Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chang Seop Hong' _publ_contact_author_address ; Department of Chemistry Korea University Seoul 136-701 SOUTH KOREA ; _publ_contact_author_email CSHONG@KOREA.AC.KR _publ_section_title ; Supramolecular WV-MnIII Bimetallic Assemblies Built by Octacyanotungstate(V) and MnIII-Schiff bases: Molecular Structures and a Spin-Flop Transition ; loop_ _publ_author_name 'Chang Seop Hong' 'Jun Sung Kang' 'Hyoung Chan Kim' 'Hyun Hee Ko' ; Eui Kwan Koh ; 'Jeong Hak Lim' 'Houng Sik Yoo' data_c2-c _database_code_depnum_ccdc_archive 'CCDC 635487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H54 Cl6 Mn3 N14 O12 W' _chemical_formula_weight 1712.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.3856(11) _cell_length_b 19.7550(6) _cell_length_c 20.7631(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.6550(10) _cell_angle_gamma 90.00 _cell_volume 14438.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6824 _exptl_absorpt_coefficient_mu 2.388 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 69834 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.35 _reflns_number_total 17932 _reflns_number_gt 10743 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0836P)^2^+36.7940P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17932 _refine_ls_number_parameters 863 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.177712(8) 0.992971(12) 0.696509(14) 0.03233(9) Uani 1 1 d . . . C1 C 0.18413(19) 1.0650(4) 0.7787(4) 0.0431(17) Uani 1 1 d . . . N1 N 0.18975(19) 1.1028(4) 0.8238(4) 0.065(2) Uani 1 1 d . . . C2 C 0.20059(19) 1.0565(3) 0.6419(4) 0.0376(15) Uani 1 1 d . . . N2 N 0.21310(17) 1.0915(3) 0.6134(3) 0.0519(16) Uani 1 1 d . . . C3 C 0.1367(2) 1.0718(4) 0.6380(4) 0.053(2) Uani 1 1 d . . . N3 N 0.1152(2) 1.1108(4) 0.6033(5) 0.085(3) Uani 1 1 d . . . C4 C 0.1388(2) 0.9458(6) 0.5981(5) 0.072(3) Uani 1 1 d . . . N4 N 0.1173(2) 0.9208(6) 0.5448(5) 0.112(4) Uani 1 1 d . . . C5 C 0.1280(2) 0.9736(4) 0.7142(4) 0.0421(17) Uani 1 1 d . . . N5 N 0.10276(18) 0.9599(4) 0.7239(3) 0.0549(17) Uani 1 1 d . . . C6 C 0.1892(2) 0.9101(4) 0.7703(4) 0.0485(19) Uani 1 1 d . . . N6 N 0.1956(2) 0.8649(4) 0.8082(4) 0.076(2) Uani 1 1 d . . . C7 C 0.2082(2) 0.9195(4) 0.6652(4) 0.0466(18) Uani 1 1 d . . . N7 N 0.2242(2) 0.8790(4) 0.6500(4) 0.070(2) Uani 1 1 d . . . C8 C 0.2377(2) 1.0028(4) 0.7683(4) 0.0468(18) Uani 1 1 d . . . N8 N 0.2692(2) 1.0101(4) 0.8035(4) 0.069(2) Uani 1 1 d . . . Mn1 Mn 0.21169(3) 1.15591(5) 0.52067(6) 0.0472(3) Uani 1 1 d . . . O1 O 0.21605(14) 1.2372(2) 0.5701(2) 0.0467(12) Uani 1 1 d . . . C9 C 0.1886(2) 1.2755(4) 0.5711(4) 0.0459(18) Uani 1 1 d . . . C10 C 0.1993(2) 1.3356(4) 0.6121(4) 0.057(2) Uani 1 1 d . . . H10 H 0.2248 1.3473 0.6358 0.068 Uiso 1 1 calc R . . C11 C 0.1726(2) 1.3776(4) 0.6178(4) 0.059(2) Uani 1 1 d . . . H11 H 0.1802 1.4163 0.6462 0.071 Uiso 1 1 calc R . . C12 C 0.1345(3) 1.3612(5) 0.5809(5) 0.066(2) Uani 1 1 d . . . Cl1 Cl 0.10102(8) 1.41530(15) 0.58611(19) 0.1046(10) Uani 1 1 d . . . C13 C 0.1231(2) 1.3039(5) 0.5398(5) 0.068(3) Uani 1 1 d . . . H13 H 0.0974 1.2941 0.5148 0.081 Uiso 1 1 calc R . . C14 C 0.1497(2) 1.2599(4) 0.5350(4) 0.053(2) Uani 1 1 d . . . C15 C 0.1360(3) 1.2011(5) 0.4916(4) 0.061(2) Uani 1 1 d . . . H15 H 0.1098 1.1955 0.4683 0.073 Uiso 1 1 calc R . . N9 N 0.15543(19) 1.1556(4) 0.4813(4) 0.0605(19) Uani 1 1 d . . . C16 C 0.1350(4) 1.0975(6) 0.4360(8) 0.136(6) Uani 1 1 d . . . H16A H 0.1191 1.0765 0.4548 0.163 Uiso 1 1 calc R . . H16B H 0.1189 1.1126 0.3872 0.163 Uiso 1 1 calc R . . C17 C 0.1611(4) 1.0522(9) 0.4360(10) 0.173(9) Uani 1 1 d . . . H17 H 0.1568 1.0667 0.3878 0.208 Uiso 1 1 calc R . . C18 C 0.1484(6) 0.9883(8) 0.4114(12) 0.190(9) Uani 1 1 d . . . H18A H 0.1571 0.9575 0.4514 0.286 Uiso 1 1 calc R . . H18B H 0.1581 0.9745 0.3785 0.286 Uiso 1 1 calc R . . H18C H 0.1212 0.9882 0.3872 0.286 Uiso 1 1 calc R . . N10 N 0.2020(2) 1.0696(4) 0.4664(4) 0.070(2) Uani 1 1 d . . . C19 C 0.2269(3) 1.0336(5) 0.4601(5) 0.072(3) Uani 1 1 d . . . H19 H 0.2186 0.9941 0.4332 0.086 Uiso 1 1 calc R . . C20 C 0.2674(3) 1.0484(4) 0.4911(4) 0.056(2) Uani 1 1 d . . . C21 C 0.2897(3) 1.0028(4) 0.4755(5) 0.064(3) Uani 1 1 d . . . H21 H 0.2787 0.9652 0.4465 0.077 Uiso 1 1 calc R . . C22 C 0.3278(3) 1.0139(4) 0.5032(5) 0.065(3) Uani 1 1 d . . . Cl2 Cl 0.35558(9) 0.95744(13) 0.48171(15) 0.0895(8) Uani 1 1 d . . . C23 C 0.3451(3) 1.0674(4) 0.5476(5) 0.062(2) Uani 1 1 d . . . H23 H 0.3713 1.0732 0.5669 0.074 Uiso 1 1 calc R . . C24 C 0.3232(2) 1.1125(4) 0.5633(4) 0.056(2) Uani 1 1 d . . . H24 H 0.3348 1.1494 0.5929 0.067 Uiso 1 1 calc R . . C25 C 0.2843(2) 1.1041(4) 0.5358(4) 0.051(2) Uani 1 1 d . . . O2 O 0.26480(15) 1.1498(3) 0.5530(3) 0.0537(14) Uani 1 1 d . . . O3 O 0.20312(17) 1.2165(3) 0.4218(3) 0.0613(15) Uani 1 1 d . . . Mn2 Mn 0.23727(3) 0.78069(5) 0.60714(6) 0.0426(3) Uani 1 1 d . . . O4 O 0.27541(15) 0.8202(2) 0.5896(3) 0.0481(12) Uani 1 1 d . . . C26 C 0.3122(2) 0.8290(3) 0.6337(4) 0.0460(18) Uani 1 1 d . . . C27 C 0.3351(2) 0.8649(4) 0.6085(4) 0.054(2) Uani 1 1 d . . . H27 H 0.3240 0.8812 0.5615 0.065 Uiso 1 1 calc R . . C28 C 0.3725(2) 0.8763(4) 0.6510(5) 0.059(2) Uani 1 1 d . . . H28 H 0.3869 0.9006 0.6335 0.071 Uiso 1 1 calc R . . C29 C 0.3895(2) 0.8511(4) 0.7217(5) 0.060(2) Uani 1 1 d . . . Cl3 Cl 0.43760(7) 0.86575(14) 0.77535(16) 0.0916(8) Uani 1 1 d . . . C30 C 0.3686(2) 0.8146(4) 0.7480(4) 0.055(2) Uani 1 1 d . . . H30 H 0.3803 0.7981 0.7950 0.066 Uiso 1 1 calc R . . C31 C 0.3300(2) 0.8020(4) 0.7049(4) 0.0473(18) Uani 1 1 d . . . C32 C 0.3105(2) 0.7642(4) 0.7359(4) 0.052(2) Uani 1 1 d . . . H32 H 0.3247 0.7467 0.7819 0.063 Uiso 1 1 calc R . . N11 N 0.2748(2) 0.7525(3) 0.7055(3) 0.0502(16) Uani 1 1 d . . . C33 C 0.2574(3) 0.7095(7) 0.7419(5) 0.104(4) Uani 1 1 d . . . C34A C 0.2192(4) 0.7274(8) 0.7214(8) 0.046(4) Uiso 0.50 1 d P . . C34B C 0.2218(5) 0.6858(9) 0.7001(9) 0.059(4) Uiso 0.50 1 d P . . C35 C 0.1971(3) 0.6769(6) 0.7419(6) 0.091(3) Uani 1 1 d . . . N12 N 0.2021(2) 0.7320(4) 0.6351(4) 0.0596(18) Uani 1 1 d . . . C36 C 0.1680(3) 0.7197(4) 0.5923(5) 0.058(2) Uani 1 1 d . . . H36 H 0.1545 0.6938 0.6106 0.069 Uiso 1 1 calc R . . C37 C 0.1474(2) 0.7409(4) 0.5189(4) 0.0503(19) Uani 1 1 d . . . C38 C 0.1093(3) 0.7227(4) 0.4816(5) 0.066(2) Uani 1 1 d . . . H38 H 0.0983 0.6965 0.5045 0.079 Uiso 1 1 calc R . . C39 C 0.0878(3) 0.7425(5) 0.4125(5) 0.067(2) Uani 1 1 d . . . Cl4 Cl 0.04037(8) 0.71781(17) 0.36581(18) 0.1103(11) Uani 1 1 d . . . C40 C 0.1030(3) 0.7840(4) 0.3789(5) 0.067(2) Uani 1 1 d . . . H40 H 0.0879 0.7995 0.3325 0.081 Uiso 1 1 calc R . . C41 C 0.1404(2) 0.8024(4) 0.4136(4) 0.055(2) Uani 1 1 d . . . H41 H 0.1504 0.8299 0.3900 0.066 Uiso 1 1 calc R . . C42 C 0.1639(2) 0.7807(3) 0.4841(4) 0.0461(18) Uani 1 1 d . . . O5 O 0.19951(15) 0.7995(3) 0.5145(3) 0.0509(13) Uani 1 1 d . . . O6 O 0.24741(15) 0.6774(3) 0.5645(3) 0.0545(13) Uani 1 1 d . . . Mn3 Mn 1.00786(3) 0.15006(6) 0.38815(7) 0.0486(3) Uani 1 1 d . . . O7 O 1.03283(15) 0.0677(3) 0.4000(4) 0.0701(17) Uani 1 1 d . . . C43 C 1.0148(3) 0.0092(4) 0.3888(6) 0.065(3) Uani 1 1 d . . . C44 C 1.0289(3) -0.0447(5) 0.3618(6) 0.085(3) Uani 1 1 d . . . H44 H 1.0506 -0.0388 0.3556 0.102 Uiso 1 1 calc R . . C45 C 1.0095(3) -0.1069(5) 0.3447(6) 0.082(3) Uani 1 1 d . . . H45 H 1.0180 -0.1424 0.3264 0.099 Uiso 1 1 calc R . . C46 C 0.9776(3) -0.1146(4) 0.3556(5) 0.064(2) Uani 1 1 d . . . Cl5 Cl 0.95348(8) -0.19214(13) 0.33012(17) 0.0953(9) Uani 1 1 d . . . C47 C 0.9643(2) -0.0648(4) 0.3830(4) 0.055(2) Uani 1 1 d . . . H47 H 0.9432 -0.0726 0.3909 0.067 Uiso 1 1 calc R . . C48 C 0.9821(2) -0.0022(4) 0.3992(4) 0.0510(19) Uani 1 1 d . . . C49 C 0.9665(2) 0.0507(4) 0.4254(4) 0.055(2) Uani 1 1 d . . . H49 H 0.9489 0.0382 0.4417 0.065 Uiso 1 1 calc R . . N13 N 0.97473(16) 0.1131(3) 0.4280(3) 0.0465(15) Uani 1 1 d . . . C50 C 0.9586(2) 0.1644(4) 0.4565(5) 0.059(2) Uani 1 1 d . . . H50A H 0.9771 0.1780 0.5044 0.071 Uiso 1 1 calc R . . H50B H 0.9365 0.1466 0.4597 0.071 Uiso 1 1 calc R . . C51 C 0.9475(3) 0.2248(4) 0.4055(5) 0.069(3) Uani 1 1 d . . . H51 H 0.9465 0.2652 0.4321 0.083 Uiso 1 1 calc R . . C52 C 0.9097(3) 0.2155(5) 0.3426(6) 0.086(3) Uani 1 1 d . . . H52A H 0.9108 0.1786 0.3137 0.129 Uiso 1 1 calc R . . H52B H 0.9027 0.2562 0.3143 0.129 Uiso 1 1 calc R . . H52C H 0.8910 0.2059 0.3593 0.129 Uiso 1 1 calc R . . N14 N 0.97914(18) 0.2333(3) 0.3845(3) 0.0515(16) Uani 1 1 d . . . C53 C 0.9877(2) 0.2927(4) 0.3700(4) 0.058(2) Uani 1 1 d . . . H53 H 0.9731 0.3289 0.3720 0.069 Uiso 1 1 calc R . . C54 C 1.0178(2) 0.3074(4) 0.3511(4) 0.055(2) Uani 1 1 d . . . C55 C 1.0233(3) 0.3771(5) 0.3401(5) 0.075(3) Uani 1 1 d . . . H55 H 1.0084 0.4101 0.3471 0.090 Uiso 1 1 calc R . . C56 C 1.0504(3) 0.3954(5) 0.3194(5) 0.077(3) Uani 1 1 d . . . Cl6 Cl 1.05601(10) 0.48013(15) 0.3048(2) 0.1272(14) Uani 1 1 d . . . C57 C 1.0726(3) 0.3485(5) 0.3104(5) 0.078(3) Uani 1 1 d . . . H57 H 1.0915 0.3617 0.2978 0.094 Uiso 1 1 calc R . . C58 C 1.0673(2) 0.2797(4) 0.3198(4) 0.063(2) Uani 1 1 d . . . H58 H 1.0826 0.2476 0.3128 0.075 Uiso 1 1 calc R . . C59 C 1.0398(2) 0.2586(4) 0.3393(4) 0.051(2) Uani 1 1 d . . . O8 O 1.03545(15) 0.1928(3) 0.3446(3) 0.0553(14) Uani 1 1 d . . . O9 O 0.96187(16) 0.1176(3) 0.2759(3) 0.0635(15) Uani 1 1 d . . . O10 O 1.05096(15) 0.1855(3) 0.5012(3) 0.0632(15) Uani 1 1 d . . . O11A O -0.0181(7) 0.5686(13) 0.0463(13) 0.119(8) Uiso 0.33 1 d P . . O11B O 0.0238(4) 0.6910(7) 0.0382(7) 0.045(3) Uiso 0.33 1 d P . . O11C O 0.0060(6) 0.6399(12) 0.0357(12) 0.096(6) Uiso 0.33 1 d P . . O12A O 0.1500(5) 0.5271(9) 0.7552(10) 0.067(5) Uiso 0.33 1 d P . . O12B O 0.1236(6) 0.5609(11) 0.7111(12) 0.084(6) Uiso 0.33 1 d P . . O12C O 0.1001(7) 0.5934(13) 0.6581(13) 0.107(7) Uiso 0.33 1 d P . . 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 W1 0.04213(15) 0.02913(14) 0.03021(15) 0.00413(12) 0.02021(12) 0.00067(11) C1 0.046(4) 0.039(4) 0.054(5) -0.003(4) 0.031(4) -0.004(3) N1 0.066(4) 0.064(5) 0.077(5) -0.027(4) 0.043(4) -0.008(4) C2 0.045(4) 0.036(4) 0.035(4) 0.007(3) 0.020(3) 0.000(3) N2 0.051(4) 0.052(4) 0.053(4) 0.014(3) 0.024(3) -0.004(3) C3 0.047(4) 0.052(5) 0.065(5) 0.032(4) 0.029(4) 0.018(4) N3 0.066(5) 0.096(6) 0.106(7) 0.056(5) 0.051(5) 0.030(4) C4 0.053(5) 0.120(9) 0.046(5) -0.030(5) 0.026(4) -0.014(5) N4 0.080(6) 0.189(11) 0.074(6) -0.054(7) 0.040(5) -0.040(7) C5 0.050(4) 0.043(4) 0.035(4) 0.004(3) 0.020(3) -0.003(3) N5 0.051(4) 0.065(4) 0.056(4) 0.006(4) 0.030(3) -0.004(3) C6 0.062(5) 0.044(4) 0.053(5) 0.014(4) 0.038(4) 0.012(4) N6 0.096(6) 0.075(5) 0.083(6) 0.049(5) 0.063(5) 0.038(4) C7 0.070(5) 0.033(4) 0.046(5) 0.001(3) 0.034(4) 0.004(3) N7 0.122(6) 0.047(4) 0.066(5) 0.006(4) 0.064(5) 0.018(4) C8 0.047(4) 0.047(4) 0.038(4) 0.002(3) 0.011(3) 0.008(3) N8 0.056(5) 0.078(5) 0.061(5) 0.010(4) 0.015(4) 0.011(4) Mn1 0.0658(7) 0.0407(6) 0.0367(6) -0.0077(5) 0.0243(6) -0.0241(5) O1 0.057(3) 0.045(3) 0.038(3) -0.013(2) 0.021(3) -0.019(2) C9 0.058(5) 0.047(4) 0.033(4) 0.004(3) 0.021(4) -0.010(4) C10 0.066(5) 0.056(5) 0.045(5) 0.000(4) 0.022(4) -0.015(4) C11 0.073(6) 0.060(5) 0.050(5) -0.001(4) 0.033(5) -0.010(4) C12 0.066(6) 0.068(6) 0.076(6) 0.008(5) 0.042(5) -0.002(5) Cl1 0.0894(19) 0.087(2) 0.156(3) 0.007(2) 0.072(2) 0.0062(15) C13 0.050(5) 0.071(6) 0.084(7) 0.014(5) 0.031(5) -0.014(4) C14 0.062(5) 0.053(5) 0.042(4) 0.003(4) 0.023(4) -0.019(4) C15 0.066(6) 0.057(5) 0.048(5) 0.006(4) 0.016(4) -0.019(4) N9 0.061(4) 0.055(4) 0.049(4) -0.004(4) 0.010(3) -0.029(4) C16 0.127(11) 0.066(8) 0.172(14) -0.041(9) 0.030(10) 0.014(7) C17 0.147(13) 0.163(15) 0.239(19) -0.167(15) 0.113(13) -0.141(12) C18 0.22(2) 0.158(17) 0.25(2) 0.029(16) 0.15(2) 0.065(15) N10 0.104(6) 0.042(4) 0.066(5) -0.020(4) 0.040(5) -0.028(4) C19 0.115(8) 0.041(5) 0.058(6) -0.023(4) 0.037(6) -0.040(5) C20 0.101(7) 0.031(4) 0.044(5) -0.006(3) 0.040(5) -0.018(4) C21 0.113(8) 0.036(5) 0.045(5) 0.001(4) 0.036(5) -0.017(5) C22 0.118(8) 0.036(4) 0.058(6) 0.006(4) 0.054(6) 0.005(5) Cl2 0.139(2) 0.0594(15) 0.0902(19) 0.0047(14) 0.0697(18) 0.0167(15) C23 0.081(6) 0.051(5) 0.057(5) 0.003(4) 0.034(5) 0.005(4) C24 0.083(6) 0.045(5) 0.042(5) -0.002(4) 0.030(5) -0.011(4) C25 0.079(6) 0.039(4) 0.039(4) 0.000(3) 0.030(4) -0.017(4) O2 0.070(4) 0.047(3) 0.050(3) -0.017(3) 0.032(3) -0.023(3) O3 0.099(4) 0.051(3) 0.044(3) -0.013(3) 0.041(3) -0.031(3) Mn2 0.0623(7) 0.0365(6) 0.0376(6) 0.0024(5) 0.0301(6) 0.0046(5) O4 0.066(3) 0.047(3) 0.039(3) 0.003(2) 0.031(3) -0.005(2) C26 0.068(5) 0.029(4) 0.041(4) -0.005(3) 0.025(4) 0.001(3) C27 0.078(6) 0.038(4) 0.050(5) 0.009(4) 0.032(5) 0.006(4) C28 0.062(5) 0.046(5) 0.067(6) 0.005(4) 0.026(5) -0.005(4) C29 0.057(5) 0.047(5) 0.071(6) 0.002(4) 0.025(5) 0.003(4) Cl3 0.0688(15) 0.0864(18) 0.099(2) 0.0241(16) 0.0191(14) -0.0081(13) C30 0.064(5) 0.049(5) 0.046(5) -0.001(4) 0.019(4) 0.005(4) C31 0.061(5) 0.042(4) 0.046(4) -0.003(4) 0.031(4) -0.001(3) C32 0.069(6) 0.051(5) 0.035(4) 0.003(4) 0.022(4) 0.006(4) N11 0.073(5) 0.051(4) 0.035(3) 0.007(3) 0.033(3) 0.000(3) C33 0.072(7) 0.176(12) 0.060(6) 0.053(7) 0.025(5) -0.024(7) C35 0.088(7) 0.111(9) 0.089(8) 0.046(7) 0.054(6) -0.007(6) N12 0.056(4) 0.069(5) 0.058(4) 0.023(4) 0.030(4) 0.005(3) C36 0.067(6) 0.059(5) 0.065(6) 0.013(4) 0.044(5) 0.004(4) C37 0.058(5) 0.040(4) 0.057(5) -0.001(4) 0.030(4) 0.006(4) C38 0.079(6) 0.055(5) 0.083(7) 0.011(5) 0.053(6) 0.002(4) C39 0.063(6) 0.063(6) 0.078(7) 0.001(5) 0.033(5) 0.002(4) Cl4 0.0665(17) 0.115(2) 0.124(3) 0.016(2) 0.0201(17) -0.0140(16) C40 0.066(6) 0.065(6) 0.060(6) 0.002(5) 0.018(5) 0.007(5) C41 0.066(5) 0.045(5) 0.054(5) 0.004(4) 0.026(4) 0.006(4) C42 0.066(5) 0.032(4) 0.049(5) 0.000(3) 0.033(4) 0.011(3) O5 0.057(3) 0.056(3) 0.045(3) 0.010(3) 0.027(3) -0.001(3) O6 0.085(4) 0.045(3) 0.043(3) -0.002(2) 0.037(3) 0.003(3) Mn3 0.0530(7) 0.0389(6) 0.0587(8) 0.0048(6) 0.0293(6) -0.0034(5) O7 0.060(3) 0.045(3) 0.117(5) 0.007(3) 0.050(4) 0.000(3) C43 0.060(5) 0.040(4) 0.099(8) 0.010(5) 0.039(5) 0.001(4) C44 0.091(7) 0.053(6) 0.142(10) 0.005(6) 0.079(7) 0.002(5) C45 0.104(8) 0.047(5) 0.119(9) -0.004(6) 0.071(7) -0.002(5) C46 0.071(6) 0.043(5) 0.067(6) 0.009(4) 0.021(5) -0.010(4) Cl5 0.103(2) 0.0606(15) 0.118(2) -0.0178(15) 0.0458(18) -0.0266(14) C47 0.066(5) 0.044(5) 0.053(5) 0.010(4) 0.024(4) -0.004(4) C48 0.049(4) 0.049(5) 0.054(5) 0.013(4) 0.021(4) -0.003(4) C49 0.053(5) 0.059(5) 0.052(5) 0.011(4) 0.024(4) -0.005(4) N13 0.045(3) 0.046(4) 0.047(4) 0.001(3) 0.020(3) -0.005(3) C50 0.060(5) 0.061(5) 0.064(6) -0.004(5) 0.035(5) -0.006(4) C51 0.069(6) 0.053(5) 0.087(7) -0.012(5) 0.036(6) -0.010(4) C52 0.073(7) 0.085(7) 0.100(8) -0.001(6) 0.039(6) 0.005(5) N14 0.051(4) 0.042(4) 0.059(4) 0.001(3) 0.022(3) 0.003(3) C53 0.061(5) 0.044(5) 0.054(5) -0.006(4) 0.014(4) -0.001(4) C54 0.058(5) 0.040(4) 0.047(5) 0.000(4) 0.007(4) -0.012(4) C55 0.081(7) 0.051(5) 0.069(6) 0.005(5) 0.014(5) -0.014(5) C56 0.080(7) 0.056(6) 0.078(7) 0.012(5) 0.021(6) -0.025(5) Cl6 0.123(3) 0.0647(17) 0.163(3) 0.037(2) 0.036(2) -0.0332(16) C57 0.070(6) 0.087(8) 0.062(6) 0.015(6) 0.015(5) -0.039(6) C58 0.072(6) 0.057(5) 0.055(5) -0.002(4) 0.024(5) -0.020(4) C59 0.059(5) 0.051(5) 0.034(4) -0.001(4) 0.013(4) -0.017(4) O8 0.068(3) 0.045(3) 0.063(4) 0.001(3) 0.039(3) -0.011(3) O9 0.073(4) 0.062(4) 0.058(4) -0.007(3) 0.031(3) -0.019(3) O10 0.054(3) 0.069(4) 0.061(4) 0.005(3) 0.021(3) -0.010(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 W1 C4 2.141(9) . ? W1 C2 2.142(7) . ? W1 C6 2.147(7) . ? W1 C1 2.148(8) . ? W1 C7 2.161(7) . ? W1 C8 2.165(8) . ? W1 C3 2.179(7) . ? W1 C5 2.180(8) . ? C1 N1 1.139(9) . ? C2 N2 1.154(8) . ? N2 Mn1 2.288(6) . ? C3 N3 1.133(9) . ? C4 N4 1.160(10) . ? C5 N5 1.134(8) . ? C6 N6 1.142(9) . ? C7 N7 1.147(9) . ? N7 Mn2 2.289(7) . ? C8 N8 1.130(10) . ? Mn1 O1 1.871(5) . ? Mn1 O2 1.893(5) . ? Mn1 N10 1.984(7) . ? Mn1 N9 1.988(7) . ? Mn1 O3 2.266(5) . ? O1 C9 1.328(9) . ? C9 C14 1.405(10) . ? C9 C10 1.409(10) . ? C10 C11 1.386(11) . ? C11 C12 1.380(11) . ? C12 C13 1.366(12) . ? C12 Cl1 1.739(9) . ? C13 C14 1.399(12) . ? C14 C15 1.419(11) . ? C15 N9 1.259(11) . ? N9 C16 1.473(13) . ? C16 C17 1.360(18) . ? C17 C18 1.368(19) . ? C17 N10 1.484(14) . ? N10 C19 1.265(12) . ? C19 C20 1.457(12) . ? C20 C21 1.395(12) . ? C20 C25 1.402(10) . ? C21 C22 1.363(14) . ? C22 C23 1.367(12) . ? C22 Cl2 1.755(10) . ? C23 C24 1.376(11) . ? C24 C25 1.386(11) . ? C25 O2 1.332(9) . ? Mn2 O5 1.866(5) . ? Mn2 O4 1.868(5) . ? Mn2 N12 1.975(7) . ? Mn2 N11 1.989(6) . ? Mn2 O6 2.329(5) . ? O4 C26 1.334(9) . ? C26 C27 1.417(10) . ? C26 C31 1.425(10) . ? C27 C28 1.356(11) . ? C28 C29 1.402(11) . ? C29 C30 1.378(11) . ? C29 Cl3 1.740(8) . ? C30 C31 1.397(10) . ? C31 C32 1.417(10) . ? C32 N11 1.278(9) . ? N11 C33 1.490(10) . ? C33 C34B 1.360(18) . ? C33 C34A 1.411(18) . ? C34A C34B 0.958(19) . ? C34A C35 1.504(17) . ? C34A N12 1.611(16) . ? C34B N12 1.523(18) . ? C34B C35 1.574(19) . ? N12 C36 1.258(10) . ? C36 C37 1.430(11) . ? C37 C38 1.394(11) . ? C37 C42 1.406(10) . ? C38 C39 1.355(12) . ? C39 C40 1.377(12) . ? C39 Cl4 1.744(9) . ? C40 C41 1.364(11) . ? C41 C42 1.404(10) . ? C42 O5 1.309(9) . ? Mn3 O7 1.860(5) . ? Mn3 O8 1.896(5) . ? Mn3 N13 1.972(6) . ? Mn3 N14 1.978(6) . ? Mn3 O10 2.304(6) . ? Mn3 O9 2.310(5) . ? O7 C43 1.320(9) . ? C43 C48 1.417(11) . ? C43 C44 1.427(13) . ? C44 C45 1.405(13) . ? C45 C46 1.379(12) . ? C46 C47 1.354(12) . ? C46 Cl5 1.754(8) . ? C47 C48 1.386(10) . ? C48 C49 1.437(11) . ? C49 N13 1.270(9) . ? N13 C50 1.456(10) . ? C50 C51 1.523(12) . ? C51 C52 1.487(12) . ? C51 N14 1.505(10) . ? N14 C53 1.293(9) . ? C53 C54 1.438(11) . ? C54 C59 1.388(11) . ? C54 C55 1.428(11) . ? C55 C56 1.367(13) . ? C56 C57 1.343(14) . ? C56 Cl6 1.732(9) . ? C57 C58 1.403(12) . ? C58 C59 1.381(11) . ? C59 O8 1.321(9) . ? O11A O11C 1.77(3) . ? O11B O11C 1.22(2) . ? O12A O12B 1.23(2) . ? O12B O12C 1.25(3) . ? 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 C4 W1 C2 92.3(3) . . ? C4 W1 C6 100.4(4) . . ? C2 W1 C6 145.1(3) . . ? C4 W1 C1 145.6(3) . . ? C2 W1 C1 96.1(3) . . ? C6 W1 C1 91.5(3) . . ? C4 W1 C7 71.2(3) . . ? C2 W1 C7 79.1(3) . . ? C6 W1 C7 74.6(3) . . ? C1 W1 C7 143.2(3) . . ? C4 W1 C8 142.2(3) . . ? C2 W1 C8 73.9(3) . . ? C6 W1 C8 76.2(3) . . ? C1 W1 C8 72.0(3) . . ? C7 W1 C8 71.7(3) . . ? C4 W1 C3 75.2(4) . . ? C2 W1 C3 70.6(3) . . ? C6 W1 C3 144.1(3) . . ? C1 W1 C3 76.3(3) . . ? C7 W1 C3 133.2(3) . . ? C8 W1 C3 128.8(3) . . ? C4 W1 C5 76.8(3) . . ? C2 W1 C5 144.5(3) . . ? C6 W1 C5 70.4(3) . . ? C1 W1 C5 77.1(3) . . ? C7 W1 C5 126.4(3) . . ? C8 W1 C5 133.3(3) . . ? C3 W1 C5 74.0(3) . . ? N1 C1 W1 176.0(7) . . ? N2 C2 W1 178.8(6) . . ? C2 N2 Mn1 155.4(6) . . ? N3 C3 W1 175.3(9) . . ? N4 C4 W1 179.2(10) . . ? N5 C5 W1 176.2(7) . . ? N6 C6 W1 178.1(7) . . ? N7 C7 W1 177.8(7) . . ? C7 N7 Mn2 161.1(7) . . ? N8 C8 W1 176.7(7) . . ? O1 Mn1 O2 92.6(2) . . ? O1 Mn1 N10 174.6(3) . . ? O2 Mn1 N10 92.7(3) . . ? O1 Mn1 N9 92.3(3) . . ? O2 Mn1 N9 175.1(3) . . ? N10 Mn1 N9 82.4(3) . . ? O1 Mn1 O3 89.1(2) . . ? O2 Mn1 O3 92.7(2) . . ? N10 Mn1 O3 91.5(3) . . ? N9 Mn1 O3 86.8(2) . . ? O1 Mn1 N2 93.1(2) . . ? O2 Mn1 N2 93.4(2) . . ? N10 Mn1 N2 85.8(3) . . ? N9 Mn1 N2 86.9(3) . . ? O3 Mn1 N2 173.4(2) . . ? C9 O1 Mn1 128.6(4) . . ? O1 C9 C14 124.5(7) . . ? O1 C9 C10 117.7(7) . . ? C14 C9 C10 117.8(8) . . ? C11 C10 C9 121.6(8) . . ? C12 C11 C10 119.2(8) . . ? C13 C12 C11 120.8(9) . . ? C13 C12 Cl1 120.1(7) . . ? C11 C12 Cl1 119.1(8) . . ? C12 C13 C14 120.9(8) . . ? C13 C14 C9 119.7(8) . . ? C13 C14 C15 118.1(8) . . ? C9 C14 C15 122.1(8) . . ? N9 C15 C14 127.3(8) . . ? C15 N9 C16 117.8(8) . . ? C15 N9 Mn1 125.2(6) . . ? C16 N9 Mn1 116.9(7) . . ? C17 C16 N9 108.5(10) . . ? C16 C17 C18 117.3(13) . . ? C16 C17 N10 121.4(10) . . ? C18 C17 N10 121.1(17) . . ? C19 N10 C17 124.7(9) . . ? C19 N10 Mn1 125.5(6) . . ? C17 N10 Mn1 109.7(8) . . ? N10 C19 C20 126.0(8) . . ? C21 C20 C25 120.0(9) . . ? C21 C20 C19 116.5(8) . . ? C25 C20 C19 123.5(8) . . ? C22 C21 C20 119.1(8) . . ? C21 C22 C23 122.2(9) . . ? C21 C22 Cl2 119.0(7) . . ? C23 C22 Cl2 118.8(9) . . ? C22 C23 C24 118.8(9) . . ? C23 C24 C25 121.4(8) . . ? O2 C25 C24 118.3(7) . . ? O2 C25 C20 123.3(8) . . ? C24 C25 C20 118.4(8) . . ? C25 O2 Mn1 128.8(5) . . ? O5 Mn2 O4 93.1(2) . . ? O5 Mn2 N12 93.4(3) . . ? O4 Mn2 N12 172.8(3) . . ? O5 Mn2 N11 174.4(3) . . ? O4 Mn2 N11 91.5(2) . . ? N12 Mn2 N11 81.8(3) . . ? O5 Mn2 N7 91.0(3) . . ? O4 Mn2 N7 93.6(2) . . ? N12 Mn2 N7 89.4(3) . . ? N11 Mn2 N7 91.8(3) . . ? O5 Mn2 O6 88.6(2) . . ? O4 Mn2 O6 90.1(2) . . ? N12 Mn2 O6 87.0(3) . . ? N11 Mn2 O6 88.3(2) . . ? N7 Mn2 O6 176.3(2) . . ? C26 O4 Mn2 129.9(5) . . ? O4 C26 C27 119.0(7) . . ? O4 C26 C31 122.8(7) . . ? C27 C26 C31 118.2(7) . . ? C28 C27 C26 121.9(8) . . ? C27 C28 C29 119.3(8) . . ? C30 C29 C28 120.9(8) . . ? C30 C29 Cl3 120.4(7) . . ? C28 C29 Cl3 118.7(7) . . ? C29 C30 C31 120.6(8) . . ? C30 C31 C32 117.3(7) . . ? C30 C31 C26 119.0(7) . . ? C32 C31 C26 123.6(7) . . ? N11 C32 C31 125.0(7) . . ? C32 N11 C33 120.4(7) . . ? C32 N11 Mn2 127.0(5) . . ? C33 N11 Mn2 112.5(5) . . ? C34B C33 C34A 40.4(8) . . ? C34B C33 N11 116.7(10) . . ? C34A C33 N11 111.9(10) . . ? C34B C34A C33 66.9(15) . . ? C34B C34A C35 75.9(15) . . ? C33 C34A C35 115.0(12) . . ? C34B C34A N12 67.2(15) . . ? C33 C34A N12 101.9(10) . . ? C35 C34A N12 110.2(10) . . ? C34A C34B C33 72.7(16) . . ? C34A C34B N12 77.3(15) . . ? C33 C34B N12 109.2(13) . . ? C34A C34B C35 67.9(15) . . ? C33 C34B C35 113.7(13) . . ? N12 C34B C35 111.2(11) . . ? C34A C35 C34B 36.2(7) . . ? C36 N12 C34B 117.8(9) . . ? C36 N12 C34A 123.7(8) . . ? C34B N12 C34A 35.5(7) . . ? C36 N12 Mn2 123.7(6) . . ? C34B N12 Mn2 114.1(7) . . ? C34A N12 Mn2 110.9(7) . . ? N12 C36 C37 127.5(8) . . ? C38 C37 C42 119.2(8) . . ? C38 C37 C36 118.1(8) . . ? C42 C37 C36 122.7(7) . . ? C39 C38 C37 121.3(8) . . ? C38 C39 C40 120.1(9) . . ? C38 C39 Cl4 120.8(8) . . ? C40 C39 Cl4 119.1(8) . . ? C41 C40 C39 120.2(9) . . ? C40 C41 C42 121.3(8) . . ? O5 C42 C41 118.6(7) . . ? O5 C42 C37 123.5(7) . . ? C41 C42 C37 117.8(8) . . ? C42 O5 Mn2 128.8(5) . . ? O7 Mn3 O8 94.1(2) . . ? O7 Mn3 N13 91.8(2) . . ? O8 Mn3 N13 173.7(2) . . ? O7 Mn3 N14 172.7(3) . . ? O8 Mn3 N14 92.9(3) . . ? N13 Mn3 N14 81.3(3) . . ? O7 Mn3 O10 91.6(2) . . ? O8 Mn3 O10 91.9(2) . . ? N13 Mn3 O10 90.5(2) . . ? N14 Mn3 O10 86.2(2) . . ? O7 Mn3 O9 91.1(2) . . ? O8 Mn3 O9 90.0(2) . . ? N13 Mn3 O9 87.3(2) . . ? N14 Mn3 O9 90.9(2) . . ? O10 Mn3 O9 176.6(2) . . ? C43 O7 Mn3 122.0(5) . . ? O7 C43 C48 124.6(8) . . ? O7 C43 C44 116.6(8) . . ? C48 C43 C44 118.8(8) . . ? C45 C44 C43 119.2(9) . . ? C46 C45 C44 119.2(9) . . ? C47 C46 C45 122.7(8) . . ? C47 C46 Cl5 120.1(7) . . ? C45 C46 Cl5 117.2(7) . . ? C46 C47 C48 120.1(8) . . ? C47 C48 C43 120.0(8) . . ? C47 C48 C49 119.0(8) . . ? C43 C48 C49 121.0(7) . . ? N13 C49 C48 125.2(8) . . ? C49 N13 C50 122.9(7) . . ? C49 N13 Mn3 123.2(6) . . ? C50 N13 Mn3 113.8(5) . . ? N13 C50 C51 107.8(7) . . ? C52 C51 N14 113.1(8) . . ? C52 C51 C50 112.1(8) . . ? N14 C51 C50 105.7(7) . . ? C53 N14 C51 120.3(7) . . ? C53 N14 Mn3 124.0(6) . . ? C51 N14 Mn3 115.5(5) . . ? N14 C53 C54 125.4(8) . . ? C59 C54 C55 119.4(9) . . ? C59 C54 C53 124.3(7) . . ? C55 C54 C53 116.1(8) . . ? C56 C55 C54 120.0(10) . . ? C57 C56 C55 120.7(9) . . ? C57 C56 Cl6 120.0(9) . . ? C55 C56 Cl6 119.3(9) . . ? C56 C57 C58 120.1(9) . . ? C59 C58 C57 121.3(9) . . ? O8 C59 C58 117.9(8) . . ? O8 C59 C54 123.7(7) . . ? C58 C59 C54 118.4(8) . . ? C59 O8 Mn3 126.9(5) . . ? O11B O11C O11A 171(2) . . ? O12A O12B O12C 168(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.532 _refine_diff_density_min -1.434 _refine_diff_density_rms 0.165 # Attachment 'complex2.cif' data_p2c _database_code_depnum_ccdc_archive 'CCDC 635488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H88 Mn3 N14 O20 W' _chemical_formula_weight 1842.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2217(4) _cell_length_b 13.3935(3) _cell_length_c 43.7623(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.799(2) _cell_angle_gamma 90.00 _cell_volume 8258.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.013 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3756 _exptl_absorpt_coefficient_mu 1.913 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 82268 _diffrn_reflns_av_R_equivalents 0.1525 _diffrn_reflns_av_sigmaI/netI 0.2453 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.40 _reflns_number_total 20390 _reflns_number_gt 7108 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20390 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2498 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2679 _refine_ls_wR_factor_gt 0.1982 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.006 _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 0.20774(10) 0.48320(11) 0.21714(3) 0.0432(4) Uani 1 1 d . . . C1 C -0.1600(8) 0.6665(10) 0.2171(3) 0.076(4) Uani 1 1 d . . . H1A H -0.2023 0.6108 0.2131 0.115 Uiso 1 1 calc R . . H1B H -0.1754 0.7165 0.2016 0.115 Uiso 1 1 calc R . . H1C H -0.1665 0.6941 0.2370 0.115 Uiso 1 1 calc R . . C2 C 0.0971(8) 0.6619(8) 0.2214(2) 0.049(3) Uani 1 1 d . . . C3 C 0.0063(8) 0.7035(8) 0.2221(2) 0.052(3) Uani 1 1 d . . . C4 C -0.0038(10) 0.8029(9) 0.2284(3) 0.073(4) Uani 1 1 d . . . H4 H -0.0640 0.8295 0.2287 0.088 Uiso 1 1 calc R . . C5 C 0.0739(10) 0.8632(9) 0.2340(3) 0.079(4) Uani 1 1 d . . . H5 H 0.0661 0.9298 0.2392 0.094 Uiso 1 1 calc R . . C6 C 0.1633(10) 0.8272(8) 0.2322(3) 0.078(4) Uani 1 1 d . . . H6 H 0.2153 0.8699 0.2351 0.093 Uiso 1 1 calc R . . C7 C 0.1757(8) 0.7246(7) 0.2259(2) 0.052(3) Uani 1 1 d . . . C8 C 0.2699(8) 0.6905(8) 0.2250(2) 0.059(3) Uani 1 1 d . . . H8 H 0.3180 0.7381 0.2272 0.071 Uiso 1 1 calc R . . C9 C 0.3937(8) 0.5735(10) 0.2185(4) 0.110(6) Uani 1 1 d . . . H9 H 0.3915 0.5731 0.1960 0.131 Uiso 1 1 calc R . . C10 C 0.4728(7) 0.6442(9) 0.2273(3) 0.078(4) Uani 1 1 d . . . H10A H 0.4749 0.6613 0.2490 0.094 Uiso 1 1 calc R . . H10B H 0.4612 0.7050 0.2154 0.094 Uiso 1 1 calc R . . C11 C 0.5697(9) 0.6006(13) 0.2220(5) 0.144(8) Uani 1 1 d . . . H11A H 0.5758 0.6074 0.2003 0.173 Uiso 1 1 calc R . . H11B H 0.6192 0.6406 0.2335 0.173 Uiso 1 1 calc R . . C12 C 0.5849(9) 0.5043(11) 0.2301(4) 0.111(6) Uani 1 1 d . . . H12A H 0.6033 0.5023 0.2522 0.133 Uiso 1 1 calc R . . H12B H 0.6390 0.4815 0.2207 0.133 Uiso 1 1 calc R . . C13 C 0.5071(8) 0.4294(9) 0.2224(3) 0.074(4) Uani 1 1 d . . . H13A H 0.5183 0.3727 0.2362 0.088 Uiso 1 1 calc R . . H13B H 0.5078 0.4057 0.2015 0.088 Uiso 1 1 calc R . . C14 C 0.4111(8) 0.4736(9) 0.2252(4) 0.095(5) Uani 1 1 d . . . H14 H 0.4147 0.4756 0.2477 0.114 Uiso 1 1 calc R . . C15 C 0.3324(7) 0.3137(8) 0.2119(2) 0.052(3) Uani 1 1 d . . . H15 H 0.3927 0.2869 0.2120 0.063 Uiso 1 1 calc R . . C16 C 0.2540(8) 0.2459(7) 0.2052(2) 0.055(3) Uani 1 1 d . . . C17 C 0.2752(9) 0.1452(8) 0.1997(3) 0.067(3) Uani 1 1 d . . . H17 H 0.3380 0.1253 0.2000 0.081 Uiso 1 1 calc R . . C18 C 0.2032(11) 0.0762(8) 0.1940(3) 0.078(4) Uani 1 1 d . . . H18 H 0.2175 0.0099 0.1903 0.093 Uiso 1 1 calc R . . C19 C 0.1093(9) 0.1051(8) 0.1937(3) 0.067(3) Uani 1 1 d . . . H19 H 0.0608 0.0581 0.1905 0.080 Uiso 1 1 calc R . . C20 C 0.0892(8) 0.2024(8) 0.1980(2) 0.058(3) Uani 1 1 d . . . C21 C 0.1606(7) 0.2770(7) 0.2052(2) 0.048(3) Uani 1 1 d . . . C22 C -0.0766(9) 0.1677(9) 0.1991(3) 0.080(4) Uani 1 1 d . . . H22A H -0.1353 0.2030 0.1991 0.120 Uiso 1 1 calc R . . H22B H -0.0642 0.1282 0.2175 0.120 Uiso 1 1 calc R . . H22C H -0.0808 0.1248 0.1814 0.120 Uiso 1 1 calc R . . N1 N 0.2942(6) 0.5981(6) 0.2214(2) 0.052(2) Uani 1 1 d . . . N2 N 0.3279(6) 0.4070(6) 0.2177(2) 0.053(2) Uani 1 1 d . . . O1 O -0.0656(5) 0.6343(6) 0.21689(17) 0.064(2) Uani 1 1 d . . . O2 O 0.1010(5) 0.5658(5) 0.21553(17) 0.0589(19) Uani 1 1 d . . . O3 O 0.1346(4) 0.3673(4) 0.21116(16) 0.0527(19) Uani 1 1 d . . . O4 O -0.0019(5) 0.2370(5) 0.19816(17) 0.059(2) Uani 1 1 d . . . O5 O 0.2176(6) 0.4725(8) 0.26908(18) 0.102(3) Uani 1 1 d . . . O6 O 0.2014(5) 0.4995(5) 0.16518(15) 0.0572(19) Uani 1 1 d . . . Mn2 Mn 0.94059(10) 0.45425(10) 0.13398(3) 0.0402(4) Uani 1 1 d . . . C23 C 1.3091(8) 0.2793(9) 0.1226(3) 0.084(4) Uani 1 1 d . . . H23A H 1.3523 0.3346 0.1258 0.126 Uiso 1 1 calc R . . H23B H 1.3121 0.2507 0.1027 0.126 Uiso 1 1 calc R . . H23C H 1.3264 0.2297 0.1382 0.126 Uiso 1 1 calc R . . C24 C 1.0543(7) 0.2810(6) 0.1243(2) 0.040(2) Uani 1 1 d . . . C25 C 1.1449(7) 0.2434(7) 0.1198(2) 0.046(3) Uani 1 1 d . . . C26 C 1.1555(9) 0.1437(9) 0.1130(3) 0.069(3) Uani 1 1 d . . . H26 H 1.2150 0.1189 0.1104 0.083 Uiso 1 1 calc R . . C27 C 1.0779(10) 0.0808(8) 0.1099(3) 0.079(4) Uani 1 1 d . . . H27 H 1.0851 0.0137 0.1053 0.095 Uiso 1 1 calc R . . C28 C 0.9906(8) 0.1173(8) 0.1138(3) 0.066(3) Uani 1 1 d . . . H28 H 0.9388 0.0743 0.1118 0.079 Uiso 1 1 calc R . . C29 C 0.9773(7) 0.2163(7) 0.1206(2) 0.047(3) Uani 1 1 d . . . C30 C 0.8819(7) 0.2486(7) 0.1258(2) 0.050(3) Uani 1 1 d . . . H30 H 0.8347 0.2001 0.1244 0.060 Uiso 1 1 calc R . . C31 C 0.7628(7) 0.3634(8) 0.1400(4) 0.082(4) Uani 1 1 d . . . H31 H 0.7715 0.3722 0.1624 0.099 Uiso 1 1 calc R . . C32 C 0.6853(7) 0.2858(8) 0.1332(3) 0.074(4) Uani 1 1 d . . . H32A H 0.7041 0.2246 0.1442 0.089 Uiso 1 1 calc R . . H32B H 0.6750 0.2712 0.1113 0.089 Uiso 1 1 calc R . . C33 C 0.5945(10) 0.3255(11) 0.1433(5) 0.154(9) Uani 1 1 d . . . H33A H 0.5432 0.2794 0.1365 0.185 Uiso 1 1 calc R . . H33B H 0.6020 0.3273 0.1657 0.185 Uiso 1 1 calc R . . C34 C 0.5682(9) 0.4227(11) 0.1318(5) 0.114(6) Uani 1 1 d . . . H34A H 0.5160 0.4458 0.1421 0.137 Uiso 1 1 calc R . . H34B H 0.5444 0.4164 0.1100 0.137 Uiso 1 1 calc R . . C35 C 0.6433(8) 0.5019(9) 0.1352(3) 0.076(4) Uani 1 1 d . . . H35A H 0.6519 0.5272 0.1561 0.091 Uiso 1 1 calc R . . H35B H 0.6237 0.5570 0.1214 0.091 Uiso 1 1 calc R . . C36 C 0.7368(8) 0.4586(8) 0.1275(3) 0.074(4) Uani 1 1 d . . . H36 H 0.7262 0.4481 0.1051 0.089 Uiso 1 1 calc R . . C37 C 0.8124(8) 0.6235(8) 0.1351(2) 0.058(3) Uani 1 1 d . . . H37 H 0.7513 0.6489 0.1346 0.070 Uiso 1 1 calc R . . C38 C 0.8893(7) 0.6951(6) 0.1384(2) 0.045(3) Uani 1 1 d . . . C39 C 0.8660(10) 0.7948(8) 0.1432(3) 0.072(4) Uani 1 1 d . . . H39 H 0.8033 0.8137 0.1437 0.086 Uiso 1 1 calc R . . C40 C 0.9384(12) 0.8648(9) 0.1471(3) 0.089(4) Uani 1 1 d . . . H40 H 0.9240 0.9315 0.1502 0.107 Uiso 1 1 calc R . . C41 C 1.0310(10) 0.8368(9) 0.1466(3) 0.074(4) Uani 1 1 d . . . H41 H 1.0786 0.8849 0.1493 0.089 Uiso 1 1 calc R . . C42 C 1.0542(9) 0.7398(8) 0.1422(3) 0.060(3) Uani 1 1 d . . . C43 C 0.9835(7) 0.6661(7) 0.1380(2) 0.047(3) Uani 1 1 d . . . C44 C 1.2159(9) 0.7746(9) 0.1431(3) 0.093(5) Uani 1 1 d . . . H44A H 1.2758 0.7418 0.1430 0.139 Uiso 1 1 calc R . . H44B H 1.2175 0.8133 0.1617 0.139 Uiso 1 1 calc R . . H44C H 1.2039 0.8179 0.1256 0.139 Uiso 1 1 calc R . . N3 N 0.8583(5) 0.3367(6) 0.1320(2) 0.050(2) Uani 1 1 d . . . N4 N 0.8200(6) 0.5282(6) 0.1327(2) 0.049(2) Uani 1 1 d . . . O7 O 1.2159(5) 0.3128(5) 0.12435(19) 0.068(2) Uani 1 1 d . . . O8 O 1.0502(4) 0.3773(5) 0.13261(16) 0.0485(17) Uani 1 1 d . . . O9 O 1.0100(4) 0.5722(4) 0.13329(17) 0.0539(19) Uani 1 1 d . . . O10 O 1.1428(5) 0.7022(5) 0.14193(19) 0.068(2) Uani 1 1 d . . . O11 O 0.9489(5) 0.4473(5) 0.18534(15) 0.0563(19) Uani 1 1 d . . . O12 O 0.9138(5) 0.4511(6) 0.08049(16) 0.066(2) Uani 1 1 d . . . Mn3 Mn 0.13295(10) 0.52008(11) 0.04321(3) 0.0425(4) Uani 1 1 d . . . C45 C -0.1317(10) 0.1885(10) 0.0289(3) 0.097(5) Uani 1 1 d . . . H45A H -0.1930 0.2186 0.0287 0.145 Uiso 1 1 calc R . . H45B H -0.1196 0.1440 0.0462 0.145 Uiso 1 1 calc R . . H45C H -0.1301 0.1518 0.0101 0.145 Uiso 1 1 calc R . . C46 C 0.0958(9) 0.3073(7) 0.0361(2) 0.057(3) Uani 1 1 d . . . C47 C 0.0287(10) 0.2322(8) 0.0313(3) 0.071(4) Uani 1 1 d . . . C48 C 0.0568(13) 0.1384(10) 0.0261(4) 0.099(5) Uani 1 1 d . . . H48 H 0.0106 0.0892 0.0223 0.118 Uiso 1 1 calc R . . C49 C 0.1486(14) 0.1120(11) 0.0263(4) 0.113(6) Uani 1 1 d . . . H49 H 0.1648 0.0456 0.0237 0.135 Uiso 1 1 calc R . . C50 C 0.2173(11) 0.1841(9) 0.0303(3) 0.091(4) Uani 1 1 d . . . H50 H 0.2804 0.1673 0.0295 0.109 Uiso 1 1 calc R . . C51 C 0.1922(9) 0.2844(7) 0.0356(3) 0.065(3) Uani 1 1 d . . . C52 C 0.2665(8) 0.3588(9) 0.0403(3) 0.068(3) Uani 1 1 d . . . H52 H 0.3286 0.3362 0.0412 0.082 Uiso 1 1 calc R . . C53 C 0.3354(10) 0.5201(12) 0.0478(5) 0.125(7) Uani 1 1 d . . . H53 H 0.3447 0.5234 0.0703 0.150 Uiso 1 1 calc R . . C54 C 0.4306(8) 0.4857(11) 0.0429(3) 0.084(4) Uani 1 1 d . . . H54A H 0.4454 0.4254 0.0549 0.101 Uiso 1 1 calc R . . H54B H 0.4295 0.4687 0.0214 0.101 Uiso 1 1 calc R . . C55 C 0.5063(11) 0.5588(13) 0.0515(6) 0.152(9) Uani 1 1 d . . . H55A H 0.5228 0.5583 0.0738 0.182 Uiso 1 1 calc R . . H55B H 0.5621 0.5386 0.0426 0.182 Uiso 1 1 calc R . . C56 C 0.4817(9) 0.6567(15) 0.0419(6) 0.184(11) Uani 1 1 d . . . H56A H 0.4847 0.6606 0.0199 0.221 Uiso 1 1 calc R . . H56B H 0.5301 0.7012 0.0520 0.221 Uiso 1 1 calc R . . C57 C 0.3825(7) 0.6982(9) 0.0478(3) 0.081(4) Uani 1 1 d . . . H57A H 0.3856 0.7209 0.0690 0.098 Uiso 1 1 calc R . . H57B H 0.3645 0.7544 0.0343 0.098 Uiso 1 1 calc R . . C58 C 0.3092(9) 0.6147(12) 0.0415(5) 0.122(7) Uani 1 1 d . . . H58 H 0.3030 0.6128 0.0190 0.146 Uiso 1 1 calc R . . C59 C 0.1837(8) 0.7278(8) 0.0509(3) 0.060(3) Uani 1 1 d . . . H59 H 0.2299 0.7773 0.0534 0.072 Uiso 1 1 calc R . . C60 C 0.0863(7) 0.7582(7) 0.0535(2) 0.050(3) Uani 1 1 d . . . C61 C 0.0666(9) 0.8587(8) 0.0591(3) 0.069(3) Uani 1 1 d . . . H61 H 0.1159 0.9048 0.0621 0.082 Uiso 1 1 calc R . . C62 C -0.0242(10) 0.8889(9) 0.0601(3) 0.086(4) Uani 1 1 d . . . H62 H -0.0372 0.9564 0.0624 0.103 Uiso 1 1 calc R . . C63 C -0.0971(9) 0.8207(9) 0.0578(3) 0.073(4) Uani 1 1 d . . . H63 H -0.1578 0.8425 0.0602 0.088 Uiso 1 1 calc R . . C64 C -0.0828(8) 0.7212(9) 0.0521(3) 0.060(3) Uani 1 1 d . . . C65 C 0.0126(7) 0.6878(7) 0.0496(2) 0.045(2) Uani 1 1 d . . . C66 C -0.2426(8) 0.6736(10) 0.0489(3) 0.084(4) Uani 1 1 d . . . H66A H -0.2810 0.6145 0.0460 0.126 Uiso 1 1 calc R . . H66B H -0.2630 0.7206 0.0328 0.126 Uiso 1 1 calc R . . H66C H -0.2490 0.7028 0.0686 0.126 Uiso 1 1 calc R . . N5 N 0.2548(6) 0.4509(6) 0.0433(2) 0.060(2) Uani 1 1 d . . . N6 N 0.2109(6) 0.6405(6) 0.04545(19) 0.050(2) Uani 1 1 d . . . O13 O -0.1484(5) 0.6487(6) 0.04800(19) 0.071(2) Uani 1 1 d . . . O14 O 0.0213(5) 0.5928(5) 0.04360(17) 0.0550(19) Uani 1 1 d . . . O15 O 0.0661(5) 0.3987(5) 0.04067(17) 0.060(2) Uani 1 1 d . . . O16 O -0.0617(7) 0.2634(6) 0.0314(2) 0.085(3) Uani 1 1 d . . . O17 O 0.1221(5) 0.5317(6) -0.00873(15) 0.065(2) Uani 1 1 d . . . O18 O 0.1572(5) 0.5165(7) 0.09471(16) 0.078(2) Uani 1 1 d . . . W1 W 0.52643(3) 0.93633(3) 0.142114(13) 0.0626(2) Uani 1 1 d . . . C67 C 0.3925(10) 0.9347(9) 0.1131(3) 0.070(3) Uani 1 1 d . . . C68 C 0.4273(9) 0.9082(8) 0.1755(3) 0.069(3) Uani 1 1 d . . . C69 C 0.4867(9) 0.7790(10) 0.1384(3) 0.075(4) Uani 1 1 d . . . C70 C 0.6129(10) 0.8674(13) 0.1794(4) 0.101(5) Uani 1 1 d . . . C71 C 0.5853(14) 0.8777(16) 0.1043(6) 0.186(12) Uani 1 1 d . . . C72 C 0.6655(11) 0.9988(11) 0.1444(5) 0.122(6) Uani 1 1 d . . . C73 C 0.5166(12) 1.0606(14) 0.1118(4) 0.112(6) Uani 1 1 d . . . C74 C 0.5196(14) 1.0632(10) 0.1709(4) 0.112(6) Uani 1 1 d . . . N7 N 0.3222(10) 0.9342(10) 0.0958(4) 0.120(5) Uani 1 1 d . . . N8 N 0.3777(8) 0.8932(8) 0.1932(3) 0.079(3) Uani 1 1 d . . . N9 N 0.4716(9) 0.6951(8) 0.1366(3) 0.108(4) Uani 1 1 d . . . N10 N 0.6619(10) 0.8328(11) 0.2007(4) 0.132(6) Uani 1 1 d . . . N11 N 0.6158(16) 0.8543(16) 0.0835(6) 0.292(17) Uani 1 1 d . . . N12 N 0.7389(10) 1.0336(9) 0.1459(5) 0.170(8) Uani 1 1 d . . . N13 N 0.5079(13) 1.1311(14) 0.0947(4) 0.170(8) Uani 1 1 d . . . N14 N 0.5141(13) 1.1319(10) 0.1849(4) 0.162(7) Uani 1 1 d . . . O19 O 0.358(2) 0.9631(15) 0.0291(6) 0.358(17) Uani 1 1 d . . . O20 O 0.3454(14) 0.5302(12) 0.1301(3) 0.215(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0421(9) 0.0411(8) 0.0467(9) -0.0011(7) 0.0072(7) 0.0055(7) C1 0.059(8) 0.102(10) 0.072(9) -0.012(7) 0.019(7) 0.025(7) C2 0.062(7) 0.048(6) 0.040(6) 0.000(5) 0.020(6) 0.014(6) C3 0.069(8) 0.044(6) 0.045(7) 0.006(5) 0.020(6) 0.020(6) C4 0.085(10) 0.070(9) 0.068(9) 0.003(7) 0.022(7) 0.036(8) C5 0.099(11) 0.046(7) 0.097(10) 0.003(7) 0.031(9) 0.007(7) C6 0.098(10) 0.049(7) 0.091(10) -0.005(6) 0.034(8) 0.012(7) C7 0.058(7) 0.039(6) 0.060(7) -0.001(5) 0.011(6) 0.010(5) C8 0.063(8) 0.045(6) 0.069(8) -0.003(6) 0.004(6) -0.009(6) C9 0.041(7) 0.074(10) 0.204(18) -0.059(11) -0.017(9) -0.008(7) C10 0.041(7) 0.080(9) 0.111(11) -0.031(8) 0.001(7) -0.009(6) C11 0.037(8) 0.106(13) 0.28(3) -0.025(15) 0.002(12) -0.003(8) C12 0.042(8) 0.080(11) 0.213(18) 0.031(12) 0.023(10) 0.000(8) C13 0.054(7) 0.075(8) 0.090(9) 0.007(7) 0.006(7) 0.023(7) C14 0.036(7) 0.063(8) 0.190(16) 0.037(9) 0.030(9) 0.007(6) C15 0.045(6) 0.050(6) 0.062(7) 0.009(6) 0.009(6) 0.009(5) C16 0.069(8) 0.037(6) 0.059(7) -0.005(5) 0.005(6) 0.018(5) C17 0.083(9) 0.046(7) 0.072(8) -0.004(6) 0.007(7) 0.020(6) C18 0.117(12) 0.041(7) 0.071(9) -0.011(6) 0.000(8) 0.024(8) C19 0.071(9) 0.036(6) 0.089(9) -0.009(6) 0.000(7) -0.004(6) C20 0.067(8) 0.056(7) 0.051(7) 0.003(6) 0.010(6) 0.005(6) C21 0.052(7) 0.048(6) 0.045(7) 0.010(5) 0.011(5) 0.004(5) C22 0.081(9) 0.063(8) 0.095(10) 0.011(7) 0.011(8) -0.018(7) N1 0.041(5) 0.046(5) 0.068(6) -0.011(4) -0.002(5) 0.012(4) N2 0.049(5) 0.046(5) 0.066(6) 0.010(4) 0.015(5) 0.004(4) O1 0.048(5) 0.066(5) 0.081(6) -0.003(4) 0.017(4) 0.013(4) O2 0.044(4) 0.048(4) 0.081(5) -0.013(4) -0.001(4) 0.007(3) O3 0.044(4) 0.033(4) 0.085(5) 0.002(3) 0.024(4) 0.002(3) O4 0.055(5) 0.051(4) 0.072(5) 0.005(4) 0.016(4) -0.010(4) O5 0.063(6) 0.188(10) 0.057(5) 0.005(6) 0.018(4) 0.031(6) O6 0.064(5) 0.063(5) 0.044(4) -0.004(4) 0.007(4) -0.008(4) Mn2 0.0376(8) 0.0353(8) 0.0487(9) -0.0024(7) 0.0097(7) -0.0027(6) C23 0.050(8) 0.065(8) 0.140(13) -0.006(8) 0.028(8) 0.006(6) C24 0.042(6) 0.031(5) 0.047(6) 0.003(4) 0.007(5) 0.005(4) C25 0.052(7) 0.033(5) 0.054(7) -0.001(5) 0.015(5) -0.001(5) C26 0.080(9) 0.068(8) 0.064(8) -0.007(6) 0.023(7) 0.019(7) C27 0.098(11) 0.031(6) 0.110(11) -0.016(6) 0.021(9) -0.009(6) C28 0.063(8) 0.040(6) 0.096(10) -0.013(6) 0.013(7) 0.005(6) C29 0.052(7) 0.031(5) 0.056(7) -0.007(5) 0.002(6) -0.011(5) C30 0.041(6) 0.045(6) 0.064(8) -0.005(5) 0.009(6) -0.015(5) C31 0.037(7) 0.057(7) 0.156(13) 0.008(8) 0.024(8) -0.006(6) C32 0.043(7) 0.051(7) 0.133(12) -0.005(7) 0.029(7) 0.003(5) C33 0.054(9) 0.078(11) 0.34(3) 0.040(14) 0.050(13) 0.002(8) C34 0.042(8) 0.106(12) 0.199(18) -0.029(12) 0.029(10) -0.017(8) C35 0.050(7) 0.059(7) 0.123(11) 0.007(7) 0.033(7) 0.007(6) C36 0.044(7) 0.061(8) 0.118(11) -0.013(7) 0.015(7) -0.001(6) C37 0.050(7) 0.062(8) 0.064(8) -0.007(6) 0.012(6) 0.009(6) C38 0.054(7) 0.025(5) 0.057(7) 0.003(4) 0.007(5) 0.000(5) C39 0.099(10) 0.042(7) 0.078(9) 0.004(6) 0.023(8) 0.010(7) C40 0.128(13) 0.032(6) 0.112(11) -0.012(7) 0.037(10) -0.003(8) C41 0.084(10) 0.048(7) 0.092(10) -0.008(7) 0.017(8) -0.014(7) C42 0.074(9) 0.045(6) 0.060(8) 0.007(5) 0.009(7) -0.014(6) C43 0.054(7) 0.040(6) 0.048(7) 0.002(5) 0.010(5) -0.003(5) C44 0.071(9) 0.072(9) 0.134(13) -0.003(8) 0.012(9) -0.043(7) N3 0.037(5) 0.042(5) 0.071(6) 0.000(4) 0.010(4) 0.004(4) N4 0.041(5) 0.039(5) 0.068(6) -0.001(4) 0.010(4) -0.002(4) O7 0.044(4) 0.048(4) 0.117(7) -0.005(4) 0.025(4) 0.009(4) O8 0.039(4) 0.039(4) 0.068(5) -0.006(3) 0.012(4) -0.006(3) O9 0.047(4) 0.033(4) 0.083(5) 0.001(3) 0.013(4) -0.001(3) O10 0.057(5) 0.047(4) 0.100(6) 0.009(4) 0.013(5) -0.024(4) O11 0.052(4) 0.068(5) 0.051(4) 0.001(4) 0.014(4) 0.003(4) O12 0.065(5) 0.087(6) 0.047(4) 0.001(4) 0.013(4) -0.004(4) Mn3 0.0407(9) 0.0423(8) 0.0446(9) -0.0027(7) 0.0061(7) -0.0034(7) C45 0.097(11) 0.073(9) 0.118(12) 0.006(8) 0.003(9) -0.024(8) C46 0.081(9) 0.035(6) 0.057(7) 0.003(5) 0.014(7) -0.003(6) C47 0.098(11) 0.036(6) 0.080(9) -0.002(6) 0.020(8) -0.017(7) C48 0.123(14) 0.053(8) 0.125(13) -0.014(8) 0.034(11) -0.031(9) C49 0.145(16) 0.047(8) 0.156(16) 0.000(9) 0.059(14) 0.000(10) C50 0.106(11) 0.053(8) 0.122(12) -0.005(8) 0.048(10) 0.019(8) C51 0.096(10) 0.034(6) 0.068(8) -0.006(5) 0.022(7) -0.002(6) C52 0.061(8) 0.064(8) 0.081(9) 0.005(7) 0.014(7) 0.017(7) C53 0.061(10) 0.074(10) 0.25(2) 0.008(12) 0.043(12) -0.003(8) C54 0.037(7) 0.103(10) 0.112(11) 0.000(9) 0.010(7) 0.006(7) C55 0.061(10) 0.093(13) 0.31(3) 0.021(15) 0.039(14) 0.004(10) C56 0.028(8) 0.151(18) 0.38(3) -0.05(2) 0.039(13) -0.046(10) C57 0.044(7) 0.079(9) 0.121(11) -0.023(8) 0.010(7) -0.027(6) C58 0.038(8) 0.096(12) 0.24(2) -0.037(13) 0.043(10) -0.015(8) C59 0.055(7) 0.058(7) 0.068(8) -0.005(6) 0.009(6) -0.018(6) C60 0.051(7) 0.041(6) 0.056(7) -0.018(5) 0.005(6) -0.001(5) C61 0.065(8) 0.051(7) 0.091(10) -0.012(6) 0.013(7) -0.010(6) C62 0.090(11) 0.048(7) 0.120(12) -0.023(8) 0.022(9) -0.002(8) C63 0.060(8) 0.064(8) 0.096(10) -0.028(7) 0.011(7) 0.017(7) C64 0.055(7) 0.066(8) 0.059(8) -0.005(6) 0.010(6) -0.004(6) C65 0.043(6) 0.050(6) 0.044(6) -0.008(5) 0.005(5) -0.005(5) C66 0.041(7) 0.098(10) 0.112(11) -0.001(8) 0.010(7) 0.012(7) N5 0.054(6) 0.050(6) 0.080(7) 0.005(5) 0.018(5) 0.003(5) N6 0.043(5) 0.044(5) 0.062(6) -0.013(4) 0.000(4) -0.005(4) O13 0.043(5) 0.064(5) 0.109(7) -0.008(5) 0.021(5) -0.007(4) O14 0.049(4) 0.035(4) 0.082(5) -0.005(4) 0.012(4) -0.002(3) O15 0.053(5) 0.038(4) 0.089(6) -0.001(4) 0.009(4) -0.007(3) O16 0.075(6) 0.056(5) 0.119(8) 0.009(5) -0.001(6) -0.027(5) O17 0.064(5) 0.091(6) 0.037(4) -0.010(4) 0.002(4) -0.017(4) O18 0.065(5) 0.131(7) 0.040(4) 0.011(5) 0.017(4) -0.010(5) W1 0.0512(3) 0.0470(3) 0.0907(4) -0.0190(3) 0.0138(3) -0.0028(2) C67 0.067(9) 0.060(7) 0.083(10) 0.016(7) 0.008(8) 0.001(7) C68 0.066(9) 0.045(7) 0.093(10) -0.013(6) 0.004(8) 0.004(6) C69 0.085(9) 0.056(8) 0.076(9) -0.012(7) -0.015(7) 0.006(7) C70 0.061(10) 0.121(14) 0.114(14) -0.066(11) -0.015(9) -0.027(9) C71 0.139(16) 0.165(18) 0.29(3) -0.147(19) 0.159(19) -0.097(14) C72 0.056(10) 0.072(10) 0.23(2) -0.029(12) -0.023(11) -0.003(8) C73 0.106(12) 0.146(16) 0.082(11) 0.011(10) 0.002(9) -0.079(11) C74 0.192(17) 0.048(8) 0.116(12) -0.025(8) 0.088(12) -0.033(9) N7 0.087(9) 0.112(11) 0.149(13) 0.045(9) -0.026(9) -0.035(8) N8 0.073(8) 0.070(7) 0.100(9) -0.009(6) 0.028(7) -0.019(6) N9 0.129(10) 0.042(6) 0.144(11) -0.020(7) -0.013(8) -0.008(7) N10 0.099(11) 0.136(13) 0.140(13) -0.022(10) -0.058(10) -0.003(9) N11 0.27(2) 0.26(2) 0.41(3) -0.25(2) 0.27(3) -0.17(2) N12 0.068(9) 0.060(8) 0.38(3) -0.042(12) 0.012(13) -0.011(7) N13 0.208(18) 0.168(16) 0.129(14) 0.033(12) 0.003(12) -0.101(14) N14 0.236(18) 0.085(10) 0.189(16) -0.061(10) 0.120(14) -0.060(11) O19 0.54(4) 0.207(19) 0.37(3) 0.14(2) 0.22(3) 0.20(2) O20 0.31(2) 0.171(14) 0.157(13) 0.004(11) 0.007(13) -0.061(14) _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 O3 1.867(6) . ? Mn1 O2 1.872(7) . ? Mn1 N1 1.963(9) . ? Mn1 N2 1.988(8) . ? Mn1 O5 2.263(8) . ? Mn1 O6 2.274(7) . ? C1 O1 1.412(11) . ? C2 O2 1.315(11) . ? C2 C7 1.391(14) . ? C2 C3 1.411(13) . ? C3 C4 1.371(14) . ? C3 O1 1.375(12) . ? C4 C5 1.363(16) . ? C5 C6 1.372(16) . ? C6 C7 1.418(14) . ? C7 C8 1.420(14) . ? C8 N1 1.301(12) . ? C9 C14 1.385(16) . ? C9 N1 1.476(14) . ? C9 C10 1.481(15) . ? C10 C11 1.542(17) . ? C11 C12 1.348(19) . ? C12 C13 1.497(17) . ? C13 C14 1.507(15) . ? C14 N2 1.483(14) . ? C15 N2 1.279(12) . ? C15 C16 1.436(14) . ? C16 C21 1.392(14) . ? C16 C17 1.410(13) . ? C17 C18 1.377(16) . ? C18 C19 1.388(16) . ? C19 C20 1.353(14) . ? C20 O4 1.377(12) . ? C20 C21 1.428(14) . ? C21 O3 1.303(11) . ? C22 O4 1.416(12) . ? Mn2 O9 1.865(6) . ? Mn2 O8 1.876(6) . ? Mn2 N3 1.956(8) . ? Mn2 N4 1.974(8) . ? Mn2 O11 2.237(7) . ? Mn2 O12 2.321(7) . ? C23 O7 1.412(12) . ? C24 O8 1.344(10) . ? C24 C29 1.388(12) . ? C24 C25 1.422(12) . ? C25 O7 1.367(11) . ? C25 C26 1.381(13) . ? C26 C27 1.380(16) . ? C27 C28 1.366(15) . ? C28 C29 1.376(13) . ? C29 C30 1.472(13) . ? C30 N3 1.267(11) . ? C31 C36 1.416(15) . ? C31 N3 1.491(12) . ? C31 C32 1.514(15) . ? C32 C33 1.517(17) . ? C33 C34 1.427(19) . ? C34 C35 1.498(16) . ? C35 C36 1.530(14) . ? C36 N4 1.499(13) . ? C37 N4 1.286(12) . ? C37 C38 1.448(14) . ? C38 C39 1.397(13) . ? C38 C43 1.398(13) . ? C39 C40 1.385(17) . ? C40 C41 1.373(16) . ? C41 C42 1.361(15) . ? C42 O10 1.358(13) . ? C42 C43 1.403(14) . ? C43 O9 1.337(11) . ? C44 O10 1.417(12) . ? Mn3 O14 1.865(7) . ? Mn3 O15 1.878(7) . ? Mn3 N6 1.952(8) . ? Mn3 N5 1.964(9) . ? Mn3 O18 2.234(7) . ? Mn3 O17 2.262(7) . ? C45 O16 1.407(13) . ? C46 O15 1.320(11) . ? C46 C47 1.382(15) . ? C46 C51 1.407(15) . ? C47 C48 1.346(17) . ? C47 O16 1.353(14) . ? C48 C49 1.352(19) . ? C49 C50 1.368(19) . ? C50 C51 1.418(14) . ? C51 C52 1.446(15) . ? C52 N5 1.254(13) . ? C53 C58 1.34(2) . ? C53 N5 1.467(16) . ? C53 C54 1.471(17) . ? C54 C55 1.465(19) . ? C55 C56 1.41(2) . ? C56 C57 1.571(18) . ? C57 C58 1.528(16) . ? C58 N6 1.472(14) . ? C59 N6 1.264(12) . ? C59 C60 1.463(14) . ? C60 C65 1.402(13) . ? C60 C61 1.403(14) . ? C61 C62 1.361(16) . ? C62 C63 1.374(16) . ? C63 C64 1.376(15) . ? C64 O13 1.341(12) . ? C64 C65 1.447(14) . ? C65 O14 1.309(11) . ? C66 O13 1.387(12) . ? W1 C71 2.104(18) . ? W1 C70 2.12(2) . ? W1 C73 2.121(18) . ? W1 C74 2.126(14) . ? W1 C72 2.137(16) . ? W1 C67 2.142(15) . ? W1 C69 2.182(13) . ? W1 C68 2.197(15) . ? C67 N7 1.170(15) . ? C68 N8 1.132(14) . ? C69 N9 1.145(14) . ? C70 N10 1.180(18) . ? C71 N11 1.11(2) . ? C72 N12 1.137(16) . ? C73 N13 1.20(2) . ? C74 N14 1.115(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn1 O2 93.0(3) . . ? O3 Mn1 N1 174.3(3) . . ? O2 Mn1 N1 92.0(3) . . ? O3 Mn1 N2 92.1(3) . . ? O2 Mn1 N2 174.5(3) . . ? N1 Mn1 N2 82.8(3) . . ? O3 Mn1 O5 92.6(4) . . ? O2 Mn1 O5 90.9(3) . . ? N1 Mn1 O5 90.1(4) . . ? N2 Mn1 O5 91.1(3) . . ? O3 Mn1 O6 89.7(3) . . ? O2 Mn1 O6 89.1(3) . . ? N1 Mn1 O6 87.6(3) . . ? N2 Mn1 O6 88.8(3) . . ? O5 Mn1 O6 177.7(3) . . ? O2 C2 C7 124.3(9) . . ? O2 C2 C3 117.0(10) . . ? C7 C2 C3 118.7(9) . . ? C4 C3 O1 126.4(10) . . ? C4 C3 C2 120.5(11) . . ? O1 C3 C2 113.1(9) . . ? C5 C4 C3 120.6(12) . . ? C4 C5 C6 121.0(12) . . ? C5 C6 C7 119.5(12) . . ? C2 C7 C6 119.6(10) . . ? C2 C7 C8 123.0(9) . . ? C6 C7 C8 117.4(11) . . ? N1 C8 C7 125.2(10) . . ? C14 C9 N1 110.1(11) . . ? C14 C9 C10 117.1(12) . . ? N1 C9 C10 122.6(10) . . ? C9 C10 C11 112.4(11) . . ? C12 C11 C10 116.0(14) . . ? C11 C12 C13 119.7(13) . . ? C12 C13 C14 111.6(11) . . ? C9 C14 N2 114.8(10) . . ? C9 C14 C13 120.0(11) . . ? N2 C14 C13 116.8(11) . . ? N2 C15 C16 126.9(10) . . ? C21 C16 C17 120.8(11) . . ? C21 C16 C15 121.7(9) . . ? C17 C16 C15 117.5(10) . . ? C18 C17 C16 120.1(11) . . ? C17 C18 C19 120.4(10) . . ? C20 C19 C18 119.2(11) . . ? C19 C20 O4 122.8(11) . . ? C19 C20 C21 123.1(11) . . ? O4 C20 C21 113.9(9) . . ? O3 C21 C16 125.1(10) . . ? O3 C21 C20 118.7(9) . . ? C16 C21 C20 116.2(10) . . ? C8 N1 C9 119.8(9) . . ? C8 N1 Mn1 125.8(7) . . ? C9 N1 Mn1 114.4(7) . . ? C15 N2 C14 124.9(9) . . ? C15 N2 Mn1 124.4(7) . . ? C14 N2 Mn1 110.7(7) . . ? C3 O1 C1 118.6(8) . . ? C2 O2 Mn1 128.8(7) . . ? C21 O3 Mn1 129.2(6) . . ? C20 O4 C22 119.3(9) . . ? O9 Mn2 O8 91.2(3) . . ? O9 Mn2 N3 174.5(3) . . ? O8 Mn2 N3 92.9(3) . . ? O9 Mn2 N4 92.0(3) . . ? O8 Mn2 N4 175.3(3) . . ? N3 Mn2 N4 83.7(3) . . ? O9 Mn2 O11 95.5(3) . . ? O8 Mn2 O11 94.5(3) . . ? N3 Mn2 O11 87.8(3) . . ? N4 Mn2 O11 88.7(3) . . ? O9 Mn2 O12 90.8(3) . . ? O8 Mn2 O12 88.9(3) . . ? N3 Mn2 O12 85.7(3) . . ? N4 Mn2 O12 87.5(3) . . ? O11 Mn2 O12 172.8(3) . . ? O8 C24 C29 124.7(8) . . ? O8 C24 C25 116.8(8) . . ? C29 C24 C25 118.5(8) . . ? O7 C25 C26 126.1(10) . . ? O7 C25 C24 113.8(8) . . ? C26 C25 C24 120.0(10) . . ? C27 C26 C25 120.1(11) . . ? C28 C27 C26 119.8(10) . . ? C27 C28 C29 121.7(11) . . ? C28 C29 C24 119.8(10) . . ? C28 C29 C30 118.3(9) . . ? C24 C29 C30 121.8(8) . . ? N3 C30 C29 125.8(9) . . ? C36 C31 N3 108.9(9) . . ? C36 C31 C32 113.5(11) . . ? N3 C31 C32 116.9(10) . . ? C31 C32 C33 109.2(10) . . ? C34 C33 C32 114.1(13) . . ? C33 C34 C35 117.6(13) . . ? C34 C35 C36 109.8(10) . . ? C31 C36 N4 110.1(10) . . ? C31 C36 C35 116.5(10) . . ? N4 C36 C35 115.1(9) . . ? N4 C37 C38 126.5(10) . . ? C39 C38 C43 120.9(10) . . ? C39 C38 C37 117.2(10) . . ? C43 C38 C37 121.8(9) . . ? C40 C39 C38 118.6(12) . . ? C41 C40 C39 120.8(11) . . ? C42 C41 C40 120.9(11) . . ? O10 C42 C41 126.7(11) . . ? O10 C42 C43 112.8(9) . . ? C41 C42 C43 120.5(12) . . ? O9 C43 C38 123.7(9) . . ? O9 C43 C42 118.0(10) . . ? C38 C43 C42 118.3(10) . . ? C30 N3 C31 123.3(8) . . ? C30 N3 Mn2 125.8(7) . . ? C31 N3 Mn2 110.8(6) . . ? C37 N4 C36 123.7(9) . . ? C37 N4 Mn2 125.3(7) . . ? C36 N4 Mn2 110.9(6) . . ? C25 O7 C23 117.1(8) . . ? C24 O8 Mn2 127.1(6) . . ? C43 O9 Mn2 129.3(6) . . ? C42 O10 C44 115.0(9) . . ? O14 Mn3 O15 91.6(3) . . ? O14 Mn3 N6 92.7(3) . . ? O15 Mn3 N6 175.7(3) . . ? O14 Mn3 N5 176.6(3) . . ? O15 Mn3 N5 91.8(3) . . ? N6 Mn3 N5 84.0(4) . . ? O14 Mn3 O18 91.0(3) . . ? O15 Mn3 O18 92.8(3) . . ? N6 Mn3 O18 87.6(3) . . ? N5 Mn3 O18 88.4(3) . . ? O14 Mn3 O17 91.8(3) . . ? O15 Mn3 O17 92.0(3) . . ? N6 Mn3 O17 87.4(3) . . ? N5 Mn3 O17 88.6(3) . . ? O18 Mn3 O17 174.4(3) . . ? O15 C46 C47 118.0(11) . . ? O15 C46 C51 122.4(10) . . ? C47 C46 C51 119.6(10) . . ? C48 C47 O16 126.3(12) . . ? C48 C47 C46 119.3(14) . . ? O16 C47 C46 114.3(10) . . ? C47 C48 C49 123.5(14) . . ? C48 C49 C50 119.3(13) . . ? C49 C50 C51 119.9(13) . . ? C46 C51 C50 118.4(11) . . ? C46 C51 C52 122.9(10) . . ? C50 C51 C52 118.7(12) . . ? N5 C52 C51 126.0(11) . . ? C58 C53 N5 112.3(12) . . ? C58 C53 C54 120.2(13) . . ? N5 C53 C54 120.1(13) . . ? C55 C54 C53 114.4(13) . . ? C56 C55 C54 113.7(16) . . ? C55 C56 C57 118.2(15) . . ? C58 C57 C56 108.5(11) . . ? C53 C58 N6 116.2(12) . . ? C53 C58 C57 119.5(13) . . ? N6 C58 C57 116.2(12) . . ? N6 C59 C60 126.1(10) . . ? C65 C60 C61 120.1(10) . . ? C65 C60 C59 120.3(9) . . ? C61 C60 C59 119.6(10) . . ? C62 C61 C60 120.3(11) . . ? C61 C62 C63 120.6(11) . . ? C62 C63 C64 121.9(11) . . ? O13 C64 C63 127.5(11) . . ? O13 C64 C65 114.1(10) . . ? C63 C64 C65 118.4(10) . . ? O14 C65 C60 126.0(9) . . ? O14 C65 C64 115.5(9) . . ? C60 C65 C64 118.4(9) . . ? C52 N5 C53 121.5(11) . . ? C52 N5 Mn3 126.4(8) . . ? C53 N5 Mn3 112.1(8) . . ? C59 N6 C58 124.0(10) . . ? C59 N6 Mn3 126.0(7) . . ? C58 N6 Mn3 110.0(8) . . ? C64 O13 C66 118.6(9) . . ? C65 O14 Mn3 127.8(6) . . ? C46 O15 Mn3 130.0(7) . . ? C47 O16 C45 116.2(10) . . ? C71 W1 C70 101.1(9) . . ? C71 W1 C73 78.5(9) . . ? C70 W1 C73 143.7(6) . . ? C71 W1 C74 145.0(6) . . ? C70 W1 C74 87.7(6) . . ? C73 W1 C74 74.9(6) . . ? C71 W1 C72 73.7(7) . . ? C70 W1 C72 72.4(6) . . ? C73 W1 C72 72.8(6) . . ? C74 W1 C72 77.0(6) . . ? C71 W1 C67 86.9(8) . . ? C70 W1 C67 146.0(5) . . ? C73 W1 C67 70.1(5) . . ? C74 W1 C67 104.6(7) . . ? C72 W1 C67 140.8(6) . . ? C71 W1 C69 73.0(6) . . ? C70 W1 C69 75.7(5) . . ? C73 W1 C69 135.8(5) . . ? C74 W1 C69 141.6(5) . . ? C72 W1 C69 127.6(5) . . ? C67 W1 C69 75.3(5) . . ? C71 W1 C68 144.9(5) . . ? C70 W1 C68 76.7(5) . . ? C73 W1 C68 123.9(6) . . ? C74 W1 C68 69.9(5) . . ? C72 W1 C68 135.1(6) . . ? C67 W1 C68 78.1(5) . . ? C69 W1 C68 72.6(4) . . ? N7 C67 W1 176.1(13) . . ? N8 C68 W1 178.6(12) . . ? N9 C69 W1 175.9(12) . . ? N10 C70 W1 177.3(14) . . ? N11 C71 W1 174(3) . . ? N12 C72 W1 178.8(16) . . ? N13 C73 W1 177.8(17) . . ? N14 C74 W1 176.9(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.056 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.149