Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Keith Murray' _publ_contact_author_address ; School of Chemistry Monash University Wellington Road Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email K.S.MURRAY@SCI.MONASH.EDU.AU _publ_section_title ; The role of diisopropanolamine (dipaH3) in cluster dimerisation and polymerisation: from spin frustrated S = 5 FeIII6 clusters to the novel 1-D covalent polymer of mixed valence [CoII3CoIII] tetramers ; loop_ _publ_author_name 'Keith Murray' 'Kevin J. Berry' 'John D. Cashion' 'Paul Jensen' 'Leigh F. Jones' 'Boujemaa Moubaraki' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 267210' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe6O2(OH)2(benz)10(dipaH2)2).5.5MeCN.H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H96.50 Fe6 N7.50 O29' _chemical_formula_weight 2118.38 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.2496(2) _cell_length_b 14.3706(2) _cell_length_c 23.8310(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.3780(10) _cell_angle_gamma 90.00 _cell_volume 4727.15(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plate' _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2190 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52860 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11600 _reflns_number_gt 8431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSEED _computing_publication_material XSEED _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^)+(0.1010P)^2^+0.4091P] 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 11600 _refine_ls_number_parameters 602 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _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 Fe1 Fe 0.25467(3) 0.57313(2) 0.123635(16) 0.02405(11) Uani 1 1 d . . . Fe2 Fe 0.12641(3) 0.42475(2) 0.065218(16) 0.02631(11) Uani 1 1 d D . . Fe3 Fe -0.08083(3) 0.33435(3) -0.025399(16) 0.02744(12) Uani 1 1 d D . . O1 O 0.14952(14) 0.55869(12) 0.05667(8) 0.0271(4) Uani 1 1 d . . . O2 O 0.04507(14) 0.40027(12) -0.01177(8) 0.0280(4) Uani 1 1 d D . . O3 O -0.06091(13) 0.28707(12) -0.10433(8) 0.0299(4) Uani 1 1 d . . . O4 O -0.18097(13) 0.35427(13) -0.17108(8) 0.0301(4) Uani 1 1 d . . . O5 O -0.31652(14) 0.30779(13) -0.10853(8) 0.0339(4) Uani 1 1 d . . . O6 O -0.19809(14) 0.24570(13) -0.03840(8) 0.0334(4) Uani 1 1 d . . . O7 O -0.00218(15) 0.22189(12) 0.01286(8) 0.0350(5) Uani 1 1 d . . . O8 O 0.11270(14) 0.28890(12) 0.08367(8) 0.0320(4) Uani 1 1 d . . . O9 O -0.10774(14) 0.35450(13) 0.05519(8) 0.0331(4) Uani 1 1 d . . . O10 O 0.00627(14) 0.45882(12) 0.09461(8) 0.0293(4) Uani 1 1 d . . . O11 O 0.20435(13) 0.45260(12) 0.14483(7) 0.0273(4) Uani 1 1 d . B . O12 O 0.34827(14) 0.50512(13) 0.08637(8) 0.0321(4) Uani 1 1 d . . . O13 O 0.25324(14) 0.38787(13) 0.04382(8) 0.0334(4) Uani 1 1 d . . . N1 N 0.36345(16) 0.54101(16) 0.20284(10) 0.0304(5) Uani 1 1 d . . . H1 H 0.4129 0.5095 0.1917 0.036 Uiso 1 1 calc R A 1 C1 C 0.3345(2) 0.42834(19) 0.05990(11) 0.0303(6) Uani 1 1 d . . . C2 C 0.4218(2) 0.3832(2) 0.04824(11) 0.0327(6) Uani 1 1 d . . . C3 C 0.5078(2) 0.4337(2) 0.05769(13) 0.0387(7) Uani 1 1 d . . . H3 H 0.5092 0.4963 0.0707 0.046 Uiso 1 1 calc R . . C4 C 0.5913(3) 0.3941(2) 0.04844(15) 0.0462(8) Uani 1 1 d . . . H4 H 0.6494 0.4293 0.0544 0.055 Uiso 1 1 calc R . . C5 C 0.5887(3) 0.3022(3) 0.03027(14) 0.0508(9) Uani 1 1 d . . . H5 H 0.6459 0.2738 0.0247 0.061 Uiso 1 1 calc R . . C6 C 0.5045(3) 0.2522(3) 0.02039(15) 0.0545(10) Uani 1 1 d . . . H6 H 0.5035 0.1898 0.0071 0.065 Uiso 1 1 calc R . . C7 C 0.4198(3) 0.2917(2) 0.02961(13) 0.0434(7) Uani 1 1 d . . . H7 H 0.3618 0.2563 0.0232 0.052 Uiso 1 1 calc R . . C8 C -0.10311(18) 0.30858(17) -0.15573(11) 0.0250(5) Uani 1 1 d . . . C9 C -0.06015(19) 0.27623(19) -0.20397(11) 0.0287(6) Uani 1 1 d . . . C10 C 0.0096(2) 0.2057(2) -0.19494(14) 0.0389(7) Uani 1 1 d . . . H10 H 0.0315 0.1782 -0.1578 0.047 Uiso 1 1 calc R . . C11 C 0.0465(3) 0.1764(3) -0.24034(15) 0.0517(9) Uani 1 1 d . . . H11 H 0.0925 0.1273 -0.2346 0.062 Uiso 1 1 calc R . . C12 C 0.0165(2) 0.2185(3) -0.29460(15) 0.0540(9) Uani 1 1 d . . . H12 H 0.0427 0.1983 -0.3255 0.065 Uiso 1 1 calc R . . C13 C -0.0509(2) 0.2892(3) -0.30340(14) 0.0431(8) Uani 1 1 d . . . H13 H -0.0705 0.3188 -0.3401 0.052 Uiso 1 1 calc R . . C14 C -0.0899(2) 0.3168(2) -0.25808(12) 0.0336(6) Uani 1 1 d . . . H14 H -0.1377 0.3643 -0.2644 0.040 Uiso 1 1 calc R . . C15 C -0.2811(2) 0.24389(18) -0.07219(12) 0.0302(6) Uani 1 1 d . . . C16 C -0.3433(2) 0.16099(19) -0.07081(12) 0.0337(6) Uani 1 1 d . . . C17 C -0.4323(2) 0.1528(2) -0.11004(16) 0.0518(9) Uani 1 1 d . . . H17 H -0.4547 0.2004 -0.1378 0.062 Uiso 1 1 calc R . . C18 C -0.4891(3) 0.0744(3) -0.1087(2) 0.0687(12) Uani 1 1 d . . . H18 H -0.5494 0.0679 -0.1364 0.082 Uiso 1 1 calc R . . C19 C -0.4597(3) 0.0080(3) -0.06869(18) 0.0619(11) Uani 1 1 d . . . H19 H -0.4999 -0.0444 -0.0678 0.074 Uiso 1 1 calc R . . C20 C -0.3729(3) 0.0153(2) -0.02955(17) 0.0559(9) Uani 1 1 d . . . H20 H -0.3526 -0.0321 -0.0013 0.067 Uiso 1 1 calc R . . C21 C -0.3137(2) 0.0913(2) -0.03046(14) 0.0419(7) Uani 1 1 d . . . H21 H -0.2526 0.0955 -0.0032 0.050 Uiso 1 1 calc R . . C22 C -0.06902(19) 0.41035(18) 0.09459(11) 0.0285(6) Uani 1 1 d . . . C23 C -0.1124(2) 0.4241(2) 0.14456(13) 0.0340(6) Uani 1 1 d . . . C24 C -0.1931(2) 0.3729(3) 0.14937(15) 0.0493(8) Uani 1 1 d . . . H24 H -0.2202 0.3282 0.1205 0.059 Uiso 1 1 calc R . . C25 C -0.2341(3) 0.3862(4) 0.19509(19) 0.0805(15) Uani 1 1 d . . . H25 H -0.2883 0.3500 0.1984 0.097 Uiso 1 1 calc R . . C26 C -0.1957(3) 0.4525(4) 0.2362(2) 0.0864(16) Uani 1 1 d . . . H26 H -0.2255 0.4640 0.2671 0.104 Uiso 1 1 calc R . . C27 C -0.1146(3) 0.5023(4) 0.23302(19) 0.0778(14) Uani 1 1 d . . . H27 H -0.0879 0.5469 0.2621 0.093 Uiso 1 1 calc R . . C28 C -0.0723(3) 0.4877(3) 0.18784(14) 0.0494(8) Uani 1 1 d . . . H28 H -0.0155 0.5211 0.1862 0.059 Uiso 1 1 calc R . . C29 C 0.0686(2) 0.21939(18) 0.05669(11) 0.0305(6) Uani 1 1 d . . . C30 C 0.1033(2) 0.12520(18) 0.07965(11) 0.0289(6) Uani 1 1 d . . . C31 C 0.1974(2) 0.11372(19) 0.11334(12) 0.0324(6) Uani 1 1 d . . . H31 H 0.2387 0.1662 0.1232 0.039 Uiso 1 1 calc R . . C32 C 0.2307(2) 0.0262(2) 0.13240(12) 0.0363(7) Uani 1 1 d . . . H32 H 0.2956 0.0179 0.1544 0.044 Uiso 1 1 calc R . . C33 C 0.1686(3) -0.04949(19) 0.11906(12) 0.0389(7) Uani 1 1 d . . . H33 H 0.1909 -0.1095 0.1330 0.047 Uiso 1 1 calc R . . C34 C 0.0754(2) -0.03922(19) 0.08611(12) 0.0367(7) Uani 1 1 d . . . H34 H 0.0337 -0.0916 0.0772 0.044 Uiso 1 1 calc R . . C35 C 0.0428(2) 0.04876(19) 0.06596(12) 0.0338(6) Uani 1 1 d . . . H35 H -0.0212 0.0564 0.0427 0.041 Uiso 1 1 calc R . . C36 C 0.1971(2) 0.3437(2) 0.22115(14) 0.0443(8) Uani 1 1 d . B . H36A H 0.1511 0.3842 0.2339 0.066 Uiso 1 1 calc R . . H36B H 0.2376 0.3113 0.2547 0.066 Uiso 1 1 calc R . . H36C H 0.1614 0.2979 0.1934 0.066 Uiso 1 1 calc R . . C37 C 0.2607(2) 0.4019(2) 0.19234(12) 0.0350(7) Uani 1 1 d . . . H37 H 0.3065 0.3603 0.1785 0.042 Uiso 1 1 calc R B . C38 C 0.3181(2) 0.4734(2) 0.23418(12) 0.0351(6) Uani 1 1 d . B . H38A H 0.2744 0.5062 0.2540 0.042 Uiso 1 1 calc R . . H38B H 0.3688 0.4415 0.2639 0.042 Uiso 1 1 calc R . . C39 C 0.4093(2) 0.6190(2) 0.23939(14) 0.0414(7) Uani 0.50 1 d P B 1 H39A H 0.3608 0.6462 0.2580 0.050 Uiso 0.50 1 calc PR B 1 H39B H 0.4258 0.6674 0.2139 0.050 Uiso 0.50 1 calc PR B 1 C40 C 0.4978(4) 0.5980(4) 0.2853(3) 0.0394(15) Uani 0.50 1 d P B 1 H40 H 0.4795 0.5553 0.3140 0.047 Uiso 0.50 1 calc PR B 1 C41 C 0.5427(6) 0.6841(5) 0.3169(3) 0.058(2) Uani 0.50 1 d P B 1 H41A H 0.5931 0.6661 0.3513 0.087 Uiso 0.50 1 calc PR B 1 H41B H 0.4927 0.7205 0.3288 0.087 Uiso 0.50 1 calc PR B 1 H41C H 0.5715 0.7217 0.2912 0.087 Uiso 0.50 1 calc PR B 1 O14 O 0.5626(6) 0.5510(6) 0.2601(3) 0.065(2) Uani 0.50 1 d P B 1 C39' C 0.4093(2) 0.6190(2) 0.23939(14) 0.0414(7) Uani 0.50 1 d P B 2 H39C H 0.4282 0.5999 0.2806 0.050 Uiso 0.50 1 calc PR B 2 H39D H 0.3639 0.6721 0.2354 0.050 Uiso 0.50 1 calc PR B 2 C40' C 0.4980(6) 0.6462(6) 0.2189(4) 0.066(2) Uani 0.50 1 d P B 2 H40' H 0.4783 0.6602 0.1765 0.080 Uiso 0.50 1 calc PR B 2 C41' C 0.5451(9) 0.7349(9) 0.2526(6) 0.119(5) Uani 0.50 1 d P B 2 H41D H 0.5394 0.7317 0.2927 0.179 Uiso 0.50 1 calc PR B 2 H41E H 0.5117 0.7906 0.2339 0.179 Uiso 0.50 1 calc PR B 2 H41F H 0.6137 0.7379 0.2523 0.179 Uiso 0.50 1 calc PR B 2 O14' O 0.5668(5) 0.5673(6) 0.2293(4) 0.068(2) Uani 0.50 1 d P B 2 H2A H 0.0475(19) 0.439(2) -0.0378(8) 0.082 Uiso 1 1 d D . . C42 C 0.2018(7) 0.3180(6) -0.0960(3) 0.111(3) Uani 0.75 1 d PU C 1 H42A H 0.1385 0.3343 -0.1213 0.167 Uiso 0.75 1 calc PR C 1 H42B H 0.2141 0.3563 -0.0609 0.167 Uiso 0.75 1 calc PR C 1 H42C H 0.2021 0.2521 -0.0854 0.167 Uiso 0.75 1 calc PR C 1 C43 C 0.2839(8) 0.3365(9) -0.1293(5) 0.222(6) Uani 0.75 1 d PU C 1 N2 N 0.3399(9) 0.3565(13) -0.1530(8) 0.305(12) Uani 0.75 1 d PU C 1 O15 O 0.1564(11) 0.2610(17) -0.0528(7) 0.135(7) Uani 0.25 1 d P D 2 O16 O 0.2839(8) 0.3365(9) -0.1293(5) 0.222(6) Uani 0.25 1 d P E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0292(2) 0.01666(19) 0.0238(2) -0.00233(14) 0.00199(15) 0.00028(14) Fe2 0.0346(2) 0.01445(19) 0.0250(2) -0.00025(14) -0.00169(16) -0.00109(15) Fe3 0.0383(2) 0.01445(19) 0.0238(2) 0.00004(13) -0.00332(16) -0.00192(15) O1 0.0364(10) 0.0161(8) 0.0253(9) -0.0011(7) 0.0010(8) 0.0010(7) O2 0.0392(10) 0.0154(9) 0.0246(9) 0.0006(7) -0.0010(8) -0.0013(7) O3 0.0369(10) 0.0207(9) 0.0283(10) -0.0021(7) 0.0010(8) 0.0042(8) O4 0.0315(10) 0.0285(10) 0.0271(9) -0.0061(8) 0.0014(8) 0.0064(8) O5 0.0383(11) 0.0237(10) 0.0352(11) 0.0018(8) 0.0006(9) -0.0057(8) O6 0.0428(11) 0.0198(9) 0.0327(10) -0.0008(8) 0.0004(9) -0.0061(8) O7 0.0487(12) 0.0161(9) 0.0304(10) 0.0014(8) -0.0089(9) -0.0010(8) O8 0.0452(11) 0.0147(9) 0.0273(9) 0.0002(7) -0.0073(8) -0.0048(8) O9 0.0424(11) 0.0245(10) 0.0273(10) 0.0021(8) -0.0011(8) -0.0062(8) O10 0.0355(10) 0.0200(9) 0.0297(10) 0.0000(8) 0.0029(8) -0.0027(8) O11 0.0333(10) 0.0210(9) 0.0228(9) 0.0026(7) -0.0017(8) 0.0009(7) O12 0.0372(10) 0.0257(10) 0.0347(10) -0.0064(8) 0.0113(8) 0.0003(8) O13 0.0392(11) 0.0255(10) 0.0329(10) -0.0085(8) 0.0040(8) 0.0032(8) N1 0.0282(12) 0.0301(12) 0.0304(12) -0.0014(10) 0.0027(9) 0.0038(9) C1 0.0427(16) 0.0266(14) 0.0208(13) -0.0003(10) 0.0061(11) 0.0055(12) C2 0.0432(16) 0.0323(15) 0.0218(13) 0.0040(11) 0.0069(11) 0.0118(13) C3 0.0463(17) 0.0347(16) 0.0361(16) 0.0035(12) 0.0121(14) 0.0105(13) C4 0.0467(18) 0.0476(19) 0.0471(18) 0.0069(16) 0.0169(15) 0.0125(16) C5 0.0485(19) 0.059(2) 0.047(2) -0.0010(16) 0.0158(16) 0.0188(17) C6 0.078(3) 0.0403(19) 0.048(2) -0.0059(16) 0.0198(18) 0.0253(18) C7 0.056(2) 0.0384(17) 0.0363(16) -0.0049(13) 0.0135(14) 0.0112(15) C8 0.0281(13) 0.0157(11) 0.0283(13) -0.0035(10) 0.0016(10) -0.0014(10) C9 0.0281(13) 0.0268(14) 0.0299(14) -0.0049(11) 0.0049(11) -0.0036(11) C10 0.0387(16) 0.0377(17) 0.0384(16) -0.0037(13) 0.0060(13) 0.0107(13) C11 0.0480(19) 0.059(2) 0.049(2) -0.0016(17) 0.0155(16) 0.0225(17) C12 0.0405(18) 0.078(3) 0.046(2) -0.0135(18) 0.0169(15) 0.0099(18) C13 0.0341(16) 0.061(2) 0.0326(16) -0.0040(15) 0.0061(13) -0.0042(15) C14 0.0295(14) 0.0376(16) 0.0305(14) -0.0027(12) 0.0014(11) 0.0013(12) C15 0.0405(15) 0.0211(13) 0.0285(14) -0.0049(11) 0.0077(12) -0.0025(11) C16 0.0420(16) 0.0274(14) 0.0317(14) -0.0043(11) 0.0089(12) -0.0079(12) C17 0.0483(19) 0.046(2) 0.055(2) 0.0064(16) 0.0019(16) -0.0188(16) C18 0.065(2) 0.059(3) 0.074(3) 0.002(2) 0.001(2) -0.032(2) C19 0.069(2) 0.050(2) 0.068(3) 0.0002(19) 0.018(2) -0.0336(19) C20 0.079(3) 0.0322(17) 0.062(2) 0.0058(16) 0.027(2) -0.0135(17) C21 0.0524(19) 0.0299(16) 0.0451(18) 0.0022(13) 0.0152(15) -0.0079(14) C22 0.0347(14) 0.0212(13) 0.0235(13) 0.0028(10) -0.0046(11) 0.0019(11) C23 0.0287(14) 0.0359(16) 0.0333(15) 0.0007(12) 0.0000(12) -0.0025(12) C24 0.0325(16) 0.064(2) 0.050(2) -0.0149(17) 0.0075(14) -0.0114(15) C25 0.045(2) 0.135(4) 0.067(3) -0.026(3) 0.024(2) -0.034(3) C26 0.059(3) 0.141(5) 0.070(3) -0.040(3) 0.037(2) -0.028(3) C27 0.082(3) 0.098(4) 0.061(3) -0.040(2) 0.032(2) -0.031(3) C28 0.0474(19) 0.058(2) 0.0436(18) -0.0130(16) 0.0119(15) -0.0160(16) C29 0.0425(16) 0.0175(12) 0.0269(14) 0.0031(10) -0.0002(12) 0.0014(11) C30 0.0446(15) 0.0161(12) 0.0224(12) -0.0006(10) 0.0017(11) -0.0008(11) C31 0.0448(16) 0.0217(13) 0.0279(14) -0.0012(11) 0.0040(12) 0.0004(12) C32 0.0463(17) 0.0293(15) 0.0311(15) 0.0017(12) 0.0053(13) 0.0113(13) C33 0.069(2) 0.0178(13) 0.0295(15) 0.0008(11) 0.0112(14) 0.0103(13) C34 0.062(2) 0.0179(13) 0.0267(14) -0.0019(11) 0.0045(13) -0.0019(13) C35 0.0506(17) 0.0205(13) 0.0245(13) 0.0001(11) -0.0014(12) -0.0014(12) C36 0.0520(19) 0.0394(18) 0.0324(16) 0.0121(13) -0.0067(14) -0.0089(15) C37 0.0411(16) 0.0257(14) 0.0314(15) 0.0048(12) -0.0037(12) 0.0018(12) C38 0.0365(15) 0.0337(16) 0.0303(14) 0.0043(12) -0.0007(12) -0.0004(12) C39 0.0429(17) 0.0351(17) 0.0387(17) -0.0058(13) -0.0044(14) -0.0047(14) C40 0.029(3) 0.040(3) 0.038(3) 0.009(3) -0.013(2) -0.012(3) C41 0.067(5) 0.039(4) 0.048(4) 0.004(3) -0.023(4) -0.013(3) O14 0.045(3) 0.058(4) 0.080(5) 0.002(4) -0.007(4) -0.002(3) C39' 0.0429(17) 0.0351(17) 0.0387(17) -0.0058(13) -0.0044(14) -0.0047(14) C40' 0.058(5) 0.064(5) 0.069(5) 0.010(4) 0.000(4) -0.010(4) C41' 0.123(10) 0.109(10) 0.110(9) -0.003(7) -0.001(8) -0.053(8) O14' 0.036(3) 0.068(5) 0.100(6) 0.016(4) 0.013(4) 0.011(3) C42 0.133(6) 0.114(6) 0.057(4) -0.016(4) -0.032(4) -0.008(5) C43 0.151(7) 0.299(14) 0.173(9) 0.088(9) -0.041(5) -0.079(8) N2 0.145(10) 0.39(2) 0.36(2) 0.281(19) 0.030(9) -0.039(11) O15 0.076(10) 0.23(2) 0.081(11) -0.038(12) -0.016(8) -0.010(12) O16 0.151(7) 0.299(14) 0.173(9) 0.088(9) -0.041(5) -0.079(8) _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 Fe1 O1 1.9098(18) . ? Fe1 O11 1.9873(18) . ? Fe1 O5 1.9980(19) 3_565 ? Fe1 O4 2.0149(19) 3_565 ? Fe1 O12 2.0276(19) . ? Fe1 N1 2.174(2) . ? Fe1 Fe2 2.9260(5) . ? Fe2 O2 1.9436(17) . ? Fe2 O1 1.9717(17) . ? Fe2 O11 1.9866(17) . ? Fe2 O8 2.0213(18) . ? Fe2 O10 2.063(2) . ? Fe2 O13 2.065(2) . ? Fe3 O1 1.8745(17) 3_565 ? Fe3 O2 1.9829(19) . ? Fe3 O7 2.0474(18) . ? Fe3 O6 2.0624(19) . ? Fe3 O9 2.070(2) . ? Fe3 O3 2.0846(19) . ? O1 Fe3 1.8745(17) 3_565 ? O3 C8 1.262(3) . ? O4 C8 1.263(3) . ? O4 Fe1 2.0149(19) 3_565 ? O5 C15 1.277(3) . ? O5 Fe1 1.9980(19) 3_565 ? O6 C15 1.255(3) . ? O7 C29 1.260(3) . ? O8 C29 1.267(3) . ? O9 C22 1.254(3) . ? O10 C22 1.279(3) . ? O11 C37 1.416(3) . ? O12 C1 1.262(3) . ? O13 C1 1.268(3) . ? N1 C38 1.469(4) . ? N1 C39 1.469(4) . ? C1 C2 1.488(4) . ? C2 C7 1.386(4) . ? C2 C3 1.394(4) . ? C3 C4 1.385(4) . ? C4 C5 1.387(5) . ? C5 C6 1.368(5) . ? C6 C7 1.400(5) . ? C8 C9 1.504(4) . ? C9 C14 1.382(4) . ? C9 C10 1.398(4) . ? C10 C11 1.381(4) . ? C11 C12 1.395(5) . ? C12 C13 1.378(5) . ? C13 C14 1.390(4) . ? C15 C16 1.490(4) . ? C16 C21 1.380(4) . ? C16 C17 1.381(4) . ? C17 C18 1.393(5) . ? C18 C19 1.340(6) . ? C19 C20 1.356(5) . ? C20 C21 1.383(4) . ? C22 C23 1.485(4) . ? C23 C28 1.390(4) . ? C23 C24 1.394(4) . ? C24 C25 1.371(5) . ? C25 C26 1.380(6) . ? C26 C27 1.377(6) . ? C27 C28 1.375(5) . ? C29 C30 1.497(4) . ? C30 C35 1.384(4) . ? C30 C31 1.391(4) . ? C31 C32 1.380(4) . ? C32 C33 1.389(4) . ? C33 C34 1.372(4) . ? C34 C35 1.391(4) . ? C36 C37 1.518(4) . ? C37 C38 1.521(4) . ? C39 C40 1.481(6) . ? C40 O14 1.394(11) . ? C40 C41 1.506(9) . ? C40' O14' 1.479(12) . ? C40' C41' 1.566(14) . ? C42 C43 1.589(14) . ? C43 N2 1.125(16) . ? 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 Fe1 O11 81.95(7) . . ? O1 Fe1 O5 103.43(8) . 3_565 ? O11 Fe1 O5 174.50(7) . 3_565 ? O1 Fe1 O4 96.61(8) . 3_565 ? O11 Fe1 O4 92.14(8) . 3_565 ? O5 Fe1 O4 88.41(8) 3_565 3_565 ? O1 Fe1 O12 92.66(8) . . ? O11 Fe1 O12 90.53(8) . . ? O5 Fe1 O12 88.07(8) 3_565 . ? O4 Fe1 O12 170.62(7) 3_565 . ? O1 Fe1 N1 160.87(8) . . ? O11 Fe1 N1 79.56(8) . . ? O5 Fe1 N1 94.99(8) 3_565 . ? O4 Fe1 N1 88.93(8) 3_565 . ? O12 Fe1 N1 82.71(8) . . ? O1 Fe1 Fe2 41.88(5) . . ? O11 Fe1 Fe2 42.57(5) . . ? O5 Fe1 Fe2 142.17(6) 3_565 . ? O4 Fe1 Fe2 107.05(6) 3_565 . ? O12 Fe1 Fe2 80.88(5) . . ? N1 Fe1 Fe2 119.00(6) . . ? O2 Fe2 O1 98.91(7) . . ? O2 Fe2 O11 177.35(8) . . ? O1 Fe2 O11 80.44(7) . . ? O2 Fe2 O8 87.89(7) . . ? O1 Fe2 O8 173.19(7) . . ? O11 Fe2 O8 92.76(7) . . ? O2 Fe2 O10 90.73(8) . . ? O1 Fe2 O10 88.71(8) . . ? O11 Fe2 O10 86.69(7) . . ? O8 Fe2 O10 91.27(8) . . ? O2 Fe2 O13 94.23(8) . . ? O1 Fe2 O13 92.65(8) . . ? O11 Fe2 O13 88.37(8) . . ? O8 Fe2 O13 86.77(8) . . ? O10 Fe2 O13 174.59(7) . . ? O2 Fe2 Fe1 137.45(6) . . ? O1 Fe2 Fe1 40.29(5) . . ? O11 Fe2 Fe1 42.59(5) . . ? O8 Fe2 Fe1 133.09(5) . . ? O10 Fe2 Fe1 97.96(5) . . ? O13 Fe2 Fe1 79.81(5) . . ? O1 Fe3 O2 92.02(8) 3_565 . ? O1 Fe3 O7 176.73(8) 3_565 . ? O2 Fe3 O7 86.06(8) . . ? O1 Fe3 O6 97.08(8) 3_565 . ? O2 Fe3 O6 170.38(8) . . ? O7 Fe3 O6 84.99(8) . . ? O1 Fe3 O9 93.17(8) 3_565 . ? O2 Fe3 O9 98.61(8) . . ? O7 Fe3 O9 84.51(8) . . ? O6 Fe3 O9 84.03(8) . . ? O1 Fe3 O3 94.78(8) 3_565 . ? O2 Fe3 O3 89.03(8) . . ? O7 Fe3 O3 87.84(8) . . ? O6 Fe3 O3 87.13(8) . . ? O9 Fe3 O3 168.77(7) . . ? Fe3 O1 Fe1 117.83(9) 3_565 . ? Fe3 O1 Fe2 139.23(10) 3_565 . ? Fe1 O1 Fe2 97.83(8) . . ? Fe2 O2 Fe3 122.98(10) . . ? C8 O3 Fe3 131.10(17) . . ? C8 O4 Fe1 130.51(17) . 3_565 ? C15 O5 Fe1 128.32(17) . 3_565 ? C15 O6 Fe3 135.11(18) . . ? C29 O7 Fe3 128.96(17) . . ? C29 O8 Fe2 135.54(16) . . ? C22 O9 Fe3 129.47(19) . . ? C22 O10 Fe2 129.59(17) . . ? C37 O11 Fe2 137.01(17) . . ? C37 O11 Fe1 118.86(16) . . ? Fe2 O11 Fe1 94.83(7) . . ? C1 O12 Fe1 127.09(19) . . ? C1 O13 Fe2 126.70(17) . . ? C38 N1 C39 113.0(2) . . ? C38 N1 Fe1 105.84(16) . . ? C39 N1 Fe1 117.98(18) . . ? O12 C1 O13 124.7(3) . . ? O12 C1 C2 116.2(3) . . ? O13 C1 C2 119.1(2) . . ? C7 C2 C3 119.5(3) . . ? C7 C2 C1 121.5(3) . . ? C3 C2 C1 119.0(3) . . ? C4 C3 C2 121.1(3) . . ? C3 C4 C5 118.9(3) . . ? C6 C5 C4 120.5(3) . . ? C5 C6 C7 120.9(3) . . ? C2 C7 C6 119.0(3) . . ? O3 C8 O4 125.5(2) . . ? O3 C8 C9 118.7(2) . . ? O4 C8 C9 115.7(2) . . ? C14 C9 C10 119.4(3) . . ? C14 C9 C8 119.6(2) . . ? C10 C9 C8 121.0(2) . . ? C11 C10 C9 119.7(3) . . ? C10 C11 C12 120.4(3) . . ? C13 C12 C11 120.1(3) . . ? C12 C13 C14 119.4(3) . . ? C9 C14 C13 121.0(3) . . ? O6 C15 O5 124.8(2) . . ? O6 C15 C16 118.3(2) . . ? O5 C15 C16 116.9(2) . . ? C21 C16 C17 118.7(3) . . ? C21 C16 C15 121.0(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 119.6(3) . . ? C19 C18 C17 120.8(4) . . ? C18 C19 C20 120.3(3) . . ? C19 C20 C21 120.4(3) . . ? C16 C21 C20 120.2(3) . . ? O9 C22 O10 124.2(3) . . ? O9 C22 C23 119.5(2) . . ? O10 C22 C23 116.3(2) . . ? C28 C23 C24 118.8(3) . . ? C28 C23 C22 120.4(3) . . ? C24 C23 C22 120.8(3) . . ? C25 C24 C23 121.0(3) . . ? C24 C25 C26 119.2(4) . . ? C27 C26 C25 120.7(4) . . ? C28 C27 C26 120.1(4) . . ? C27 C28 C23 120.2(3) . . ? O7 C29 O8 126.3(2) . . ? O7 C29 C30 116.9(2) . . ? O8 C29 C30 116.8(2) . . ? C35 C30 C31 119.7(2) . . ? C35 C30 C29 120.1(2) . . ? C31 C30 C29 120.1(2) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 119.4(3) . . ? C34 C33 C32 121.2(3) . . ? C33 C34 C35 119.2(3) . . ? C30 C35 C34 120.4(3) . . ? O11 C37 C36 111.2(2) . . ? O11 C37 C38 106.4(2) . . ? C36 C37 C38 111.1(3) . . ? N1 C38 C37 110.3(2) . . ? N1 C39 C40 117.0(3) . . ? O14 C40 C39 108.2(5) . . ? O14 C40 C41 111.6(6) . . ? C39 C40 C41 112.3(5) . . ? O14' C40' C41' 110.9(8) . . ? N2 C43 C42 174.7(17) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.832 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.096 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.255 -0.035 0.873 110.8 46.6 2 0.245 0.465 0.627 110.8 46.6 3 0.745 0.035 0.127 110.8 46.2 4 0.755 0.535 0.373 110.8 46.0 _platon_squeeze_details ; ? ; # END data_lfj21\pbca1s _database_code_depnum_ccdc_archive 'CCDC 267211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe6O2(OH)2(piv)10(dipaH2)2).2MeCN.3H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H132 Fe6 N4 O31' _chemical_formula_weight 1812.87 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.6547(2) _cell_length_b 19.9776(2) _cell_length_c 21.4828(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8864.48(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plate' _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 109403 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.19 _reflns_number_total 10878 _reflns_number_gt 8184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSEED _computing_publication_material XSEED _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^)+(0.0981P)^2^+5.9180P] 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 10878 _refine_ls_number_parameters 504 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.119 _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 Fe3 Fe 0.45799(2) 0.46173(2) 0.392753(18) 0.01813(12) Uani 1 1 d D . . Fe1 Fe 0.42310(2) 0.46903(2) 0.678747(19) 0.02393(13) Uani 1 1 d . . . Fe2 Fe 0.40617(2) 0.44733(2) 0.544718(18) 0.01800(12) Uani 1 1 d D . . O1 O 0.46000(10) 0.49826(10) 0.60315(9) 0.0197(4) Uani 1 1 d . . . O2 O 0.42991(9) 0.50156(10) 0.47245(9) 0.0181(4) Uani 1 1 d D . . H2A H 0.4472(8) 0.5375(6) 0.4793(7) 0.022 Uiso 1 1 d D . . O7 O 0.34819(11) 0.39124(11) 0.49002(10) 0.0290(5) Uani 1 1 d . . . O8 O 0.36839(11) 0.41759(12) 0.39053(9) 0.0281(5) Uani 1 1 d . . . O5 O 0.41604(10) 0.54100(11) 0.34704(10) 0.0258(5) Uani 1 1 d . . . O6 O 0.49735(11) 0.58059(12) 0.28952(10) 0.0302(5) Uani 1 1 d . . . O3 O 0.46844(12) 0.41867(12) 0.30688(10) 0.0335(6) Uani 1 1 d . . . O4 O 0.55657(13) 0.45876(13) 0.26133(11) 0.0369(6) Uani 1 1 d . . . O12 O 0.33931(11) 0.52380(12) 0.66305(10) 0.0287(5) Uani 1 1 d . . . O13 O 0.32895(10) 0.51015(11) 0.56008(9) 0.0257(5) Uani 1 1 d . . . O11 O 0.38611(11) 0.39693(11) 0.62406(10) 0.0264(5) Uani 1 1 d . . . O9 O 0.48907(12) 0.37168(10) 0.42628(10) 0.0286(5) Uani 1 1 d . . . O10 O 0.48165(11) 0.38259(11) 0.52939(10) 0.0268(5) Uani 1 1 d . . . O15 O 0.30049(14) 0.55762(17) 0.43031(13) 0.0494(7) Uani 1 1 d D . . N1 N 0.36443(15) 0.41754(16) 0.74697(13) 0.0356(7) Uani 1 1 d . . . H1 H 0.3277 0.4440 0.7519 0.043 Uiso 1 1 calc R A 1 C1 C 0.33500(15) 0.39074(15) 0.43205(14) 0.0248(6) Uani 1 1 d . . . C2 C 0.27430(17) 0.35186(19) 0.41261(16) 0.0360(8) Uani 1 1 d . . . C3 C 0.2876(2) 0.2780(2) 0.4250(2) 0.0600(13) Uani 1 1 d . . . H3A H 0.3270 0.2645 0.4030 0.090 Uiso 1 1 calc R . . H3B H 0.2509 0.2512 0.4101 0.090 Uiso 1 1 calc R . . H3C H 0.2932 0.2709 0.4698 0.090 Uiso 1 1 calc R . . C4 C 0.21635(19) 0.3769(3) 0.4518(2) 0.0548(11) Uani 1 1 d . . . H4A H 0.2111 0.4252 0.4458 0.082 Uiso 1 1 calc R . . H4B H 0.2244 0.3675 0.4959 0.082 Uiso 1 1 calc R . . H4C H 0.1768 0.3538 0.4385 0.082 Uiso 1 1 calc R . . C5 C 0.2600(2) 0.3630(3) 0.34312(19) 0.0561(12) Uani 1 1 d . . . H5A H 0.2983 0.3514 0.3185 0.084 Uiso 1 1 calc R . . H5B H 0.2489 0.4101 0.3361 0.084 Uiso 1 1 calc R . . H5C H 0.2236 0.3346 0.3305 0.084 Uiso 1 1 calc R . . C6 C 0.43842(16) 0.57597(15) 0.30342(14) 0.0243(6) Uani 1 1 d . . . C7 C 0.38898(17) 0.61382(18) 0.26345(15) 0.0331(8) Uani 1 1 d . . . C8 C 0.3552(2) 0.6661(2) 0.3041(2) 0.0531(11) Uani 1 1 d . . . H8A H 0.3318 0.6436 0.3378 0.080 Uiso 1 1 calc R . . H8B H 0.3245 0.6917 0.2787 0.080 Uiso 1 1 calc R . . H8C H 0.3876 0.6965 0.3218 0.080 Uiso 1 1 calc R . . C9 C 0.3376(2) 0.5625(2) 0.2423(2) 0.0516(11) Uani 1 1 d . . . H9A H 0.3150 0.5446 0.2788 0.077 Uiso 1 1 calc R . . H9B H 0.3589 0.5258 0.2199 0.077 Uiso 1 1 calc R . . H9C H 0.3064 0.5845 0.2147 0.077 Uiso 1 1 calc R . . C10 C 0.4203(2) 0.6446(3) 0.2063(2) 0.0756(18) Uani 1 1 d . . . H10A H 0.4565 0.6731 0.2192 0.113 Uiso 1 1 calc R . . H10B H 0.3883 0.6717 0.1839 0.113 Uiso 1 1 calc R . . H10C H 0.4363 0.6090 0.1790 0.113 Uiso 1 1 calc R . . C11 C 0.50906(16) 0.41829(16) 0.26474(14) 0.0269(7) Uani 1 1 d . . . C12 C 0.50142(19) 0.36856(19) 0.21112(16) 0.0386(8) Uani 1 1 d . . . C13 C 0.4636(4) 0.3083(3) 0.2334(3) 0.108(3) Uani 1 1 d . . . H13A H 0.4881 0.2853 0.2660 0.162 Uiso 1 1 calc R . . H13B H 0.4563 0.2777 0.1985 0.162 Uiso 1 1 calc R . . H13C H 0.4218 0.3230 0.2502 0.162 Uiso 1 1 calc R . . C14 C 0.4652(3) 0.4073(3) 0.1600(2) 0.094(2) Uani 1 1 d . . . H14A H 0.4221 0.4197 0.1751 0.141 Uiso 1 1 calc R . . H14B H 0.4610 0.3790 0.1230 0.141 Uiso 1 1 calc R . . H14C H 0.4895 0.4479 0.1495 0.141 Uiso 1 1 calc R . . C15 C 0.5667(2) 0.3486(3) 0.1858(3) 0.0673(14) Uani 1 1 d . . . H15A H 0.5922 0.3274 0.2188 0.101 Uiso 1 1 calc R . . H15B H 0.5895 0.3885 0.1707 0.101 Uiso 1 1 calc R . . H15C H 0.5609 0.3170 0.1513 0.101 Uiso 1 1 calc R . . C19 C 0.3415(2) 0.3556(2) 0.71807(17) 0.0437(9) Uani 1 1 d . . . H19A H 0.3007 0.3411 0.7383 0.052 Uiso 1 1 calc R . . H19B H 0.3741 0.3198 0.7238 0.052 Uiso 1 1 calc R . . C20 C 0.32981(18) 0.36713(19) 0.64908(16) 0.0364(8) Uani 1 1 d . . . H20 H 0.2926 0.3986 0.6439 0.044 Uiso 1 1 calc R B . C21 C 0.3136(2) 0.3015(2) 0.61789(19) 0.0535(11) Uani 1 1 d . . . H21A H 0.3130 0.3077 0.5726 0.080 Uiso 1 1 calc R . . H21B H 0.2709 0.2863 0.6319 0.080 Uiso 1 1 calc R . . H21C H 0.3463 0.2680 0.6289 0.080 Uiso 1 1 calc R . . C22 C 0.31210(16) 0.53535(16) 0.61188(14) 0.0260(7) Uani 1 1 d . . . C23 C 0.25351(19) 0.58197(19) 0.61083(15) 0.0371(8) Uani 1 1 d . . . C24 C 0.2366(2) 0.6059(2) 0.67691(17) 0.0507(11) Uani 1 1 d . . . H24A H 0.2286 0.5670 0.7037 0.076 Uiso 1 1 calc R . . H24B H 0.1977 0.6339 0.6754 0.076 Uiso 1 1 calc R . . H24C H 0.2728 0.6320 0.6938 0.076 Uiso 1 1 calc R . . C25 C 0.1963(2) 0.5440(3) 0.5819(2) 0.0553(12) Uani 1 1 d . . . H25A H 0.2079 0.5290 0.5399 0.083 Uiso 1 1 calc R . . H25B H 0.1586 0.5737 0.5795 0.083 Uiso 1 1 calc R . . H25C H 0.1857 0.5051 0.6077 0.083 Uiso 1 1 calc R . . C26 C 0.2689(3) 0.6426(2) 0.5696(2) 0.0619(14) Uani 1 1 d . . . H26A H 0.3071 0.6659 0.5859 0.093 Uiso 1 1 calc R . . H26B H 0.2319 0.6733 0.5694 0.093 Uiso 1 1 calc R . . H26C H 0.2776 0.6275 0.5270 0.093 Uiso 1 1 calc R . . C27 C 0.49513(14) 0.34938(14) 0.48092(13) 0.0207(6) Uani 1 1 d . . . C28 C 0.52109(19) 0.27976(16) 0.48981(15) 0.0324(8) Uani 1 1 d . . . C29 C 0.5362(3) 0.2465(2) 0.4273(2) 0.0695(17) Uani 1 1 d . . . H29A H 0.5718 0.2704 0.4069 0.104 Uiso 1 1 calc R . . H29B H 0.4977 0.2480 0.4007 0.104 Uiso 1 1 calc R . . H29C H 0.5488 0.1998 0.4343 0.104 Uiso 1 1 calc R . . C30 C 0.5816(2) 0.2843(3) 0.5308(2) 0.0654(14) Uani 1 1 d . . . H30A H 0.6140 0.3127 0.5104 0.098 Uiso 1 1 calc R . . H30B H 0.5995 0.2394 0.5371 0.098 Uiso 1 1 calc R . . H30C H 0.5700 0.3037 0.5712 0.098 Uiso 1 1 calc R . . C31 C 0.4689(3) 0.2392(2) 0.5241(2) 0.0604(13) Uani 1 1 d . . . H31A H 0.4603 0.2597 0.5647 0.091 Uiso 1 1 calc R . . H31B H 0.4840 0.1932 0.5300 0.091 Uiso 1 1 calc R . . H31C H 0.4290 0.2390 0.4994 0.091 Uiso 1 1 calc R . . H15D H 0.3331(12) 0.557(2) 0.4072(16) 0.035(11) Uiso 1 1 d D . . H15E H 0.315(3) 0.548(3) 0.4654(13) 0.09(2) Uiso 1 1 d D . . O14 O 0.3017(3) 0.4628(2) 0.8556(3) 0.0609(14) Uani 0.80 1 d PD B 1 H14 H 0.2721 0.4610 0.8824 0.073 Uiso 0.80 1 calc PR B 1 C16 C 0.3730(3) 0.3965(4) 0.9227(2) 0.0561(17) Uani 0.80 1 d PD B 1 H16A H 0.4052 0.3605 0.9224 0.084 Uiso 0.80 1 calc PR B 1 H16B H 0.3397 0.3867 0.9540 0.084 Uiso 0.80 1 calc PR B 1 H16C H 0.3942 0.4390 0.9330 0.084 Uiso 0.80 1 calc PR B 1 C17 C 0.3420(3) 0.4017(3) 0.8597(2) 0.0391(11) Uani 0.80 1 d PD B 1 H17 H 0.3155 0.3610 0.8507 0.047 Uiso 0.80 1 calc PR B 1 C18 C 0.3927(3) 0.4118(2) 0.8096(3) 0.0367(14) Uani 0.80 1 d PD B 1 H18A H 0.4176 0.4529 0.8190 0.044 Uiso 0.80 1 calc PR B 1 H18B H 0.4232 0.3736 0.8103 0.044 Uiso 0.80 1 calc PR B 1 O14' O 0.2957(10) 0.4375(12) 0.8479(13) 0.0609(14) Uani 0.20 1 d PD B 2 H14' H 0.2764 0.4663 0.8696 0.073 Uiso 0.20 1 calc PR B 2 C16' C 0.3901(13) 0.4338(15) 0.9190(7) 0.057(8) Uani 0.20 1 d PD B 2 H16D H 0.3650 0.3969 0.9369 0.086 Uiso 0.20 1 calc PR B 2 H16E H 0.3842 0.4741 0.9444 0.086 Uiso 0.20 1 calc PR B 2 H16F H 0.4361 0.4216 0.9182 0.086 Uiso 0.20 1 calc PR B 2 C17' C 0.3672(9) 0.4472(11) 0.8537(7) 0.044(5) Uani 0.20 1 d PD B 2 H17' H 0.3816 0.4919 0.8379 0.053 Uiso 0.20 1 calc PR B 2 C18' C 0.3884(15) 0.3895(13) 0.8111(12) 0.0367(14) Uani 0.20 1 d PD B 2 H18C H 0.3667 0.3470 0.8220 0.044 Uiso 0.20 1 calc PR B 2 H18D H 0.4360 0.3831 0.8117 0.044 Uiso 0.20 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe3 0.0240(2) 0.0192(2) 0.0112(2) -0.00047(15) 0.00105(15) -0.00224(16) Fe1 0.0250(2) 0.0353(3) 0.0115(2) 0.00054(17) 0.00244(16) 0.00105(18) Fe2 0.0234(2) 0.0192(2) 0.0114(2) -0.00154(15) 0.00152(15) -0.00263(16) O1 0.0208(10) 0.0255(11) 0.0127(9) 0.0003(8) 0.0000(8) -0.0015(8) O2 0.0239(10) 0.0180(10) 0.0126(9) -0.0013(8) 0.0007(8) -0.0037(8) O7 0.0334(12) 0.0367(12) 0.0169(10) -0.0029(9) 0.0006(9) -0.0154(10) O8 0.0300(12) 0.0370(13) 0.0174(10) -0.0018(9) 0.0002(9) -0.0120(10) O5 0.0259(11) 0.0329(12) 0.0187(11) 0.0077(9) -0.0009(8) 0.0028(9) O6 0.0284(12) 0.0404(13) 0.0218(11) 0.0123(10) 0.0005(9) 0.0004(10) O3 0.0453(14) 0.0397(13) 0.0157(11) -0.0076(10) 0.0052(10) -0.0077(11) O4 0.0411(14) 0.0504(15) 0.0193(12) -0.0109(10) 0.0043(10) -0.0090(12) O12 0.0291(12) 0.0397(13) 0.0173(10) -0.0047(9) 0.0034(9) 0.0068(10) O13 0.0240(11) 0.0360(12) 0.0172(10) -0.0006(9) 0.0004(8) 0.0043(9) O11 0.0327(12) 0.0277(11) 0.0187(10) 0.0007(9) 0.0044(9) -0.0052(9) O9 0.0455(14) 0.0193(10) 0.0208(11) 0.0014(8) 0.0060(10) 0.0026(10) O10 0.0379(12) 0.0242(11) 0.0183(10) -0.0031(8) -0.0002(9) 0.0069(9) O15 0.0404(16) 0.079(2) 0.0291(15) 0.0084(14) 0.0005(13) 0.0251(15) N1 0.0335(16) 0.0512(18) 0.0219(14) 0.0040(13) 0.0034(12) 0.0005(13) C1 0.0272(16) 0.0258(15) 0.0213(15) -0.0057(12) -0.0011(12) -0.0034(12) C2 0.0351(18) 0.045(2) 0.0277(17) -0.0021(15) -0.0077(14) -0.0154(16) C3 0.075(3) 0.037(2) 0.069(3) -0.007(2) -0.026(3) -0.021(2) C4 0.033(2) 0.074(3) 0.057(3) -0.001(2) 0.0020(19) -0.017(2) C5 0.046(2) 0.084(3) 0.038(2) 0.000(2) -0.0181(19) -0.026(2) C6 0.0312(17) 0.0254(15) 0.0163(14) 0.0018(12) -0.0017(12) 0.0007(12) C7 0.0333(18) 0.0399(19) 0.0261(17) 0.0127(14) -0.0041(14) 0.0044(15) C8 0.063(3) 0.038(2) 0.058(3) 0.0008(19) -0.012(2) 0.017(2) C9 0.051(3) 0.059(3) 0.045(2) -0.008(2) -0.026(2) 0.008(2) C10 0.055(3) 0.112(4) 0.060(3) 0.061(3) 0.003(2) 0.016(3) C11 0.0346(17) 0.0286(16) 0.0174(15) -0.0026(12) -0.0028(13) 0.0048(13) C12 0.048(2) 0.041(2) 0.0268(17) -0.0154(15) 0.0028(16) 0.0037(17) C13 0.166(7) 0.069(4) 0.090(5) -0.052(3) 0.050(4) -0.060(4) C14 0.116(5) 0.117(5) 0.050(3) -0.051(3) -0.046(3) 0.052(4) C15 0.062(3) 0.066(3) 0.074(3) -0.039(3) 0.007(3) 0.012(2) C19 0.048(2) 0.051(2) 0.0325(19) 0.0094(17) 0.0072(17) -0.0111(18) C20 0.041(2) 0.041(2) 0.0275(17) 0.0073(15) 0.0056(15) -0.0100(16) C21 0.071(3) 0.046(2) 0.043(2) -0.0007(18) 0.008(2) -0.022(2) C22 0.0263(16) 0.0303(17) 0.0213(15) 0.0016(12) 0.0062(12) 0.0032(13) C23 0.040(2) 0.046(2) 0.0252(17) 0.0062(15) 0.0107(15) 0.0193(17) C24 0.063(3) 0.060(3) 0.0299(19) -0.0033(18) 0.0140(19) 0.023(2) C25 0.034(2) 0.093(4) 0.039(2) 0.003(2) 0.0033(18) 0.020(2) C26 0.102(4) 0.038(2) 0.045(2) 0.0084(19) 0.024(3) 0.022(2) C27 0.0256(15) 0.0199(14) 0.0165(13) -0.0010(11) -0.0001(11) -0.0016(11) C28 0.052(2) 0.0235(16) 0.0217(16) -0.0002(13) 0.0068(14) 0.0112(15) C29 0.135(5) 0.036(2) 0.037(2) -0.0005(18) 0.027(3) 0.037(3) C30 0.065(3) 0.067(3) 0.065(3) 0.008(2) -0.008(2) 0.036(3) C31 0.102(4) 0.027(2) 0.053(3) 0.0072(18) 0.015(3) -0.008(2) O14 0.067(2) 0.066(4) 0.049(2) -0.005(3) 0.0158(19) 0.029(3) C16 0.059(4) 0.086(5) 0.023(3) 0.007(3) 0.006(3) 0.011(4) C17 0.058(3) 0.037(3) 0.023(2) 0.0055(19) 0.008(2) 0.010(2) C18 0.049(3) 0.042(4) 0.0198(17) 0.008(3) 0.0000(17) 0.004(3) O14' 0.067(2) 0.066(4) 0.049(2) -0.005(3) 0.0158(19) 0.029(3) C16' 0.071(17) 0.09(2) 0.010(9) -0.005(11) 0.018(10) -0.025(16) C17' 0.054(12) 0.067(14) 0.010(8) 0.013(8) 0.009(8) 0.026(11) C18' 0.049(3) 0.042(4) 0.0198(17) 0.008(3) 0.0000(17) 0.004(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 Fe3 O1 1.875(2) 5_666 ? Fe3 O2 1.9751(19) . ? Fe3 O9 2.041(2) . ? Fe3 O3 2.047(2) . ? Fe3 O8 2.051(2) . ? Fe3 O5 2.055(2) . ? Fe1 O1 1.887(2) . ? Fe1 O4 1.979(2) 5_666 ? Fe1 O11 2.010(2) . ? Fe1 O6 2.036(2) 5_666 ? Fe1 O12 2.075(2) . ? Fe1 N1 2.162(3) . ? Fe1 Fe2 2.9327(6) . ? Fe2 O2 1.9556(19) . ? Fe2 O1 1.961(2) . ? Fe2 O7 2.018(2) . ? Fe2 O11 2.022(2) . ? Fe2 O10 2.052(2) . ? Fe2 O13 2.056(2) . ? O1 Fe3 1.875(2) 5_666 ? O7 C1 1.275(4) . ? O8 C1 1.249(4) . ? O5 C6 1.257(4) . ? O6 C6 1.257(4) . ? O6 Fe1 2.036(2) 5_666 ? O3 C11 1.234(4) . ? O4 C11 1.274(4) . ? O4 Fe1 1.979(2) 5_666 ? O12 C22 1.256(4) . ? O13 C22 1.270(4) . ? O11 C20 1.413(4) . ? O9 C27 1.262(4) . ? O10 C27 1.266(3) . ? N1 C19 1.463(5) . ? N1 C18 1.472(7) . ? N1 C18' 1.57(3) . ? C1 C2 1.533(4) . ? C2 C3 1.523(6) . ? C2 C5 1.538(5) . ? C2 C4 1.546(6) . ? C6 C7 1.534(4) . ? C7 C10 1.518(5) . ? C7 C8 1.530(5) . ? C7 C9 1.544(5) . ? C11 C12 1.529(4) . ? C12 C15 1.509(6) . ? C12 C13 1.513(7) . ? C12 C14 1.536(7) . ? C19 C20 1.519(5) . ? C20 C21 1.510(5) . ? C22 C23 1.527(5) . ? C23 C26 1.535(5) . ? C23 C25 1.536(6) . ? C23 C24 1.538(5) . ? C27 C28 1.503(4) . ? C28 C29 1.530(5) . ? C28 C30 1.532(6) . ? C28 C31 1.537(6) . ? O14 C17 1.481(6) . ? C16 C17 1.502(7) . ? C17 C18 1.514(7) . ? O14' C17' 1.496(18) . ? C16' C17' 1.503(16) . ? C17' C18' 1.536(17) . ? 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 Fe3 O2 93.03(8) 5_666 . ? O1 Fe3 O9 94.30(9) 5_666 . ? O2 Fe3 O9 98.14(8) . . ? O1 Fe3 O3 97.25(9) 5_666 . ? O2 Fe3 O3 168.97(9) . . ? O9 Fe3 O3 85.09(9) . . ? O1 Fe3 O8 178.63(8) 5_666 . ? O2 Fe3 O8 85.89(8) . . ? O9 Fe3 O8 85.01(10) . . ? O3 Fe3 O8 83.88(9) . . ? O1 Fe3 O5 94.30(9) 5_666 . ? O2 Fe3 O5 88.85(8) . . ? O9 Fe3 O5 168.61(9) . . ? O3 Fe3 O5 86.43(10) . . ? O8 Fe3 O5 86.54(9) . . ? O1 Fe1 O4 104.40(10) . 5_666 ? O1 Fe1 O11 82.65(9) . . ? O4 Fe1 O11 169.63(10) 5_666 . ? O1 Fe1 O6 96.48(9) . 5_666 ? O4 Fe1 O6 88.04(11) 5_666 5_666 ? O11 Fe1 O6 98.83(10) . 5_666 ? O1 Fe1 O12 91.94(9) . . ? O4 Fe1 O12 84.17(10) 5_666 . ? O11 Fe1 O12 88.04(9) . . ? O6 Fe1 O12 169.73(9) 5_666 . ? O1 Fe1 N1 163.18(10) . . ? O4 Fe1 N1 91.42(11) 5_666 . ? O11 Fe1 N1 80.92(10) . . ? O6 Fe1 N1 89.64(10) 5_666 . ? O12 Fe1 N1 83.89(11) . . ? O1 Fe1 Fe2 41.30(6) . . ? O4 Fe1 Fe2 140.52(8) 5_666 . ? O11 Fe1 Fe2 43.51(6) . . ? O6 Fe1 Fe2 110.66(7) 5_666 . ? O12 Fe1 Fe2 79.57(6) . . ? N1 Fe1 Fe2 121.90(8) . . ? O2 Fe2 O1 94.51(8) . . ? O2 Fe2 O7 89.66(8) . . ? O1 Fe2 O7 175.80(9) . . ? O2 Fe2 O11 174.99(9) . . ? O1 Fe2 O11 80.50(8) . . ? O7 Fe2 O11 95.32(9) . . ? O2 Fe2 O10 91.79(8) . . ? O1 Fe2 O10 89.94(9) . . ? O7 Fe2 O10 90.43(9) . . ? O11 Fe2 O10 88.69(9) . . ? O2 Fe2 O13 89.07(8) . . ? O1 Fe2 O13 91.17(8) . . ? O7 Fe2 O13 88.39(9) . . ? O11 Fe2 O13 90.55(9) . . ? O10 Fe2 O13 178.54(9) . . ? O2 Fe2 Fe1 131.89(6) . . ? O1 Fe2 Fe1 39.41(6) . . ? O7 Fe2 Fe1 136.44(6) . . ? O11 Fe2 Fe1 43.16(6) . . ? O10 Fe2 Fe1 99.21(6) . . ? O13 Fe2 Fe1 81.07(6) . . ? Fe3 O1 Fe1 117.16(10) 5_666 . ? Fe3 O1 Fe2 139.75(11) 5_666 . ? Fe1 O1 Fe2 99.28(9) . . ? Fe2 O2 Fe3 122.59(10) . . ? C1 O7 Fe2 134.4(2) . . ? C1 O8 Fe3 131.8(2) . . ? C6 O5 Fe3 129.0(2) . . ? C6 O6 Fe1 131.8(2) . 5_666 ? C11 O3 Fe3 137.3(2) . . ? C11 O4 Fe1 126.1(2) . 5_666 ? C22 O12 Fe1 127.8(2) . . ? C22 O13 Fe2 126.5(2) . . ? C20 O11 Fe1 113.12(19) . . ? C20 O11 Fe2 134.4(2) . . ? Fe1 O11 Fe2 93.33(9) . . ? C27 O9 Fe3 132.11(19) . . ? C27 O10 Fe2 129.01(19) . . ? C19 N1 C18 116.8(3) . . ? C19 N1 C18' 100.0(10) . . ? C18 N1 C18' 16.8(10) . . ? C19 N1 Fe1 107.2(2) . . ? C18 N1 Fe1 115.8(3) . . ? C18' N1 Fe1 126.0(12) . . ? O8 C1 O7 125.2(3) . . ? O8 C1 C2 118.4(3) . . ? O7 C1 C2 116.4(3) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 C5 110.1(4) . . ? C1 C2 C5 110.4(3) . . ? C3 C2 C4 110.9(4) . . ? C1 C2 C4 108.7(3) . . ? C5 C2 C4 109.4(3) . . ? O6 C6 O5 125.0(3) . . ? O6 C6 C7 118.4(3) . . ? O5 C6 C7 116.5(3) . . ? C10 C7 C8 112.3(4) . . ? C10 C7 C6 111.7(3) . . ? C8 C7 C6 108.7(3) . . ? C10 C7 C9 108.9(4) . . ? C8 C7 C9 108.0(3) . . ? C6 C7 C9 107.2(3) . . ? O3 C11 O4 124.2(3) . . ? O3 C11 C12 119.1(3) . . ? O4 C11 C12 116.7(3) . . ? C15 C12 C13 111.5(4) . . ? C15 C12 C11 110.6(3) . . ? C13 C12 C11 109.4(3) . . ? C15 C12 C14 108.1(4) . . ? C13 C12 C14 112.1(5) . . ? C11 C12 C14 105.1(3) . . ? N1 C19 C20 109.7(3) . . ? O11 C20 C21 112.3(3) . . ? O11 C20 C19 107.7(3) . . ? C21 C20 C19 109.7(3) . . ? O12 C22 O13 124.8(3) . . ? O12 C22 C23 118.7(3) . . ? O13 C22 C23 116.5(3) . . ? C22 C23 C26 109.0(3) . . ? C22 C23 C25 108.4(3) . . ? C26 C23 C25 108.4(4) . . ? C22 C23 C24 110.8(3) . . ? C26 C23 C24 109.6(3) . . ? C25 C23 C24 110.6(3) . . ? O9 C27 O10 124.0(3) . . ? O9 C27 C28 118.7(3) . . ? O10 C27 C28 117.3(3) . . ? C27 C28 C29 111.3(3) . . ? C27 C28 C30 108.0(3) . . ? C29 C28 C30 111.4(4) . . ? C27 C28 C31 107.3(3) . . ? C29 C28 C31 109.6(4) . . ? C30 C28 C31 109.2(3) . . ? O14 C17 C16 110.4(5) . . ? O14 C17 C18 103.7(4) . . ? C16 C17 C18 110.8(5) . . ? N1 C18 C17 112.6(5) . . ? O14' C17' C16' 111.4(17) . . ? O14' C17' C18' 97.7(17) . . ? C16' C17' C18' 109.4(17) . . ? C17' C18' N1 99.6(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.894 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.120 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 136.2 53.7 2 0.500 0.000 0.500 136.2 53.9 3 0.000 0.500 0.500 136.0 53.8 4 0.500 0.500 1.000 136.1 53.8 _platon_squeeze_details ; ? ; # END data_lfj17s _database_code_depnum_ccdc_archive 'CCDC 267212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety {[Co4OH(piv)4(pivH)2(dipaH)2].2MeCN}n _chemical_formula_sum 'C46 H89 Co4 N4 O17' _chemical_formula_weight 1205.93 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.92460(10) _cell_length_b 20.0660(2) _cell_length_c 17.2700(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.03 _cell_angle_gamma 90.00 _cell_volume 5690.09(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour purple _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 _exptl_absorpt_coefficient_mu 1.213 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57686 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9986 _reflns_number_gt 7852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XSEED _computing_publication_material XSEED _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^)+(0.0822P)^2^+10.5726P] 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 9986 _refine_ls_number_parameters 630 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _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 Co1 Co 0.57843(3) 0.23755(3) 0.24051(3) 0.02362(15) Uani 1 1 d D . . Co2 Co 0.42074(3) 0.26937(3) 0.10104(3) 0.02556(15) Uani 1 1 d D A . Co3 Co 0.24720(3) 0.23069(3) 0.09565(4) 0.02902(16) Uani 1 1 d . A . Co4 Co 0.37148(3) 0.18430(3) 0.23942(3) 0.02865(16) Uani 1 1 d D A . O1 O 0.73318(19) 0.13041(16) 0.2749(2) 0.0507(9) Uani 1 1 d . . . H1 H 0.6841 0.1282 0.2766 0.061 Uiso 1 1 calc R . . O2 O 0.70793(17) 0.23815(14) 0.27360(19) 0.0347(7) Uani 1 1 d . . . O3 O 0.58620(19) 0.19816(16) 0.13119(18) 0.0400(8) Uani 1 1 d . . . O4 O 0.47959(19) 0.22245(16) 0.03164(18) 0.0398(8) Uani 1 1 d . . . O5 O 0.59128(17) 0.33320(14) 0.20381(19) 0.0345(7) Uani 1 1 d . . . O6 O 0.48131(18) 0.35712(15) 0.10799(19) 0.0370(7) Uani 1 1 d . . . O7 O 0.45574(16) 0.24909(13) 0.21697(16) 0.0246(6) Uani 1 1 d D . . H7 H 0.4496(8) 0.2836(6) 0.2420(8) 0.029 Uiso 1 1 d D . . O8 O 0.30645(16) 0.29430(13) 0.05005(17) 0.0280(6) Uani 1 1 d . A . O9 O 0.08514(17) 0.22754(14) -0.14174(17) 0.0317(7) Uani 1 1 d . . . O10 O 0.34203(16) 0.17718(13) 0.11202(17) 0.0287(6) Uani 1 1 d . . . O11 O 0.28888(16) 0.26545(14) 0.19816(18) 0.0310(7) Uani 1 1 d . . . O12 O 0.18208(17) 0.16669(15) 0.1360(2) 0.0394(8) Uani 1 1 d . . . O13 O 0.27364(18) 0.12531(16) 0.2409(2) 0.0431(8) Uani 1 1 d . . . O14 O 0.39668(19) 0.21267(17) 0.35732(18) 0.0408(8) Uani 1 1 d . . . O15 O 0.5096(2) 0.2158(2) 0.4544(2) 0.0556(10) Uani 1 1 d . . . H15 H 0.5245 0.2408 0.4215 0.067 Uiso 1 1 calc R A . O16 O 0.45219(17) 0.10446(14) 0.25913(18) 0.0351(7) Uani 1 1 d . . . O17 O 0.58179(17) 0.13826(13) 0.27908(18) 0.0327(7) Uani 1 1 d . . . N1 N 0.2138(2) 0.19105(18) -0.0118(2) 0.0367(9) Uani 1 1 d . . . H1N H 0.2083 0.2263 -0.0476 0.044 Uiso 1 1 calc R A . N2 N 0.1612(2) 0.29795(18) 0.0855(2) 0.0371(9) Uani 1 1 d . . . H2N H 0.1114 0.2798 0.0589 0.045 Uiso 1 1 calc R A . C1 C 0.8976(3) 0.1820(3) 0.3509(3) 0.0538(14) Uani 1 1 d . . . H1A H 0.8866 0.2098 0.3937 0.081 Uiso 1 1 calc R . . H1B H 0.9550 0.1866 0.3497 0.081 Uiso 1 1 calc R . . H1C H 0.8861 0.1353 0.3606 0.081 Uiso 1 1 calc R . . C2 C 0.8605(4) 0.1621(4) 0.2021(4) 0.080(2) Uani 1 1 d . . . H2A H 0.8504 0.1151 0.2115 0.120 Uiso 1 1 calc R . . H2B H 0.9175 0.1680 0.2003 0.120 Uiso 1 1 calc R . . H2C H 0.8248 0.1763 0.1512 0.120 Uiso 1 1 calc R . . C3 C 0.8561(3) 0.2784(3) 0.2572(4) 0.0618(17) Uani 1 1 d . . . H3A H 0.8213 0.2924 0.2058 0.093 Uiso 1 1 calc R . . H3B H 0.9133 0.2861 0.2574 0.093 Uiso 1 1 calc R . . H3C H 0.8421 0.3042 0.3002 0.093 Uiso 1 1 calc R . . C4 C 0.8429(3) 0.2045(3) 0.2700(3) 0.0402(11) Uani 1 1 d . . . C5 C 0.7547(3) 0.1931(2) 0.2732(3) 0.0334(10) Uani 1 1 d . . . C6 C 0.6522(5) 0.1164(4) 0.0345(4) 0.093(3) Uani 1 1 d . . . H6A H 0.6206 0.0776 0.0437 0.140 Uiso 1 1 calc R . . H6B H 0.6871 0.1315 0.0853 0.140 Uiso 1 1 calc R . . H6C H 0.6861 0.1043 -0.0020 0.140 Uiso 1 1 calc R . . C7 C 0.6469(8) 0.2289(4) -0.0175(7) 0.158(6) Uani 1 1 d . . . H7A H 0.6938 0.2116 -0.0351 0.237 Uiso 1 1 calc R . . H7B H 0.6660 0.2549 0.0316 0.237 Uiso 1 1 calc R . . H7C H 0.6144 0.2576 -0.0592 0.237 Uiso 1 1 calc R . . C8 C 0.5377(5) 0.1484(6) -0.0750(5) 0.147(5) Uani 1 1 d . . . H8A H 0.5014 0.1851 -0.0983 0.221 Uiso 1 1 calc R . . H8B H 0.5053 0.1114 -0.0621 0.221 Uiso 1 1 calc R . . H8C H 0.5681 0.1333 -0.1134 0.221 Uiso 1 1 calc R . . C9 C 0.5951(3) 0.1716(3) -0.0017(3) 0.0445(12) Uani 1 1 d . . . C10 C 0.5496(3) 0.1992(2) 0.0591(3) 0.0332(10) Uani 1 1 d . . . C11 C 0.6623(4) 0.4541(3) 0.2028(5) 0.097(3) Uani 1 1 d . . . H11A H 0.7060 0.4210 0.2095 0.146 Uiso 1 1 calc R . . H11B H 0.6423 0.4561 0.2514 0.146 Uiso 1 1 calc R . . H11C H 0.6833 0.4979 0.1925 0.146 Uiso 1 1 calc R . . C12 C 0.6231(5) 0.4186(3) 0.0585(5) 0.091(3) Uani 1 1 d . . . H12A H 0.6659 0.3847 0.0716 0.137 Uiso 1 1 calc R . . H12B H 0.6452 0.4591 0.0401 0.137 Uiso 1 1 calc R . . H12C H 0.5780 0.4018 0.0161 0.137 Uiso 1 1 calc R . . C13 C 0.5315(4) 0.4895(2) 0.1137(4) 0.0674(18) Uani 1 1 d . . . H13A H 0.5567 0.5288 0.0959 0.101 Uiso 1 1 calc R . . H13B H 0.5131 0.5007 0.1617 0.101 Uiso 1 1 calc R . . H13C H 0.4848 0.4754 0.0713 0.101 Uiso 1 1 calc R . . C14 C 0.5925(3) 0.4343(2) 0.1321(3) 0.0417(12) Uani 1 1 d . . . C15 C 0.5518(2) 0.3693(2) 0.1503(3) 0.0285(9) Uani 1 1 d . . . C16 C 0.3962(5) 0.0779(3) 0.0588(5) 0.0490(19) Uani 0.69 1 d PD A 1 H16A H 0.4371 0.1041 0.0406 0.073 Uiso 0.69 1 calc PR A 1 H16B H 0.3790 0.0402 0.0225 0.073 Uiso 0.69 1 calc PR A 1 H16C H 0.4197 0.0612 0.1128 0.073 Uiso 0.69 1 calc PR A 1 C17 C 0.3223(7) 0.1220(5) 0.0594(9) 0.025(2) Uani 0.69 1 d PDU A 1 H17 H 0.2802 0.0943 0.0762 0.030 Uiso 0.69 1 calc PR A 1 C16' C 0.3083(10) 0.0619(7) 0.0831(11) 0.050(4) Uani 0.31 1 d PD A 2 H16D H 0.3447 0.0479 0.1337 0.075 Uiso 0.31 1 calc PR A 2 H16E H 0.3008 0.0249 0.0450 0.075 Uiso 0.31 1 calc PR A 2 H16F H 0.2555 0.0748 0.0922 0.075 Uiso 0.31 1 calc PR A 2 C17' C 0.3459(19) 0.1213(15) 0.049(3) 0.050(10) Uani 0.31 1 d PDU A 2 H17' H 0.4014 0.1130 0.0409 0.060 Uiso 0.31 1 calc PR A 2 C18 C 0.2852(3) 0.1513(2) -0.0222(3) 0.0450(12) Uani 1 1 d . A . H18A H 0.3249 0.1801 -0.0399 0.054 Uiso 1 1 calc R B 1 H18B H 0.2674 0.1155 -0.0621 0.054 Uiso 1 1 calc R B 1 C19 C 0.1341(3) 0.1543(2) -0.0320(3) 0.0452(12) Uani 1 1 d . A . H19A H 0.1432 0.1072 -0.0152 0.054 Uiso 1 1 calc R . . H19B H 0.0965 0.1743 -0.0026 0.054 Uiso 1 1 calc R . . C20 C 0.0965(3) 0.1574(2) -0.1197(3) 0.0457(12) Uani 1 1 d D . . H20 H 0.1345 0.1367 -0.1491 0.055 Uiso 1 1 calc R A . C21 C 0.0157(3) 0.1202(3) -0.1402(3) 0.0559(15) Uani 1 1 d D A . H21A H -0.0226 0.1417 -0.1136 0.084 Uiso 1 1 calc R . . H21B H 0.0244 0.0739 -0.1221 0.084 Uiso 1 1 calc R . . H21C H -0.0069 0.1210 -0.1981 0.084 Uiso 1 1 calc R . . C22 C 0.3035(3) 0.4075(2) 0.0009(3) 0.0413(11) Uani 1 1 d . A . H22A H 0.3631 0.4096 0.0150 0.062 Uiso 1 1 calc R . . H22B H 0.2812 0.4520 0.0056 0.062 Uiso 1 1 calc R . . H22C H 0.2844 0.3917 -0.0542 0.062 Uiso 1 1 calc R . . C23 C 0.2754(2) 0.3601(2) 0.0565(3) 0.0318(10) Uani 1 1 d . . . H23 H 0.2954 0.3762 0.1126 0.038 Uiso 1 1 calc R A . C24 C 0.1835(3) 0.3534(2) 0.0374(3) 0.0383(11) Uani 1 1 d . A . H24A H 0.1590 0.3956 0.0500 0.046 Uiso 1 1 calc R . . H24B H 0.1623 0.3441 -0.0202 0.046 Uiso 1 1 calc R . . C25 C 0.1580(3) 0.3180(3) 0.1671(3) 0.0477(13) Uani 1 1 d . A . H25A H 0.1075 0.3000 0.1784 0.057 Uiso 1 1 calc R . . H25B H 0.1549 0.3672 0.1692 0.057 Uiso 1 1 calc R . . C26 C 0.2297(3) 0.2949(4) 0.2317(4) 0.079(2) Uani 1 1 d . A . H26 H 0.2057 0.2540 0.2500 0.095 Uiso 1 1 calc R . . C27 C 0.2544(5) 0.3278(4) 0.3030(4) 0.095(3) Uani 1 1 d . . . H27A H 0.2963 0.3015 0.3394 0.142 Uiso 1 1 calc R A . H27B H 0.2078 0.3341 0.3265 0.142 Uiso 1 1 calc R . . H27C H 0.2769 0.3713 0.2939 0.142 Uiso 1 1 calc R . . C28 C 0.1090(5) 0.1227(4) 0.2854(6) 0.104(3) Uani 1 1 d . A . H28A H 0.0708 0.0946 0.3054 0.157 Uiso 1 1 calc R . . H28B H 0.0821 0.1644 0.2645 0.157 Uiso 1 1 calc R . . H28C H 0.1566 0.1325 0.3291 0.157 Uiso 1 1 calc R . . C29 C 0.0639(4) 0.0803(4) 0.1481(5) 0.088(2) Uani 1 1 d . A . H29A H 0.0768 0.0513 0.1072 0.132 Uiso 1 1 calc R . . H29B H 0.0495 0.1248 0.1257 0.132 Uiso 1 1 calc R . . H29C H 0.0179 0.0616 0.1661 0.132 Uiso 1 1 calc R . . C30 C 0.1721(4) 0.0193(3) 0.2473(6) 0.104(3) Uani 1 1 d . A . H30A H 0.1301 -0.0083 0.2618 0.155 Uiso 1 1 calc R . . H30B H 0.2173 0.0258 0.2943 0.155 Uiso 1 1 calc R . . H30C H 0.1921 -0.0029 0.2053 0.155 Uiso 1 1 calc R . . C31 C 0.1368(3) 0.0853(3) 0.2177(4) 0.0555(15) Uani 1 1 d . . . C32 C 0.2038(3) 0.1288(2) 0.1973(3) 0.0405(11) Uani 1 1 d . A . C33 C 0.3099(5) 0.1633(8) 0.4563(7) 0.218(9) Uani 1 1 d . A . H33A H 0.2988 0.2075 0.4318 0.326 Uiso 1 1 calc R . . H33B H 0.2903 0.1617 0.5052 0.326 Uiso 1 1 calc R . . H33C H 0.2818 0.1293 0.4188 0.326 Uiso 1 1 calc R . . C34 C 0.4331(6) 0.1635(4) 0.5635(4) 0.100(3) Uani 1 1 d . A . H34A H 0.4341 0.2116 0.5733 0.150 Uiso 1 1 calc R . . H34B H 0.4886 0.1457 0.5799 0.150 Uiso 1 1 calc R . . H34C H 0.3988 0.1417 0.5942 0.150 Uiso 1 1 calc R . . C35 C 0.4185(10) 0.0809(4) 0.4551(7) 0.192(7) Uani 1 1 d . A . H35A H 0.3980 0.0491 0.4887 0.288 Uiso 1 1 calc R . . H35B H 0.4776 0.0758 0.4640 0.288 Uiso 1 1 calc R . . H35C H 0.3924 0.0722 0.3988 0.288 Uiso 1 1 calc R . . C36 C 0.3992(3) 0.1504(3) 0.4760(3) 0.0516(14) Uani 1 1 d . . . C37 C 0.4382(3) 0.1965(2) 0.4253(3) 0.0388(11) Uani 1 1 d . A . C38 C 0.4841(3) -0.0270(2) 0.2763(3) 0.0507(14) Uani 1 1 d . A . H38A H 0.4634 -0.0181 0.3236 0.076 Uiso 1 1 calc R . . H38B H 0.5028 -0.0733 0.2774 0.076 Uiso 1 1 calc R . . H38C H 0.4406 -0.0195 0.2281 0.076 Uiso 1 1 calc R . . C39 C 0.6226(3) 0.0109(2) 0.3522(3) 0.0486(13) Uani 1 1 d . A . H39A H 0.6686 0.0400 0.3506 0.073 Uiso 1 1 calc R . . H39B H 0.6407 -0.0356 0.3566 0.073 Uiso 1 1 calc R . . H39C H 0.6014 0.0225 0.3985 0.073 Uiso 1 1 calc R . . C40 C 0.5904(4) 0.0053(3) 0.2037(3) 0.0548(14) Uani 1 1 d . A . H40A H 0.5475 0.0106 0.1546 0.082 Uiso 1 1 calc R . . H40B H 0.6110 -0.0406 0.2072 0.082 Uiso 1 1 calc R . . H40C H 0.6350 0.0363 0.2032 0.082 Uiso 1 1 calc R . . C41 C 0.5556(3) 0.0200(2) 0.2759(3) 0.0369(11) Uani 1 1 d . . . C42 C 0.5266(3) 0.0930(2) 0.2710(2) 0.0301(10) Uani 1 1 d . A . 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 Co1 0.0175(3) 0.0228(3) 0.0291(3) 0.0048(2) 0.0027(2) -0.0008(2) Co2 0.0176(3) 0.0286(3) 0.0284(3) 0.0059(2) 0.0017(2) -0.0014(2) Co3 0.0177(3) 0.0257(3) 0.0401(4) 0.0041(2) 0.0000(2) -0.0035(2) Co4 0.0192(3) 0.0299(3) 0.0353(3) 0.0111(2) 0.0034(2) -0.0043(2) O1 0.0284(17) 0.0338(19) 0.090(3) 0.0041(17) 0.0145(18) 0.0051(14) O2 0.0215(15) 0.0309(16) 0.050(2) 0.0033(14) 0.0060(14) 0.0012(13) O3 0.0364(18) 0.051(2) 0.0326(19) -0.0030(14) 0.0075(15) 0.0090(15) O4 0.0315(18) 0.053(2) 0.0340(18) -0.0013(15) 0.0062(14) 0.0076(15) O5 0.0213(15) 0.0317(16) 0.0470(19) 0.0133(14) 0.0017(14) -0.0061(13) O6 0.0283(17) 0.0340(17) 0.0457(19) 0.0148(14) 0.0030(14) -0.0066(13) O7 0.0203(14) 0.0231(14) 0.0298(15) 0.0056(11) 0.0050(12) -0.0013(11) O8 0.0217(14) 0.0225(14) 0.0363(17) 0.0049(12) 0.0003(12) -0.0012(12) O9 0.0278(16) 0.0307(16) 0.0319(17) 0.0040(12) -0.0016(13) -0.0031(12) O10 0.0217(14) 0.0258(14) 0.0345(16) 0.0010(12) -0.0007(12) -0.0020(12) O11 0.0213(15) 0.0342(16) 0.0381(17) 0.0057(13) 0.0079(13) -0.0015(12) O12 0.0221(15) 0.0364(17) 0.057(2) 0.0083(15) 0.0037(14) -0.0090(13) O13 0.0261(17) 0.0422(19) 0.059(2) 0.0182(16) 0.0057(16) -0.0068(14) O14 0.0367(18) 0.053(2) 0.0307(18) 0.0113(15) 0.0051(14) 0.0053(15) O15 0.036(2) 0.092(3) 0.038(2) 0.0278(19) 0.0074(16) -0.0038(19) O16 0.0257(16) 0.0310(16) 0.0444(19) 0.0120(13) 0.0001(13) -0.0025(13) O17 0.0263(15) 0.0230(15) 0.0466(19) 0.0055(13) 0.0048(13) -0.0023(12) N1 0.029(2) 0.033(2) 0.040(2) 0.0004(16) -0.0073(17) -0.0072(16) N2 0.0192(18) 0.031(2) 0.057(3) 0.0029(17) 0.0017(17) -0.0015(15) C1 0.030(3) 0.061(3) 0.065(4) 0.010(3) 0.000(2) 0.005(2) C2 0.041(3) 0.128(6) 0.077(5) -0.039(4) 0.027(3) 0.001(4) C3 0.033(3) 0.070(4) 0.084(4) 0.028(3) 0.016(3) -0.008(3) C4 0.025(2) 0.055(3) 0.040(3) 0.000(2) 0.008(2) 0.005(2) C5 0.029(2) 0.038(3) 0.032(2) -0.0004(19) 0.0031(19) 0.002(2) C6 0.091(5) 0.117(6) 0.070(5) -0.018(4) 0.016(4) 0.065(5) C7 0.277(15) 0.074(5) 0.204(11) -0.023(6) 0.215(12) -0.019(7) C8 0.079(6) 0.273(13) 0.074(5) -0.101(7) -0.010(4) 0.057(7) C9 0.045(3) 0.055(3) 0.034(3) -0.010(2) 0.011(2) 0.007(2) C10 0.035(3) 0.030(2) 0.035(3) -0.0061(18) 0.010(2) -0.0001(19) C11 0.067(4) 0.064(4) 0.132(7) 0.043(4) -0.033(4) -0.046(4) C12 0.111(6) 0.058(4) 0.135(7) 0.027(4) 0.088(6) -0.005(4) C13 0.055(4) 0.026(3) 0.119(6) 0.011(3) 0.017(4) -0.007(2) C14 0.029(2) 0.031(2) 0.062(3) 0.017(2) 0.006(2) -0.005(2) C15 0.023(2) 0.024(2) 0.039(3) 0.0047(18) 0.0077(19) -0.0023(17) C16 0.052(5) 0.029(4) 0.055(5) -0.008(3) -0.008(4) 0.009(4) C17 0.016(7) 0.025(4) 0.035(5) -0.006(3) 0.007(5) 0.008(4) C16' 0.041(9) 0.029(8) 0.067(12) -0.008(7) -0.014(8) 0.005(7) C17' 0.014(15) 0.063(16) 0.08(2) -0.008(12) 0.019(11) -0.001(11) C18 0.047(3) 0.036(3) 0.044(3) -0.012(2) -0.003(2) 0.003(2) C19 0.044(3) 0.039(3) 0.047(3) 0.003(2) 0.000(2) -0.011(2) C20 0.044(3) 0.038(3) 0.046(3) 0.006(2) -0.008(2) -0.008(2) C21 0.049(3) 0.052(3) 0.056(3) 0.012(3) -0.007(3) -0.021(3) C22 0.032(3) 0.036(3) 0.051(3) 0.014(2) 0.001(2) -0.001(2) C23 0.024(2) 0.024(2) 0.042(3) 0.0031(18) -0.0028(19) -0.0013(17) C24 0.031(2) 0.031(2) 0.049(3) 0.008(2) 0.003(2) 0.0049(19) C25 0.039(3) 0.053(3) 0.053(3) 0.005(2) 0.016(2) 0.012(2) C26 0.037(3) 0.125(6) 0.067(4) -0.032(4) -0.004(3) 0.035(4) C27 0.103(6) 0.133(7) 0.046(4) -0.010(4) 0.014(4) 0.062(5) C28 0.089(6) 0.111(6) 0.140(8) -0.018(5) 0.082(6) -0.040(5) C29 0.054(4) 0.089(5) 0.119(6) 0.020(4) 0.019(4) -0.038(4) C30 0.055(4) 0.059(4) 0.201(10) 0.057(5) 0.039(5) -0.010(3) C31 0.036(3) 0.050(3) 0.078(4) 0.016(3) 0.011(3) -0.015(2) C32 0.033(3) 0.032(2) 0.055(3) 0.009(2) 0.007(2) -0.007(2) C33 0.042(4) 0.42(2) 0.188(11) 0.215(14) 0.032(6) -0.013(8) C34 0.143(7) 0.122(6) 0.038(4) 0.007(4) 0.026(4) -0.070(6) C35 0.41(2) 0.053(5) 0.180(11) 0.017(6) 0.208(14) -0.012(8) C36 0.042(3) 0.068(4) 0.045(3) 0.021(3) 0.011(2) -0.004(3) C37 0.029(3) 0.054(3) 0.033(3) 0.009(2) 0.008(2) 0.006(2) C38 0.047(3) 0.028(2) 0.068(4) 0.011(2) -0.004(3) -0.008(2) C39 0.044(3) 0.032(3) 0.062(3) 0.017(2) -0.002(3) -0.001(2) C40 0.063(4) 0.034(3) 0.065(4) -0.007(2) 0.011(3) 0.000(3) C41 0.034(2) 0.022(2) 0.048(3) 0.0045(19) -0.003(2) -0.0026(18) C42 0.033(3) 0.026(2) 0.029(2) 0.0077(17) 0.0035(19) -0.0041(19) _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 Co1 O7 2.030(3) . ? Co1 O5 2.049(3) . ? Co1 O3 2.080(3) . ? Co1 O17 2.097(3) . ? Co1 O2 2.127(3) . ? Co1 O9 2.128(3) 4_666 ? Co2 O4 1.973(3) . ? Co2 O8 1.985(3) . ? Co2 O7 1.987(3) . ? Co2 O6 2.026(3) . ? Co2 O10 2.314(3) . ? Co3 O11 1.874(3) . ? Co3 O10 1.894(3) . ? Co3 O8 1.907(3) . ? Co3 O12 1.929(3) . ? Co3 N2 1.962(4) . ? Co3 N1 1.971(4) . ? Co3 Co4 2.9872(8) . ? Co4 O7 2.035(3) . ? Co4 O13 2.041(3) . ? Co4 O14 2.057(3) . ? Co4 O16 2.079(3) . ? Co4 O10 2.140(3) . ? Co4 O11 2.152(3) . ? O1 C5 1.312(5) . ? O2 C5 1.203(5) . ? O3 C10 1.249(5) . ? O4 C10 1.254(5) . ? O5 C15 1.236(5) . ? O6 C15 1.262(5) . ? O8 C23 1.435(5) . ? O9 C20 1.459(5) . ? O9 Co1 2.128(3) 4_565 ? O10 C17 1.420(14) . ? O10 C17' 1.57(4) . ? O11 C26 1.403(6) . ? O12 C32 1.283(6) . ? O13 C32 1.241(6) . ? O14 C37 1.256(5) . ? O15 C37 1.251(6) . ? O16 C42 1.247(5) . ? O17 C42 1.285(5) . ? N1 C18 1.495(6) . ? N1 C19 1.502(6) . ? N2 C25 1.480(6) . ? N2 C24 1.492(6) . ? C1 C4 1.544(7) . ? C2 C4 1.535(8) . ? C3 C4 1.525(8) . ? C4 C5 1.524(6) . ? C6 C9 1.501(8) . ? C7 C9 1.511(9) . ? C8 C9 1.472(8) . ? C9 C10 1.549(6) . ? C11 C14 1.532(8) . ? C12 C14 1.518(9) . ? C13 C14 1.495(7) . ? C14 C15 1.542(6) . ? C16 C17 1.535(10) . ? C17 C18 1.515(14) . ? C16' C17' 1.530(16) . ? C17' C18 1.53(4) . ? C19 C20 1.496(7) . ? C20 C21 1.524(6) . ? C22 C23 1.507(6) . ? C23 C24 1.515(6) . ? C25 C26 1.509(8) . ? C26 C27 1.370(9) . ? C28 C31 1.554(10) . ? C29 C31 1.502(9) . ? C30 C31 1.492(8) . ? C31 C32 1.538(6) . ? C33 C36 1.490(10) . ? C34 C36 1.503(8) . ? C35 C36 1.497(11) . ? C36 C37 1.530(7) . ? C38 C41 1.535(6) . ? C39 C41 1.527(7) . ? C40 C41 1.532(7) . ? C41 C42 1.541(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Co1 O5 90.65(11) . . ? O7 Co1 O3 98.53(12) . . ? O5 Co1 O3 92.32(13) . . ? O7 Co1 O17 96.87(11) . . ? O5 Co1 O17 172.43(11) . . ? O3 Co1 O17 85.67(12) . . ? O7 Co1 O2 172.13(12) . . ? O5 Co1 O2 84.15(11) . . ? O3 Co1 O2 87.61(12) . . ? O17 Co1 O2 88.47(11) . . ? O7 Co1 O9 88.21(11) . 4_666 ? O5 Co1 O9 90.13(12) . 4_666 ? O3 Co1 O9 172.80(11) . 4_666 ? O17 Co1 O9 91.04(12) . 4_666 ? O2 Co1 O9 85.90(12) . 4_666 ? O4 Co2 O8 115.58(13) . . ? O4 Co2 O7 116.30(12) . . ? O8 Co2 O7 121.26(12) . . ? O4 Co2 O6 97.35(13) . . ? O8 Co2 O6 103.40(11) . . ? O7 Co2 O6 95.47(12) . . ? O4 Co2 O10 93.08(12) . . ? O8 Co2 O10 73.71(10) . . ? O7 Co2 O10 77.92(10) . . ? O6 Co2 O10 169.35(12) . . ? O11 Co3 O10 87.63(12) . . ? O11 Co3 O8 91.48(12) . . ? O10 Co3 O8 85.96(12) . . ? O11 Co3 O12 91.38(13) . . ? O10 Co3 O12 96.10(12) . . ? O8 Co3 O12 176.54(13) . . ? O11 Co3 N2 85.97(15) . . ? O10 Co3 N2 170.71(14) . . ? O8 Co3 N2 87.47(14) . . ? O12 Co3 N2 90.79(14) . . ? O11 Co3 N1 174.61(14) . . ? O10 Co3 N1 87.20(14) . . ? O8 Co3 N1 86.62(14) . . ? O12 Co3 N1 90.70(15) . . ? N2 Co3 N1 98.97(16) . . ? O11 Co3 Co4 45.81(9) . . ? O10 Co3 Co4 45.49(9) . . ? O8 Co3 Co4 102.53(8) . . ? O12 Co3 Co4 80.87(9) . . ? N2 Co3 Co4 130.29(12) . . ? N1 Co3 Co4 129.80(11) . . ? O7 Co4 O13 168.86(12) . . ? O7 Co4 O14 91.44(12) . . ? O13 Co4 O14 97.00(14) . . ? O7 Co4 O16 93.47(11) . . ? O13 Co4 O16 93.08(12) . . ? O14 Co4 O16 94.64(12) . . ? O7 Co4 O10 81.14(11) . . ? O13 Co4 O10 89.26(12) . . ? O14 Co4 O10 167.72(12) . . ? O16 Co4 O10 95.56(11) . . ? O7 Co4 O11 83.26(10) . . ? O13 Co4 O11 88.81(12) . . ? O14 Co4 O11 94.62(12) . . ? O16 Co4 O11 170.25(12) . . ? O10 Co4 O11 74.89(11) . . ? O7 Co4 Co3 91.57(8) . . ? O13 Co4 Co3 77.37(9) . . ? O14 Co4 Co3 132.21(9) . . ? O16 Co4 Co3 132.72(9) . . ? O10 Co4 Co3 39.16(7) . . ? O11 Co4 Co3 38.64(8) . . ? C5 O2 Co1 129.1(3) . . ? C10 O3 Co1 140.6(3) . . ? C10 O4 Co2 121.1(3) . . ? C15 O5 Co1 134.6(3) . . ? C15 O6 Co2 126.6(3) . . ? Co2 O7 Co1 105.41(12) . . ? Co2 O7 Co4 105.73(12) . . ? Co1 O7 Co4 128.24(13) . . ? C23 O8 Co3 110.2(2) . . ? C23 O8 Co2 122.2(2) . . ? Co3 O8 Co2 101.63(12) . . ? C20 O9 Co1 122.7(3) . 4_565 ? C17 O10 C17' 17.2(10) . . ? C17 O10 Co3 106.7(5) . . ? C17' O10 Co3 118.5(14) . . ? C17 O10 Co4 132.1(5) . . ? C17' O10 Co4 135.9(13) . . ? Co3 O10 Co4 95.35(12) . . ? C17 O10 Co2 128.4(5) . . ? C17' O10 Co2 113.2(7) . . ? Co3 O10 Co2 91.06(11) . . ? Co4 O10 Co2 92.04(10) . . ? C26 O11 Co3 113.8(3) . . ? C26 O11 Co4 130.8(4) . . ? Co3 O11 Co4 95.55(12) . . ? C32 O12 Co3 128.2(3) . . ? C32 O13 Co4 128.1(3) . . ? C37 O14 Co4 142.1(3) . . ? C42 O16 Co4 140.0(3) . . ? C42 O17 Co1 132.3(3) . . ? C18 N1 C19 114.6(4) . . ? C18 N1 Co3 105.9(3) . . ? C19 N1 Co3 117.0(3) . . ? C25 N2 C24 113.6(4) . . ? C25 N2 Co3 107.4(3) . . ? C24 N2 Co3 106.3(3) . . ? C5 C4 C3 109.3(4) . . ? C5 C4 C2 108.5(4) . . ? C3 C4 C2 111.4(5) . . ? C5 C4 C1 107.6(4) . . ? C3 C4 C1 109.8(4) . . ? C2 C4 C1 110.2(5) . . ? O2 C5 O1 122.3(4) . . ? O2 C5 C4 122.6(4) . . ? O1 C5 C4 115.1(4) . . ? C8 C9 C6 110.5(6) . . ? C8 C9 C7 112.1(8) . . ? C6 C9 C7 107.1(7) . . ? C8 C9 C10 111.3(5) . . ? C6 C9 C10 110.9(4) . . ? C7 C9 C10 104.8(4) . . ? O3 C10 O4 125.3(4) . . ? O3 C10 C9 117.5(4) . . ? O4 C10 C9 117.2(4) . . ? C13 C14 C12 109.5(5) . . ? C13 C14 C11 109.6(5) . . ? C12 C14 C11 111.5(6) . . ? C13 C14 C15 110.6(4) . . ? C12 C14 C15 104.8(4) . . ? C11 C14 C15 110.7(4) . . ? O5 C15 O6 125.7(4) . . ? O5 C15 C14 117.4(4) . . ? O6 C15 C14 116.9(4) . . ? O10 C17 C18 105.9(6) . . ? O10 C17 C16 112.8(9) . . ? C18 C17 C16 111.8(9) . . ? C18 C17' C16' 111(2) . . ? C18 C17' O10 98.3(17) . . ? C16' C17' O10 102(2) . . ? N1 C18 C17 105.0(5) . . ? N1 C18 C17' 121.1(13) . . ? C17 C18 C17' 17.8(10) . . ? C20 C19 N1 110.6(4) . . ? O9 C20 C19 107.5(4) . . ? O9 C20 C21 111.0(4) . . ? C19 C20 C21 110.6(4) . . ? O8 C23 C22 110.7(4) . . ? O8 C23 C24 106.1(3) . . ? C22 C23 C24 112.5(4) . . ? N2 C24 C23 109.3(3) . . ? N2 C25 C26 114.3(4) . . ? C27 C26 O11 118.7(5) . . ? C27 C26 C25 122.1(6) . . ? O11 C26 C25 110.6(5) . . ? C30 C31 C29 113.5(6) . . ? C30 C31 C32 109.0(4) . . ? C29 C31 C32 111.2(5) . . ? C30 C31 C28 109.9(6) . . ? C29 C31 C28 107.2(6) . . ? C32 C31 C28 105.9(5) . . ? O13 C32 O12 125.1(4) . . ? O13 C32 C31 118.4(4) . . ? O12 C32 C31 116.5(4) . . ? C33 C36 C35 112.1(10) . . ? C33 C36 C34 108.6(7) . . ? C35 C36 C34 110.7(7) . . ? C33 C36 C37 108.6(5) . . ? C35 C36 C37 106.0(5) . . ? C34 C36 C37 110.9(5) . . ? O15 C37 O14 124.2(4) . . ? O15 C37 C36 117.8(4) . . ? O14 C37 C36 118.0(4) . . ? C39 C41 C40 109.1(4) . . ? C39 C41 C38 110.1(4) . . ? C40 C41 C38 110.1(4) . . ? C39 C41 C42 108.7(4) . . ? C40 C41 C42 108.6(4) . . ? C38 C41 C42 110.1(4) . . ? O16 C42 O17 124.5(4) . . ? O16 C42 C41 118.6(4) . . ? O17 C42 C41 116.9(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.569 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.094 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.145 0.932 -0.028 95.8 44.6 2 0.355 0.432 0.528 95.2 44.5 3 0.647 0.569 0.472 95.4 46.8 4 0.853 0.069 0.028 94.7 46.8 #_platon_squeeze_details # END OF CIF