Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'George Christou' 'Khalil A. Abboud' 'Anastasios J. Tasiopoulos' _publ_contact_author_name 'Prof George Christou' _publ_contact_author_address ; Department of Chemistry University of Florida PO Box 117200 Gainesville FL 32611-7200 UNITED STATES OF AMERICA ; _publ_contact_author_email CHRISTOU@CHEM.UFL.EDU _publ_section_title ; A Novel Aggregate of [Mn2(μ-O)2] Units: [Mn8O10(O2CMe)6(H2O)2(bpy)6]4+ with a Serpentine Core ; data_ts30 _database_code_CSD 192829 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H86 Cl4 Mn8 N12 O48' _chemical_formula_weight 2540.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.1494(7) _cell_length_b 13.7254(7) _cell_length_c 15.8387(8) _cell_angle_alpha 65.623(2) _cell_angle_beta 79.268(2) _cell_angle_gamma 73.316(2) _cell_volume 2486.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 67 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8106 _exptl_absorpt_correction_T_max 0.9539 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 22247 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11071 _reflns_number_gt 6093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^] 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 11071 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _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 0.54254(4) 0.43389(4) 0.45182(3) 0.01841(12) Uani 1 1 d . . . Mn2 Mn 0.53706(4) 0.21218(4) 0.52799(3) 0.02101(12) Uani 1 1 d . . . Mn3 Mn 0.76896(4) 0.22585(4) 0.41057(3) 0.02055(12) Uani 1 1 d . . . Mn4 Mn 0.90513(4) 0.30366(4) 0.26577(3) 0.02270(13) Uani 1 1 d . . . Cl1 Cl 1.16329(7) -0.42275(9) 0.28946(7) 0.0424(3) Uani 1 1 d . . . Cl2 Cl 0.58622(7) -0.18517(8) -0.08143(6) 0.0376(2) Uani 1 1 d . . . O1 O 0.55824(15) 0.44058(16) 0.55950(13) 0.0187(5) Uani 1 1 d . . . O2 O 0.44839(15) 0.34355(16) 0.49809(13) 0.0209(5) Uani 1 1 d . . . O3 O 0.64025(15) 0.28758(16) 0.47241(13) 0.0199(5) Uani 1 1 d . . . O4 O 0.62742(17) 0.05771(17) 0.56704(14) 0.0248(5) Uani 1 1 d . . . O5 O 0.50552(16) 0.19477(17) 0.42321(15) 0.0256(5) Uani 1 1 d . . . O6 O 0.79306(17) 0.08166(18) 0.51634(14) 0.0267(5) Uani 1 1 d . . . O7 O 0.89010(16) 0.17126(17) 0.34531(14) 0.0239(5) Uani 1 1 d . . . O8 O 0.77634(15) 0.35536(16) 0.30859(13) 0.0215(5) Uani 1 1 d . . . O9 O 0.66928(17) 0.16890(17) 0.35146(14) 0.0272(5) Uani 1 1 d . . . O10 O 0.87057(17) 0.27256(18) 0.47726(14) 0.0266(5) Uani 1 1 d . . . O11 O 0.97723(16) 0.32847(17) 0.34631(14) 0.0249(5) Uani 1 1 d . . . O12 O 1.0503(2) 0.2471(2) 0.20915(16) 0.0279(6) Uani 1 1 d . . . H12A H 1.104(3) 0.263(3) 0.210(3) 0.061(16) Uiso 1 1 d . . . H12B H 1.076(3) 0.172(3) 0.215(3) 0.064(14) Uiso 1 1 d . . . O13 O 1.2070(2) 0.3431(2) 0.20141(17) 0.0390(7) Uani 1 1 d . . . H13A H 1.2036 0.3937 0.2409 0.059 Uiso 1 1 d R . . H13B H 1.277(4) 0.313(4) 0.185(4) 0.13(2) Uiso 1 1 d . . . O14 O 1.1930(2) -0.3668(3) 0.19417(18) 0.0738(10) Uani 1 1 d . . . O15 O 1.2106(2) -0.3925(2) 0.34579(17) 0.0567(8) Uani 1 1 d . . . O16 O 1.04940(19) -0.3975(2) 0.30745(19) 0.0556(8) Uani 1 1 d . . . O17 O 1.2006(2) -0.5411(2) 0.3138(2) 0.0646(9) Uani 1 1 d . . . O18 O 0.6348(2) -0.1910(2) -0.00472(16) 0.0481(7) Uani 1 1 d . . . O19 O 0.4739(2) -0.1421(2) -0.07198(17) 0.0553(8) Uani 1 1 d . . . O20 O 0.6304(2) -0.1153(2) -0.16695(17) 0.0546(8) Uani 1 1 d . . . O21 O 0.6084(2) -0.2942(2) -0.08171(16) 0.0464(7) Uani 1 1 d . . . N1 N 0.65985(18) 0.5170(2) 0.38602(16) 0.0181(6) Uani 1 1 d . . . N2 N 0.52764(19) 0.4709(2) 0.31322(17) 0.0189(6) Uani 1 1 d . . . N3 N 0.5556(2) 0.1979(2) 0.65703(17) 0.0233(6) Uani 1 1 d . . . N4 N 0.4125(2) 0.1433(2) 0.60427(18) 0.0251(6) Uani 1 1 d . . . N5 N 0.91782(19) 0.4545(2) 0.16297(17) 0.0215(6) Uani 1 1 d . . . N6 N 0.8410(2) 0.3019(2) 0.15991(18) 0.0257(7) Uani 1 1 d . . . C1 C 0.7274(2) 0.5311(3) 0.4307(2) 0.0219(7) Uani 1 1 d . . . H1A H 0.7256 0.4965 0.4966 0.026 Uiso 1 1 calc R . . C2 C 0.7997(2) 0.5946(3) 0.3840(2) 0.0260(8) Uani 1 1 d . . . H2A H 0.8492 0.6013 0.4168 0.031 Uiso 1 1 calc R . . C3 C 0.7992(3) 0.6482(3) 0.2892(2) 0.0282(8) Uani 1 1 d . . . H3A H 0.8459 0.6955 0.2561 0.034 Uiso 1 1 calc R . . C4 C 0.7302(2) 0.6328(3) 0.2423(2) 0.0243(8) Uani 1 1 d . . . H4A H 0.7299 0.6682 0.1765 0.029 Uiso 1 1 calc R . . C5 C 0.6617(2) 0.5650(2) 0.2928(2) 0.0199(7) Uani 1 1 d . . . C6 C 0.5891(2) 0.5362(2) 0.2512(2) 0.0203(7) Uani 1 1 d . . . C7 C 0.5824(3) 0.5714(3) 0.1561(2) 0.0272(8) Uani 1 1 d . . . H7A H 0.6265 0.6170 0.1129 0.033 Uiso 1 1 calc R . . C8 C 0.5114(3) 0.5395(3) 0.1255(2) 0.0326(9) Uani 1 1 d . . . H8A H 0.5069 0.5617 0.0608 0.039 Uiso 1 1 calc R . . C9 C 0.4465(3) 0.4750(3) 0.1890(2) 0.0309(9) Uani 1 1 d . . . H9A H 0.3959 0.4535 0.1688 0.037 Uiso 1 1 calc R . . C10 C 0.4567(2) 0.4424(3) 0.2824(2) 0.0245(8) Uani 1 1 d . . . H10A H 0.4120 0.3983 0.3264 0.029 Uiso 1 1 calc R . . C11 C 0.6344(2) 0.2265(2) 0.6782(2) 0.0243(8) Uani 1 1 d . . . H11A H 0.6853 0.2561 0.6302 0.029 Uiso 1 1 calc R . . C12 C 0.6433(3) 0.2139(3) 0.7674(2) 0.0325(9) Uani 1 1 d . . . H12C H 0.6996 0.2346 0.7809 0.039 Uiso 1 1 calc R . . C13 C 0.5696(3) 0.1709(3) 0.8370(2) 0.0371(9) Uani 1 1 d . . . H13C H 0.5743 0.1623 0.8990 0.044 Uiso 1 1 calc R . . C14 C 0.4894(3) 0.1407(3) 0.8166(2) 0.0331(9) Uani 1 1 d . . . H14A H 0.4386 0.1103 0.8642 0.040 Uiso 1 1 calc R . . C15 C 0.4834(3) 0.1548(3) 0.7260(2) 0.0252(8) Uani 1 1 d . . . C16 C 0.4009(3) 0.1273(3) 0.6949(2) 0.0274(8) Uani 1 1 d . . . C17 C 0.3139(3) 0.0914(3) 0.7523(3) 0.0372(9) Uani 1 1 d . . . H17A H 0.3063 0.0802 0.8162 0.045 Uiso 1 1 calc R . . C18 C 0.2390(3) 0.0726(3) 0.7136(3) 0.0466(11) Uani 1 1 d . . . H18A H 0.1786 0.0488 0.7510 0.056 Uiso 1 1 calc R . . C19 C 0.2517(3) 0.0884(3) 0.6206(3) 0.0405(10) Uani 1 1 d . . . H19A H 0.2009 0.0753 0.5934 0.049 Uiso 1 1 calc R . . C20 C 0.3398(3) 0.1235(3) 0.5685(3) 0.0342(9) Uani 1 1 d . . . H20A H 0.3494 0.1340 0.5046 0.041 Uiso 1 1 calc R . . C21 C 0.7277(3) 0.0228(3) 0.5639(2) 0.0254(8) Uani 1 1 d . . . C22 C 0.7720(3) -0.0956(3) 0.6221(2) 0.0321(9) Uani 1 1 d . . . H22A H 0.7610 -0.1061 0.6879 0.048 Uiso 1 1 calc R . . H22B H 0.8483 -0.1158 0.6049 0.048 Uiso 1 1 calc R . . H22C H 0.7355 -0.1421 0.6116 0.048 Uiso 1 1 calc R . . C23 C 0.5723(3) 0.1741(3) 0.3592(2) 0.0239(8) Uani 1 1 d . . . C24 C 0.5234(3) 0.1560(3) 0.2900(2) 0.0316(9) Uani 1 1 d . . . H24A H 0.5797 0.1332 0.2472 0.047 Uiso 1 1 calc R . . H24B H 0.4748 0.2246 0.2547 0.047 Uiso 1 1 calc R . . H24C H 0.4838 0.0986 0.3228 0.047 Uiso 1 1 calc R . . C25 C 0.9487(3) 0.3102(3) 0.4334(2) 0.0255(8) Uani 1 1 d . . . C26 C 1.0168(3) 0.3385(3) 0.4816(2) 0.0353(9) Uani 1 1 d . . . H26A H 0.9738 0.3585 0.5322 0.053 Uiso 1 1 calc R . . H26B H 1.0457 0.4008 0.4371 0.053 Uiso 1 1 calc R . . H26C H 1.0755 0.2748 0.5071 0.053 Uiso 1 1 calc R . . C27 C 0.9675(2) 0.5235(3) 0.1692(2) 0.0259(8) Uani 1 1 d . . . H27A H 1.0032 0.5018 0.2234 0.031 Uiso 1 1 calc R . . C28 C 0.9685(3) 0.6253(3) 0.0994(2) 0.0313(9) Uani 1 1 d . . . H28A H 1.0042 0.6730 0.1053 0.038 Uiso 1 1 calc R . . C29 C 0.9173(3) 0.6561(3) 0.0217(2) 0.0328(9) Uani 1 1 d . . . H29A H 0.9157 0.7264 -0.0267 0.039 Uiso 1 1 calc R . . C30 C 0.8677(3) 0.5844(3) 0.0138(2) 0.0311(9) Uani 1 1 d . . . H30A H 0.8323 0.6047 -0.0402 0.037 Uiso 1 1 calc R . . C31 C 0.8700(2) 0.4830(3) 0.0850(2) 0.0240(8) Uani 1 1 d . . . C32 C 0.8253(2) 0.3975(3) 0.0833(2) 0.0260(8) Uani 1 1 d . . . C33 C 0.7742(3) 0.4072(3) 0.0104(2) 0.0354(9) Uani 1 1 d . . . H33A H 0.7641 0.4737 -0.0430 0.043 Uiso 1 1 calc R . . C34 C 0.7378(3) 0.3197(3) 0.0157(2) 0.0402(10) Uani 1 1 d . . . H34A H 0.7027 0.3257 -0.0341 0.048 Uiso 1 1 calc R . . C35 C 0.7528(3) 0.2242(3) 0.0931(2) 0.0397(10) Uani 1 1 d . . . H35A H 0.7277 0.1636 0.0979 0.048 Uiso 1 1 calc R . . C36 C 0.8051(3) 0.2173(3) 0.1644(2) 0.0314(9) Uani 1 1 d . . . H36A H 0.8159 0.1510 0.2180 0.038 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 0.0147(3) 0.0193(3) 0.0198(3) -0.0080(2) -0.0005(2) -0.0017(2) Mn2 0.0182(3) 0.0202(3) 0.0229(3) -0.0079(2) -0.0003(2) -0.0033(2) Mn3 0.0171(3) 0.0204(3) 0.0210(3) -0.0074(2) -0.0008(2) -0.0010(2) Mn4 0.0194(3) 0.0260(3) 0.0205(3) -0.0094(2) -0.0001(2) -0.0023(2) Cl1 0.0311(6) 0.0688(8) 0.0396(6) -0.0302(6) 0.0027(4) -0.0190(5) Cl2 0.0392(6) 0.0445(6) 0.0260(5) -0.0154(5) 0.0003(4) -0.0040(5) O1 0.0158(11) 0.0191(12) 0.0190(12) -0.0065(10) -0.0020(9) -0.0014(9) O2 0.0164(12) 0.0200(13) 0.0260(12) -0.0087(10) -0.0016(9) -0.0037(10) O3 0.0164(12) 0.0213(12) 0.0184(11) -0.0072(10) -0.0013(9) 0.0001(9) O4 0.0238(13) 0.0187(13) 0.0280(13) -0.0073(11) -0.0008(10) -0.0025(10) O5 0.0198(12) 0.0280(14) 0.0308(13) -0.0149(11) -0.0016(10) -0.0029(10) O6 0.0231(13) 0.0235(13) 0.0264(13) -0.0040(11) -0.0001(10) -0.0046(11) O7 0.0220(12) 0.0235(13) 0.0233(12) -0.0085(10) 0.0004(10) -0.0030(10) O8 0.0175(12) 0.0220(13) 0.0224(12) -0.0086(10) -0.0011(9) -0.0009(10) O9 0.0234(13) 0.0318(14) 0.0305(13) -0.0162(11) 0.0002(11) -0.0077(11) O10 0.0241(13) 0.0321(14) 0.0243(13) -0.0115(11) -0.0005(10) -0.0075(11) O11 0.0187(12) 0.0356(15) 0.0217(13) -0.0129(11) -0.0008(10) -0.0057(11) O12 0.0220(15) 0.0309(17) 0.0274(14) -0.0113(12) 0.0007(11) -0.0029(13) O13 0.0333(16) 0.0416(17) 0.0428(16) -0.0178(14) 0.0029(13) -0.0108(13) O14 0.064(2) 0.124(3) 0.0291(16) -0.0264(18) 0.0024(15) -0.023(2) O15 0.064(2) 0.085(2) 0.0409(16) -0.0254(16) -0.0130(14) -0.0387(17) O16 0.0256(15) 0.090(2) 0.071(2) -0.0534(18) 0.0078(14) -0.0157(15) O17 0.0498(19) 0.063(2) 0.092(2) -0.0437(19) 0.0098(17) -0.0168(16) O18 0.0527(18) 0.063(2) 0.0336(15) -0.0230(14) -0.0093(13) -0.0100(15) O19 0.0337(16) 0.082(2) 0.0499(17) -0.0380(17) -0.0022(13) 0.0054(15) O20 0.071(2) 0.0556(19) 0.0321(15) -0.0132(14) 0.0090(14) -0.0212(16) O21 0.0579(18) 0.0360(17) 0.0415(16) -0.0142(13) -0.0063(14) -0.0048(14) N1 0.0143(14) 0.0200(15) 0.0192(15) -0.0098(12) 0.0004(11) -0.0006(12) N2 0.0152(14) 0.0179(15) 0.0228(15) -0.0087(12) -0.0007(12) -0.0016(12) N3 0.0222(16) 0.0186(15) 0.0233(15) -0.0073(13) 0.0011(12) 0.0011(12) N4 0.0220(16) 0.0198(16) 0.0299(17) -0.0081(13) 0.0020(13) -0.0042(13) N5 0.0161(14) 0.0260(16) 0.0200(15) -0.0096(13) 0.0015(12) -0.0022(12) N6 0.0213(16) 0.0333(18) 0.0211(15) -0.0112(14) 0.0029(12) -0.0059(13) C1 0.0181(18) 0.0245(19) 0.0244(18) -0.0138(16) 0.0011(15) -0.0018(15) C2 0.0129(17) 0.034(2) 0.037(2) -0.0205(18) 0.0004(15) -0.0056(16) C3 0.0222(19) 0.025(2) 0.037(2) -0.0129(17) 0.0047(16) -0.0079(16) C4 0.0222(19) 0.0211(19) 0.0251(19) -0.0079(16) 0.0003(15) -0.0013(15) C5 0.0147(17) 0.0186(18) 0.0249(19) -0.0117(15) -0.0011(14) 0.0032(14) C6 0.0198(18) 0.0176(18) 0.0228(18) -0.0096(15) -0.0003(14) -0.0014(14) C7 0.0234(19) 0.028(2) 0.0233(19) -0.0054(16) 0.0014(15) -0.0054(16) C8 0.033(2) 0.041(2) 0.0223(19) -0.0128(18) -0.0085(16) -0.0018(18) C9 0.024(2) 0.038(2) 0.033(2) -0.0139(18) -0.0082(16) -0.0057(17) C10 0.0190(18) 0.026(2) 0.0262(19) -0.0084(16) -0.0027(15) -0.0033(15) C11 0.0236(19) 0.0209(19) 0.0253(19) -0.0079(16) -0.0032(15) -0.0014(15) C12 0.035(2) 0.038(2) 0.027(2) -0.0145(18) -0.0026(17) -0.0090(18) C13 0.049(3) 0.036(2) 0.023(2) -0.0111(18) -0.0048(18) -0.006(2) C14 0.036(2) 0.026(2) 0.028(2) -0.0079(17) 0.0067(17) -0.0024(17) C15 0.0258(19) 0.0178(19) 0.0238(19) -0.0061(15) 0.0045(15) 0.0002(15) C16 0.0230(19) 0.0140(18) 0.037(2) -0.0064(16) 0.0057(16) -0.0020(15) C17 0.042(2) 0.026(2) 0.039(2) -0.0106(18) 0.0100(19) -0.0119(18) C18 0.036(2) 0.030(2) 0.069(3) -0.019(2) 0.018(2) -0.0140(19) C19 0.032(2) 0.030(2) 0.058(3) -0.014(2) -0.002(2) -0.0105(18) C20 0.027(2) 0.030(2) 0.044(2) -0.0110(18) -0.0021(18) -0.0090(17) C21 0.029(2) 0.025(2) 0.0178(18) -0.0062(16) -0.0098(16) 0.0019(17) C22 0.030(2) 0.026(2) 0.033(2) -0.0026(17) -0.0056(17) -0.0070(17) C23 0.026(2) 0.0183(19) 0.0249(19) -0.0056(15) -0.0033(16) -0.0055(15) C24 0.029(2) 0.038(2) 0.035(2) -0.0214(18) -0.0046(16) -0.0045(17) C25 0.0224(19) 0.023(2) 0.026(2) -0.0077(16) -0.0047(16) 0.0014(16) C26 0.031(2) 0.046(3) 0.034(2) -0.0165(19) -0.0041(17) -0.0119(19) C27 0.0194(18) 0.029(2) 0.0275(19) -0.0133(17) 0.0026(15) -0.0025(16) C28 0.031(2) 0.029(2) 0.031(2) -0.0084(17) 0.0025(17) -0.0097(17) C29 0.033(2) 0.030(2) 0.026(2) -0.0065(17) 0.0064(17) -0.0065(17) C30 0.026(2) 0.035(2) 0.0230(19) -0.0057(17) -0.0012(16) -0.0029(17) C31 0.0171(18) 0.028(2) 0.0221(19) -0.0087(16) -0.0012(15) 0.0008(15) C32 0.0164(18) 0.041(2) 0.0197(18) -0.0132(17) 0.0029(14) -0.0055(16) C33 0.029(2) 0.044(3) 0.027(2) -0.0093(18) -0.0032(17) -0.0056(18) C34 0.037(2) 0.063(3) 0.029(2) -0.019(2) -0.0044(18) -0.020(2) C35 0.044(2) 0.051(3) 0.034(2) -0.018(2) 0.0020(19) -0.026(2) C36 0.034(2) 0.037(2) 0.028(2) -0.0150(18) 0.0021(17) -0.0124(18) _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 1.7974(19) . ? Mn1 O1 1.811(2) 2_666 ? Mn1 O2 1.844(2) . ? Mn1 O3 1.981(2) . ? Mn1 N1 2.049(2) . ? Mn1 N2 2.073(2) . ? Mn1 Mn1 2.7126(9) 2_666 ? Mn1 Mn2 2.7900(7) . ? Mn2 O2 1.769(2) . ? Mn2 O3 1.816(2) . ? Mn2 O5 1.904(2) . ? Mn2 O4 2.008(2) . ? Mn2 N3 2.026(3) . ? Mn2 N4 2.060(3) . ? Mn3 O8 1.857(2) . ? Mn3 O7 1.873(2) . ? Mn3 O3 1.946(2) . ? Mn3 O6 1.981(2) . ? Mn3 O9 2.203(2) . ? Mn3 O10 2.211(2) . ? Mn3 Mn4 2.6746(7) . ? Mn4 O8 1.764(2) . ? Mn4 O7 1.775(2) . ? Mn4 O11 1.907(2) . ? Mn4 N6 2.024(3) . ? Mn4 O12 2.034(2) . ? Mn4 N5 2.068(3) . ? Cl1 O14 1.420(3) . ? Cl1 O15 1.420(2) . ? Cl1 O16 1.438(2) . ? Cl1 O17 1.457(3) . ? Cl2 O19 1.429(3) . ? Cl2 O20 1.430(2) . ? Cl2 O18 1.438(2) . ? Cl2 O21 1.442(3) . ? O1 Mn1 1.811(2) 2_666 ? O4 C21 1.266(4) . ? O5 C23 1.282(4) . ? O6 C21 1.270(4) . ? O9 C23 1.242(4) . ? O10 C25 1.245(4) . ? O11 C25 1.296(4) . ? O12 H12A 0.80(4) . ? O12 H12B 0.96(4) . ? O13 H13A 1.0974 . ? O13 H13B 0.93(5) . ? N1 C1 1.332(4) . ? N1 C5 1.345(4) . ? N2 C10 1.340(4) . ? N2 C6 1.346(4) . ? N3 C11 1.346(4) . ? N3 C15 1.360(4) . ? N4 C20 1.337(4) . ? N4 C16 1.345(4) . ? N5 C27 1.339(4) . ? N5 C31 1.350(4) . ? N6 C36 1.344(4) . ? N6 C32 1.364(4) . ? C1 C2 1.376(4) . ? C1 H1A 0.9500 . ? C2 C3 1.372(4) . ? C2 H2A 0.9500 . ? C3 C4 1.382(4) . ? C3 H3A 0.9500 . ? C4 C5 1.384(4) . ? C4 H4A 0.9500 . ? C5 C6 1.473(4) . ? C6 C7 1.392(4) . ? C7 C8 1.370(4) . ? C7 H7A 0.9500 . ? C8 C9 1.379(4) . ? C8 H8A 0.9500 . ? C9 C10 1.379(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.374(4) . ? C11 H11A 0.9500 . ? C12 C13 1.377(5) . ? C12 H12C 0.9500 . ? C13 C14 1.371(5) . ? C13 H13C 0.9500 . ? C14 C15 1.380(4) . ? C14 H14A 0.9500 . ? C15 C16 1.466(4) . ? C16 C17 1.394(4) . ? C17 C18 1.384(5) . ? C17 H17A 0.9500 . ? C18 C19 1.381(5) . ? C18 H18A 0.9500 . ? C19 C20 1.375(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.500(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.503(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.495(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.380(4) . ? C27 H27A 0.9500 . ? C28 C29 1.365(4) . ? C28 H28A 0.9500 . ? C29 C30 1.383(4) . ? C29 H29A 0.9500 . ? C30 C31 1.379(4) . ? C30 H30A 0.9500 . ? C31 C32 1.466(4) . ? C32 C33 1.383(4) . ? C33 C34 1.382(5) . ? C33 H33A 0.9500 . ? C34 C35 1.369(5) . ? C34 H34A 0.9500 . ? C35 C36 1.386(4) . ? C35 H35A 0.9500 . ? C36 H36A 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 82.51(9) . 2_666 ? O1 Mn1 O2 97.56(9) . . ? O1 Mn1 O2 95.06(9) 2_666 . ? O1 Mn1 O3 96.92(8) . . ? O1 Mn1 O3 173.55(9) 2_666 . ? O2 Mn1 O3 78.62(8) . . ? O1 Mn1 N1 90.51(9) . . ? O1 Mn1 N1 92.82(9) 2_666 . ? O2 Mn1 N1 169.38(9) . . ? O3 Mn1 N1 93.61(9) . . ? O1 Mn1 N2 164.16(10) . . ? O1 Mn1 N2 87.13(9) 2_666 . ? O2 Mn1 N2 95.26(9) . . ? O3 Mn1 N2 94.70(9) . . ? N1 Mn1 N2 78.02(10) . . ? O1 Mn1 Mn1 41.44(6) . 2_666 ? O1 Mn1 Mn1 41.07(6) 2_666 2_666 ? O2 Mn1 Mn1 98.40(7) . 2_666 ? O3 Mn1 Mn1 138.00(6) . 2_666 ? N1 Mn1 Mn1 92.22(7) . 2_666 ? N2 Mn1 Mn1 127.16(7) . 2_666 ? O1 Mn1 Mn2 95.63(7) . . ? O1 Mn1 Mn2 133.13(7) 2_666 . ? O2 Mn1 Mn2 38.47(6) . . ? O3 Mn1 Mn2 40.45(6) . . ? N1 Mn1 Mn2 134.04(7) . . ? N2 Mn1 Mn2 100.20(7) . . ? Mn1 Mn1 Mn2 121.42(3) 2_666 . ? O2 Mn2 O3 85.16(9) . . ? O2 Mn2 O5 91.49(9) . . ? O3 Mn2 O5 98.97(9) . . ? O2 Mn2 O4 175.31(9) . . ? O3 Mn2 O4 99.52(9) . . ? O5 Mn2 O4 87.98(9) . . ? O2 Mn2 N3 95.11(10) . . ? O3 Mn2 N3 93.96(10) . . ? O5 Mn2 N3 165.93(10) . . ? O4 Mn2 N3 84.43(9) . . ? O2 Mn2 N4 88.92(10) . . ? O3 Mn2 N4 170.14(10) . . ? O5 Mn2 N4 89.04(10) . . ? O4 Mn2 N4 86.41(9) . . ? N3 Mn2 N4 78.70(11) . . ? O2 Mn2 Mn1 40.44(6) . . ? O3 Mn2 Mn1 45.06(6) . . ? O5 Mn2 Mn1 101.04(7) . . ? O4 Mn2 Mn1 144.19(6) . . ? N3 Mn2 Mn1 92.00(7) . . ? N4 Mn2 Mn1 127.87(7) . . ? O8 Mn3 O7 81.27(9) . . ? O8 Mn3 O3 96.35(9) . . ? O7 Mn3 O3 177.12(9) . . ? O8 Mn3 O6 168.35(9) . . ? O7 Mn3 O6 89.31(9) . . ? O3 Mn3 O6 93.24(9) . . ? O8 Mn3 O9 96.79(8) . . ? O7 Mn3 O9 90.17(8) . . ? O3 Mn3 O9 88.49(8) . . ? O6 Mn3 O9 90.04(9) . . ? O8 Mn3 O10 86.82(8) . . ? O7 Mn3 O10 89.75(8) . . ? O3 Mn3 O10 91.74(8) . . ? O6 Mn3 O10 86.30(9) . . ? O9 Mn3 O10 176.34(8) . . ? O8 Mn3 Mn4 41.05(6) . . ? O7 Mn3 Mn4 41.45(6) . . ? O3 Mn3 Mn4 136.52(6) . . ? O6 Mn3 Mn4 128.16(7) . . ? O9 Mn3 Mn4 102.38(6) . . ? O10 Mn3 Mn4 79.93(6) . . ? O8 Mn4 O7 86.69(9) . . ? O8 Mn4 O11 94.86(9) . . ? O7 Mn4 O11 95.38(9) . . ? O8 Mn4 N6 89.39(10) . . ? O7 Mn4 N6 95.60(10) . . ? O11 Mn4 N6 168.43(10) . . ? O8 Mn4 O12 176.70(10) . . ? O7 Mn4 O12 94.75(10) . . ? O11 Mn4 O12 87.96(10) . . ? N6 Mn4 O12 87.52(10) . . ? O8 Mn4 N5 93.98(10) . . ? O7 Mn4 N5 174.20(10) . . ? O11 Mn4 N5 90.31(10) . . ? N6 Mn4 N5 78.65(11) . . ? O12 Mn4 N5 84.29(10) . . ? O8 Mn4 Mn3 43.75(7) . . ? O7 Mn4 Mn3 44.30(7) . . ? O11 Mn4 Mn3 88.45(6) . . ? N6 Mn4 Mn3 101.98(7) . . ? O12 Mn4 Mn3 138.24(8) . . ? N5 Mn4 Mn3 137.33(7) . . ? O14 Cl1 O15 109.90(17) . . ? O14 Cl1 O16 110.79(18) . . ? O15 Cl1 O16 109.71(17) . . ? O14 Cl1 O17 109.37(19) . . ? O15 Cl1 O17 108.70(17) . . ? O16 Cl1 O17 108.33(17) . . ? O19 Cl2 O20 109.55(17) . . ? O19 Cl2 O18 109.63(16) . . ? O20 Cl2 O18 109.69(16) . . ? O19 Cl2 O21 110.35(17) . . ? O20 Cl2 O21 108.90(16) . . ? O18 Cl2 O21 108.70(16) . . ? Mn1 O1 Mn1 97.49(9) . 2_666 ? Mn2 O2 Mn1 101.09(10) . . ? Mn2 O3 Mn3 120.99(11) . . ? Mn2 O3 Mn1 94.50(9) . . ? Mn3 O3 Mn1 137.34(11) . . ? C21 O4 Mn2 130.4(2) . . ? C23 O5 Mn2 126.8(2) . . ? C21 O6 Mn3 129.6(2) . . ? Mn4 O7 Mn3 94.25(10) . . ? Mn4 O8 Mn3 95.20(9) . . ? C23 O9 Mn3 133.5(2) . . ? C25 O10 Mn3 121.3(2) . . ? C25 O11 Mn4 125.3(2) . . ? Mn4 O12 H12A 124(3) . . ? Mn4 O12 H12B 123(2) . . ? H12A O12 H12B 102(3) . . ? H13A O13 H13B 111.2 . . ? C1 N1 C5 119.9(3) . . ? C1 N1 Mn1 123.6(2) . . ? C5 N1 Mn1 116.3(2) . . ? C10 N2 C6 119.2(3) . . ? C10 N2 Mn1 125.0(2) . . ? C6 N2 Mn1 115.64(19) . . ? C11 N3 C15 118.9(3) . . ? C11 N3 Mn2 124.5(2) . . ? C15 N3 Mn2 116.5(2) . . ? C20 N4 C16 119.5(3) . . ? C20 N4 Mn2 124.7(2) . . ? C16 N4 Mn2 115.5(2) . . ? C27 N5 C31 119.5(3) . . ? C27 N5 Mn4 125.2(2) . . ? C31 N5 Mn4 115.3(2) . . ? C36 N6 C32 119.3(3) . . ? C36 N6 Mn4 124.2(2) . . ? C32 N6 Mn4 116.2(2) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 124.4(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 114.6(3) . . ? C7 C6 C5 124.3(3) . . ? C8 C7 C6 119.1(3) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C7 C8 C9 119.8(3) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C8 C9 C10 118.5(3) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 120.7 . . ? N2 C10 C9 122.2(3) . . ? N2 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? N3 C11 C12 121.8(3) . . ? N3 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C13 119.1(3) . . ? C11 C12 H12C 120.4 . . ? C13 C12 H12C 120.4 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13C 120.2 . . ? C12 C13 H13C 120.2 . . ? C13 C14 C15 119.3(3) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? N3 C15 C14 121.2(3) . . ? N3 C15 C16 114.2(3) . . ? C14 C15 C16 124.6(3) . . ? N4 C16 C17 121.3(3) . . ? N4 C16 C15 114.8(3) . . ? C17 C16 C15 123.8(3) . . ? C18 C17 C16 118.2(3) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 118.2(4) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? N4 C20 C19 122.5(4) . . ? N4 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? O4 C21 O6 124.5(3) . . ? O4 C21 C22 117.5(3) . . ? O6 C21 C22 118.0(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 C23 O5 125.6(3) . . ? O9 C23 C24 120.5(3) . . ? O5 C23 C24 113.9(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O10 C25 O11 125.0(3) . . ? O10 C25 C26 119.6(3) . . ? O11 C25 C26 115.4(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 122.0(3) . . ? N5 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C29 C28 C27 118.8(3) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? C28 C29 C30 119.6(3) . . ? C28 C29 H29A 120.2 . . ? C30 C29 H29A 120.2 . . ? C31 C30 C29 119.4(3) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? N5 C31 C30 120.6(3) . . ? N5 C31 C32 114.5(3) . . ? C30 C31 C32 124.8(3) . . ? N6 C32 C33 120.5(3) . . ? N6 C32 C31 114.5(3) . . ? C33 C32 C31 124.9(3) . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 119.0(3) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? N6 C36 C35 121.9(3) . . ? N6 C36 H36A 119.1 . . ? C35 C36 H36A 119.1 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.472 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.079