(4) . . ? O1 C1 C6 121.2(4) . . ? C2 C1 C6 118.7(4) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 121.8(4) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 118.9(4) . . ? C5 C6 C7 121.2(4) . . ? C1 C6 C7 119.8(4) . . ? C8 C7 C12 118.6(4) . . ? C8 C7 C6 119.7(4) . . ? C12 C7 C6 121.7(4) . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.6(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? O2 C12 C11 119.2(4) . . ? O2 C12 C7 121.5(3) . . ? C11 C12 C7 119.3(4) . . ? O3 C13 C18 122.9(4) . . ? O3 C13 C14 118.0(4) . . ? C18 C13 C14 119.0(4) . . ? C15 C14 C13 120.4(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.8(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C18 122.5(5) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 118.4(4) . . ? C17 C18 C19 118.4(4) . . ? C13 C18 C19 123.2(4) . . ? C20 C19 C24 118.0(4) . . ? C20 C19 C18 120.4(4) . . ? C24 C19 C18 121.4(4) . . ? C21 C20 C19 122.4(4) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 118.7(4) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? O4 C24 C23 119.0(4) . . ? O4 C24 C19 121.3(4) . . ? C23 C24 C19 119.6(4) . . ? N1 C25 C26 122.7(4) . . ? N1 C25 H25 118.7 . . ? C26 C25 H25 118.7 . . ? C27 C26 C25 118.7(5) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 118.7(5) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? N1 C29 C28 122.5(4) . . ? N1 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? N2 C30 C31 123.6(4) . . ? N2 C30 H30 118.2 . . ? C31 C30 H30 118.2 . . ? C32 C31 C30 118.8(4) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 118.3(4) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C34 C33 C32 119.2(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? N2 C34 C33 123.4(4) . . ? N2 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? C36B C35 O5 118.3(7) . . ? C36B C35 C36A 68.8(8) . . ? O5 C35 C36A 117.5(7) . . ? C35 C36A H36A 109.5 . . ? C35 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C35 C36B H36D 109.5 . . ? C35 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? O7 C37 C42 119.5(4) . . ? O7 C37 C38 120.8(4) . . ? C42 C37 C38 119.6(4) . . ? C39 C38 C37 118.1(4) . . ? C39 C38 C48 121.5(4) . . ? C37 C38 C48 120.4(3) . . ? C40 C39 C38 122.6(4) . . ? C40 C39 H40 118.7 . . ? C38 C39 H40 118.7 . . ? C39 C40 C41 118.9(4) . . ? C39 C40 H41 120.6 . . ? C41 C40 H41 120.6 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H42 119.9 . . ? C40 C41 H42 119.9 . . ? C41 C42 C37 120.6(4) . . ? C41 C42 H43 119.7 . . ? C37 C42 H43 119.7 . . ? O6 C43 C44 120.4(4) . . ? O6 C43 C48 120.4(4) . . ? C44 C43 C48 119.1(4) . . ? C45 C44 C43 121.1(5) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C46 C45 C44 121.0(5) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 119.1(4) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? C46 C47 C48 122.1(5) . . ? C46 C47 H47 118.9 . . ? C48 C47 H47 118.9 . . ? C47 C48 C43 117.5(4) . . ? C47 C48 C38 121.0(4) . . ? C43 C48 C38 121.5(4) . . ? C50 C49 N3 127.3(7) . . ? C50 C49 H49 116.4 . . ? N3 C49 H49 116.4 . . ? C49 C50 C51 120.1(8) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 115.3(7) . . ? C50 C51 H51 122.4 . . ? C52 C51 H51 122.4 . . ? C53 C52 C51 116.6(8) . . ? C53 C52 H52 121.7 . . ? C51 C52 H52 121.7 . . ? N3 C53 C52 135.3(8) . . ? N3 C53 H53 112.3 . . ? C52 C53 H53 112.3 . . ? O8 C54 C55 120.2(5) . . ? O8 C54 C59 120.0(4) . . ? C55 C54 C59 119.8(5) . . ? C56 C55 C54 120.5(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 120.4(6) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C58 C57 C56 120.3(6) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C57 C58 C59 121.2(6) . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C58 C59 C54 117.8(5) . . ? C58 C59 C60 121.3(5) . . ? C54 C59 C60 120.9(4) . . ? C61 C60 C65 118.8(5) . . ? C61 C60 C59 121.1(4) . . ? C65 C60 C59 120.2(4) . . ? C62 C61 C60 121.2(5) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C63 C62 C61 119.2(5) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C62 C63 C64 121.0(5) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C63 C64 C65 120.4(5) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? O9 C65 C64 120.2(4) . . ? O9 C65 C60 120.5(4) . . ? C64 C65 C60 119.3(4) . . ? O10 C66 C67 127.3(6) . . ? O10 C66 H67 105.5 . . ? C67 C66 H67 105.5 . . ? O10 C66 H66 105.5 . . ? C67 C66 H66 105.5 . . ? H67 C66 H66 106.1 . . ? C66 C67 H70 109.5 . . ? C66 C67 H68 109.5 . . ? H70 C67 H68 109.5 . . ? C66 C67 H69 109.5 . . ? H70 C67 H69 109.5 . . ? H68 C67 H69 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.738 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.069 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 778269' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Na2Mn2(biphen)4(EtOH)3(3-cnp)2)n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H58 Mn2 N4 Na2 O11' _chemical_formula_weight 1239.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.293(2) _cell_length_b 15.606(3) _cell_length_c 17.596(4) _cell_angle_alpha 84.81(3) _cell_angle_beta 77.73(3) _cell_angle_gamma 81.07(3) _cell_volume 2988.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 0.502 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9590 _cell_measurement_reflns_used 6267 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.82628 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 23677 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.9590 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0026780000 _diffrn_orient_matrix_UB_12 0.0262090000 _diffrn_orient_matrix_UB_13 -0.0348607000 _diffrn_orient_matrix_UB_21 -0.0218384000 _diffrn_orient_matrix_UB_22 0.0371446000 _diffrn_orient_matrix_UB_23 0.0220516000 _diffrn_orient_matrix_UB_31 0.0610700000 _diffrn_orient_matrix_UB_32 0.0075870000 _diffrn_orient_matrix_UB_33 -0.0025014000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 -47.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -17.2341 127.0000 70.0000 29 #__ type_ start__ end____ width___ exp.time_ 2 omega -78.00 -37.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -17.2341 179.0000 90.0000 41 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 90.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 4 omega -53.00 38.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 -37.0000 90.0000 91 #__ type_ start__ end____ width___ exp.time_ 5 omega -45.00 48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 -77.0000 -120.0000 93 #__ type_ start__ end____ width___ exp.time_ 6 omega 67.00 94.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 179.0000 -180.0000 27 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 10920 _reflns_number_gt 5906 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0364P)^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 10920 _refine_ls_number_parameters 780 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1580 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.5000 0.5000 0.5000 0.0237(3) Uani 1 2 d S . . Mn2 Mn 0.71638(7) 0.24034(6) 0.24646(5) 0.0261(2) Uani 1 1 d . . . Mn3 Mn 1.0000 0.0000 0.0000 0.0301(3) Uani 1 2 d S . . Na1 Na 0.62116(19) 0.41592(14) 0.33856(11) 0.0286(5) Uani 1 1 d . . . Na2 Na 0.86848(19) 0.16660(15) 0.07849(12) 0.0323(6) Uani 1 1 d . . . N1 N 0.7280(4) 0.4691(3) 0.4711(3) 0.0260(11) Uani 1 1 d . . . N2 N 1.0451(5) 0.6113(4) 0.3091(3) 0.0579(17) Uani 1 1 d . . . N3 N 0.6616(4) 0.1289(3) 0.3236(2) 0.0260(11) Uani 1 1 d . . . N4 N 0.2762(5) 0.0288(4) 0.4238(3) 0.0618(18) Uani 1 1 d . . . O1 O 0.4822(3) 0.6135(2) 0.53573(19) 0.0255(9) Uani 1 1 d . . . O2 O 0.5234(3) 0.5432(2) 0.39378(19) 0.0251(9) Uani 1 1 d . . . O3 O 0.7759(4) 0.4754(3) 0.2462(3) 0.0448(12) Uani 1 1 d D . . O4 O 0.7536(3) 0.2923(2) 0.3293(2) 0.0280(10) Uani 1 1 d . . . O5 O 0.8836(3) 0.2225(2) 0.1946(2) 0.0270(9) Uani 1 1 d . . . O6 O 0.5648(3) 0.3186(2) 0.2582(2) 0.0292(10) Uani 1 1 d . . . O7 O 0.6849(3) 0.1855(3) 0.1627(2) 0.0312(10) Uani 1 1 d . . . O8 O 0.7710(5) 0.2959(4) 0.0265(3) 0.0575(14) Uani 1 1 d D . . O9 O 0.9379(3) 0.0224(3) 0.1067(2) 0.0352(10) Uani 1 1 d . . . O10 O 0.9766(3) -0.1177(3) 0.0188(2) 0.0334(10) Uani 1 1 d . . . O11 O 0.7962(4) 0.0555(3) -0.0016(3) 0.0617(15) Uani 1 1 d . . . H11A H 0.7480 0.0186 0.0392 0.074 Uiso 1 1 calc R . . C1 C 0.5718(5) 0.6630(3) 0.5107(3) 0.0214(12) Uani 1 1 d . . . C2 C 0.6491(5) 0.6749(4) 0.5599(3) 0.0308(14) Uani 1 1 d . . . H2 H 0.6365 0.6496 0.6117 0.037 Uiso 1 1 calc R . . C3 C 0.7434(5) 0.7230(4) 0.5338(4) 0.0401(17) Uani 1 1 d . . . H3 H 0.7959 0.7297 0.5678 0.048 Uiso 1 1 calc R . . C4 C 0.7636(5) 0.7613(4) 0.4605(4) 0.0342(15) Uani 1 1 d . . . H4 H 0.8304 0.7933 0.4432 0.041 Uiso 1 1 calc R . . C5 C 0.6846(5) 0.7529(4) 0.4110(3) 0.0321(15) Uani 1 1 d . . . H5 H 0.6976 0.7796 0.3598 0.038 Uiso 1 1 calc R . . C6 C 0.5866(5) 0.7054(4) 0.4367(3) 0.0255(13) Uani 1 1 d . . . C7 C 0.4998(5) 0.7011(4) 0.3836(3) 0.0254(13) Uani 1 1 d . . . C8 C 0.4450(5) 0.7766(4) 0.3513(3) 0.0325(15) Uani 1 1 d . . . H8 H 0.4646 0.8304 0.3627 0.039 Uiso 1 1 calc R . . C9 C 0.3623(5) 0.7774(4) 0.3028(3) 0.0376(16) Uani 1 1 d . . . H9 H 0.3240 0.8306 0.2827 0.045 Uiso 1 1 calc R . . C10 C 0.3376(5) 0.6984(4) 0.2849(3) 0.0378(16) Uani 1 1 d . . . H10 H 0.2827 0.6971 0.2510 0.045 Uiso 1 1 calc R . . C11 C 0.3912(5) 0.6220(4) 0.3154(3) 0.0314(15) Uani 1 1 d . . . H11 H 0.3729 0.5686 0.3021 0.038 Uiso 1 1 calc R . . C12 C 0.4731(5) 0.6208(4) 0.3662(3) 0.0234(13) Uani 1 1 d . . . C13 C 0.7952(5) 0.5226(4) 0.4214(3) 0.0269(14) Uani 1 1 d . . . H13 H 0.7551 0.5726 0.3975 0.032 Uiso 1 1 calc R . . C14 C 0.9237(5) 0.5057(4) 0.4045(3) 0.0293(14) Uani 1 1 d . . . C15 C 0.9920(5) 0.5638(5) 0.3514(4) 0.0400(17) Uani 1 1 d . . . C16 C 0.9819(5) 0.4338(4) 0.4399(3) 0.0289(14) Uani 1 1 d . . . H16 H 1.0687 0.4226 0.4306 0.035 Uiso 1 1 calc R . . C17 C 0.9122(5) 0.3784(4) 0.4889(3) 0.0290(14) Uani 1 1 d . . . H17 H 0.9504 0.3276 0.5128 0.035 Uiso 1 1 calc R . . C18 C 0.7854(5) 0.3980(4) 0.5030(3) 0.0299(14) Uani 1 1 d . . . H18 H 0.7377 0.3593 0.5365 0.036 Uiso 1 1 calc R . . C19 C 0.7871(7) 0.5572(5) 0.2039(4) 0.061(2) Uani 1 1 d . . . H19A H 0.8587 0.5800 0.2145 0.073 Uiso 1 1 calc R . . H19B H 0.7133 0.5988 0.2228 0.073 Uiso 1 1 calc R . . C20 C 0.8017(7) 0.5518(5) 0.1187(4) 0.075(3) Uani 1 1 d . . . H20A H 0.8816 0.5189 0.0981 0.112 Uiso 1 1 calc R . . H20B H 0.7965 0.6105 0.0935 0.112 Uiso 1 1 calc R . . H20C H 0.7367 0.5225 0.1082 0.112 Uiso 1 1 calc R . . C21 C 0.8308(5) 0.2424(4) 0.3700(3) 0.0256(13) Uani 1 1 d . . . C22 C 0.7839(5) 0.2043(4) 0.4432(3) 0.0320(15) Uani 1 1 d . . . H22 H 0.6985 0.2138 0.4642 0.038 Uiso 1 1 calc R . . C23 C 0.8623(6) 0.1528(4) 0.4848(3) 0.0380(16) Uani 1 1 d . . . H23 H 0.8301 0.1281 0.5349 0.046 Uiso 1 1 calc R . . C24 C 0.9859(6) 0.1366(4) 0.4551(3) 0.0394(17) Uani 1 1 d . . . H24 H 1.0386 0.0995 0.4833 0.047 Uiso 1 1 calc R . . C25 C 1.0323(5) 0.1756(4) 0.3829(3) 0.0330(15) Uani 1 1 d . . . H25 H 1.1177 0.1647 0.3621 0.040 Uiso 1 1 calc R . . C26 C 0.9577(5) 0.2296(4) 0.3406(3) 0.0238(13) Uani 1 1 d . . . C27 C 1.0073(5) 0.2787(4) 0.2682(3) 0.0285(14) Uani 1 1 d . . . C28 C 1.0965(5) 0.3314(4) 0.2667(3) 0.0311(15) Uani 1 1 d . . . H28 H 1.1289 0.3320 0.3122 0.037 Uiso 1 1 calc R . . C29 C 1.1401(5) 0.3831(4) 0.2017(4) 0.0426(18) Uani 1 1 d . . . H29 H 1.1984 0.4203 0.2034 0.051 Uiso 1 1 calc R . . C30 C 1.0974(5) 0.3794(4) 0.1346(3) 0.0399(17) Uani 1 1 d . . . H30 H 1.1274 0.4135 0.0891 0.048 Uiso 1 1 calc R . . C31 C 1.0116(5) 0.3265(4) 0.1334(3) 0.0321(15) Uani 1 1 d . . . H31 H 0.9832 0.3247 0.0866 0.038 Uiso 1 1 calc R . . C32 C 0.9651(5) 0.2758(4) 0.1980(3) 0.0256(13) Uani 1 1 d . . . C33 C 0.7444(5) 0.0618(4) 0.3380(3) 0.0301(15) Uani 1 1 d . . . H33 H 0.8285 0.0676 0.3204 0.036 Uiso 1 1 calc R . . C34 C 0.7158(5) -0.0147(4) 0.3765(3) 0.0408(17) Uani 1 1 d . . . H34 H 0.7780 -0.0606 0.3856 0.049 Uiso 1 1 calc R . . C35 C 0.5933(6) -0.0229(4) 0.4018(3) 0.0369(15) Uani 1 1 d . . . H35 H 0.5697 -0.0751 0.4288 0.044 Uiso 1 1 calc R . . C36 C 0.5057(5) 0.0450(4) 0.3877(3) 0.0303(14) Uani 1 1 d . . . C37 C 0.3775(6) 0.0378(4) 0.4073(4) 0.0438(17) Uani 1 1 d . . . C38 C 0.5433(5) 0.1202(4) 0.3489(3) 0.0298(14) Uani 1 1 d . . . H38 H 0.4830 0.1675 0.3399 0.036 Uiso 1 1 calc R . . C39 C 0.5154(5) 0.3512(4) 0.1968(3) 0.0286(14) Uani 1 1 d . . . C40 C 0.5083(5) 0.4407(4) 0.1779(3) 0.0332(15) Uani 1 1 d . . . H40 H 0.5393 0.4756 0.2084 0.040 Uiso 1 1 calc R . . C41 C 0.4575(5) 0.4801(5) 0.1160(3) 0.0447(17) Uani 1 1 d . . . H41 H 0.4535 0.5410 0.1041 0.054 Uiso 1 1 calc R . . C42 C 0.4124(5) 0.4277(5) 0.0718(4) 0.0446(18) Uani 1 1 d . . . H42 H 0.3772 0.4529 0.0290 0.054 Uiso 1 1 calc R . . C43 C 0.4186(5) 0.3405(5) 0.0897(3) 0.0426(18) Uani 1 1 d . . . H43 H 0.3876 0.3058 0.0588 0.051 Uiso 1 1 calc R . . C44 C 0.4687(5) 0.3007(4) 0.1516(3) 0.0317(15) Uani 1 1 d . . . C45 C 0.4696(5) 0.2064(4) 0.1672(3) 0.0294(15) Uani 1 1 d . . . C46 C 0.3627(5) 0.1678(4) 0.1769(3) 0.0429(18) Uani 1 1 d . . . H46 H 0.2867 0.2036 0.1761 0.051 Uiso 1 1 calc R . . C47 C 0.3660(6) 0.0788(5) 0.1875(4) 0.050(2) Uani 1 1 d . . . H47 H 0.2922 0.0542 0.1953 0.060 Uiso 1 1 calc R . . C48 C 0.4765(6) 0.0247(5) 0.1870(4) 0.052(2) Uani 1 1 d . . . H48 H 0.4791 -0.0367 0.1924 0.062 Uiso 1 1 calc R . . C49 C 0.5828(5) 0.0620(4) 0.1786(3) 0.0371(17) Uani 1 1 d . . . H49 H 0.6588 0.0259 0.1781 0.044 Uiso 1 1 calc R . . C50 C 0.5791(5) 0.1507(4) 0.1709(3) 0.0310(15) Uani 1 1 d . . . C51 C 0.7732(9) 0.3500(7) -0.0414(6) 0.114(4) Uani 1 1 d . . . H51A H 0.7501 0.4110 -0.0268 0.136 Uiso 1 1 calc R . . H51B H 0.7108 0.3362 -0.0686 0.136 Uiso 1 1 calc R . . C52 C 0.8869(8) 0.3426(7) -0.0933(5) 0.112(4) Uani 1 1 d . . . H52A H 0.9488 0.3586 -0.0677 0.169 Uiso 1 1 calc R . . H52B H 0.8809 0.3816 -0.1396 0.169 Uiso 1 1 calc R . . H52C H 0.9104 0.2826 -0.1086 0.169 Uiso 1 1 calc R . . C53 C 0.7286(8) 0.0725(8) -0.0580(6) 0.176(7) Uani 1 1 d . . . H53A H 0.7178 0.0158 -0.0747 0.211 Uiso 1 1 calc R . . H53B H 0.7787 0.1014 -0.1032 0.211 Uiso 1 1 calc R . . C54 C 0.6139(8) 0.1220(7) -0.0435(5) 0.128(5) Uani 1 1 d . . . H54A H 0.5543 0.0866 -0.0126 0.191 Uiso 1 1 calc R . . H54B H 0.5895 0.1423 -0.0930 0.191 Uiso 1 1 calc R . . H54C H 0.6170 0.1721 -0.0146 0.191 Uiso 1 1 calc R . . C55 C 0.9680(5) -0.0280(4) 0.1670(3) 0.0311(14) Uani 1 1 d . . . C56 C 1.0347(5) 0.0029(4) 0.2147(3) 0.0384(17) Uani 1 1 d . . . H56 H 1.0583 0.0593 0.2035 0.046 Uiso 1 1 calc R . . C57 C 1.0666(5) -0.0471(5) 0.2778(4) 0.0465(19) Uani 1 1 d . . . H57 H 1.1129 -0.0255 0.3092 0.056 Uiso 1 1 calc R . . C58 C 1.0311(5) -0.1293(5) 0.2955(3) 0.0435(18) Uani 1 1 d . . . H58 H 1.0539 -0.1645 0.3384 0.052 Uiso 1 1 calc R . . C59 C 0.9628(5) -0.1586(4) 0.2501(3) 0.0402(16) Uani 1 1 d . . . H59 H 0.9377 -0.2144 0.2628 0.048 Uiso 1 1 calc R . . C60 C 0.9287(5) -0.1091(4) 0.1858(3) 0.0312(15) Uani 1 1 d . . . C61 C 0.8445(5) -0.1419(4) 0.1434(3) 0.0322(15) Uani 1 1 d . . . C62 C 0.7379(5) -0.1705(4) 0.1833(3) 0.0417(17) Uani 1 1 d . . . H62 H 0.7178 -0.1683 0.2384 0.050 Uiso 1 1 calc R . . C63 C 0.6595(6) -0.2021(4) 0.1464(4) 0.0488(19) Uani 1 1 d . . . H63 H 0.5868 -0.2219 0.1755 0.059 Uiso 1 1 calc R . . C64 C 0.6882(6) -0.2046(5) 0.0664(4) 0.054(2) Uani 1 1 d . . . H64 H 0.6354 -0.2267 0.0399 0.065 Uiso 1 1 calc R . . C65 C 0.7927(6) -0.1752(4) 0.0249(4) 0.0439(18) Uani 1 1 d . . . H65 H 0.8101 -0.1761 -0.0303 0.053 Uiso 1 1 calc R . . C66 C 0.8739(5) -0.1441(4) 0.0611(3) 0.0338(15) Uani 1 1 d . . . H8A H 0.709(7) 0.288(9) 0.062(5) 0.23(7) Uiso 1 1 d D . . H3A H 0.828(4) 0.430(2) 0.236(3) 0.05(2) Uiso 1 1 d 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 0.0301(7) 0.0202(7) 0.0207(7) -0.0066(6) -0.0042(5) -0.0010(5) Mn2 0.0247(5) 0.0286(6) 0.0251(5) -0.0122(4) -0.0022(4) -0.0013(4) Mn3 0.0356(8) 0.0307(8) 0.0216(7) -0.0098(6) -0.0023(5) 0.0021(6) Na1 0.0367(13) 0.0231(14) 0.0242(12) -0.0084(10) -0.0022(10) -0.0001(10) Na2 0.0348(14) 0.0335(15) 0.0267(12) -0.0108(11) -0.0021(10) 0.0007(11) N1 0.036(3) 0.014(3) 0.029(3) -0.007(2) -0.006(2) -0.002(2) N2 0.048(4) 0.064(5) 0.059(4) 0.013(4) -0.001(3) -0.019(3) N3 0.026(3) 0.022(3) 0.029(3) -0.005(2) -0.006(2) 0.002(2) N4 0.035(4) 0.063(5) 0.082(5) 0.015(4) -0.004(3) -0.014(3) O1 0.028(2) 0.026(2) 0.021(2) -0.0070(18) 0.0040(16) -0.0098(18) O2 0.032(2) 0.019(2) 0.021(2) -0.0049(18) -0.0018(17) 0.0035(17) O3 0.054(3) 0.029(3) 0.048(3) -0.003(2) -0.007(2) 0.001(3) O4 0.029(2) 0.029(3) 0.028(2) -0.0152(19) -0.0072(17) 0.0018(18) O5 0.022(2) 0.028(2) 0.030(2) -0.0109(19) -0.0007(16) 0.0001(17) O6 0.029(2) 0.033(3) 0.025(2) -0.012(2) -0.0101(17) 0.0073(18) O7 0.018(2) 0.047(3) 0.030(2) -0.025(2) 0.0003(16) -0.0048(19) O8 0.059(4) 0.058(4) 0.048(3) 0.007(3) -0.009(3) 0.007(3) O9 0.053(3) 0.026(3) 0.023(2) -0.0068(19) -0.0038(19) 0.004(2) O10 0.042(3) 0.026(3) 0.027(2) -0.0082(19) 0.0068(18) -0.006(2) O11 0.048(3) 0.071(4) 0.073(3) -0.032(3) -0.030(3) 0.014(3) C1 0.025(3) 0.014(3) 0.024(3) -0.006(3) -0.003(2) 0.002(2) C2 0.036(4) 0.028(4) 0.028(3) -0.009(3) -0.009(3) 0.001(3) C3 0.035(4) 0.036(4) 0.055(4) -0.010(4) -0.020(3) -0.004(3) C4 0.027(3) 0.023(4) 0.054(4) 0.004(3) -0.011(3) -0.009(3) C5 0.042(4) 0.017(3) 0.038(4) -0.003(3) -0.015(3) 0.002(3) C6 0.028(3) 0.016(3) 0.032(3) -0.004(3) -0.004(3) 0.000(2) C7 0.026(3) 0.027(4) 0.022(3) -0.005(3) -0.003(2) 0.001(3) C8 0.030(3) 0.031(4) 0.037(4) -0.005(3) -0.010(3) 0.000(3) C9 0.037(4) 0.040(4) 0.036(4) 0.000(3) -0.015(3) 0.004(3) C10 0.034(4) 0.047(5) 0.035(4) -0.006(3) -0.014(3) 0.001(3) C11 0.038(4) 0.033(4) 0.026(3) -0.005(3) -0.012(3) -0.005(3) C12 0.024(3) 0.028(4) 0.014(3) -0.002(3) 0.002(2) 0.001(3) C13 0.040(4) 0.014(3) 0.027(3) -0.002(3) -0.008(3) -0.001(3) C14 0.025(3) 0.036(4) 0.029(3) -0.010(3) -0.006(3) -0.006(3) C15 0.028(4) 0.052(5) 0.041(4) -0.014(4) 0.001(3) -0.013(3) C16 0.022(3) 0.035(4) 0.030(3) -0.012(3) -0.003(3) -0.001(3) C17 0.038(4) 0.024(4) 0.027(3) -0.004(3) -0.013(3) 0.001(3) C18 0.037(4) 0.018(4) 0.032(3) -0.006(3) -0.001(3) -0.002(3) C19 0.087(6) 0.044(5) 0.054(5) 0.010(4) -0.008(4) -0.033(4) C20 0.067(6) 0.092(8) 0.054(5) 0.005(5) 0.002(4) 0.000(5) C21 0.038(4) 0.023(4) 0.018(3) -0.009(3) -0.005(3) -0.005(3) C22 0.034(4) 0.037(4) 0.029(3) -0.013(3) -0.007(3) -0.011(3) C23 0.048(4) 0.038(4) 0.032(4) -0.003(3) -0.012(3) -0.009(3) C24 0.047(4) 0.040(4) 0.038(4) 0.004(3) -0.024(3) -0.009(3) C25 0.030(4) 0.039(4) 0.032(4) -0.010(3) -0.008(3) -0.005(3) C26 0.031(3) 0.020(3) 0.023(3) -0.011(3) -0.010(3) -0.002(3) C27 0.025(3) 0.029(4) 0.030(3) -0.011(3) -0.005(3) 0.002(3) C28 0.027(3) 0.034(4) 0.031(3) -0.013(3) -0.002(3) -0.002(3) C29 0.036(4) 0.045(5) 0.048(4) -0.017(4) 0.000(3) -0.012(3) C30 0.041(4) 0.045(5) 0.032(4) 0.000(3) 0.004(3) -0.018(3) C31 0.038(4) 0.034(4) 0.024(3) 0.001(3) -0.008(3) -0.006(3) C32 0.019(3) 0.024(4) 0.034(3) -0.007(3) -0.005(2) -0.002(2) C33 0.028(3) 0.022(4) 0.041(4) -0.016(3) -0.006(3) 0.002(3) C34 0.034(4) 0.038(4) 0.052(4) -0.014(4) -0.013(3) 0.003(3) C35 0.055(4) 0.020(4) 0.036(4) 0.000(3) -0.011(3) -0.003(3) C36 0.029(4) 0.024(4) 0.038(4) -0.009(3) -0.006(3) -0.001(3) C37 0.040(4) 0.040(5) 0.052(4) -0.003(4) -0.009(3) -0.009(3) C38 0.028(3) 0.028(4) 0.033(3) -0.009(3) -0.010(3) 0.007(3) C39 0.015(3) 0.037(4) 0.032(3) -0.008(3) 0.001(2) 0.000(3) C40 0.038(4) 0.029(4) 0.032(4) 0.003(3) -0.006(3) -0.007(3) C41 0.041(4) 0.045(5) 0.044(4) 0.014(4) -0.005(3) -0.007(3) C42 0.042(4) 0.058(5) 0.033(4) 0.005(4) -0.017(3) 0.001(4) C43 0.035(4) 0.061(5) 0.035(4) -0.014(4) -0.009(3) -0.005(3) C44 0.022(3) 0.049(5) 0.024(3) -0.016(3) 0.000(2) -0.006(3) C45 0.029(3) 0.035(4) 0.028(3) -0.020(3) -0.008(3) -0.001(3) C46 0.028(4) 0.052(5) 0.051(4) -0.024(4) -0.003(3) -0.008(3) C47 0.038(4) 0.058(5) 0.060(5) -0.032(4) -0.007(3) -0.017(4) C48 0.053(5) 0.046(5) 0.061(5) -0.029(4) -0.006(4) -0.016(4) C49 0.035(4) 0.037(4) 0.042(4) -0.026(3) -0.006(3) -0.003(3) C50 0.029(3) 0.034(4) 0.031(3) -0.023(3) -0.003(3) -0.001(3) C51 0.102(9) 0.131(11) 0.085(8) 0.041(7) -0.014(6) 0.019(7) C52 0.100(9) 0.140(11) 0.071(7) 0.020(7) 0.011(6) 0.008(7) C53 0.080(7) 0.296(16) 0.172(10) -0.197(11) -0.097(7) 0.116(8) C54 0.098(8) 0.176(12) 0.119(8) -0.070(8) -0.078(7) 0.060(7) C55 0.027(3) 0.030(4) 0.033(4) -0.011(3) -0.002(3) 0.006(3) C56 0.029(4) 0.046(5) 0.039(4) -0.017(3) -0.004(3) 0.003(3) C57 0.034(4) 0.071(6) 0.037(4) -0.017(4) -0.011(3) 0.001(4) C58 0.036(4) 0.058(5) 0.034(4) 0.006(4) -0.014(3) 0.009(3) C59 0.039(4) 0.042(5) 0.037(4) 0.001(3) -0.008(3) 0.001(3) C60 0.024(3) 0.035(4) 0.032(4) -0.004(3) -0.002(3) 0.002(3) C61 0.030(4) 0.035(4) 0.028(3) -0.001(3) 0.002(3) -0.004(3) C62 0.046(4) 0.052(5) 0.024(3) -0.003(3) -0.002(3) -0.002(3) C63 0.039(4) 0.053(5) 0.054(5) -0.016(4) 0.004(3) -0.017(4) C64 0.053(5) 0.062(5) 0.055(5) -0.032(4) -0.014(4) -0.013(4) C65 0.048(4) 0.048(5) 0.035(4) -0.014(3) -0.001(3) -0.008(3) C66 0.036(4) 0.031(4) 0.031(3) -0.008(3) 0.006(3) -0.008(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 O1 1.900(3) . ? Mn1 O1 1.900(3) 2_666 ? Mn1 O2 1.906(3) . ? Mn1 O2 1.906(3) 2_666 ? Mn1 N1 2.495(4) 2_666 ? Mn1 N1 2.495(4) . ? Mn1 Na1 3.183(2) . ? Mn1 Na1 3.183(2) 2_666 ? Mn2 O4 1.882(3) . ? Mn2 O7 1.891(3) . ? Mn2 O5 1.905(3) . ? Mn2 O6 1.926(4) . ? Mn2 N3 2.191(5) . ? Mn2 Na1 3.231(2) . ? Mn2 Na2 3.295(2) . ? Mn3 O10 1.886(4) . ? Mn3 O10 1.886(4) 2_755 ? Mn3 O9 1.903(4) . ? Mn3 O9 1.903(4) 2_755 ? Mn3 O11 2.335(4) . ? Mn3 O11 2.335(4) 2_755 ? Mn3 Na2 3.075(2) . ? Mn3 Na2 3.075(2) 2_755 ? Na1 O4 2.246(4) . ? Na1 O2 2.306(4) . ? Na1 O1 2.313(4) 2_666 ? Na1 O3 2.362(5) . ? Na1 O6 2.405(4) . ? Na1 H3A 2.67(5) . ? Na2 O10 2.264(4) 2_755 ? Na2 O7 2.273(4) . ? Na2 O9 2.311(5) . ? Na2 O5 2.341(4) . ? Na2 O8 2.350(6) . ? Na2 O11 2.650(4) . ? Na2 H8A 2.45(13) . ? N1 C18 1.336(7) . ? N1 C13 1.350(6) . ? N2 C15 1.145(7) . ? N3 C33 1.336(7) . ? N3 C38 1.339(6) . ? N4 C37 1.146(7) . ? O1 C1 1.344(6) . ? O1 Na1 2.313(4) 2_666 ? O2 C12 1.350(6) . ? O3 C19 1.428(8) . ? O3 H3A 0.852(10) . ? O4 C21 1.353(6) . ? O5 C32 1.346(5) . ? O6 C39 1.344(6) . ? O7 C50 1.363(6) . ? O8 C51 1.398(9) . ? O8 H8A 0.849(10) . ? O9 C55 1.334(7) . ? O10 C66 1.340(6) . ? O10 Na2 2.264(4) 2_755 ? O11 C53 1.361(8) . ? O11 H11A 1.0000 . ? C1 C6 1.394(7) . ? C1 C2 1.396(6) . ? C2 C3 1.374(7) . ? C2 H2 0.9500 . ? C3 C4 1.360(8) . ? C3 H3 0.9500 . ? C4 C5 1.399(7) . ? C4 H4 0.9500 . ? C5 C6 1.401(7) . ? C5 H5 0.9500 . ? C6 C7 1.503(6) . ? C7 C8 1.377(7) . ? C7 C12 1.408(7) . ? C8 C9 1.391(6) . ? C8 H8 0.9500 . ? C9 C10 1.384(8) . ? C9 H9 0.9500 . ? C10 C11 1.368(8) . ? C10 H10 0.9500 . ? C11 C12 1.414(6) . ? C11 H11 0.9500 . ? C13 C14 1.405(7) . ? C13 H13 0.9500 . ? C14 C16 1.377(8) . ? C14 C15 1.431(8) . ? C16 C17 1.377(7) . ? C16 H16 0.9500 . ? C17 C18 1.391(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.481(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.401(7) . ? C21 C26 1.406(7) . ? C22 C23 1.383(8) . ? C22 H22 0.9500 . ? C23 C24 1.376(8) . ? C23 H23 0.9500 . ? C24 C25 1.391(8) . ? C24 H24 0.9500 . ? C25 C26 1.382(7) . ? C25 H25 0.9500 . ? C26 C27 1.475(7) . ? C27 C28 1.391(7) . ? C27 C32 1.421(7) . ? C28 C29 1.384(8) . ? C28 H28 0.9500 . ? C29 C30 1.376(7) . ? C29 H29 0.9500 . ? C30 C31 1.372(7) . ? C30 H30 0.9500 . ? C31 C32 1.381(7) . ? C31 H31 0.9500 . ? C33 C34 1.367(8) . ? C33 H33 0.9500 . ? C34 C35 1.383(7) . ? C34 H34 0.9500 . ? C35 C36 1.377(8) . ? C35 H35 0.9500 . ? C36 C38 1.382(8) . ? C36 C37 1.435(8) . ? C38 H38 0.9500 . ? C39 C44 1.397(7) . ? C39 C40 1.399(8) . ? C40 C41 1.389(7) . ? C40 H40 0.9500 . ? C41 C42 1.395(8) . ? C41 H41 0.9500 . ? C42 C43 1.363(9) . ? C42 H42 0.9500 . ? C43 C44 1.387(8) . ? C43 H43 0.9500 . ? C44 C45 1.471(8) . ? C45 C46 1.404(7) . ? C45 C50 1.407(7) . ? C46 C47 1.381(9) . ? C46 H46 0.9500 . ? C47 C48 1.393(9) . ? C47 H47 0.9500 . ? C48 C49 1.389(7) . ? C48 H48 0.9500 . ? C49 C50 1.373(8) . ? C49 H49 0.9500 . ? C51 C52 1.403(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.387(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.394(8) . ? C55 C56 1.401(7) . ? C56 C57 1.377(8) . ? C56 H56 0.9500 . ? C57 C58 1.392(8) . ? C57 H57 0.9500 . ? C58 C59 1.371(7) . ? C58 H58 0.9500 . ? C59 C60 1.401(8) . ? C59 H59 0.9500 . ? C60 C61 1.499(7) . ? C61 C62 1.376(7) . ? C61 C66 1.418(7) . ? C62 C63 1.374(7) . ? C62 H62 0.9500 . ? C63 C64 1.380(8) . ? C63 H63 0.9500 . ? C64 C65 1.371(8) . ? C64 H64 0.9500 . ? C65 C66 1.386(7) . ? C65 H65 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.00(18) . 2_666 ? O1 Mn1 O2 92.05(15) . . ? O1 Mn1 O2 87.95(15) 2_666 . ? O1 Mn1 O2 87.95(15) . 2_666 ? O1 Mn1 O2 92.05(15) 2_666 2_666 ? O2 Mn1 O2 180.000(1) . 2_666 ? O1 Mn1 N1 81.37(14) . 2_666 ? O1 Mn1 N1 98.63(14) 2_666 2_666 ? O2 Mn1 N1 96.70(15) . 2_666 ? O2 Mn1 N1 83.30(15) 2_666 2_666 ? O1 Mn1 N1 98.63(14) . . ? O1 Mn1 N1 81.37(14) 2_666 . ? O2 Mn1 N1 83.30(15) . . ? O2 Mn1 N1 96.70(15) 2_666 . ? N1 Mn1 N1 180.0(2) 2_666 . ? O1 Mn1 Na1 133.91(11) . . ? O1 Mn1 Na1 46.09(11) 2_666 . ? O2 Mn1 Na1 45.90(11) . . ? O2 Mn1 Na1 134.10(11) 2_666 . ? N1 Mn1 Na1 115.80(10) 2_666 . ? N1 Mn1 Na1 64.20(10) . . ? O1 Mn1 Na1 46.09(11) . 2_666 ? O1 Mn1 Na1 133.91(11) 2_666 2_666 ? O2 Mn1 Na1 134.10(11) . 2_666 ? O2 Mn1 Na1 45.90(11) 2_666 2_666 ? N1 Mn1 Na1 64.20(10) 2_666 2_666 ? N1 Mn1 Na1 115.80(10) . 2_666 ? Na1 Mn1 Na1 180.000(1) . 2_666 ? O4 Mn2 O7 177.82(16) . . ? O4 Mn2 O5 92.28(14) . . ? O7 Mn2 O5 85.84(14) . . ? O4 Mn2 O6 88.42(15) . . ? O7 Mn2 O6 93.75(15) . . ? O5 Mn2 O6 145.39(17) . . ? O4 Mn2 N3 91.17(16) . . ? O7 Mn2 N3 88.55(16) . . ? O5 Mn2 N3 113.03(17) . . ? O6 Mn2 N3 101.55(17) . . ? O4 Mn2 Na1 42.70(12) . . ? O7 Mn2 Na1 139.34(13) . . ? O5 Mn2 Na1 117.39(11) . . ? O6 Mn2 Na1 47.76(10) . . ? N3 Mn2 Na1 109.11(12) . . ? O4 Mn2 Na2 136.27(12) . . ? O7 Mn2 Na2 41.97(11) . . ? O5 Mn2 Na2 44.17(10) . . ? O6 Mn2 Na2 123.71(11) . . ? N3 Mn2 Na2 107.88(12) . . ? Na1 Mn2 Na2 143.01(7) . . ? O10 Mn3 O10 180.00(5) . 2_755 ? O10 Mn3 O9 91.69(16) . . ? O10 Mn3 O9 88.31(16) 2_755 . ? O10 Mn3 O9 88.31(16) . 2_755 ? O10 Mn3 O9 91.69(16) 2_755 2_755 ? O9 Mn3 O9 180.0(3) . 2_755 ? O10 Mn3 O11 96.56(17) . . ? O10 Mn3 O11 83.44(17) 2_755 . ? O9 Mn3 O11 78.57(16) . . ? O9 Mn3 O11 101.43(16) 2_755 . ? O10 Mn3 O11 83.44(17) . 2_755 ? O10 Mn3 O11 96.56(17) 2_755 2_755 ? O9 Mn3 O11 101.43(16) . 2_755 ? O9 Mn3 O11 78.57(16) 2_755 2_755 ? O11 Mn3 O11 180.0(2) . 2_755 ? O10 Mn3 Na2 132.85(12) . . ? O10 Mn3 Na2 47.15(12) 2_755 . ? O9 Mn3 Na2 48.63(13) . . ? O9 Mn3 Na2 131.37(13) 2_755 . ? O11 Mn3 Na2 56.70(11) . . ? O11 Mn3 Na2 123.30(11) 2_755 . ? O10 Mn3 Na2 47.15(12) . 2_755 ? O10 Mn3 Na2 132.85(12) 2_755 2_755 ? O9 Mn3 Na2 131.37(13) . 2_755 ? O9 Mn3 Na2 48.63(13) 2_755 2_755 ? O11 Mn3 Na2 123.30(11) . 2_755 ? O11 Mn3 Na2 56.70(11) 2_755 2_755 ? Na2 Mn3 Na2 180.00(7) . 2_755 ? O4 Na1 O2 155.16(14) . . ? O4 Na1 O1 96.79(16) . 2_666 ? O2 Na1 O1 69.79(14) . 2_666 ? O4 Na1 O3 84.87(17) . . ? O2 Na1 O3 97.97(17) . . ? O1 Na1 O3 153.17(15) 2_666 . ? O4 Na1 O6 69.55(13) . . ? O2 Na1 O6 133.40(15) . . ? O1 Na1 O6 106.31(14) 2_666 . ? O3 Na1 O6 99.38(15) . . ? O4 Na1 Mn1 122.98(12) . . ? O2 Na1 Mn1 36.42(9) . . ? O1 Na1 Mn1 36.27(9) 2_666 . ? O3 Na1 Mn1 122.69(12) . . ? O6 Na1 Mn1 135.71(12) . . ? O4 Na1 Mn2 34.63(8) . . ? O2 Na1 Mn2 169.72(11) . . ? O1 Na1 Mn2 111.48(12) 2_666 . ? O3 Na1 Mn2 84.91(12) . . ? O6 Na1 Mn2 36.38(9) . . ? Mn1 Na1 Mn2 147.23(8) . . ? O4 Na1 H3A 66.7(7) . . ? O2 Na1 H3A 115.1(8) . . ? O1 Na1 H3A 150.8(11) 2_666 . ? O3 Na1 H3A 18.3(7) . . ? O6 Na1 H3A 90.7(11) . . ? Mn1 Na1 H3A 133.5(11) . . ? Mn2 Na1 H3A 69.1(8) . . ? O10 Na2 O7 162.51(15) 2_755 . ? O10 Na2 O9 70.46(15) 2_755 . ? O7 Na2 O9 101.58(17) . . ? O10 Na2 O5 127.52(14) 2_755 . ? O7 Na2 O5 68.13(12) . . ? O9 Na2 O5 98.40(15) . . ? O10 Na2 O8 105.38(19) 2_755 . ? O7 Na2 O8 77.83(19) . . ? O9 Na2 O8 163.90(17) . . ? O5 Na2 O8 96.28(17) . . ? O10 Na2 O11 69.79(14) 2_755 . ? O7 Na2 O11 92.78(14) . . ? O9 Na2 O11 65.64(14) . . ? O5 Na2 O11 152.89(17) . . ? O8 Na2 O11 98.26(17) . . ? O10 Na2 Mn3 37.65(10) 2_755 . ? O7 Na2 Mn3 127.96(13) . . ? O9 Na2 Mn3 38.16(9) . . ? O5 Na2 Mn3 130.76(12) . . ? O8 Na2 Mn3 130.69(15) . . ? O11 Na2 Mn3 47.43(10) . . ? O10 Na2 Mn2 161.85(12) 2_755 . ? O7 Na2 Mn2 33.81(8) . . ? O9 Na2 Mn2 105.00(12) . . ? O5 Na2 Mn2 34.54(9) . . ? O8 Na2 Mn2 83.61(15) . . ? O11 Na2 Mn2 125.32(13) . . ? Mn3 Na2 Mn2 142.81(8) . . ? O10 Na2 H8A 123.9(14) 2_755 . ? O7 Na2 H8A 57.7(10) . . ? O9 Na2 H8A 153.4(19) . . ? O5 Na2 H8A 89(2) . . ? O8 Na2 H8A 20.2(9) . . ? O11 Na2 H8A 97(3) . . ? Mn3 Na2 H8A 140(3) . . ? Mn2 Na2 H8A 68.0(18) . . ? C18 N1 C13 118.9(5) . . ? C18 N1 Mn1 120.5(4) . . ? C13 N1 Mn1 120.6(4) . . ? C33 N3 C38 117.5(5) . . ? C33 N3 Mn2 120.9(4) . . ? C38 N3 Mn2 121.0(4) . . ? C1 O1 Mn1 119.8(3) . . ? C1 O1 Na1 129.2(3) . 2_666 ? Mn1 O1 Na1 97.64(16) . 2_666 ? C12 O2 Mn1 126.4(3) . . ? C12 O2 Na1 134.8(3) . . ? Mn1 O2 Na1 97.68(17) . . ? C19 O3 Na1 135.6(4) . . ? C19 O3 H3A 122(4) . . ? Na1 O3 H3A 101(4) . . ? C21 O4 Mn2 116.1(3) . . ? C21 O4 Na1 140.1(3) . . ? Mn2 O4 Na1 102.67(16) . . ? C32 O5 Mn2 123.9(3) . . ? C32 O5 Na2 123.0(3) . . ? Mn2 O5 Na2 101.29(14) . . ? C39 O6 Mn2 122.0(3) . . ? C39 O6 Na1 119.4(3) . . ? Mn2 O6 Na1 95.86(13) . . ? C50 O7 Mn2 120.1(3) . . ? C50 O7 Na2 133.7(3) . . ? Mn2 O7 Na2 104.22(15) . . ? C51 O8 Na2 142.9(6) . . ? C51 O8 H8A 127(9) . . ? Na2 O8 H8A 87(9) . . ? C55 O9 Mn3 125.1(4) . . ? C55 O9 Na2 138.5(3) . . ? Mn3 O9 Na2 93.21(17) . . ? C66 O10 Mn3 123.6(4) . . ? C66 O10 Na2 137.9(3) . 2_755 ? Mn3 O10 Na2 95.20(16) . 2_755 ? C53 O11 Mn3 134.5(5) . . ? C53 O11 Na2 128.8(6) . . ? Mn3 O11 Na2 75.87(12) . . ? C53 O11 H11A 104.3 . . ? Mn3 O11 H11A 104.3 . . ? Na2 O11 H11A 104.3 . . ? O1 C1 C6 121.0(4) . . ? O1 C1 C2 119.9(5) . . ? C6 C1 C2 119.1(5) . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 121.8(5) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 119.5(5) . . ? C1 C6 C7 121.5(5) . . ? C5 C6 C7 119.1(5) . . ? C8 C7 C12 119.1(5) . . ? C8 C7 C6 119.8(5) . . ? C12 C7 C6 121.1(5) . . ? C7 C8 C9 122.9(5) . . ? C7 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? C10 C9 C8 117.9(6) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 121.6(5) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? O2 C12 C7 123.7(4) . . ? O2 C12 C11 118.6(5) . . ? C7 C12 C11 117.7(5) . . ? N1 C13 C14 121.0(5) . . ? N1 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C16 C14 C13 119.4(5) . . ? C16 C14 C15 121.0(6) . . ? C13 C14 C15 119.5(6) . . ? N2 C15 C14 178.9(8) . . ? C14 C16 C17 119.0(5) . . ? C14 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N1 C18 C17 122.4(5) . . ? N1 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? O3 C19 C20 112.9(6) . . ? O3 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? O3 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C22 119.6(5) . . ? O4 C21 C26 121.0(5) . . ? C22 C21 C26 119.5(5) . . ? C23 C22 C21 119.8(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 121.3(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 118.7(6) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 121.8(6) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C21 118.9(5) . . ? C25 C26 C27 122.2(5) . . ? C21 C26 C27 118.8(5) . . ? C28 C27 C32 117.3(5) . . ? C28 C27 C26 120.7(5) . . ? C32 C27 C26 122.0(5) . . ? C29 C28 C27 122.8(5) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C30 C29 C28 118.7(5) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 122.3(5) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? O5 C32 C31 121.0(4) . . ? O5 C32 C27 120.1(5) . . ? C31 C32 C27 118.9(5) . . ? N3 C33 C34 124.1(5) . . ? N3 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C33 C34 C35 117.7(6) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C36 C35 C34 119.6(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C38 118.6(5) . . ? C35 C36 C37 122.0(6) . . ? C38 C36 C37 119.2(6) . . ? N4 C37 C36 177.3(8) . . ? N3 C38 C36 122.5(5) . . ? N3 C38 H38 118.8 . . ? C36 C38 H38 118.8 . . ? O6 C39 C44 123.4(6) . . ? O6 C39 C40 118.4(5) . . ? C44 C39 C40 118.2(5) . . ? C41 C40 C39 122.3(5) . . ? C41 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C40 C41 C42 118.0(6) . . ? C40 C41 H41 121.0 . . ? C42 C41 H41 121.0 . . ? C43 C42 C41 120.3(6) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 122.0(6) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C43 C44 C39 119.2(6) . . ? C43 C44 C45 118.1(5) . . ? C39 C44 C45 122.7(5) . . ? C46 C45 C50 117.1(6) . . ? C46 C45 C44 121.8(5) . . ? C50 C45 C44 121.1(5) . . ? C47 C46 C45 121.1(6) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 120.7(6) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 118.8(7) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C50 C49 C48 120.6(6) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? O7 C50 C49 119.3(5) . . ? O7 C50 C45 119.0(5) . . ? C49 C50 C45 121.6(5) . . ? O8 C51 C52 114.3(8) . . ? O8 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? O8 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O11 C53 C54 120.6(7) . . ? O11 C53 H53A 107.2 . . ? C54 C53 H53A 107.2 . . ? O11 C53 H53B 107.2 . . ? C54 C53 H53B 107.2 . . ? H53A C53 H53B 106.8 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O9 C55 C60 121.2(5) . . ? O9 C55 C56 119.5(6) . . ? C60 C55 C56 119.3(6) . . ? C57 C56 C55 121.0(6) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C56 C57 C58 120.0(6) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 119.0(6) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C58 C59 C60 122.2(6) . . ? C58 C59 H59 118.9 . . ? C60 C59 H59 118.9 . . ? C55 C60 C59 118.4(5) . . ? C55 C60 C61 122.3(5) . . ? C59 C60 C61 119.2(6) . . ? C62 C61 C66 118.9(5) . . ? C62 C61 C60 120.8(5) . . ? C66 C61 C60 120.3(5) . . ? C63 C62 C61 122.4(6) . . ? C63 C62 H62 118.8 . . ? C61 C62 H62 118.8 . . ? C62 C63 C64 118.8(6) . . ? C62 C63 H63 120.6 . . ? C64 C63 H63 120.6 . . ? C65 C64 C63 120.1(5) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 122.0(6) . . ? C64 C65 H65 119.0 . . ? C66 C65 H65 119.0 . . ? O10 C66 C65 120.4(5) . . ? O10 C66 C61 121.8(5) . . ? C65 C66 C61 117.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.994 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.086 # Attachment '- 2.cif' data_p21n _database_code_depnum_ccdc_archive 'CCDC 778270' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Na(biphenH2)(EtOH)2(H2O))(Mn(biphen)2(4-cnp)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 Mn N4 Na O9' _chemical_formula_weight 948.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.377(2) _cell_length_b 21.331(4) _cell_length_c 23.121(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.53(3) _cell_angle_gamma 90.00 _cell_volume 5047.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.328 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.8806 _cell_measurement_reflns_used 8021 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.97503 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 23519 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.8806 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0375522000 _diffrn_orient_matrix_UB_12 0.0158021000 _diffrn_orient_matrix_UB_13 -0.0240993000 _diffrn_orient_matrix_UB_21 -0.0035155000 _diffrn_orient_matrix_UB_22 0.0267956000 _diffrn_orient_matrix_UB_23 0.0178368000 _diffrn_orient_matrix_UB_31 0.0580870000 _diffrn_orient_matrix_UB_32 0.0118020000 _diffrn_orient_matrix_UB_33 -0.0083238000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -25.00 22.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -17.3903 -96.0000 -114.0000 47 #__ type_ start__ end____ width___ exp.time_ 2 omega -35.00 92.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 0.0000 -180.0000 127 #__ type_ start__ end____ width___ exp.time_ 3 omega -5.00 42.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -77.0000 150.0000 47 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 9233 _reflns_number_gt 5854 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1682P)^2^+1.6381P] 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 9233 _refine_ls_number_parameters 622 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2652 _refine_ls_wR_factor_gt 0.2473 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _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 0.88092(6) 0.22134(3) 0.80537(3) 0.0226(2) Uani 1 1 d . . . Na1 Na 1.36764(18) 0.19641(11) 0.77257(9) 0.0393(5) Uani 1 1 d . . . N1 N 0.7689(6) 0.0233(3) 0.5221(2) 0.0548(14) Uani 1 1 d . . . N2 N 0.8430(4) 0.16244(18) 0.71723(17) 0.0252(9) Uani 1 1 d . . . N3 N 0.9186(4) 0.28006(19) 0.89367(18) 0.0276(9) Uani 1 1 d . . . N4 N 0.9922(5) 0.4034(3) 1.0973(3) 0.0600(16) Uani 1 1 d . . . O1 O 0.7278(3) 0.27172(16) 0.77919(14) 0.0268(8) Uani 1 1 d . . . O2 O 0.9866(3) 0.27781(15) 0.77058(15) 0.0254(7) Uani 1 1 d . . . O3 O 1.0341(3) 0.17115(15) 0.83282(15) 0.0273(8) Uani 1 1 d . . . O4 O 0.7739(3) 0.16437(16) 0.83822(14) 0.0279(8) Uani 1 1 d . . . O5 O 1.5231(3) 0.26040(16) 0.83087(15) 0.0295(8) Uani 1 1 d D . . O6 O 1.2657(3) 0.22001(17) 0.85245(15) 0.0329(8) Uani 1 1 d D . . O7 O 1.2138(4) 0.2663(2) 0.7250(2) 0.0603(13) Uani 1 1 d D . . O8 O 1.3200(4) 0.1416(2) 0.6842(2) 0.0595(12) Uani 1 1 d D . . O9 O 1.5288(4) 0.1207(2) 0.7929(2) 0.0603(13) Uani 1 1 d . . . C1 C 0.7008(4) 0.2948(2) 0.7244(2) 0.0241(10) Uani 1 1 d . . . C2 C 0.5989(4) 0.2689(2) 0.6848(2) 0.0290(11) Uani 1 1 d . . . H2 H 0.5511 0.2344 0.6963 0.035 Uiso 1 1 calc R . . C3 C 0.5668(5) 0.2935(3) 0.6282(2) 0.0343(12) Uani 1 1 d . . . H3 H 0.4956 0.2763 0.6018 0.041 Uiso 1 1 calc R . . C4 C 0.6363(5) 0.3416(3) 0.6105(2) 0.0386(13) Uani 1 1 d . . . H4 H 0.6153 0.3574 0.5717 0.046 Uiso 1 1 calc R . . C5 C 0.7384(5) 0.3678(3) 0.6497(2) 0.0346(12) Uani 1 1 d . . . H5 H 0.7870 0.4014 0.6370 0.042 Uiso 1 1 calc R . . C6 C 0.7710(4) 0.3459(2) 0.7069(2) 0.0266(11) Uani 1 1 d . . . C7 C 0.8766(5) 0.3759(2) 0.7488(2) 0.0313(12) Uani 1 1 d . . . C8 C 0.8761(6) 0.4411(3) 0.7562(3) 0.0528(17) Uani 1 1 d . . . H8 H 0.8064 0.4653 0.7356 0.063 Uiso 1 1 calc R . . C9 C 0.9776(6) 0.4711(3) 0.7938(4) 0.068(2) Uani 1 1 d . . . H9 H 0.9778 0.5154 0.7981 0.081 Uiso 1 1 calc R . . C10 C 1.0769(6) 0.4355(3) 0.8244(3) 0.060(2) Uani 1 1 d . . . H10 H 1.1447 0.4554 0.8506 0.072 Uiso 1 1 calc R . . C11 C 1.0791(5) 0.3698(3) 0.8174(3) 0.0380(13) Uani 1 1 d . . . H11 H 1.1488 0.3459 0.8382 0.046 Uiso 1 1 calc R . . C12 C 0.9792(4) 0.3403(2) 0.7799(2) 0.0265(11) Uani 1 1 d . . . C13 C 0.8052(4) 0.1461(2) 0.8949(2) 0.0279(11) Uani 1 1 d . . . C14 C 0.7354(5) 0.1700(3) 0.9363(2) 0.0366(13) Uani 1 1 d . . . H14 H 0.6677 0.1996 0.9248 0.044 Uiso 1 1 calc R . . C15 C 0.7641(6) 0.1507(3) 0.9942(2) 0.0461(15) Uani 1 1 d . . . H15 H 0.7158 0.1674 1.0222 0.055 Uiso 1 1 calc R . . C16 C 0.8608(6) 0.1082(3) 1.0116(3) 0.0516(17) Uani 1 1 d . . . H16 H 0.8812 0.0962 1.0517 0.062 Uiso 1 1 calc R . . C17 C 0.9295(5) 0.0824(3) 0.9707(2) 0.0392(13) Uani 1 1 d . . . H17 H 0.9952 0.0520 0.9828 0.047 Uiso 1 1 calc R . . C18 C 0.9030(5) 0.1008(2) 0.9117(2) 0.0313(11) Uani 1 1 d . . . C19 C 0.9720(4) 0.0717(2) 0.8674(2) 0.0279(11) Uani 1 1 d . . . C20 C 0.9743(5) 0.0065(3) 0.8625(3) 0.0388(13) Uani 1 1 d . . . H20 H 0.9313 -0.0184 0.8875 0.047 Uiso 1 1 calc R . . C21 C 1.0379(6) -0.0225(3) 0.8218(3) 0.0473(15) Uani 1 1 d . . . H21 H 1.0362 -0.0669 0.8182 0.057 Uiso 1 1 calc R . . C22 C 1.1035(6) 0.0129(3) 0.7867(3) 0.0454(15) Uani 1 1 d . . . H22 H 1.1510 -0.0070 0.7601 0.055 Uiso 1 1 calc R . . C23 C 1.1005(5) 0.0784(3) 0.7900(2) 0.0354(12) Uani 1 1 d . . . H23 H 1.1445 0.1029 0.7651 0.042 Uiso 1 1 calc R . . C24 C 1.0338(4) 0.1075(2) 0.8295(2) 0.0261(11) Uani 1 1 d . . . C25 C 0.7851(5) 0.0534(3) 0.5633(2) 0.0373(13) Uani 1 1 d . . . C26 C 0.8062(4) 0.0910(2) 0.6158(2) 0.0272(11) Uani 1 1 d . . . C27 C 0.8473(5) 0.1526(2) 0.6147(2) 0.0295(11) Uani 1 1 d . . . H27 H 0.8628 0.1713 0.5791 0.035 Uiso 1 1 calc R . . C28 C 0.8652(4) 0.1865(2) 0.6665(2) 0.0286(11) Uani 1 1 d . . . H28 H 0.8946 0.2286 0.6660 0.034 Uiso 1 1 calc R . . C29 C 0.8030(4) 0.1029(2) 0.7174(2) 0.0274(11) Uani 1 1 d . . . H29 H 0.7877 0.0853 0.7534 0.033 Uiso 1 1 calc R . . C30 C 0.7829(5) 0.0656(2) 0.6679(2) 0.0294(11) Uani 1 1 d . . . H30 H 0.7537 0.0235 0.6697 0.035 Uiso 1 1 calc R . . C31 C 0.9794(5) 0.3796(3) 1.0531(3) 0.0448(15) Uani 1 1 d . . . C32 C 0.9618(5) 0.3457(3) 0.9976(2) 0.0372(13) Uani 1 1 d . . . C33 C 0.8651(5) 0.3651(3) 0.9517(2) 0.0368(13) Uani 1 1 d . . . H33 H 0.8118 0.4005 0.9558 0.044 Uiso 1 1 calc R . . C34 C 0.8494(5) 0.3316(3) 0.9008(2) 0.0338(12) Uani 1 1 d . . . H34 H 0.7864 0.3456 0.8688 0.041 Uiso 1 1 calc R . . C35 C 1.0086(4) 0.2626(3) 0.9379(2) 0.0303(11) Uani 1 1 d . . . H35 H 1.0576 0.2258 0.9335 0.036 Uiso 1 1 calc R . . C36 C 1.0357(5) 0.2950(3) 0.9904(2) 0.0336(12) Uani 1 1 d . . . H36 H 1.1040 0.2819 1.0206 0.040 Uiso 1 1 calc R . . C37 C 1.4950(4) 0.3169(2) 0.8542(2) 0.0280(11) Uani 1 1 d . . . C38 C 1.5233(5) 0.3726(3) 0.8296(2) 0.0358(13) Uani 1 1 d . . . H38 H 1.5619 0.3726 0.7951 0.043 Uiso 1 1 calc R . . C39 C 1.4957(5) 0.4293(3) 0.8549(3) 0.0475(15) Uani 1 1 d . . . H39 H 1.5145 0.4679 0.8375 0.057 Uiso 1 1 calc R . . C40 C 1.4409(6) 0.4294(3) 0.9055(3) 0.0490(16) Uani 1 1 d . . . H40 H 1.4233 0.4678 0.9235 0.059 Uiso 1 1 calc R . . C41 C 1.4127(5) 0.3740(3) 0.9290(3) 0.0426(14) Uani 1 1 d . . . H41 H 1.3738 0.3746 0.9635 0.051 Uiso 1 1 calc R . . C42 C 1.4379(5) 0.3164(2) 0.9053(2) 0.0315(12) Uani 1 1 d . . . C43 C 1.4075(5) 0.2580(3) 0.9357(2) 0.0322(12) Uani 1 1 d . . . C44 C 1.4625(6) 0.2501(3) 0.9952(2) 0.0475(16) Uani 1 1 d . . . H44 H 1.5234 0.2798 1.0142 0.057 Uiso 1 1 calc R . . C45 C 1.4273(6) 0.1983(4) 1.0264(3) 0.0575(19) Uani 1 1 d . . . H45 H 1.4626 0.1937 1.0668 0.069 Uiso 1 1 calc R . . C46 C 1.3433(6) 0.1545(3) 0.9995(3) 0.0509(17) Uani 1 1 d . . . H46 H 1.3205 0.1195 1.0210 0.061 Uiso 1 1 calc R . . C47 C 1.2911(5) 0.1606(3) 0.9413(3) 0.0416(14) Uani 1 1 d . . . H47 H 1.2336 0.1293 0.9227 0.050 Uiso 1 1 calc R . . C48 C 1.3210(4) 0.2116(3) 0.9095(2) 0.0311(12) Uani 1 1 d . . . C51 C 1.2228(7) 0.1523(4) 0.6330(3) 0.068(2) Uani 1 1 d . . . H51A H 1.2631 0.1753 0.6033 0.081 Uiso 1 1 calc R . . H51B H 1.1523 0.1789 0.6438 0.081 Uiso 1 1 calc R . . C49 C 1.2585(7) 0.3308(4) 0.7082(4) 0.069(2) Uani 1 1 d . . . H49A H 1.2669 0.3587 0.7428 0.083 Uiso 1 1 calc R . . H49B H 1.3459 0.3270 0.6966 0.083 Uiso 1 1 calc R . . C50 C 1.1723(9) 0.3583(5) 0.6619(4) 0.101(3) Uani 1 1 d . . . H50A H 1.1550 0.3288 0.6290 0.151 Uiso 1 1 calc R . . H50B H 1.2118 0.3965 0.6490 0.151 Uiso 1 1 calc R . . H50C H 1.0901 0.3689 0.6752 0.151 Uiso 1 1 calc R . . C52 C 1.1667(6) 0.0943(4) 0.6075(4) 0.076(2) Uani 1 1 d . . . H52A H 1.2353 0.0688 0.5947 0.114 Uiso 1 1 calc R . . H52B H 1.0991 0.1038 0.5738 0.114 Uiso 1 1 calc R . . H52C H 1.1278 0.0711 0.6369 0.114 Uiso 1 1 calc R . . H6A H 1.1814(15) 0.212(3) 0.846(3) 0.048(18) Uiso 1 1 d D . . H5A H 1.585(5) 0.273(3) 0.812(3) 0.07(2) Uiso 1 1 d D . . H7A H 1.143(5) 0.268(4) 0.742(3) 0.09(3) Uiso 1 1 d D . . H8A H 1.384(5) 0.122(3) 0.672(3) 0.08(2) Uiso 1 1 d 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 0.0177(4) 0.0266(4) 0.0238(4) -0.0006(3) 0.0045(3) 0.0007(3) Na1 0.0272(10) 0.0519(14) 0.0395(13) -0.0072(11) 0.0078(9) -0.0034(9) N1 0.079(4) 0.050(3) 0.036(3) -0.012(3) 0.014(3) -0.014(3) N2 0.025(2) 0.025(2) 0.027(2) 0.0010(18) 0.0064(16) -0.0006(16) N3 0.023(2) 0.031(2) 0.029(2) -0.0012(19) 0.0043(17) 0.0033(17) N4 0.043(3) 0.084(4) 0.053(3) -0.036(3) 0.008(3) -0.007(3) O1 0.0183(15) 0.039(2) 0.0235(18) 0.0024(15) 0.0044(13) 0.0038(13) O2 0.0211(16) 0.0235(18) 0.0330(19) -0.0018(15) 0.0084(14) -0.0007(13) O3 0.0190(15) 0.0254(18) 0.038(2) -0.0005(15) 0.0051(14) -0.0017(13) O4 0.0196(16) 0.040(2) 0.0242(18) 0.0053(16) 0.0033(13) -0.0006(14) O5 0.0245(17) 0.031(2) 0.035(2) -0.0033(16) 0.0121(15) -0.0027(14) O6 0.0240(18) 0.044(2) 0.031(2) 0.0028(17) 0.0058(15) -0.0061(15) O7 0.048(3) 0.083(4) 0.054(3) 0.005(3) 0.024(2) 0.023(2) O8 0.046(3) 0.074(3) 0.053(3) -0.018(2) -0.007(2) 0.014(2) O9 0.035(2) 0.055(3) 0.086(4) -0.021(3) -0.006(2) 0.0039(19) C1 0.021(2) 0.031(3) 0.022(2) -0.003(2) 0.0077(18) 0.0046(19) C2 0.021(2) 0.039(3) 0.028(3) -0.008(2) 0.006(2) -0.003(2) C3 0.028(3) 0.048(3) 0.026(3) -0.006(2) 0.001(2) -0.001(2) C4 0.036(3) 0.054(4) 0.026(3) 0.008(3) 0.004(2) 0.011(3) C5 0.036(3) 0.030(3) 0.039(3) 0.009(2) 0.012(2) 0.003(2) C6 0.025(2) 0.025(3) 0.030(3) -0.004(2) 0.006(2) 0.0051(19) C7 0.030(3) 0.024(3) 0.041(3) -0.007(2) 0.007(2) 0.001(2) C8 0.036(3) 0.032(3) 0.087(5) -0.014(3) -0.001(3) 0.011(2) C9 0.049(4) 0.028(3) 0.118(7) -0.034(4) -0.010(4) 0.007(3) C10 0.036(3) 0.050(4) 0.089(5) -0.034(4) -0.006(3) -0.002(3) C11 0.029(3) 0.034(3) 0.050(4) -0.009(3) 0.002(2) -0.001(2) C12 0.023(2) 0.023(3) 0.034(3) -0.006(2) 0.006(2) 0.0024(19) C13 0.021(2) 0.037(3) 0.027(3) 0.004(2) 0.0061(19) -0.004(2) C14 0.025(3) 0.054(4) 0.031(3) 0.003(3) 0.007(2) 0.005(2) C15 0.042(3) 0.067(4) 0.031(3) 0.002(3) 0.013(3) 0.009(3) C16 0.041(3) 0.083(5) 0.029(3) 0.012(3) 0.002(3) 0.000(3) C17 0.031(3) 0.047(4) 0.039(3) 0.011(3) 0.001(2) 0.002(2) C18 0.028(3) 0.036(3) 0.029(3) 0.002(2) 0.002(2) -0.007(2) C19 0.023(2) 0.029(3) 0.030(3) 0.001(2) 0.000(2) -0.0009(19) C20 0.045(3) 0.027(3) 0.042(3) 0.004(3) 0.000(3) -0.005(2) C21 0.057(4) 0.023(3) 0.058(4) -0.004(3) 0.000(3) 0.007(3) C22 0.046(3) 0.039(3) 0.050(4) -0.014(3) 0.007(3) 0.008(3) C23 0.033(3) 0.036(3) 0.036(3) -0.004(3) 0.004(2) 0.003(2) C24 0.021(2) 0.025(3) 0.031(3) -0.001(2) -0.0018(19) -0.0001(18) C25 0.046(3) 0.034(3) 0.034(3) -0.001(3) 0.011(2) -0.008(2) C26 0.025(2) 0.028(3) 0.030(3) -0.001(2) 0.006(2) 0.0004(19) C27 0.034(3) 0.030(3) 0.027(3) 0.002(2) 0.013(2) 0.001(2) C28 0.027(2) 0.025(3) 0.036(3) 0.000(2) 0.009(2) 0.0001(19) C29 0.023(2) 0.034(3) 0.026(3) 0.005(2) 0.0057(19) 0.000(2) C30 0.030(3) 0.026(3) 0.032(3) 0.000(2) 0.006(2) -0.001(2) C31 0.031(3) 0.066(4) 0.037(3) -0.017(3) 0.003(2) -0.005(3) C32 0.031(3) 0.048(4) 0.033(3) -0.011(3) 0.007(2) -0.010(2) C33 0.033(3) 0.037(3) 0.041(3) -0.010(3) 0.008(2) 0.007(2) C34 0.025(2) 0.043(3) 0.031(3) -0.003(3) 0.000(2) 0.006(2) C35 0.021(2) 0.037(3) 0.033(3) -0.002(2) 0.003(2) 0.003(2) C36 0.027(3) 0.046(3) 0.026(3) -0.002(2) 0.001(2) 0.003(2) C37 0.017(2) 0.030(3) 0.036(3) -0.007(2) 0.0010(19) 0.0017(19) C38 0.027(3) 0.041(3) 0.040(3) 0.001(3) 0.006(2) 0.001(2) C39 0.036(3) 0.034(3) 0.071(4) 0.002(3) 0.001(3) -0.001(2) C40 0.045(3) 0.043(4) 0.058(4) -0.020(3) 0.007(3) 0.006(3) C41 0.039(3) 0.052(4) 0.037(3) -0.016(3) 0.006(2) 0.007(3) C42 0.023(2) 0.038(3) 0.032(3) -0.008(2) 0.002(2) 0.001(2) C43 0.025(2) 0.045(3) 0.029(3) -0.003(2) 0.011(2) 0.013(2) C44 0.040(3) 0.075(5) 0.027(3) -0.005(3) 0.005(2) 0.015(3) C45 0.052(4) 0.096(6) 0.027(3) 0.015(4) 0.012(3) 0.033(4) C46 0.039(3) 0.067(4) 0.050(4) 0.020(3) 0.016(3) 0.015(3) C47 0.030(3) 0.047(4) 0.050(4) 0.014(3) 0.015(2) 0.007(2) C48 0.019(2) 0.042(3) 0.034(3) 0.002(2) 0.009(2) 0.008(2) C51 0.054(4) 0.071(5) 0.072(5) -0.025(4) -0.005(3) 0.019(3) C49 0.050(4) 0.079(6) 0.081(6) -0.001(5) 0.018(4) -0.001(4) C50 0.086(6) 0.151(10) 0.063(5) 0.027(6) 0.006(5) -0.029(6) C52 0.038(4) 0.076(5) 0.110(7) -0.033(5) 0.003(4) -0.002(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 O4 1.888(3) . ? Mn1 O2 1.896(3) . ? Mn1 O1 1.930(3) . ? Mn1 O3 1.935(3) . ? Mn1 N2 2.371(4) . ? Mn1 N3 2.372(4) . ? Na1 O9 2.316(5) . ? Na1 O7 2.323(5) . ? Na1 O6 2.330(4) . ? Na1 O8 2.335(5) . ? Na1 O5 2.358(4) . ? N1 C25 1.137(7) . ? N2 C28 1.334(6) . ? N2 C29 1.337(6) . ? N3 C35 1.320(6) . ? N3 C34 1.339(6) . ? N4 C31 1.128(7) . ? O1 C1 1.346(6) . ? O2 C12 1.354(5) . ? O3 C24 1.360(6) . ? O4 C13 1.354(6) . ? O5 C37 1.372(6) . ? O5 H5A 0.877(10) . ? O6 C48 1.359(6) . ? O6 H6A 0.879(10) . ? O7 C49 1.524(9) . ? O7 H7A 0.883(10) . ? O8 C51 1.441(8) . ? O8 H8A 0.880(10) . ? C1 C2 1.394(7) . ? C1 C6 1.406(7) . ? C2 C3 1.398(7) . ? C2 H2 0.9500 . ? C3 C4 1.355(8) . ? C3 H3 0.9500 . ? C4 C5 1.392(8) . ? C4 H4 0.9500 . ? C5 C6 1.392(7) . ? C5 H5 0.9500 . ? C6 C7 1.481(7) . ? C7 C8 1.402(7) . ? C7 C12 1.405(7) . ? C8 C9 1.403(9) . ? C8 H8 0.9500 . ? C9 C10 1.378(10) . ? C9 H9 0.9500 . ? C10 C11 1.411(8) . ? C10 H10 0.9500 . ? C11 C12 1.388(7) . ? C11 H11 0.9500 . ? C13 C14 1.389(7) . ? C13 C18 1.408(7) . ? C14 C15 1.386(8) . ? C14 H14 0.9500 . ? C15 C16 1.363(8) . ? C15 H15 0.9500 . ? C16 C17 1.389(8) . ? C16 H16 0.9500 . ? C17 C18 1.402(7) . ? C17 H17 0.9500 . ? C18 C19 1.480(7) . ? C19 C24 1.394(7) . ? C19 C20 1.397(7) . ? C20 C21 1.381(8) . ? C20 H20 0.9500 . ? C21 C22 1.369(9) . ? C21 H21 0.9500 . ? C22 C23 1.401(8) . ? C22 H22 0.9500 . ? C23 C24 1.381(7) . ? C23 H23 0.9500 . ? C25 C26 1.441(8) . ? C26 C30 1.377(7) . ? C26 C27 1.384(7) . ? C27 C28 1.386(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.382(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.458(8) . ? C32 C36 1.352(8) . ? C32 C33 1.397(8) . ? C33 C34 1.363(7) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.385(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.370(7) . ? C37 C42 1.406(7) . ? C38 C39 1.395(8) . ? C38 H38 0.9500 . ? C39 C40 1.383(9) . ? C39 H39 0.9500 . ? C40 C41 1.352(9) . ? C40 H40 0.9500 . ? C41 C42 1.389(8) . ? C41 H41 0.9500 . ? C42 C43 1.489(8) . ? C43 C48 1.403(8) . ? C43 C44 1.411(8) . ? C44 C45 1.400(10) . ? C44 H44 0.9500 . ? C45 C46 1.355(10) . ? C45 H45 0.9500 . ? C46 C47 1.371(9) . ? C46 H46 0.9500 . ? C47 C48 1.378(7) . ? C47 H47 0.9500 . ? C51 C52 1.449(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C49 C50 1.405(12) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 178.62(15) . . ? O4 Mn1 O1 88.63(14) . . ? O2 Mn1 O1 90.98(14) . . ? O4 Mn1 O3 91.03(14) . . ? O2 Mn1 O3 89.37(13) . . ? O1 Mn1 O3 179.14(14) . . ? O4 Mn1 N2 88.84(14) . . ? O2 Mn1 N2 89.84(14) . . ? O1 Mn1 N2 90.84(14) . . ? O3 Mn1 N2 89.94(14) . . ? O4 Mn1 N3 91.02(14) . . ? O2 Mn1 N3 90.30(14) . . ? O1 Mn1 N3 89.19(14) . . ? O3 Mn1 N3 90.03(14) . . ? N2 Mn1 N3 179.86(15) . . ? O9 Na1 O7 163.67(19) . . ? O9 Na1 O6 113.41(18) . . ? O7 Na1 O6 82.53(15) . . ? O9 Na1 O8 82.52(17) . . ? O7 Na1 O8 82.96(18) . . ? O6 Na1 O8 138.05(17) . . ? O9 Na1 O5 83.39(15) . . ? O7 Na1 O5 104.51(18) . . ? O6 Na1 O5 77.25(13) . . ? O8 Na1 O5 144.64(17) . . ? C28 N2 C29 117.9(4) . . ? C28 N2 Mn1 121.5(3) . . ? C29 N2 Mn1 120.6(3) . . ? C35 N3 C34 117.5(4) . . ? C35 N3 Mn1 120.8(3) . . ? C34 N3 Mn1 121.6(3) . . ? C1 O1 Mn1 122.1(3) . . ? C12 O2 Mn1 120.4(3) . . ? C24 O3 Mn1 122.7(3) . . ? C13 O4 Mn1 120.8(3) . . ? C37 O5 Na1 124.3(3) . . ? C37 O5 H5A 98(4) . . ? Na1 O5 H5A 113(5) . . ? C48 O6 Na1 124.5(3) . . ? C48 O6 H6A 112(4) . . ? Na1 O6 H6A 114(4) . . ? C49 O7 Na1 119.1(4) . . ? C49 O7 H7A 112(5) . . ? Na1 O7 H7A 112(5) . . ? C51 O8 Na1 131.1(4) . . ? C51 O8 H8A 106(5) . . ? Na1 O8 H8A 118(5) . . ? O1 C1 C2 119.4(4) . . ? O1 C1 C6 121.1(4) . . ? C2 C1 C6 119.5(4) . . ? C1 C2 C3 120.2(5) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.5(5) . . ? C5 C6 C7 120.8(5) . . ? C1 C6 C7 120.7(4) . . ? C8 C7 C12 119.4(5) . . ? C8 C7 C6 119.5(5) . . ? C12 C7 C6 121.1(4) . . ? C7 C8 C9 120.7(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.2(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.8(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? O2 C12 C11 119.3(4) . . ? O2 C12 C7 120.6(4) . . ? C11 C12 C7 119.9(5) . . ? O4 C13 C14 119.5(4) . . ? O4 C13 C18 120.8(4) . . ? C14 C13 C18 119.7(5) . . ? C15 C14 C13 120.3(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.9(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.8(5) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 118.5(5) . . ? C17 C18 C19 121.1(5) . . ? C13 C18 C19 120.4(4) . . ? C24 C19 C20 118.5(5) . . ? C24 C19 C18 122.1(5) . . ? C20 C19 C18 119.4(5) . . ? C21 C20 C19 121.2(5) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.0(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? O3 C24 C23 119.2(4) . . ? O3 C24 C19 120.5(4) . . ? C23 C24 C19 120.2(5) . . ? N1 C25 C26 179.4(7) . . ? C30 C26 C27 119.3(5) . . ? C30 C26 C25 119.6(5) . . ? C27 C26 C25 121.1(5) . . ? C26 C27 C28 118.4(5) . . ? C26 C27 H27 120.8 . . ? C28 C27 H27 120.8 . . ? N2 C28 C27 122.8(5) . . ? N2 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? N2 C29 C30 123.3(4) . . ? N2 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C26 C30 C29 118.3(5) . . ? C26 C30 H30 120.9 . . ? C29 C30 H30 120.9 . . ? N4 C31 C32 177.0(7) . . ? C36 C32 C33 119.6(5) . . ? C36 C32 C31 120.9(5) . . ? C33 C32 C31 119.5(5) . . ? C34 C33 C32 118.0(5) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? N3 C34 C33 123.1(5) . . ? N3 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? N3 C35 C36 123.6(5) . . ? N3 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C32 C36 C35 118.0(5) . . ? C32 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C38 C37 O5 121.6(5) . . ? C38 C37 C42 120.4(5) . . ? O5 C37 C42 118.0(4) . . ? C37 C38 C39 120.3(5) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.9(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 119.1(5) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 123.2(5) . . ? C40 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C41 C42 C37 117.2(5) . . ? C41 C42 C43 119.1(5) . . ? C37 C42 C43 123.7(4) . . ? C48 C43 C44 117.7(5) . . ? C48 C43 C42 123.8(5) . . ? C44 C43 C42 118.5(5) . . ? C45 C44 C43 119.9(6) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 120.7(6) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.3(6) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 120.8(6) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? O6 C48 C47 121.7(5) . . ? O6 C48 C43 117.6(5) . . ? C47 C48 C43 120.7(5) . . ? O8 C51 C52 112.2(7) . . ? O8 C51 H51A 109.2 . . ? C52 C51 H51A 109.2 . . ? O8 C51 H51B 109.2 . . ? C52 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? C50 C49 O7 113.0(7) . . ? C50 C49 H49A 109.0 . . ? O7 C49 H49A 109.0 . . ? C50 C49 H49B 109.0 . . ? O7 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.130 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.113