Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jeffrey Long' _publ_contact_author_address ; Department of Chemistry University of California, Berkeley Berkeley CA 94720-1460 UNITED STATES OF AMERICA ; _publ_contact_author_email JRLONG@BERKELEY.EDU _publ_section_title ; Symmetry-breaking substitutions of [Re(CN)8]3- into the centered, face-capped octahedral clusters (CH3OH)24M9M'6(CN)48 (M = Mn, Co; M' = Mo, W) ; loop_ _publ_author_name 'Jeff Long' 'Miriam V. Bennett' 'Danna E. Freedman' # Attachment '1c.cif' data_mvb1d _database_code_depnum_ccdc_archive 'CCDC 292902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H0 Mn9 N48 O32.80 Re6' _chemical_formula_weight 3685.67 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 29.235(5) _cell_length_b 18.748(3) _cell_length_c 32.554(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.856(2) _cell_angle_gamma 90.00 _cell_volume 16190(5) _cell_formula_units_Z 4 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 15360 _cell_measurement_theta_min 4.744 _cell_measurement_theta_max 46.500 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6846 _exptl_absorpt_coefficient_mu 5.204 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 135 _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 'Bruker SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 31957 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.34 _reflns_number_total 15360 _reflns_number_gt 14692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0885P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.505(17) _refine_ls_number_reflns 15360 _refine_ls_number_parameters 769 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.2143 _refine_ls_goodness_of_fit_ref 1.845 _refine_ls_restrained_S_all 1.845 _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 Re1 Re 0.35075(4) -0.85147(5) -0.55150(4) 0.0285(3) Uani 1 1 d . . . Re2 Re 0.71258(4) -0.83878(5) -0.56684(4) 0.0348(3) Uani 1 1 d . . . Re3 Re 0.61298(4) -0.67251(5) -0.41975(4) 0.0296(3) Uani 1 1 d . . . Re4 Re 0.45460(4) -0.65244(6) -0.68685(4) 0.0336(3) Uani 1 1 d . . . Re5 Re 0.58810(4) -1.08057(5) -0.44024(3) 0.0244(3) Uani 1 1 d . . . Re6 Re 0.47390(4) -1.05688(5) -0.69280(3) 0.0245(3) Uani 1 1 d . . . Mn7 Mn 0.53191(14) -0.85973(17) -0.55972(13) 0.0165(7) Uani 1 1 d . . . Mn8 Mn 0.66113(15) -1.11963(19) -0.56674(14) 0.0246(8) Uani 1 1 d . . . Mn9 Mn 0.39888(15) -1.1260(2) -0.56804(13) 0.0251(9) Uani 1 1 d . . . Mn10 Mn 0.31915(17) -0.8721(2) -0.72764(16) 0.0387(11) Uani 1 1 d . . . Mn11 Mn 0.50123(17) -0.8693(2) -0.38157(14) 0.0352(10) Uani 1 1 d . . . Mn12 Mn 0.56586(18) -0.8340(2) -0.73719(15) 0.0372(11) Uani 1 1 d . . . Mn13 Mn 0.64155(17) -0.5718(2) -0.56276(18) 0.0400(11) Uani 1 1 d . . . Mn14 Mn 0.74345(16) -0.8934(2) -0.39289(16) 0.0395(11) Uani 1 1 d . . . Mn15 Mn 0.42694(15) -0.5842(2) -0.53623(15) 0.0310(10) Uani 1 1 d . . . C1 C 0.4182(10) -0.8538(13) -0.5546(9) 0.025(6) Uiso 1 1 d . . . C2 C 0.3789(11) -0.7458(15) -0.5394(10) 0.037(7) Uiso 1 1 d . . . C3 C 0.4041(10) -0.8690(13) -0.4863(9) 0.024(5) Uiso 1 1 d . . . C4 C 0.2864(15) -0.9136(19) -0.5659(13) 0.058(9) Uiso 1 1 d . . . C5 C 0.2909(12) -0.7847(15) -0.5874(10) 0.039(7) Uiso 1 1 d . . . C6 C 0.3239(18) -0.829(2) -0.5068(15) 0.074(12) Uiso 1 1 d . . . C7 C 0.3347(13) -0.8556(16) -0.6200(11) 0.046(8) Uiso 1 1 d . . . C8 C 0.3685(11) -0.9590(14) -0.5514(9) 0.033(6) Uiso 1 1 d . . . C9 C 0.6858(10) -0.7320(14) -0.5656(9) 0.030(6) Uiso 1 1 d . . . C10 C 0.6427(11) -0.8482(14) -0.5628(9) 0.032(6) Uiso 1 1 d . . . C11 C 0.6611(9) -0.8492(12) -0.6334(8) 0.020(5) Uiso 1 1 d . . . C12 C 0.6956(11) -0.9475(14) -0.5728(10) 0.034(6) Uiso 1 1 d . . . C13 C 0.7781(15) -0.7764(19) -0.5247(13) 0.057(9) Uiso 1 1 d . . . C14 C 0.7310(10) -0.8707(13) -0.5013(9) 0.027(6) Uiso 1 1 d . . . C15 C 0.7720(10) -0.9002(14) -0.5639(9) 0.030(6) Uiso 1 1 d . . . C16 C 0.7435(12) -0.7797(16) -0.6070(11) 0.045(8) Uiso 1 1 d . . . C17 C 0.6684(9) -0.7526(12) -0.4081(8) 0.022(5) Uiso 1 1 d . . . C18 C 0.5646(10) -0.7392(12) -0.4048(8) 0.022(5) Uiso 1 1 d . . . C19 C 0.6779(11) -0.6168(14) -0.3952(10) 0.034(6) Uiso 1 1 d . . . C20 C 0.5955(12) -0.5774(16) -0.3996(11) 0.045(8) Uiso 1 1 d . . . C21 C 0.5837(11) -0.7452(15) -0.4727(10) 0.037(7) Uiso 1 1 d . . . C22 C 0.6455(11) -0.6863(15) -0.3478(10) 0.035(7) Uiso 1 1 d . . . C23 C 0.6247(9) -0.6260(12) -0.4718(8) 0.022(5) Uiso 1 1 d . . . C24 C 0.5452(10) -0.6356(13) -0.4635(9) 0.028(6) Uiso 1 1 d . . . C25 C 0.4991(12) -0.7124(16) -0.7041(10) 0.041(7) Uiso 1 1 d . . . C26 C 0.3802(15) -0.599(2) -0.7106(13) 0.062(10) Uiso 1 1 d . . . C27 C 0.4179(17) -0.650(2) -0.7589(15) 0.072(11) Uiso 1 1 d . . . C28 C 0.4055(13) -0.7378(17) -0.7044(11) 0.049(8) Uiso 1 1 d . . . C29 C 0.4428(12) -0.6205(15) -0.6312(10) 0.038(7) Uiso 1 1 d . . . C30 C 0.5293(13) -0.6175(16) -0.6386(11) 0.043(7) Uiso 1 1 d . . . C31 C 0.4842(9) -0.7321(12) -0.6384(8) 0.019(5) Uiso 1 1 d . . . C32 C 0.4636(16) -0.550(2) -0.7004(14) 0.068(10) Uiso 1 1 d . . . C33 C 0.5906(13) -1.1937(17) -0.4536(11) 0.048(8) Uiso 1 1 d . . . C34 C 0.5647(10) -0.9949(14) -0.4879(9) 0.028(6) Uiso 1 1 d . . . C35 C 0.6460(9) -1.0091(12) -0.4210(8) 0.019(5) Uiso 1 1 d . . . C36 C 0.5553(11) -1.1247(15) -0.4032(10) 0.037(7) Uiso 1 1 d . . . C37 C 0.5621(10) -1.0023(13) -0.4110(9) 0.027(6) Uiso 1 1 d . . . C38 C 0.5143(9) -1.1034(12) -0.4892(8) 0.019(5) Uiso 1 1 d . . . C39 C 0.6202(9) -1.0994(11) -0.4855(8) 0.015(5) Uiso 1 1 d . . . C40 C 0.6480(14) -1.1121(18) -0.3832(12) 0.053(9) Uiso 1 1 d . . . C41 C 0.4972(10) -0.9792(13) -0.6412(9) 0.024(5) Uiso 1 1 d . . . C42 C 0.4599(11) -1.1664(15) -0.7002(10) 0.037(7) Uiso 1 1 d . . . C43 C 0.4461(10) -1.0878(13) -0.6462(9) 0.025(6) Uiso 1 1 d . . . C44 C 0.4295(11) -1.0701(14) -0.7616(10) 0.034(6) Uiso 1 1 d . . . C45 C 0.4074(11) -0.9946(14) -0.7093(9) 0.032(6) Uiso 1 1 d . . . C46 C 0.5417(9) -1.0893(12) -0.6432(8) 0.020(5) Uiso 1 1 d . . . C47 C 0.5041(11) -0.9723(15) -0.7181(10) 0.037(7) Uiso 1 1 d . . . C48 C 0.5189(13) -1.1007(17) -0.7217(12) 0.050(8) Uiso 1 1 d . . . C201 C 0.7866(17) -1.113(2) -0.5202(15) 0.073(11) Uiso 1 1 d . . . C202 C 0.6755(18) -1.293(2) -0.5436(15) 0.081(12) Uiso 1 1 d . . . C203 C 0.6687(17) -1.097(2) -0.6634(14) 0.067(10) Uiso 1 1 d . . . C204 C 0.2924(19) -1.081(2) -0.6519(16) 0.111(18) Uiso 1 1 d D . . C205 C 0.387(3) -1.284(4) -0.555(3) 0.17(3) Uiso 1 1 d . . . C206 C 0.388(2) -1.119(3) -0.4659(18) 0.094(15) Uiso 1 1 d . . . C207 C 0.353(3) -0.921(3) -0.812(2) 0.14(2) Uiso 1 1 d . . . C208 C 0.252(2) -0.739(3) -0.713(2) 0.110(17) Uiso 1 1 d . . . C210 C 0.4520(16) -1.018(2) -0.3640(14) 0.073(11) Uiso 1 1 d . . . C211 C 0.4121(11) -0.777(4) -0.372(2) 0.15(2) Uiso 1 1 d D . . C212 C 0.6141(16) -0.854(2) -0.3009(14) 0.068(10) Uiso 1 1 d . . . C213 C 0.4581(17) -0.794(2) -0.8324(15) 0.074(11) Uiso 1 1 d . . . C214 C 0.5895(14) -0.9735(18) -0.7808(12) 0.058(9) Uiso 1 1 d . . . C215 C 0.649(3) -0.752(4) -0.746(3) 0.16(3) Uiso 1 1 d . . . C216 C 0.758(4) -0.573(5) -0.487(4) 0.21(4) Uiso 1 1 d . . . C217 C 0.649(2) -0.564(3) -0.653(2) 0.104(17) Uiso 1 1 d . . . C218 C 0.571(2) -0.438(3) -0.6003(18) 0.094(14) Uiso 1 1 d . . . C219 C 0.818(4) -0.759(5) -0.369(3) 0.22(4) Uiso 1 1 d . . . C220 C 0.772(3) -1.016(3) -0.420(2) 0.14(2) Uiso 1 1 d . . . C221 C 0.760(4) -0.847(3) -0.297(3) 0.08(3) Uiso 0.50 1 d PD . . C222 C 0.504(3) -0.456(3) -0.510(2) 0.13(2) Uiso 1 1 d . . . C223 C 0.4234(15) -0.604(2) -0.4381(13) 0.064(10) Uiso 1 1 d . . . C224 C 0.3158(14) -0.5804(18) -0.6237(13) 0.056(9) Uiso 1 1 d . . . C321 C 0.730(3) -0.956(4) -0.308(4) 0.10(3) Uiso 0.50 1 d PD . . C804 C 0.740(3) -1.260(3) -0.404(2) 0.13(2) Uiso 1 1 d . . . O806 O 0.4778(13) -1.2786(18) -0.6067(12) 0.102(10) Uiso 1 1 d . . . O808 O 0.7074(19) -0.913(2) -0.7332(16) 0.149(16) Uiso 1 1 d . . . N1 N 0.4590(9) -0.8565(12) -0.5567(8) 0.035(5) Uiso 1 1 d . . . N2 N 0.3956(11) -0.6875(14) -0.5372(9) 0.049(7) Uiso 1 1 d . . . N3 N 0.4361(10) -0.8737(13) -0.4470(9) 0.044(6) Uiso 1 1 d . . . N4 N 0.2480(12) -0.9417(15) -0.5861(10) 0.057(7) Uiso 1 1 d . . . N5 N 0.2566(9) -0.7449(12) -0.6059(8) 0.036(5) Uiso 1 1 d . . . N6 N 0.3026(19) -0.819(2) -0.4826(16) 0.112(14) Uiso 1 1 d . . . N7 N 0.3296(11) -0.8700(14) -0.6568(10) 0.049(7) Uiso 1 1 d . . . N8 N 0.3813(9) -1.0178(11) -0.5533(8) 0.030(5) Uiso 1 1 d . . . N9 N 0.6734(10) -0.6757(13) -0.5637(9) 0.041(6) Uiso 1 1 d . . . N10 N 0.6048(8) -0.8523(10) -0.5624(7) 0.025(5) Uiso 1 1 d . . . N11 N 0.6280(10) -0.8537(13) -0.6694(9) 0.042(6) Uiso 1 1 d . . . N12 N 0.6807(8) -1.0039(11) -0.5710(7) 0.029(5) Uiso 1 1 d . . . N13 N 0.8114(13) -0.7473(16) -0.5000(11) 0.065(8) Uiso 1 1 d . . . N14 N 0.7382(10) -0.8761(12) -0.4611(8) 0.038(6) Uiso 1 1 d . . . N15 N 0.8031(14) -0.9362(18) -0.5694(12) 0.075(9) Uiso 1 1 d . . . N16 N 0.7527(12) -0.7442(15) -0.6327(10) 0.060(8) Uiso 1 1 d . . . N17 N 0.6948(10) -0.7978(13) -0.4012(9) 0.045(6) Uiso 1 1 d . . . N18 N 0.5392(9) -0.7777(12) -0.3974(8) 0.036(6) Uiso 1 1 d . . . N19 N 0.7174(15) -0.5830(19) -0.3774(13) 0.083(10) Uiso 1 1 d . . . N20 N 0.5848(13) -0.5299(17) -0.3802(12) 0.073(9) Uiso 1 1 d . . . N21 N 0.5650(9) -0.7857(12) -0.5020(8) 0.036(6) Uiso 1 1 d . . . N22 N 0.6642(11) -0.6951(14) -0.3079(10) 0.053(7) Uiso 1 1 d . . . N23 N 0.6276(11) -0.6013(14) -0.5003(9) 0.048(7) Uiso 1 1 d . . . N24 N 0.5016(11) -0.6177(14) -0.4907(9) 0.049(7) Uiso 1 1 d . . . N25 N 0.5278(9) -0.7480(12) -0.7183(8) 0.035(5) Uiso 1 1 d . . . N26 N 0.3436(17) -0.555(2) -0.7073(15) 0.104(13) Uiso 1 1 d . . . N27 N 0.4059(15) -0.6529(18) -0.7975(13) 0.079(10) Uiso 1 1 d . . . N28 N 0.3740(11) -0.7822(15) -0.7152(10) 0.055(7) Uiso 1 1 d . . . N29 N 0.4387(10) -0.6035(13) -0.5997(9) 0.043(6) Uiso 1 1 d . . . N30 N 0.5660(10) -0.6027(12) -0.6148(8) 0.039(6) Uiso 1 1 d . . . N31 N 0.5020(9) -0.7756(11) -0.6123(7) 0.030(5) Uiso 1 1 d . . . N32 N 0.4714(18) -0.491(2) -0.7074(15) 0.111(14) Uiso 1 1 d . . . N33 N 0.5898(10) -1.2569(14) -0.4564(9) 0.049(7) Uiso 1 1 d . . . N34 N 0.5519(8) -0.9496(11) -0.5140(7) 0.024(5) Uiso 1 1 d . . . N35 N 0.6781(11) -0.9658(14) -0.4112(10) 0.054(7) Uiso 1 1 d . . . N36 N 0.5352(10) -1.1537(12) -0.3799(9) 0.040(6) Uiso 1 1 d . . . N37 N 0.5448(10) -0.9582(13) -0.3985(8) 0.041(6) Uiso 1 1 d . . . N38 N 0.4758(8) -1.1139(10) -0.5177(7) 0.025(5) Uiso 1 1 d . . . N39 N 0.6405(10) -1.1082(12) -0.5097(8) 0.039(6) Uiso 1 1 d . . . N40 N 0.6823(15) -1.1373(19) -0.3500(13) 0.079(10) Uiso 1 1 d . . . N41 N 0.5073(9) -0.9354(12) -0.6152(8) 0.032(5) Uiso 1 1 d . . . N42 N 0.4474(12) -1.2228(17) -0.7036(11) 0.066(8) Uiso 1 1 d . . . N43 N 0.4292(8) -1.1009(11) -0.6193(7) 0.026(5) Uiso 1 1 d . . . N44 N 0.4073(11) -1.0705(14) -0.8005(10) 0.053(7) Uiso 1 1 d . . . N45 N 0.3765(8) -0.9570(10) -0.7150(7) 0.023(4) Uiso 1 1 d . . . N46 N 0.5789(9) -1.1063(11) -0.6177(8) 0.032(5) Uiso 1 1 d . . . N47 N 0.5233(9) -0.9224(12) -0.7271(8) 0.036(6) Uiso 1 1 d . . . N48 N 0.5432(11) -1.1207(15) -0.7442(10) 0.058(7) Uiso 1 1 d . . . O1 O 0.7394(7) -1.1347(9) -0.5186(6) 0.031(4) Uiso 1 1 d . . . O2 O 0.6486(9) -1.2350(13) -0.5710(8) 0.060(6) Uiso 1 1 d . . . O3 O 0.6880(8) -1.1334(10) -0.6197(7) 0.041(5) Uiso 1 1 d . . . O4 O 0.3223(8) -1.1333(11) -0.6219(7) 0.046(5) Uiso 1 1 d D . . O5 O 0.4040(8) -1.2384(10) -0.5783(7) 0.043(5) Uiso 1 1 d . . . O6 O 0.3763(8) -1.1522(10) -0.5122(7) 0.043(5) Uiso 1 1 d . . . O7 O 0.3069(9) -0.8820(11) -0.7992(8) 0.051(6) Uiso 1 1 d . . . O8 O 0.2608(11) -0.7911(14) -0.7436(9) 0.072(7) Uiso 1 1 d . . . O9 O 0.2580(9) -0.9476(12) -0.7434(8) 0.055(6) Uiso 1 1 d D . . O10 O 0.4625(9) -0.9455(12) -0.3550(8) 0.057(6) Uiso 1 1 d . . . O11 O 0.4636(9) -0.7913(12) -0.3578(8) 0.053(6) Uiso 1 1 d D . . O12 O 0.5613(9) -0.8654(12) -0.3139(8) 0.055(6) Uiso 1 1 d . . . O13 O 0.5149(9) -0.8230(11) -0.8091(8) 0.051(6) Uiso 1 1 d . . . O14 O 0.6072(9) -0.9031(12) -0.7667(8) 0.059(6) Uiso 1 1 d . . . O15 O 0.6074(11) -0.7456(14) -0.7507(9) 0.072(7) Uiso 1 1 d . . . O16 O 0.7190(11) -0.5346(14) -0.5175(9) 0.071(7) Uiso 1 1 d . . . O17 O 0.6613(9) -0.5302(12) -0.6150(8) 0.055(6) Uiso 1 1 d . . . O18 O 0.6132(8) -0.4650(11) -0.5581(7) 0.047(5) Uiso 1 1 d . . . O19 O 0.8122(12) -0.8357(15) -0.3637(10) 0.080(8) Uiso 1 1 d . . . O20 O 0.7906(8) -0.9877(11) -0.3829(7) 0.046(5) Uiso 1 1 d . . . O21 O 0.7599(11) -0.9096(14) -0.3207(10) 0.076(8) Uiso 1 1 d D . . O22 O 0.4518(9) -0.4739(12) -0.5349(8) 0.053(6) Uiso 1 1 d . . . O23 O 0.4093(10) -0.5557(13) -0.4801(9) 0.063(7) Uiso 1 1 d . . . O24 O 0.3537(8) -0.5442(11) -0.5807(7) 0.045(5) Uiso 1 1 d . . . O800 O 0.5080(10) -1.3418(13) -0.7155(9) 0.066(7) Uiso 1 1 d . . . O801 O 0.641(2) -0.416(3) -0.448(2) 0.084(17) Uiso 0.50 1 d P . . O802 O 0.6094(11) -1.2966(15) -0.6570(10) 0.083(8) Uiso 1 1 d . . . O803 O 0.504(4) -0.597(5) -0.821(3) 0.07(2) Uiso 0.30 1 d P . . O804 O 0.7665(12) -1.2155(16) -0.4368(11) 0.092(9) Uiso 1 1 d . . . O805 O 0.754(2) -0.424(3) -0.4462(19) 0.072(14) Uiso 0.50 1 d P . . O807 O 0.5157(15) -1.3159(18) -0.7999(13) 0.112(11) Uiso 1 1 d . . . O810 O 0.826(3) -1.084(4) -0.313(3) 0.13(3) Uiso 0.50 1 d P . . O811 O 0.560(2) -0.611(3) -0.7796(18) 0.071(14) Uiso 0.50 1 d P . . O813 O 0.904(2) -1.083(3) -0.146(2) 0.089(18) Uiso 0.50 1 d P . . C209 C 0.2126(14) -0.952(3) -0.738(2) 0.110(17) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0171(6) 0.0268(5) 0.0482(7) -0.0017(5) 0.0202(5) -0.0017(4) Re2 0.0187(6) 0.0284(6) 0.0642(8) 0.0108(6) 0.0243(6) 0.0037(4) Re3 0.0246(6) 0.0191(5) 0.0380(7) -0.0087(5) 0.0062(5) -0.0010(4) Re4 0.0267(7) 0.0331(6) 0.0396(7) 0.0166(5) 0.0127(5) 0.0093(5) Re5 0.0228(6) 0.0307(6) 0.0251(6) 0.0092(5) 0.0154(5) 0.0051(4) Re6 0.0237(6) 0.0344(6) 0.0171(5) -0.0055(4) 0.0104(4) -0.0001(4) Mn7 0.0114(16) 0.0229(18) 0.0202(19) 0.0007(16) 0.0115(15) 0.0016(16) Mn8 0.020(2) 0.0238(19) 0.031(2) 0.0018(17) 0.0107(18) 0.0041(16) Mn9 0.023(2) 0.026(2) 0.029(2) -0.0012(17) 0.0141(18) -0.0077(16) Mn10 0.024(2) 0.040(2) 0.038(3) 0.000(2) -0.001(2) 0.0038(19) Mn11 0.043(3) 0.048(3) 0.026(2) -0.001(2) 0.026(2) 0.005(2) Mn12 0.042(3) 0.049(3) 0.031(2) 0.005(2) 0.026(2) 0.006(2) Mn13 0.025(2) 0.027(2) 0.069(3) 0.006(2) 0.021(2) 0.0000(18) Mn14 0.022(2) 0.027(2) 0.050(3) -0.008(2) -0.004(2) 0.0007(17) Mn15 0.021(2) 0.025(2) 0.047(3) -0.0005(19) 0.014(2) 0.0063(16) _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 Re1 C6 1.97(4) . ? Re1 C1 2.02(3) . ? Re1 C3 2.06(3) . ? Re1 C5 2.07(3) . ? Re1 C7 2.08(3) . ? Re1 C8 2.08(3) . ? Re1 C4 2.09(4) . ? Re1 C2 2.12(3) . ? Re2 C15 2.05(3) . ? Re2 C14 2.06(3) . ? Re2 C11 2.06(2) . ? Re2 C12 2.09(3) . ? Re2 C10 2.11(3) . ? Re2 C9 2.16(3) . ? Re2 C13 2.17(4) . ? Re2 C16 2.18(3) . ? Re3 C19 2.01(3) . ? Re3 C24 2.02(3) . ? Re3 C20 2.04(3) . ? Re3 C23 2.06(2) . ? Re3 C21 2.08(3) . ? Re3 C18 2.09(2) . ? Re3 C17 2.12(2) . ? Re3 C22 2.14(3) . ? Re4 C25 1.97(3) . ? Re4 C32 2.02(4) . ? Re4 C28 2.06(3) . ? Re4 C29 2.07(3) . ? Re4 C31 2.08(2) . ? Re4 C27 2.13(5) . ? Re4 C30 2.19(3) . ? Re4 C26 2.22(4) . ? Re5 C36 2.01(3) . ? Re5 C40 2.03(4) . ? Re5 C35 2.04(2) . ? Re5 C37 2.06(2) . ? Re5 C39 2.08(2) . ? Re5 C38 2.12(2) . ? Re5 C34 2.14(3) . ? Re5 C33 2.17(3) . ? Re6 C46 2.05(2) . ? Re6 C44 2.08(3) . ? Re6 C48 2.08(3) . ? Re6 C43 2.08(2) . ? Re6 C42 2.09(3) . ? Re6 C41 2.11(2) . ? Re6 C45 2.13(3) . ? Re6 C47 2.14(3) . ? Mn7 N34 2.16(2) . ? Mn7 N41 2.17(2) . ? Mn7 N10 2.17(2) . ? Mn7 N1 2.18(2) . ? Mn7 N21 2.21(2) . ? Mn7 N31 2.22(2) . ? Mn8 O1 2.18(2) . ? Mn8 O3 2.19(2) . ? Mn8 O2 2.19(2) . ? Mn8 N39 2.19(2) . ? Mn8 N12 2.26(2) . ? Mn8 N46 2.29(2) . ? Mn9 O5 2.15(2) . ? Mn9 N38 2.17(2) . ? Mn9 O4 2.19(2) . ? Mn9 N8 2.20(2) . ? Mn9 O6 2.23(2) . ? Mn9 N43 2.24(2) . ? Mn10 O9 2.17(2) . ? Mn10 O8 2.18(3) . ? Mn10 N7 2.20(3) . ? Mn10 O7 2.21(2) . ? Mn10 N45 2.22(2) . ? Mn10 N28 2.24(3) . ? Mn11 O11 2.16(2) . ? Mn11 O12 2.17(2) . ? Mn11 N3 2.18(3) . ? Mn11 O10 2.21(2) . ? Mn11 N18 2.22(2) . ? Mn11 N37 2.30(2) . ? Mn12 N47 2.18(2) . ? Mn12 N25 2.19(2) . ? Mn12 O13 2.19(2) . ? Mn12 O15 2.20(3) . ? Mn12 N11 2.22(3) . ? Mn12 O14 2.24(2) . ? Mn13 O17 2.16(2) . ? Mn13 N9 2.16(2) . ? Mn13 O18 2.20(2) . ? Mn13 N30 2.22(3) . ? Mn13 O16 2.23(3) . ? Mn13 N23 2.30(3) . ? Mn14 O19 2.12(3) . ? Mn14 O20 2.18(2) . ? Mn14 N14 2.18(2) . ? Mn14 N35 2.21(3) . ? Mn14 O21 2.21(3) . ? Mn14 N17 2.23(3) . ? Mn15 N2 2.14(3) . ? Mn15 O24 2.15(2) . ? Mn15 N24 2.15(3) . ? Mn15 O23 2.16(2) . ? Mn15 O22 2.19(2) . ? Mn15 N29 2.26(3) . ? C1 N1 1.22(3) . ? C2 N2 1.19(4) . ? C3 N3 1.23(4) . ? C4 N4 1.16(5) . ? C5 N5 1.19(4) . ? C6 N6 1.21(5) . ? C7 N7 1.17(4) . ? C8 N8 1.17(3) . ? C9 N9 1.13(3) . ? C10 N10 1.12(3) . ? C11 N11 1.17(4) . ? C12 N12 1.16(3) . ? C13 N13 1.11(4) . ? C14 N14 1.24(3) . ? C15 N15 1.21(4) . ? C16 N16 1.18(4) . ? C17 N17 1.10(3) . ? C18 N18 1.13(3) . ? C19 N19 1.23(5) . ? C20 N20 1.20(4) . ? C21 N21 1.16(4) . ? C22 N22 1.19(4) . ? C23 N23 1.07(3) . ? C24 N24 1.25(4) . ? C25 N25 1.30(4) . ? C26 N26 1.39(5) . ? C27 N27 1.16(5) . ? C28 N28 1.18(4) . ? C29 N29 1.13(4) . ? C30 N30 1.06(4) . ? C31 N31 1.14(3) . ? C32 N32 1.17(5) . ? C33 N33 1.19(4) . ? C34 N34 1.15(3) . ? C35 N35 1.18(3) . ? C36 N36 1.26(4) . ? C37 N37 1.13(3) . ? C38 N38 1.14(3) . ? C39 N39 1.18(3) . ? C40 N40 1.22(5) . ? C41 N41 1.13(3) . ? C42 N42 1.11(4) . ? C43 N43 1.20(3) . ? C44 N44 1.16(4) . ? C45 N45 1.10(3) . ? C46 N46 1.10(3) . ? C47 N47 1.19(3) . ? C48 N48 1.27(4) . ? C201 O1 1.46(5) . ? C202 O2 1.41(5) . ? C203 O3 1.46(4) . ? C204 O4 1.403(10) . ? C205 O5 1.36(8) . ? C206 O6 1.53(5) . ? C207 O7 1.74(7) . ? C208 O8 1.48(6) . ? C210 O10 1.39(4) . ? C211 O11 1.401(10) . ? C212 O12 1.43(5) . ? C213 O13 1.60(5) . ? C214 O14 1.42(4) . ? C215 O15 1.18(8) . ? C216 O16 1.37(10) . ? C217 O17 1.29(6) . ? C218 O18 1.50(6) . ? C219 O19 1.47(9) . ? C220 O20 1.23(7) . ? C221 O21 1.40(3) . ? C222 O22 1.43(7) . ? C223 O23 1.54(4) . ? C224 O24 1.53(4) . ? C321 O21 1.42(3) . ? C804 O804 1.76(7) . ? O9 C209 1.405(10) . ? O803 O811 1.65(11) . ? 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 C6 Re1 C1 138.0(15) . . ? C6 Re1 C3 68.7(15) . . ? C1 Re1 C3 73.5(10) . . ? C6 Re1 C5 77.4(15) . . ? C1 Re1 C5 126.7(11) . . ? C3 Re1 C5 140.4(10) . . ? C6 Re1 C7 145.2(17) . . ? C1 Re1 C7 74.4(12) . . ? C3 Re1 C7 146.1(11) . . ? C5 Re1 C7 70.1(12) . . ? C6 Re1 C8 112.7(14) . . ? C1 Re1 C8 74.4(10) . . ? C3 Re1 C8 76.4(10) . . ? C5 Re1 C8 137.6(12) . . ? C7 Re1 C8 84.8(11) . . ? C6 Re1 C4 71.8(16) . . ? C1 Re1 C4 141.5(12) . . ? C3 Re1 C4 111.2(12) . . ? C5 Re1 C4 75.1(13) . . ? C7 Re1 C4 87.8(14) . . ? C8 Re1 C4 70.2(13) . . ? C6 Re1 C2 84.5(14) . . ? C1 Re1 C2 73.6(10) . . ? C3 Re1 C2 83.8(10) . . ? C5 Re1 C2 73.1(12) . . ? C7 Re1 C2 97.4(12) . . ? C8 Re1 C2 145.9(11) . . ? C4 Re1 C2 143.7(13) . . ? C15 Re2 C14 86.6(10) . . ? C15 Re2 C11 103.0(10) . . ? C14 Re2 C11 145.0(10) . . ? C15 Re2 C12 67.7(11) . . ? C14 Re2 C12 76.1(11) . . ? C11 Re2 C12 76.7(10) . . ? C15 Re2 C10 140.6(10) . . ? C14 Re2 C10 75.4(11) . . ? C11 Re2 C10 76.1(10) . . ? C12 Re2 C10 74.0(11) . . ? C15 Re2 C9 145.8(10) . . ? C14 Re2 C9 100.9(10) . . ? C11 Re2 C9 89.8(10) . . ? C12 Re2 C9 146.5(11) . . ? C10 Re2 C9 73.0(10) . . ? C15 Re2 C13 76.6(12) . . ? C14 Re2 C13 74.0(12) . . ? C11 Re2 C13 140.8(11) . . ? C12 Re2 C13 134.2(13) . . ? C10 Re2 C13 128.8(12) . . ? C9 Re2 C13 73.7(12) . . ? C15 Re2 C16 76.0(11) . . ? C14 Re2 C16 141.0(11) . . ? C11 Re2 C16 73.8(11) . . ? C12 Re2 C16 125.7(11) . . ? C10 Re2 C16 137.5(11) . . ? C9 Re2 C16 77.6(10) . . ? C13 Re2 C16 68.1(13) . . ? C19 Re3 C24 125.8(11) . . ? C19 Re3 C20 75.0(12) . . ? C24 Re3 C20 67.8(12) . . ? C19 Re3 C23 69.6(11) . . ? C24 Re3 C23 74.2(10) . . ? C20 Re3 C23 92.6(11) . . ? C19 Re3 C21 131.3(11) . . ? C24 Re3 C21 72.5(11) . . ? C20 Re3 C21 140.2(13) . . ? C23 Re3 C21 75.4(10) . . ? C19 Re3 C18 146.5(11) . . ? C24 Re3 C18 79.0(10) . . ? C20 Re3 C18 99.4(11) . . ? C23 Re3 C18 143.8(10) . . ? C21 Re3 C18 73.6(10) . . ? C19 Re3 C17 76.9(10) . . ? C24 Re3 C17 145.0(10) . . ? C20 Re3 C17 146.8(12) . . ? C23 Re3 C17 93.9(9) . . ? C21 Re3 C17 72.7(10) . . ? C18 Re3 C17 94.3(9) . . ? C19 Re3 C22 73.6(11) . . ? C24 Re3 C22 131.8(10) . . ? C20 Re3 C22 79.0(12) . . ? C23 Re3 C22 143.2(10) . . ? C21 Re3 C22 131.8(11) . . ? C18 Re3 C22 72.9(10) . . ? C17 Re3 C22 76.4(10) . . ? C25 Re4 C32 108.7(14) . . ? C25 Re4 C28 86.8(13) . . ? C32 Re4 C28 145.0(15) . . ? C25 Re4 C29 141.9(12) . . ? C32 Re4 C29 90.0(14) . . ? C28 Re4 C29 96.5(12) . . ? C25 Re4 C31 72.1(11) . . ? C32 Re4 C31 143.2(14) . . ? C28 Re4 C31 70.9(11) . . ? C29 Re4 C31 73.3(10) . . ? C25 Re4 C27 77.7(15) . . ? C32 Re4 C27 77.8(16) . . ? C28 Re4 C27 75.2(15) . . ? C29 Re4 C27 139.8(14) . . ? C31 Re4 C27 135.2(13) . . ? C25 Re4 C30 78.2(12) . . ? C32 Re4 C30 71.9(15) . . ? C28 Re4 C30 143.1(13) . . ? C29 Re4 C30 76.7(12) . . ? C31 Re4 C30 72.5(10) . . ? C27 Re4 C30 132.2(14) . . ? C25 Re4 C26 145.6(14) . . ? C32 Re4 C26 72.0(15) . . ? C28 Re4 C26 77.7(13) . . ? C29 Re4 C26 71.0(13) . . ? C31 Re4 C26 128.6(12) . . ? C27 Re4 C26 68.8(15) . . ? C30 Re4 C26 130.8(13) . . ? C36 Re5 C40 77.1(13) . . ? C36 Re5 C35 129.0(11) . . ? C40 Re5 C35 68.0(12) . . ? C36 Re5 C37 69.8(11) . . ? C40 Re5 C37 97.4(12) . . ? C35 Re5 C37 79.0(9) . . ? C36 Re5 C39 145.7(10) . . ? C40 Re5 C39 97.2(11) . . ? C35 Re5 C39 76.5(9) . . ? C37 Re5 C39 144.2(9) . . ? C36 Re5 C38 77.1(11) . . ? C40 Re5 C38 147.4(11) . . ? C35 Re5 C38 144.6(9) . . ? C37 Re5 C38 92.0(10) . . ? C39 Re5 C38 93.0(9) . . ? C36 Re5 C34 131.2(11) . . ? C40 Re5 C34 140.5(12) . . ? C35 Re5 C34 72.5(10) . . ? C37 Re5 C34 74.5(10) . . ? C39 Re5 C34 73.4(9) . . ? C38 Re5 C34 72.1(9) . . ? C36 Re5 C33 77.4(11) . . ? C40 Re5 C33 79.0(13) . . ? C35 Re5 C33 127.6(11) . . ? C37 Re5 C33 146.9(11) . . ? C39 Re5 C33 68.3(10) . . ? C38 Re5 C33 76.2(11) . . ? C34 Re5 C33 128.1(11) . . ? C46 Re6 C44 140.5(10) . . ? C46 Re6 C48 69.7(12) . . ? C44 Re6 C48 72.1(13) . . ? C46 Re6 C43 83.6(10) . . ? C44 Re6 C43 119.6(11) . . ? C48 Re6 C43 137.2(11) . . ? C46 Re6 C42 82.9(10) . . ? C44 Re6 C42 75.9(11) . . ? C48 Re6 C42 71.9(12) . . ? C43 Re6 C42 72.1(10) . . ? C46 Re6 C41 72.3(9) . . ? C44 Re6 C41 141.9(10) . . ? C48 Re6 C41 125.4(12) . . ? C43 Re6 C41 72.9(9) . . ? C42 Re6 C41 138.9(11) . . ? C46 Re6 C45 146.8(10) . . ? C44 Re6 C45 72.7(11) . . ? C48 Re6 C45 141.6(12) . . ? C43 Re6 C45 75.1(10) . . ? C42 Re6 C45 113.3(11) . . ? C41 Re6 C45 77.1(10) . . ? C46 Re6 C47 95.9(11) . . ? C44 Re6 C47 81.1(11) . . ? C48 Re6 C47 71.2(12) . . ? C43 Re6 C47 146.8(10) . . ? C42 Re6 C47 140.9(11) . . ? C41 Re6 C47 75.4(10) . . ? C45 Re6 C47 88.7(10) . . ? N34 Mn7 N41 87.9(8) . . ? N34 Mn7 N10 95.3(8) . . ? N41 Mn7 N10 89.8(8) . . ? N34 Mn7 N1 88.6(8) . . ? N41 Mn7 N1 93.8(9) . . ? N10 Mn7 N1 174.7(7) . . ? N34 Mn7 N21 90.5(8) . . ? N41 Mn7 N21 174.1(9) . . ? N10 Mn7 N21 84.7(8) . . ? N1 Mn7 N21 91.8(9) . . ? N34 Mn7 N31 172.2(8) . . ? N41 Mn7 N31 86.4(8) . . ? N10 Mn7 N31 90.0(8) . . ? N1 Mn7 N31 86.5(8) . . ? N21 Mn7 N31 95.7(8) . . ? O1 Mn8 O3 86.3(7) . . ? O1 Mn8 O2 90.8(8) . . ? O3 Mn8 O2 86.5(8) . . ? O1 Mn8 N39 89.0(8) . . ? O3 Mn8 N39 175.3(9) . . ? O2 Mn8 N39 93.0(9) . . ? O1 Mn8 N12 87.3(8) . . ? O3 Mn8 N12 83.2(7) . . ? O2 Mn8 N12 169.6(8) . . ? N39 Mn8 N12 97.2(8) . . ? O1 Mn8 N46 178.7(8) . . ? O3 Mn8 N46 93.3(8) . . ? O2 Mn8 N46 88.0(9) . . ? N39 Mn8 N46 91.4(9) . . ? N12 Mn8 N46 93.8(8) . . ? O5 Mn9 N38 95.9(8) . . ? O5 Mn9 O4 85.9(8) . . ? N38 Mn9 O4 176.1(8) . . ? O5 Mn9 N8 168.1(8) . . ? N38 Mn9 N8 90.1(8) . . ? O4 Mn9 N8 88.8(8) . . ? O5 Mn9 O6 88.6(7) . . ? N38 Mn9 O6 88.6(8) . . ? O4 Mn9 O6 95.0(8) . . ? N8 Mn9 O6 81.3(8) . . ? O5 Mn9 N43 90.8(7) . . ? N38 Mn9 N43 86.0(8) . . ? O4 Mn9 N43 90.4(8) . . ? N8 Mn9 N43 99.8(8) . . ? O6 Mn9 N43 174.5(8) . . ? O9 Mn10 O8 85.0(10) . . ? O9 Mn10 N7 89.8(9) . . ? O8 Mn10 N7 89.2(10) . . ? O9 Mn10 O7 86.8(8) . . ? O8 Mn10 O7 92.5(9) . . ? N7 Mn10 O7 176.0(9) . . ? O9 Mn10 N45 93.4(8) . . ? O8 Mn10 N45 177.0(9) . . ? N7 Mn10 N45 93.3(9) . . ? O7 Mn10 N45 84.8(8) . . ? O9 Mn10 N28 171.9(10) . . ? O8 Mn10 N28 87.0(10) . . ? N7 Mn10 N28 91.3(10) . . ? O7 Mn10 N28 92.3(9) . . ? N45 Mn10 N28 94.5(9) . . ? O11 Mn11 O12 86.0(9) . . ? O11 Mn11 N3 90.5(9) . . ? O12 Mn11 N3 175.1(9) . . ? O11 Mn11 O10 82.9(8) . . ? O12 Mn11 O10 87.4(9) . . ? N3 Mn11 O10 88.7(9) . . ? O11 Mn11 N18 86.5(8) . . ? O12 Mn11 N18 86.4(9) . . ? N3 Mn11 N18 96.8(9) . . ? O10 Mn11 N18 168.1(8) . . ? O11 Mn11 N37 173.3(9) . . ? O12 Mn11 N37 88.5(9) . . ? N3 Mn11 N37 94.8(9) . . ? O10 Mn11 N37 93.0(9) . . ? N18 Mn11 N37 97.1(8) . . ? N47 Mn12 N25 97.4(9) . . ? N47 Mn12 O13 93.3(9) . . ? N25 Mn12 O13 91.9(9) . . ? N47 Mn12 O15 177.4(10) . . ? N25 Mn12 O15 83.7(9) . . ? O13 Mn12 O15 84.3(9) . . ? N47 Mn12 N11 90.2(9) . . ? N25 Mn12 N11 98.2(9) . . ? O13 Mn12 N11 168.8(9) . . ? O15 Mn12 N11 92.0(10) . . ? N47 Mn12 O14 94.0(9) . . ? N25 Mn12 O14 167.0(9) . . ? O13 Mn12 O14 81.0(9) . . ? O15 Mn12 O14 84.7(9) . . ? N11 Mn12 O14 88.1(9) . . ? O17 Mn13 N9 93.1(9) . . ? O17 Mn13 O18 87.7(8) . . ? N9 Mn13 O18 176.6(10) . . ? O17 Mn13 N30 90.2(9) . . ? N9 Mn13 N30 92.8(9) . . ? O18 Mn13 N30 90.5(9) . . ? O17 Mn13 O16 82.8(9) . . ? N9 Mn13 O16 88.1(10) . . ? O18 Mn13 O16 88.7(9) . . ? N30 Mn13 O16 172.9(9) . . ? O17 Mn13 N23 171.0(10) . . ? N9 Mn13 N23 91.9(9) . . ? O18 Mn13 N23 86.9(8) . . ? N30 Mn13 N23 97.0(9) . . ? O16 Mn13 N23 89.9(10) . . ? O19 Mn14 O20 85.7(10) . . ? O19 Mn14 N14 91.7(10) . . ? O20 Mn14 N14 92.4(8) . . ? O19 Mn14 N35 168.9(11) . . ? O20 Mn14 N35 87.9(9) . . ? N14 Mn14 N35 97.6(10) . . ? O19 Mn14 O21 81.5(11) . . ? O20 Mn14 O21 83.6(9) . . ? N14 Mn14 O21 172.3(10) . . ? N35 Mn14 O21 88.8(10) . . ? O19 Mn14 N17 94.6(10) . . ? O20 Mn14 N17 178.2(9) . . ? N14 Mn14 N17 89.3(9) . . ? N35 Mn14 N17 91.5(10) . . ? O21 Mn14 N17 94.7(10) . . ? N2 Mn15 O24 90.4(9) . . ? N2 Mn15 N24 92.9(10) . . ? O24 Mn15 N24 176.5(9) . . ? N2 Mn15 O23 89.1(10) . . ? O24 Mn15 O23 87.6(9) . . ? N24 Mn15 O23 91.4(10) . . ? N2 Mn15 O22 173.9(9) . . ? O24 Mn15 O22 85.0(8) . . ? N24 Mn15 O22 91.7(9) . . ? O23 Mn15 O22 86.8(9) . . ? N2 Mn15 N29 94.0(9) . . ? O24 Mn15 N29 86.1(9) . . ? N24 Mn15 N29 94.7(10) . . ? O23 Mn15 N29 173.0(10) . . ? O22 Mn15 N29 89.6(9) . . ? N1 C1 Re1 179(2) . . ? N2 C2 Re1 172(3) . . ? N3 C3 Re1 175(2) . . ? N4 C4 Re1 161(3) . . ? N5 C5 Re1 176(2) . . ? N6 C6 Re1 173(4) . . ? N7 C7 Re1 168(3) . . ? N8 C8 Re1 174(2) . . ? N9 C9 Re2 178(3) . . ? N10 C10 Re2 177(2) . . ? N11 C11 Re2 172(2) . . ? N12 C12 Re2 166(2) . . ? N13 C13 Re2 174(3) . . ? N14 C14 Re2 167(2) . . ? N15 C15 Re2 170(3) . . ? N16 C16 Re2 170(3) . . ? N17 C17 Re3 174(2) . . ? N18 C18 Re3 177(2) . . ? N19 C19 Re3 176(3) . . ? N20 C20 Re3 166(3) . . ? N21 C21 Re3 176(2) . . ? N22 C22 Re3 179(3) . . ? N23 C23 Re3 175(3) . . ? N24 C24 Re3 175(2) . . ? N25 C25 Re4 175(2) . . ? N26 C26 Re4 156(3) . . ? N27 C27 Re4 168(4) . . ? N28 C28 Re4 174(3) . . ? N29 C29 Re4 177(3) . . ? N30 C30 Re4 178(3) . . ? N31 C31 Re4 177(2) . . ? N32 C32 Re4 176(4) . . ? N33 C33 Re5 171(3) . . ? N34 C34 Re5 179(3) . . ? N35 C35 Re5 177(2) . . ? N36 C36 Re5 179(2) . . ? N37 C37 Re5 174(3) . . ? N38 C38 Re5 175(2) . . ? N39 C39 Re5 177(2) . . ? N40 C40 Re5 174(3) . . ? N41 C41 Re6 176(2) . . ? N42 C42 Re6 172(3) . . ? N43 C43 Re6 176(2) . . ? N44 C44 Re6 172(3) . . ? N45 C45 Re6 172(3) . . ? N46 C46 Re6 177(2) . . ? N47 C47 Re6 172(3) . . ? N48 C48 Re6 171(3) . . ? C1 N1 Mn7 179(2) . . ? C2 N2 Mn15 177(2) . . ? C3 N3 Mn11 169(2) . . ? C7 N7 Mn10 168(3) . . ? C8 N8 Mn9 171(2) . . ? C9 N9 Mn13 174(2) . . ? C10 N10 Mn7 179(2) . . ? C11 N11 Mn12 166(2) . . ? C12 N12 Mn8 173(2) . . ? C14 N14 Mn14 174(2) . . ? C17 N17 Mn14 175(3) . . ? C18 N18 Mn11 168(2) . . ? C21 N21 Mn7 177(2) . . ? C23 N23 Mn13 167(2) . . ? C24 N24 Mn15 178(2) . . ? C25 N25 Mn12 163(2) . . ? C28 N28 Mn10 173(3) . . ? C29 N29 Mn15 172(2) . . ? C30 N30 Mn13 178(3) . . ? C31 N31 Mn7 176(2) . . ? C34 N34 Mn7 176(2) . . ? C35 N35 Mn14 174(2) . . ? C37 N37 Mn11 173(3) . . ? C38 N38 Mn9 173(2) . . ? C39 N39 Mn8 167(2) . . ? C41 N41 Mn7 174(2) . . ? C43 N43 Mn9 179(2) . . ? C45 N45 Mn10 174(2) . . ? C46 N46 Mn8 169(2) . . ? C47 N47 Mn12 174(2) . . ? C201 O1 Mn8 131(2) . . ? C202 O2 Mn8 133(2) . . ? C203 O3 Mn8 126(2) . . ? C204 O4 Mn9 130(3) . . ? C205 O5 Mn9 117(4) . . ? C206 O6 Mn9 134(2) . . ? C207 O7 Mn10 120(3) . . ? C208 O8 Mn10 130(3) . . ? C209 O9 Mn10 137(3) . . ? C210 O10 Mn11 131(2) . . ? C211 O11 Mn11 130(3) . . ? C212 O12 Mn11 128(2) . . ? C213 O13 Mn12 129.8(19) . . ? C214 O14 Mn12 119(2) . . ? C215 O15 Mn12 122(4) . . ? C216 O16 Mn13 129(5) . . ? C217 O17 Mn13 121(3) . . ? C218 O18 Mn13 116(2) . . ? C219 O19 Mn14 125(5) . . ? C220 O20 Mn14 103(3) . . ? C221 O21 C321 102(6) . . ? C221 O21 Mn14 114(4) . . ? C321 O21 Mn14 121(5) . . ? C222 O22 Mn15 120(3) . . ? C223 O23 Mn15 122(2) . . ? C224 O24 Mn15 126.4(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.739 _refine_diff_density_min -2.053 _refine_diff_density_rms 0.277 # Attachment '2b.cif' data_df38v _database_code_depnum_ccdc_archive 'CCDC 292903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common na _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76.5 H125 Mn9 Mo5.17 N48 O34 Re0.83' _chemical_formula_weight 3404.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 29.366(3) _cell_length_b 19.029(2) _cell_length_c 32.886(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.532(2) _cell_angle_gamma 90.00 _cell_volume 16718(3) _cell_formula_units_Z 6 _cell_measurement_temperature 178 _cell_measurement_reflns_used 7945 _cell_measurement_theta_min 4.495 _cell_measurement_theta_max 46.495 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max .20 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6285 _exptl_absorpt_coefficient_mu 1.688 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 178(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 'Bruker SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36892 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 23.35 _reflns_number_total 17232 _reflns_number_gt 13773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(4) _refine_ls_number_reflns 17232 _refine_ls_number_parameters 789 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2270 _refine_ls_wR_factor_gt 0.2166 _refine_ls_goodness_of_fit_ref 1.579 _refine_ls_restrained_S_all 1.579 _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 Re1 Re 0.38062(5) 1.44401(8) 0.93816(5) 0.0253(4) Uani 0.14 1 d P . . Re2 Re 0.61930(6) 1.66058(8) 1.05851(5) 0.0313(4) Uani 0.14 1 d P . . Re3 Re 0.25901(5) 1.65255(8) 1.08014(5) 0.0276(4) Uani 0.14 1 d P . . Re4 Re 0.49615(6) 1.42672(9) 1.19056(5) 0.0311(4) Uani 0.14 1 d P . . Re5 Re 0.36244(6) 1.84519(10) 0.94191(5) 0.0417(5) Uani 0.14 1 d P . . Re6 Re 0.52252(5) 1.83070(7) 1.20758(5) 0.0283(4) Uani 0.14 1 d P . . Mo1 Mo 0.38062(5) 1.44401(8) 0.93816(5) 0.0253(4) Uani 0.86 1 d P . . Mo2 Mo 0.61930(6) 1.66058(8) 1.05851(5) 0.0313(4) Uani 0.86 1 d P . . Mo3 Mo 0.25901(5) 1.65255(8) 1.08014(5) 0.0276(4) Uani 0.86 1 d P . . Mo4 Mo 0.49615(6) 1.42672(9) 1.19056(5) 0.0311(4) Uani 0.86 1 d P . . Mo5 Mo 0.36244(6) 1.84519(10) 0.94191(5) 0.0417(5) Uani 0.86 1 d P . . Mo6 Mo 0.52252(5) 1.83070(7) 1.20758(5) 0.0283(4) Uani 0.86 1 d P . . Mn1 Mn 0.30678(12) 1.37901(17) 1.06327(11) 0.0328(8) Uani 1 1 d . . . Mn2 Mn 0.43965(12) 1.64266(12) 1.06976(10) 0.0207(6) Uani 1 1 d . . . Mn3 Mn 0.56861(12) 1.38279(16) 1.06333(10) 0.0277(8) Uani 1 1 d . . . Mn4 Mn 0.47182(13) 1.66279(18) 0.88937(10) 0.0387(9) Uani 1 1 d . . . Mn5 Mn 0.33563(11) 1.91820(15) 1.09174(10) 0.0262(7) Uani 1 1 d . . . Mn6 Mn 0.65267(12) 1.60998(16) 1.23270(11) 0.0337(8) Uani 1 1 d . . . Mn7 Mn 0.40930(13) 1.63827(19) 1.24907(11) 0.0398(9) Uani 1 1 d . . . Mn8 Mn 0.22588(13) 1.62934(19) 0.90429(11) 0.0446(10) Uani 1 1 d . . . Mn9 Mn 0.54965(15) 1.9271(2) 1.06341(16) 0.0653(13) Uani 1 1 d . . . C1 C 0.3508(7) 1.4156(11) 0.9858(7) 0.030(5) Uiso 1 1 d . . . C2 C 0.4487(8) 1.4089(11) 0.9873(7) 0.038(6) Uiso 1 1 d . . . C3 C 0.4034(7) 1.5236(10) 0.9870(6) 0.027(5) Uiso 1 1 d . . . C4 C 0.4119(7) 1.5296(10) 0.9131(6) 0.026(5) Uiso 1 1 d . . . C5 C 0.3143(8) 1.5075(11) 0.9229(7) 0.033(5) Uiso 1 1 d . . . C6 C 0.3608(10) 1.3391(15) 0.9304(9) 0.068(8) Uiso 1 1 d . . . C7 C 0.4227(8) 1.4003(11) 0.9064(7) 0.039(5) Uiso 1 1 d . . . C8 C 0.3357(11) 1.4358(14) 0.8703(10) 0.070(8) Uiso 1 1 d . . . C9 C 0.5495(10) 1.6538(12) 1.0648(8) 0.043(6) Uiso 1 1 d . . . C10 C 0.5645(9) 1.6505(12) 0.9914(8) 0.042(6) Uiso 1 1 d . . . C11 C 0.5985(8) 1.5525(11) 1.0532(6) 0.028(5) Uiso 1 1 d . . . C12 C 0.6846(10) 1.7184(13) 1.0987(8) 0.049(6) Uiso 1 1 d . . . C13 C 0.5937(10) 1.7676(13) 1.0597(8) 0.054(7) Uiso 1 1 d . . . C14 C 0.6789(8) 1.5980(11) 1.0588(7) 0.038(5) Uiso 1 1 d . . . C15 C 0.6474(8) 1.7192(12) 1.0188(7) 0.046(6) Uiso 1 1 d . . . C16 C 0.6391(7) 1.6362(10) 1.1282(7) 0.028(5) Uiso 1 1 d . . . C17 C 0.3285(7) 1.6495(9) 1.0756(6) 0.020(4) Uiso 1 1 d . . . C18 C 0.2444(8) 1.6398(11) 1.0119(7) 0.036(5) Uiso 1 1 d . . . C19 C 0.3155(9) 1.6417(11) 1.1479(7) 0.038(6) Uiso 1 1 d . . . C20 C 0.2768(9) 1.5453(12) 1.0762(7) 0.041(6) Uiso 1 1 d . . . C21 C 0.2894(8) 1.7569(11) 1.0894(7) 0.032(5) Uiso 1 1 d . . . C22 C 0.1977(8) 1.7207(11) 1.0419(7) 0.034(5) Uiso 1 1 d . . . C23 C 0.1953(13) 1.5889(17) 1.0639(11) 0.085(10) Uiso 1 1 d . . . C24 C 0.2311(11) 1.6793(15) 1.1238(9) 0.070(8) Uiso 1 1 d . . . C25 C 0.4739(7) 1.5111(10) 1.1412(6) 0.025(5) Uiso 1 1 d . . . C26 C 0.5537(8) 1.5022(11) 1.2091(7) 0.036(5) Uiso 1 1 d . . . C27 C 0.5290(7) 1.4035(10) 1.1442(6) 0.029(5) Uiso 1 1 d . . . C28 C 0.4232(8) 1.4018(10) 1.1423(6) 0.029(5) Uiso 1 1 d . . . C29 C 0.4669(8) 1.5102(11) 1.2175(7) 0.036(5) Uiso 1 1 d . . . C30 C 0.4587(8) 1.3751(11) 1.2266(7) 0.039(6) Uiso 1 1 d . . . C31 C 0.5023(10) 1.3189(15) 1.1837(9) 0.069(8) Uiso 1 1 d . . . C32 C 0.5557(11) 1.3963(15) 1.2517(10) 0.077(8) Uiso 1 1 d . . . C33 C 0.3941(8) 1.7685(11) 0.9916(7) 0.036(5) Uiso 1 1 d . . . C34 C 0.4074(9) 1.7811(12) 0.9174(8) 0.046(6) Uiso 1 1 d . . . C35 C 0.3517(8) 1.8823(11) 0.9985(7) 0.040(6) Uiso 1 1 d . . . C36 C 0.4380(8) 1.8800(11) 0.9899(7) 0.037(5) Uiso 1 1 d . . . C37 C 0.3075(9) 1.7618(12) 0.9259(8) 0.047(6) Uiso 1 1 d . . . C38 C 0.3801(13) 1.9501(18) 0.9244(11) 0.087(10) Uiso 1 1 d . . . C39 C 0.3257(16) 1.843(2) 0.8679(15) 0.120(14) Uiso 1 1 d . . . C40 C 0.2931(12) 1.9000(16) 0.9201(10) 0.079(9) Uiso 1 1 d . . . C41 C 0.4744(7) 1.7628(9) 1.2247(6) 0.019(4) Uiso 1 1 d . . . C42 C 0.5757(7) 1.7470(10) 1.2195(6) 0.028(5) Uiso 1 1 d . . . C43 C 0.4508(6) 1.8678(9) 1.1640(6) 0.016(4) Uiso 1 1 d . . . C44 C 0.4909(7) 1.7526(10) 1.1544(6) 0.025(5) Uiso 1 1 d . . . C45 C 0.5344(8) 1.8755(11) 1.1512(7) 0.035(5) Uiso 1 1 d . . . C46 C 0.5899(8) 1.8853(11) 1.2328(7) 0.038(5) Uiso 1 1 d . . . C47 C 0.5558(8) 1.8160(11) 1.2775(7) 0.033(5) Uiso 1 1 d . . . C48 C 0.5063(11) 1.9220(16) 1.2313(10) 0.073(8) Uiso 1 1 d . . . C201 C 0.2051(16) 1.428(2) 0.9794(14) 0.132(14) Uiso 1 1 d . . . C202 C 0.3095(11) 1.3836(15) 1.1653(10) 0.074(9) Uiso 1 1 d . . . C203 C 0.3037(18) 1.214(2) 1.0795(16) 0.148(17) Uiso 1 1 d . . . C204 C 0.5773(12) 1.3953(16) 0.9703(7) 0.085(10) Uiso 1 1 d D . . C205 C 0.6910(9) 1.3941(12) 1.1106(8) 0.050(6) Uiso 1 1 d . . . C206 C 0.5811(14) 1.215(2) 1.0754(12) 0.102(11) Uiso 1 1 d . . . C207 C 0.4984(11) 1.5182(16) 0.8492(10) 0.078(8) Uiso 1 1 d . . . C208 C 0.3669(11) 1.7002(15) 0.8014(9) 0.074(8) Uiso 1 1 d . . . C210 C 0.3562(13) 1.4893(18) 1.2574(11) 0.100(11) Uiso 1 1 d . . . C211 C 0.5180(11) 1.6624(14) 1.3300(9) 0.071(8) Uiso 1 1 d . . . C212 C 0.3214(8) 1.7351(16) 1.2606(10) 0.088(9) Uiso 1 1 d D . . C213 C 0.3339(11) 1.8969(15) 1.1890(9) 0.072(8) Uiso 1 1 d . . . C214 C 0.2288(9) 1.9218(13) 1.0072(8) 0.052(7) Uiso 1 1 d . . . C215 C 0.4082(14) 2.0489(18) 1.1230(12) 0.102(11) Uiso 1 1 d . . . C216 C 0.7310(16) 1.728(2) 1.2274(14) 0.126(14) Uiso 1 1 d . . . C218 C 0.6793(14) 1.4642(19) 1.2089(13) 0.112(12) Uiso 1 1 d . . . C219 C 0.2510(19) 1.625(2) 0.8180(16) 0.149(17) Uiso 1 1 d . . . C220 C 0.1619(10) 1.7622(14) 0.9187(9) 0.063(7) Uiso 1 1 d . . . C221 C 0.118(2) 1.534(3) 0.8887(16) 0.166(19) Uiso 1 1 d . . . C222 C 0.4778(14) 2.0658(18) 1.0342(12) 0.098(11) Uiso 1 1 d . . . C223 C 0.5585(15) 1.933(2) 0.9778(13) 0.109(13) Uiso 1 1 d . . . C224 C 0.6684(15) 1.920(2) 1.1240(13) 0.116(13) Uiso 1 1 d . . . O801 O 0.8388(11) 1.5889(15) 1.0119(10) 0.148(10) Uiso 1 1 d . . . C804 C 0.6375(14) 1.2515(19) 1.2090(12) 0.110(12) Uiso 1 1 d . . . C807 C 0.428(2) 1.898(3) 0.839(2) 0.087(19) Uiso 0.50 1 d P . . C808 C 0.453(2) 1.125(3) 0.8194(18) 0.17(2) Uiso 1 1 d . . . C810 C 0.6126(11) 1.5886(15) 0.8872(10) 0.075(8) Uiso 1 1 d . . . C812 C 0.5575(16) 1.076(2) 1.1816(15) 0.121(13) Uiso 1 1 d . . . N1 N 0.3357(7) 1.3997(9) 1.0109(6) 0.035(4) Uiso 1 1 d . . . N2 N 0.4899(6) 1.3975(9) 1.0163(5) 0.032(4) Uiso 1 1 d . . . N3 N 0.4138(6) 1.5673(8) 1.0151(5) 0.025(4) Uiso 1 1 d . . . N4 N 0.4287(7) 1.5761(9) 0.9026(6) 0.040(5) Uiso 1 1 d . . . N5 N 0.2833(8) 1.5475(10) 0.9142(6) 0.048(5) Uiso 1 1 d . . . N6 N 0.3559(10) 1.2792(15) 0.9329(9) 0.095(8) Uiso 1 1 d . . . N7 N 0.4476(9) 1.3710(12) 0.8888(8) 0.069(7) Uiso 1 1 d . . . N8 N 0.3134(8) 1.4353(11) 0.8299(8) 0.070(6) Uiso 1 1 d . . . N9 N 0.5117(6) 1.6491(8) 1.0666(5) 0.027(4) Uiso 1 1 d . . . N10 N 0.5351(8) 1.6508(10) 0.9561(7) 0.050(5) Uiso 1 1 d . . . N11 N 0.5874(7) 1.4961(10) 1.0564(6) 0.044(5) Uiso 1 1 d . . . N12 N 0.7207(9) 1.7512(12) 1.1236(7) 0.070(7) Uiso 1 1 d . . . N13 N 0.5773(7) 1.8255(10) 1.0587(6) 0.047(5) Uiso 1 1 d . . . N14 N 0.7123(8) 1.5619(11) 1.0588(7) 0.062(6) Uiso 1 1 d . . . N15 N 0.6629(8) 1.7531(11) 0.9962(7) 0.062(6) Uiso 1 1 d . . . N16 N 0.6454(7) 1.6217(9) 1.1617(6) 0.036(4) Uiso 1 1 d . . . N17 N 0.3668(6) 1.6464(8) 1.0731(5) 0.029(4) Uiso 1 1 d . . . N18 N 0.2339(9) 1.6311(12) 0.9723(8) 0.067(7) Uiso 1 1 d . . . N19 N 0.3470(8) 1.6379(10) 1.1831(7) 0.047(5) Uiso 1 1 d . . . N20 N 0.2884(7) 1.4890(10) 1.0770(6) 0.046(5) Uiso 1 1 d . . . N21 N 0.3043(7) 1.8132(10) 1.0918(6) 0.044(5) Uiso 1 1 d . . . N22 N 0.1667(7) 1.7589(9) 1.0247(6) 0.039(4) Uiso 1 1 d . . . N23 N 0.1588(15) 1.560(2) 1.0541(12) 0.147(14) Uiso 1 1 d . . . N24 N 0.2169(10) 1.7006(14) 1.1526(9) 0.094(8) Uiso 1 1 d . . . N25 N 0.4617(6) 1.5529(8) 1.1163(5) 0.028(4) Uiso 1 1 d . . . N26 N 0.5891(8) 1.5399(11) 1.2172(7) 0.055(6) Uiso 1 1 d . . . N27 N 0.5469(6) 1.3969(9) 1.1190(5) 0.033(4) Uiso 1 1 d . . . N28 N 0.3831(7) 1.3853(9) 1.1135(6) 0.036(4) Uiso 1 1 d . . . N29 N 0.4492(7) 1.5543(10) 1.2310(6) 0.048(5) Uiso 1 1 d . . . N30 N 0.4422(8) 1.3526(10) 1.2492(7) 0.054(5) Uiso 1 1 d . . . N31 N 0.5007(10) 1.2526(15) 1.1731(9) 0.099(8) Uiso 1 1 d . . . N32 N 0.5899(14) 1.3849(19) 1.2892(13) 0.144(12) Uiso 1 1 d . . . N33 N 0.4108(6) 1.7248(9) 1.0198(5) 0.032(4) Uiso 1 1 d . . . N34 N 0.4320(7) 1.7444(10) 0.9085(6) 0.043(5) Uiso 1 1 d . . . N35 N 0.3472(7) 1.8961(10) 1.0309(6) 0.046(5) Uiso 1 1 d . . . N36 N 0.4755(7) 1.8947(9) 1.0134(6) 0.044(5) Uiso 1 1 d . . . N37 N 0.2791(8) 1.7161(11) 0.9162(7) 0.059(6) Uiso 1 1 d . . . N38 N 0.3926(14) 2.008(2) 0.9172(12) 0.146(13) Uiso 1 1 d . . . N39 N 0.3035(12) 1.8311(16) 0.8268(11) 0.113(10) Uiso 1 1 d . . . N40 N 0.2537(11) 1.9325(14) 0.9072(9) 0.097(9) Uiso 1 1 d . . . N41 N 0.4499(7) 1.7268(9) 1.2348(6) 0.038(4) Uiso 1 1 d . . . N42 N 0.6047(8) 1.7055(10) 1.2236(6) 0.052(5) Uiso 1 1 d . . . N43 N 0.4119(7) 1.8865(9) 1.1402(6) 0.044(5) Uiso 1 1 d . . . N44 N 0.4720(6) 1.7180(8) 1.1260(5) 0.031(4) Uiso 1 1 d . . . N45 N 0.5381(7) 1.9002(10) 1.1231(6) 0.045(5) Uiso 1 1 d . . . N46 N 0.6291(9) 1.9119(12) 1.2495(8) 0.071(6) Uiso 1 1 d . . . N47 N 0.5758(8) 1.8097(11) 1.3155(7) 0.059(6) Uiso 1 1 d . . . N48 N 0.4970(13) 1.9756(18) 1.2444(11) 0.132(11) Uiso 1 1 d . . . O1 O 0.2306(6) 1.3704(8) 1.0128(5) 0.052(4) Uiso 1 1 d . . . O2 O 0.2863(6) 1.3485(7) 1.1197(5) 0.044(4) Uiso 1 1 d . . . O3 O 0.3125(5) 1.2686(8) 1.0536(5) 0.044(4) Uiso 1 1 d . . . O4 O 0.5947(6) 1.3614(8) 1.0118(5) 0.053(4) Uiso 1 1 d D . . O5 O 0.6455(6) 1.3657(7) 1.1119(5) 0.041(4) Uiso 1 1 d . . . O6 O 0.5595(8) 1.2705(11) 1.0656(7) 0.080(6) Uiso 1 1 d . . . O7 O 0.5112(6) 1.5890(9) 0.8627(5) 0.057(5) Uiso 1 1 d . . . O8 O 0.4172(6) 1.6726(8) 0.8198(5) 0.051(4) Uiso 1 1 d . . . O9 O 0.5122(6) 1.7447(9) 0.8742(6) 0.063(5) Uiso 1 1 d D . . O10 O 0.3700(7) 1.5626(9) 1.2747(6) 0.066(5) Uiso 1 1 d . . . O11 O 0.4688(6) 1.6421(8) 1.3169(5) 0.049(4) Uiso 1 1 d . . . O12 O 0.3708(7) 1.7130(9) 1.2728(6) 0.073(5) Uiso 1 1 d D . . O13 O 0.3229(6) 1.9460(9) 1.1499(5) 0.059(5) Uiso 1 1 d . . . O14 O 0.2623(5) 1.9549(7) 1.0478(5) 0.039(4) Uiso 1 1 d . . . O15 O 0.3595(6) 2.0276(8) 1.0931(5) 0.057(4) Uiso 1 1 d . . . O16 O 0.7207(6) 1.6756(8) 1.2533(5) 0.050(4) Uiso 1 1 d . . . O17 O 0.6696(8) 1.6033(10) 1.3036(7) 0.077(6) Uiso 1 1 d D . . O18 O 0.6973(7) 1.5194(9) 1.2423(6) 0.070(5) Uiso 1 1 d . . . O19 O 0.2118(6) 1.6265(8) 0.8339(5) 0.057(5) Uiso 1 1 d . . . O20 O 0.1645(7) 1.7062(9) 0.8875(6) 0.070(5) Uiso 1 1 d . . . O21 O 0.1684(8) 1.5445(10) 0.8872(6) 0.078(6) Uiso 1 1 d . . . O22 O 0.5221(8) 2.0304(10) 1.0667(7) 0.083(6) Uiso 1 1 d . . . O23 O 0.5681(8) 1.9723(11) 1.0122(7) 0.094(7) Uiso 1 1 d . . . O24 O 0.6238(8) 1.9595(11) 1.1080(7) 0.082(6) Uiso 1 1 d . . . O802 O 0.4208(9) 1.1565(12) 0.9151(8) 0.118(8) Uiso 1 1 d . . . O803 O 0.3340(9) 2.0698(12) 1.1923(8) 0.025(6) Uiso 0.50 1 d P . . O804 O 0.6705(8) 1.2923(11) 1.1890(7) 0.102(7) Uiso 1 1 d . . . O805 O 0.4283(14) 1.2443(16) 1.0572(12) 0.181(12) Uiso 1 1 d . . . O807 O 0.460(2) 1.860(3) 0.8307(17) 0.119(16) Uiso 0.50 1 d P . . O808 O 0.4216(11) 1.1831(16) 0.8297(10) 0.153(11) Uiso 1 1 d . . . O809 O 0.6473(19) 1.566(3) 0.9256(17) 0.117(16) Uiso 0.50 1 d P . . O810 O 0.3212(19) 2.033(3) 0.8017(17) 0.122(16) Uiso 0.50 1 d P . . O812 O 0.5335(12) 1.1027(15) 1.1497(11) 0.141(10) Uiso 1 1 d . . . O813 O 0.201(2) 1.456(3) 0.719(2) 0.15(2) Uiso 0.50 1 d P . . O814 O 0.223(3) 1.263(4) 0.920(2) 0.18(3) Uiso 0.50 1 d P . . O816 O 0.4366(14) 1.9029(19) 0.7504(12) 0.077(11) Uiso 0.50 1 d P . . O818 O 0.5139(15) 1.202(2) 0.9706(13) 0.090(12) Uiso 0.50 1 d P . . C209 C 0.537(3) 1.797(3) 0.9060(19) 0.28(3) Uiso 1 1 d D . . C217 C 0.631(3) 1.602(5) 1.319(3) 0.32(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0256(9) 0.0269(9) 0.0211(8) -0.0042(7) 0.0073(6) 0.0035(6) Re2 0.0198(9) 0.0385(10) 0.0407(9) 0.0122(8) 0.0178(7) 0.0070(7) Re3 0.0178(9) 0.0284(9) 0.0438(10) -0.0038(8) 0.0199(7) -0.0059(7) Re4 0.0268(9) 0.0401(10) 0.0295(8) 0.0136(7) 0.0148(7) 0.0049(7) Re5 0.0452(12) 0.0548(12) 0.0309(9) 0.0218(8) 0.0217(8) 0.0285(9) Re6 0.0188(8) 0.0158(8) 0.0370(9) -0.0036(7) -0.0015(7) 0.0018(6) Mo1 0.0256(9) 0.0269(9) 0.0211(8) -0.0042(7) 0.0073(6) 0.0035(6) Mo2 0.0198(9) 0.0385(10) 0.0407(9) 0.0122(8) 0.0178(7) 0.0070(7) Mo3 0.0178(9) 0.0284(9) 0.0438(10) -0.0038(8) 0.0199(7) -0.0059(7) Mo4 0.0268(9) 0.0401(10) 0.0295(8) 0.0136(7) 0.0148(7) 0.0049(7) Mo5 0.0452(12) 0.0548(12) 0.0309(9) 0.0218(8) 0.0217(8) 0.0285(9) Mo6 0.0188(8) 0.0158(8) 0.0370(9) -0.0036(7) -0.0015(7) 0.0018(6) Mn1 0.0263(19) 0.0345(19) 0.037(2) 0.0019(15) 0.0130(15) -0.0097(14) Mn2 0.0168(12) 0.0261(15) 0.0212(13) -0.0003(14) 0.0097(11) 0.0008(15) Mn3 0.0274(18) 0.0272(18) 0.0272(17) 0.0045(14) 0.0101(14) 0.0088(13) Mn4 0.044(2) 0.052(2) 0.0293(18) 0.0147(16) 0.0245(16) 0.0212(17) Mn5 0.0165(16) 0.0218(17) 0.0382(18) 0.0002(14) 0.0094(14) 0.0073(12) Mn6 0.0270(19) 0.0264(18) 0.0385(19) -0.0064(15) 0.0045(15) 0.0033(14) Mn7 0.045(2) 0.049(2) 0.0327(19) 0.0046(16) 0.0229(17) 0.0070(17) Mn8 0.028(2) 0.056(2) 0.035(2) -0.0069(17) -0.0024(15) 0.0138(17) Mn9 0.035(2) 0.054(3) 0.115(4) 0.044(2) 0.039(2) 0.0114(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C6 2.07(3) . ? Re1 C8 2.07(3) . ? Re1 C2 2.09(2) . ? Re1 C7 2.09(2) . ? Re1 C3 2.11(2) . ? Re1 C1 2.16(2) . ? Re1 C5 2.17(2) . ? Re1 C4 2.19(2) . ? Re2 C14 2.11(2) . ? Re2 C15 2.13(2) . ? Re2 C12 2.13(3) . ? Re2 C11 2.13(2) . ? Re2 C10 2.13(2) . ? Re2 C9 2.15(3) . ? Re2 C16 2.17(2) . ? Re2 C13 2.18(3) . ? Re3 C24 1.99(3) . ? Re3 C23 2.10(4) . ? Re3 C17 2.11(2) . ? Re3 C18 2.12(2) . ? Re3 C20 2.12(2) . ? Re3 C21 2.15(2) . ? Re3 C22 2.15(2) . ? Re3 C19 2.16(2) . ? Re4 C31 2.08(3) . ? Re4 C26 2.11(2) . ? Re4 C28 2.12(2) . ? Re4 C32 2.12(3) . ? Re4 C30 2.16(2) . ? Re4 C27 2.16(2) . ? Re4 C29 2.16(2) . ? Re4 C25 2.18(2) . ? Re5 C33 2.10(2) . ? Re5 C40 2.13(3) . ? Re5 C35 2.13(2) . ? Re5 C37 2.17(2) . ? Re5 C34 2.18(2) . ? Re5 C38 2.20(3) . ? Re5 C39 2.22(4) . ? Re5 C36 2.22(2) . ? Re6 C48 2.04(3) . ? Re6 C46 2.08(2) . ? Re6 C47 2.11(2) . ? Re6 C43 2.116(17) . ? Re6 C42 2.15(2) . ? Re6 C41 2.155(19) . ? Re6 C44 2.186(19) . ? Re6 C45 2.20(2) . ? Mn1 O3 2.141(15) . ? Mn1 N28 2.165(18) . ? Mn1 O1 2.168(16) . ? Mn1 N1 2.249(18) . ? Mn1 O2 2.251(15) . ? Mn1 N20 2.25(2) . ? Mn2 N9 2.163(18) . ? Mn2 N33 2.169(17) . ? Mn2 N3 2.175(16) . ? Mn2 N17 2.188(18) . ? Mn2 N25 2.204(17) . ? Mn2 N44 2.219(17) . ? Mn3 O6 2.16(2) . ? Mn3 O4 2.167(16) . ? Mn3 O5 2.181(15) . ? Mn3 N27 2.190(17) . ? Mn3 N2 2.202(17) . ? Mn3 N11 2.260(19) . ? Mn4 O9 2.138(18) . ? Mn4 N34 2.187(19) . ? Mn4 O8 2.190(16) . ? Mn4 O7 2.219(17) . ? Mn4 N10 2.22(2) . ? Mn4 N4 2.229(18) . ? Mn5 O14 2.151(14) . ? Mn5 O13 2.160(16) . ? Mn5 O15 2.192(16) . ? Mn5 N21 2.20(2) . ? Mn5 N35 2.204(19) . ? Mn5 N43 2.225(19) . ? Mn6 O18 2.109(18) . ? Mn6 N26 2.18(2) . ? Mn6 O17 2.18(2) . ? Mn6 O16 2.210(16) . ? Mn6 N42 2.24(2) . ? Mn6 N16 2.267(18) . ? Mn7 O12 2.155(18) . ? Mn7 N19 2.18(2) . ? Mn7 O11 2.190(16) . ? Mn7 N29 2.20(2) . ? Mn7 O10 2.220(19) . ? Mn7 N41 2.224(18) . ? Mn8 N18 2.15(2) . ? Mn8 O19 2.176(17) . ? Mn8 N37 2.19(2) . ? Mn8 O20 2.207(18) . ? Mn8 N5 2.22(2) . ? Mn8 O21 2.23(2) . ? Mn9 N13 2.13(2) . ? Mn9 O22 2.15(2) . ? Mn9 O24 2.15(2) . ? Mn9 O23 2.15(2) . ? Mn9 N45 2.188(19) . ? Mn9 N36 2.20(2) . ? C1 N1 1.13(2) . ? C2 N2 1.21(3) . ? C3 N3 1.18(2) . ? C4 N4 1.13(2) . ? C5 N5 1.13(3) . ? C6 N6 1.16(3) . ? C7 N7 1.24(3) . ? C8 N8 1.21(3) . ? C9 N9 1.14(3) . ? C10 N10 1.12(3) . ? C11 N11 1.14(2) . ? C12 N12 1.21(3) . ? C13 N13 1.20(3) . ? C14 N14 1.20(3) . ? C15 N15 1.21(3) . ? C16 N16 1.07(2) . ? C17 N17 1.16(2) . ? C18 N18 1.22(3) . ? C19 N19 1.15(3) . ? C20 N20 1.12(3) . ? C21 N21 1.15(2) . ? C22 N22 1.12(2) . ? C23 N23 1.13(4) . ? C24 N24 1.25(3) . ? C25 N25 1.09(2) . ? C26 N26 1.20(3) . ? C27 N27 1.16(2) . ? C28 N28 1.21(2) . ? C29 N29 1.17(2) . ? C30 N30 1.13(3) . ? C31 N31 1.31(3) . ? C32 N32 1.25(4) . ? C33 N33 1.19(2) . ? C34 N34 1.13(3) . ? C35 N35 1.16(3) . ? C36 N36 1.09(2) . ? C37 N37 1.15(3) . ? C38 N38 1.21(4) . ? C39 N39 1.25(4) . ? C40 N40 1.22(4) . ? C41 N41 1.14(2) . ? C42 N42 1.13(3) . ? C43 N43 1.14(2) . ? C44 N44 1.09(2) . ? C45 N45 1.08(2) . ? C46 N46 1.16(3) . ? C47 N47 1.15(2) . ? C48 N48 1.18(4) . ? C201 O1 1.51(4) . ? C202 O2 1.52(3) . ? C203 O3 1.44(5) . ? C204 O4 1.401(10) . ? C205 O5 1.46(3) . ? C206 O6 1.20(4) . ? C207 O7 1.42(3) . ? C208 O8 1.44(3) . ? C210 O10 1.50(4) . ? C211 O11 1.38(3) . ? C212 O12 1.401(10) . ? C213 O13 1.51(3) . ? C214 O14 1.43(3) . ? C215 O15 1.42(4) . ? C216 O16 1.42(4) . ? C218 O18 1.45(4) . ? C219 O19 1.45(5) . ? C220 O20 1.50(3) . ? C221 O21 1.50(5) . ? C222 O22 1.46(4) . ? C223 O23 1.28(4) . ? C224 O24 1.41(4) . ? C804 O804 1.58(4) . ? C807 O807 1.32(7) . ? C808 O808 1.57(5) . ? C810 O809 1.32(5) . ? C812 O812 1.11(4) . ? O9 C209 1.400(10) . ? O17 C217 1.402(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Re1 C8 76.9(11) . . ? C6 Re1 C2 85.2(10) . . ? C8 Re1 C2 141.7(10) . . ? C6 Re1 C7 75.4(9) . . ? C8 Re1 C7 71.1(10) . . ? C2 Re1 C7 71.8(8) . . ? C6 Re1 C3 140.7(9) . . ? C8 Re1 C3 137.2(9) . . ? C2 Re1 C3 75.0(8) . . ? C7 Re1 C3 126.9(8) . . ? C6 Re1 C1 70.7(9) . . ? C8 Re1 C1 119.6(10) . . ? C2 Re1 C1 84.5(8) . . ? C7 Re1 C1 139.9(8) . . ? C3 Re1 C1 73.8(7) . . ? C6 Re1 C5 109.3(9) . . ? C8 Re1 C5 71.6(9) . . ? C2 Re1 C5 146.7(8) . . ? C7 Re1 C5 140.0(8) . . ? C3 Re1 C5 75.3(8) . . ? C1 Re1 C5 73.2(8) . . ? C6 Re1 C4 144.3(9) . . ? C8 Re1 C4 80.2(9) . . ? C2 Re1 C4 96.5(8) . . ? C7 Re1 C4 71.4(8) . . ? C3 Re1 C4 72.7(7) . . ? C1 Re1 C4 145.0(7) . . ? C5 Re1 C4 88.6(7) . . ? C14 Re2 C15 76.5(8) . . ? C14 Re2 C12 76.0(9) . . ? C15 Re2 C12 68.3(9) . . ? C14 Re2 C11 70.4(8) . . ? C15 Re2 C11 128.8(8) . . ? C12 Re2 C11 134.7(9) . . ? C14 Re2 C10 102.8(9) . . ? C15 Re2 C10 74.3(9) . . ? C12 Re2 C10 141.9(9) . . ? C11 Re2 C10 76.2(8) . . ? C14 Re2 C9 141.9(8) . . ? C15 Re2 C9 136.0(9) . . ? C12 Re2 C9 128.4(9) . . ? C11 Re2 C9 72.4(8) . . ? C10 Re2 C9 75.8(9) . . ? C14 Re2 C16 91.0(8) . . ? C15 Re2 C16 139.4(8) . . ? C12 Re2 C16 71.2(8) . . ? C11 Re2 C16 79.7(7) . . ? C10 Re2 C16 146.2(8) . . ? C9 Re2 C16 74.5(8) . . ? C14 Re2 C13 144.9(9) . . ? C15 Re2 C13 75.2(9) . . ? C12 Re2 C13 74.6(10) . . ? C11 Re2 C13 144.6(9) . . ? C10 Re2 C13 89.2(9) . . ? C9 Re2 C13 72.8(9) . . ? C16 Re2 C13 97.1(8) . . ? C24 Re3 C23 75.0(12) . . ? C24 Re3 C17 139.3(10) . . ? C23 Re3 C17 138.7(10) . . ? C24 Re3 C18 146.1(10) . . ? C23 Re3 C18 84.1(10) . . ? C17 Re3 C18 72.5(8) . . ? C24 Re3 C20 118.3(10) . . ? C23 Re3 C20 69.3(11) . . ? C17 Re3 C20 72.5(8) . . ? C18 Re3 C20 76.8(8) . . ? C24 Re3 C21 86.1(10) . . ? C23 Re3 C21 147.4(11) . . ? C17 Re3 C21 71.2(7) . . ? C18 Re3 C21 98.5(8) . . ? C20 Re3 C21 143.1(9) . . ? C24 Re3 C22 76.8(10) . . ? C23 Re3 C22 76.1(11) . . ? C17 Re3 C22 125.1(7) . . ? C18 Re3 C22 72.4(8) . . ? C20 Re3 C22 135.4(9) . . ? C21 Re3 C22 73.9(8) . . ? C24 Re3 C19 69.6(10) . . ? C23 Re3 C19 115.3(11) . . ? C17 Re3 C19 73.7(8) . . ? C18 Re3 C19 144.3(9) . . ? C20 Re3 C19 82.4(8) . . ? C21 Re3 C19 81.1(8) . . ? C22 Re3 C19 139.1(8) . . ? C31 Re4 C26 127.5(10) . . ? C31 Re4 C28 78.7(10) . . ? C26 Re4 C28 143.9(8) . . ? C31 Re4 C32 76.1(11) . . ? C26 Re4 C32 70.4(10) . . ? C28 Re4 C32 145.6(10) . . ? C31 Re4 C30 72.4(9) . . ? C26 Re4 C30 133.0(8) . . ? C28 Re4 C30 73.9(8) . . ? C32 Re4 C30 76.3(10) . . ? C31 Re4 C27 68.8(9) . . ? C26 Re4 C27 78.7(8) . . ? C28 Re4 C27 92.0(8) . . ? C32 Re4 C27 100.3(9) . . ? C30 Re4 C27 140.6(8) . . ? C31 Re4 C29 146.7(9) . . ? C26 Re4 C29 77.8(8) . . ? C28 Re4 C29 91.3(8) . . ? C32 Re4 C29 97.0(10) . . ? C30 Re4 C29 74.3(8) . . ? C27 Re4 C29 144.0(8) . . ? C31 Re4 C25 131.1(9) . . ? C26 Re4 C25 70.7(8) . . ? C28 Re4 C25 73.2(7) . . ? C32 Re4 C25 141.2(10) . . ? C30 Re4 C25 132.8(8) . . ? C27 Re4 C25 73.1(7) . . ? C29 Re4 C25 73.6(7) . . ? C33 Re5 C40 131.0(10) . . ? C33 Re5 C35 74.3(8) . . ? C40 Re5 C35 70.4(10) . . ? C33 Re5 C37 74.0(8) . . ? C40 Re5 C37 76.4(10) . . ? C35 Re5 C37 95.1(9) . . ? C33 Re5 C34 76.0(8) . . ? C40 Re5 C34 142.2(10) . . ? C35 Re5 C34 147.0(9) . . ? C37 Re5 C34 90.3(9) . . ? C33 Re5 C38 139.4(11) . . ? C40 Re5 C38 76.3(12) . . ? C35 Re5 C38 93.7(10) . . ? C37 Re5 C38 146.5(11) . . ? C34 Re5 C38 99.6(10) . . ? C33 Re5 C39 134.2(12) . . ? C40 Re5 C39 71.3(13) . . ? C35 Re5 C39 141.6(12) . . ? C37 Re5 C39 75.1(12) . . ? C34 Re5 C39 71.1(12) . . ? C38 Re5 C39 78.0(13) . . ? C33 Re5 C36 70.4(8) . . ? C40 Re5 C36 128.7(10) . . ? C35 Re5 C36 75.4(8) . . ? C37 Re5 C36 144.5(8) . . ? C34 Re5 C36 81.4(8) . . ? C38 Re5 C36 69.0(10) . . ? C39 Re5 C36 132.3(12) . . ? C48 Re6 C46 75.9(10) . . ? C48 Re6 C47 76.8(10) . . ? C46 Re6 C47 72.4(8) . . ? C48 Re6 C43 69.6(10) . . ? C46 Re6 C43 128.2(8) . . ? C47 Re6 C43 131.5(7) . . ? C48 Re6 C42 146.0(10) . . ? C46 Re6 C42 78.4(8) . . ? C47 Re6 C42 74.4(7) . . ? C43 Re6 C42 144.4(7) . . ? C48 Re6 C41 97.4(9) . . ? C46 Re6 C41 144.5(7) . . ? C47 Re6 C41 72.2(7) . . ? C43 Re6 C41 78.5(7) . . ? C42 Re6 C41 90.8(7) . . ? C48 Re6 C44 142.7(10) . . ? C46 Re6 C44 132.5(8) . . ? C47 Re6 C44 129.3(7) . . ? C43 Re6 C44 73.3(7) . . ? C42 Re6 C44 71.1(7) . . ? C41 Re6 C44 72.3(7) . . ? C48 Re6 C45 97.8(10) . . ? C46 Re6 C45 71.6(8) . . ? C47 Re6 C45 143.8(8) . . ? C43 Re6 C45 76.1(7) . . ? C42 Re6 C45 94.8(7) . . ? C41 Re6 C45 143.5(7) . . ? C44 Re6 C45 75.6(7) . . ? O3 Mn1 N28 92.7(6) . . ? O3 Mn1 O1 86.1(6) . . ? N28 Mn1 O1 178.8(6) . . ? O3 Mn1 N1 88.8(6) . . ? N28 Mn1 N1 88.5(7) . . ? O1 Mn1 N1 91.4(6) . . ? O3 Mn1 O2 86.2(5) . . ? N28 Mn1 O2 86.1(6) . . ? O1 Mn1 O2 93.9(6) . . ? N1 Mn1 O2 172.5(6) . . ? O3 Mn1 N20 168.8(7) . . ? N28 Mn1 N20 93.1(7) . . ? O1 Mn1 N20 88.1(7) . . ? N1 Mn1 N20 100.9(7) . . ? O2 Mn1 N20 84.6(6) . . ? N9 Mn2 N33 90.3(6) . . ? N9 Mn2 N3 90.6(6) . . ? N33 Mn2 N3 87.5(6) . . ? N9 Mn2 N17 174.9(5) . . ? N33 Mn2 N17 86.2(6) . . ? N3 Mn2 N17 92.9(6) . . ? N9 Mn2 N25 93.8(6) . . ? N33 Mn2 N25 173.9(6) . . ? N3 Mn2 N25 87.9(5) . . ? N17 Mn2 N25 90.1(6) . . ? N9 Mn2 N44 85.1(6) . . ? N33 Mn2 N44 93.6(5) . . ? N3 Mn2 N44 175.6(6) . . ? N17 Mn2 N44 91.5(6) . . ? N25 Mn2 N44 91.2(6) . . ? O6 Mn3 O4 86.0(7) . . ? O6 Mn3 O5 86.1(7) . . ? O4 Mn3 O5 87.2(6) . . ? O6 Mn3 N27 90.6(7) . . ? O4 Mn3 N27 174.8(6) . . ? O5 Mn3 N27 88.7(6) . . ? O6 Mn3 N2 92.4(7) . . ? O4 Mn3 N2 94.8(6) . . ? O5 Mn3 N2 177.5(6) . . ? N27 Mn3 N2 89.3(6) . . ? O6 Mn3 N11 170.6(7) . . ? O4 Mn3 N11 85.4(6) . . ? O5 Mn3 N11 89.7(6) . . ? N27 Mn3 N11 97.8(7) . . ? N2 Mn3 N11 92.1(7) . . ? O9 Mn4 N34 87.9(7) . . ? O9 Mn4 O8 86.1(6) . . ? N34 Mn4 O8 89.6(6) . . ? O9 Mn4 O7 86.5(6) . . ? N34 Mn4 O7 172.6(6) . . ? O8 Mn4 O7 85.2(6) . . ? O9 Mn4 N10 89.3(7) . . ? N34 Mn4 N10 96.7(7) . . ? O8 Mn4 N10 172.1(7) . . ? O7 Mn4 N10 88.1(7) . . ? O9 Mn4 N4 178.0(7) . . ? N34 Mn4 N4 93.2(7) . . ? O8 Mn4 N4 92.2(6) . . ? O7 Mn4 N4 92.3(6) . . ? N10 Mn4 N4 92.3(7) . . ? O14 Mn5 O13 91.3(6) . . ? O14 Mn5 O15 85.8(6) . . ? O13 Mn5 O15 85.5(6) . . ? O14 Mn5 N21 89.6(6) . . ? O13 Mn5 N21 89.7(7) . . ? O15 Mn5 N21 173.3(6) . . ? O14 Mn5 N35 86.6(6) . . ? O13 Mn5 N35 176.7(7) . . ? O15 Mn5 N35 91.8(6) . . ? N21 Mn5 N35 92.8(7) . . ? O14 Mn5 N43 176.1(6) . . ? O13 Mn5 N43 85.7(7) . . ? O15 Mn5 N43 91.4(6) . . ? N21 Mn5 N43 92.9(7) . . ? N35 Mn5 N43 96.3(7) . . ? O18 Mn6 N26 87.3(8) . . ? O18 Mn6 O17 86.6(7) . . ? N26 Mn6 O17 90.4(8) . . ? O18 Mn6 O16 89.4(7) . . ? N26 Mn6 O16 175.2(7) . . ? O17 Mn6 O16 85.9(7) . . ? O18 Mn6 N42 178.8(7) . . ? N26 Mn6 N42 92.0(8) . . ? O17 Mn6 N42 92.4(7) . . ? O16 Mn6 N42 91.2(7) . . ? O18 Mn6 N16 91.2(6) . . ? N26 Mn6 N16 96.6(7) . . ? O17 Mn6 N16 172.6(7) . . ? O16 Mn6 N16 87.0(6) . . ? N42 Mn6 N16 89.9(7) . . ? O12 Mn7 N19 90.8(7) . . ? O12 Mn7 O11 85.7(6) . . ? N19 Mn7 O11 176.4(7) . . ? O12 Mn7 N29 173.6(7) . . ? N19 Mn7 N29 92.8(7) . . ? O11 Mn7 N29 90.6(6) . . ? O12 Mn7 O10 81.8(7) . . ? N19 Mn7 O10 91.3(7) . . ? O11 Mn7 O10 87.4(6) . . ? N29 Mn7 O10 92.9(7) . . ? O12 Mn7 N41 89.1(7) . . ? N19 Mn7 N41 95.4(7) . . ? O11 Mn7 N41 85.4(6) . . ? N29 Mn7 N41 95.8(7) . . ? O10 Mn7 N41 168.8(6) . . ? N18 Mn8 O19 175.7(8) . . ? N18 Mn8 N37 92.3(8) . . ? O19 Mn8 N37 90.9(7) . . ? N18 Mn8 O20 88.5(8) . . ? O19 Mn8 O20 88.6(6) . . ? N37 Mn8 O20 89.6(7) . . ? N18 Mn8 N5 96.3(8) . . ? O19 Mn8 N5 86.3(7) . . ? N37 Mn8 N5 93.5(8) . . ? O20 Mn8 N5 174.1(7) . . ? N18 Mn8 O21 91.1(8) . . ? O19 Mn8 O21 85.7(7) . . ? N37 Mn8 O21 175.8(8) . . ? O20 Mn8 O21 87.9(7) . . ? N5 Mn8 O21 88.8(7) . . ? N13 Mn9 O22 178.5(8) . . ? N13 Mn9 O24 90.1(8) . . ? O22 Mn9 O24 89.9(8) . . ? N13 Mn9 O23 94.5(8) . . ? O22 Mn9 O23 84.0(8) . . ? O24 Mn9 O23 84.7(8) . . ? N13 Mn9 N45 93.4(7) . . ? O22 Mn9 N45 88.1(7) . . ? O24 Mn9 N45 86.8(7) . . ? O23 Mn9 N45 168.4(8) . . ? N13 Mn9 N36 88.8(7) . . ? O22 Mn9 N36 91.0(7) . . ? O24 Mn9 N36 175.5(7) . . ? O23 Mn9 N36 91.1(8) . . ? N45 Mn9 N36 97.6(7) . . ? N1 C1 Re1 178.8(19) . . ? N2 C2 Re1 171.6(19) . . ? N3 C3 Re1 175.9(16) . . ? N4 C4 Re1 175.5(17) . . ? N5 C5 Re1 171(2) . . ? N6 C6 Re1 169(3) . . ? N7 C7 Re1 176.4(19) . . ? N8 C8 Re1 173(2) . . ? N9 C9 Re2 177(2) . . ? N10 C10 Re2 174(2) . . ? N11 C11 Re2 169.9(18) . . ? N12 C12 Re2 176(2) . . ? N13 C13 Re2 177(2) . . ? N14 C14 Re2 179(2) . . ? N15 C15 Re2 179(2) . . ? N16 C16 Re2 174.4(19) . . ? N17 C17 Re3 178.6(16) . . ? N18 C18 Re3 177(2) . . ? N19 C19 Re3 176(2) . . ? N20 C20 Re3 176(2) . . ? N21 C21 Re3 176.0(19) . . ? N22 C22 Re3 175.1(19) . . ? N23 C23 Re3 174(4) . . ? N24 C24 Re3 174(3) . . ? N25 C25 Re4 178.4(18) . . ? N26 C26 Re4 172(2) . . ? N27 C27 Re4 174.5(17) . . ? N28 C28 Re4 176.1(18) . . ? N29 C29 Re4 177(2) . . ? N30 C30 Re4 173(2) . . ? N31 C31 Re4 171(2) . . ? N32 C32 Re4 174(3) . . ? N33 C33 Re5 178.1(18) . . ? N34 C34 Re5 173(2) . . ? N35 C35 Re5 173(2) . . ? N36 C36 Re5 178(2) . . ? N37 C37 Re5 177(2) . . ? N38 C38 Re5 176(3) . . ? N39 C39 Re5 171(3) . . ? N40 C40 Re5 179(3) . . ? N41 C41 Re6 178.2(17) . . ? N42 C42 Re6 175.0(19) . . ? N43 C43 Re6 178.7(17) . . ? N44 C44 Re6 173.7(18) . . ? N45 C45 Re6 176(2) . . ? N46 C46 Re6 175(2) . . ? N47 C47 Re6 177(2) . . ? N48 C48 Re6 179(3) . . ? C1 N1 Mn1 174.3(17) . . ? C2 N2 Mn3 172.9(17) . . ? C3 N3 Mn2 174.6(16) . . ? C4 N4 Mn4 172.1(17) . . ? C5 N5 Mn8 174.2(18) . . ? C9 N9 Mn2 178.8(17) . . ? C10 N10 Mn4 172(2) . . ? C11 N11 Mn3 177.6(18) . . ? C13 N13 Mn9 174.5(19) . . ? C16 N16 Mn6 169.8(17) . . ? C17 N17 Mn2 178.5(16) . . ? C18 N18 Mn8 170(2) . . ? C19 N19 Mn7 175.6(19) . . ? C20 N20 Mn1 168.1(19) . . ? C21 N21 Mn5 174.7(18) . . ? C25 N25 Mn2 176.0(17) . . ? C26 N26 Mn6 179(2) . . ? C27 N27 Mn3 170.9(17) . . ? C28 N28 Mn1 167.6(16) . . ? C29 N29 Mn7 173.9(18) . . ? C33 N33 Mn2 178.2(18) . . ? C34 N34 Mn4 172(2) . . ? C35 N35 Mn5 177.1(19) . . ? C36 N36 Mn9 176.8(19) . . ? C37 N37 Mn8 175(2) . . ? C41 N41 Mn7 167.8(16) . . ? C42 N42 Mn6 170(2) . . ? C43 N43 Mn5 177.1(17) . . ? C44 N44 Mn2 175.0(17) . . ? C45 N45 Mn9 167.5(19) . . ? C201 O1 Mn1 123.1(19) . . ? C202 O2 Mn1 122.5(14) . . ? C203 O3 Mn1 126(2) . . ? C204 O4 Mn3 124.9(17) . . ? C205 O5 Mn3 127.3(12) . . ? C206 O6 Mn3 145(2) . . ? C207 O7 Mn4 127.6(15) . . ? C208 O8 Mn4 130.4(15) . . ? C209 O9 Mn4 120(3) . . ? C210 O10 Mn7 124.2(17) . . ? C211 O11 Mn7 128.0(15) . . ? C212 O12 Mn7 137.0(18) . . ? C213 O13 Mn5 123.2(14) . . ? C214 O14 Mn5 126.3(13) . . ? C215 O15 Mn5 120.5(18) . . ? C216 O16 Mn6 127(2) . . ? C217 O17 Mn6 121(4) . . ? C218 O18 Mn6 118.0(19) . . ? C219 O19 Mn8 124(2) . . ? C220 O20 Mn8 124.6(15) . . ? C221 O21 Mn8 138(2) . . ? C222 O22 Mn9 128.7(19) . . ? C223 O23 Mn9 115(2) . . ? C224 O24 Mn9 129(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.772 _refine_diff_density_min -1.749 _refine_diff_density_rms 0.190 # Attachment '3b.cif' data_df40u _database_code_depnum_ccdc_archive 'CCDC 292904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common na _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H124 Co9 Mo4.74 N48 O35 Re1.26' _chemical_formula_weight 3476.98 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 28.963(3) _cell_length_b 18.8097(17) _cell_length_c 32.276(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.586(2) _cell_angle_gamma 90.00 _cell_volume 15990(2) _cell_formula_units_Z 4 _cell_measurement_temperature 147 _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.548 _cell_measurement_theta_max 50.143 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6410 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.827368 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 147 _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 'Bruker SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45344 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.42 _reflns_number_total 24489 _reflns_number_gt 16209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 24489 _refine_ls_number_parameters 777 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2673 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.004 _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 Re1 Re 0.07831(7) 0.15659(8) 0.46718(7) 0.0413(5) Uani 0.21 1 d P . . Re2 Re 0.43260(7) 0.15194(8) 0.44085(6) 0.0344(4) Uani 0.21 1 d P . . Re3 Re 0.19668(7) -0.06608(9) 0.33090(6) 0.0362(4) Uani 0.21 1 d P . . Re4 Re 0.17383(7) 0.33187(8) 0.32078(7) 0.0404(4) Uani 0.21 1 d P . . Re5 Re 0.31531(7) -0.05901(8) 0.58279(6) 0.0360(4) Uani 0.21 1 d P . . Re6 Re 0.33581(7) 0.33857(8) 0.58440(7) 0.0428(5) Uani 0.21 1 d P . . Mo1 Mo 0.07831(7) 0.15659(8) 0.46718(7) 0.0413(5) Uani 0.79 1 d P . . Mo2 Mo 0.43260(7) 0.15194(8) 0.44085(6) 0.0344(4) Uani 0.79 1 d PD . . Mo3 Mo 0.19668(7) -0.06608(9) 0.33090(6) 0.0362(4) Uani 0.79 1 d P . . Mo4 Mo 0.17383(7) 0.33187(8) 0.32078(7) 0.0404(4) Uani 0.79 1 d P . . Mo5 Mo 0.31531(7) -0.05901(8) 0.58279(6) 0.0360(4) Uani 0.79 1 d P . . Mo6 Mo 0.33581(7) 0.33857(8) 0.58440(7) 0.0428(5) Uani 0.79 1 d PD . . Co7 Co 0.25573(13) 0.14193(8) 0.45494(12) 0.0198(3) Uani 1 1 d . . . Co8 Co 0.38548(12) -0.12014(16) 0.45565(11) 0.0332(7) Uani 1 1 d . . . Co9 Co 0.04114(13) 0.11679(17) 0.29199(12) 0.0438(9) Uani 1 1 d . . . Co10 Co 0.12661(12) -0.11769(15) 0.45882(10) 0.0308(7) Uani 1 1 d . . . Co11 Co 0.46929(12) 0.12373(18) 0.61714(11) 0.0412(8) Uani 1 1 d . . . Co12 Co 0.36071(12) 0.41661(15) 0.43403(11) 0.0361(7) Uani 1 1 d . . . Co13 Co 0.14867(13) 0.41999(18) 0.46799(15) 0.0633(12) Uani 1 1 d . . . Co14 Co 0.28171(14) 0.14419(19) 0.27262(12) 0.0478(9) Uani 1 1 d . . . Co15 Co 0.22719(15) 0.15497(18) 0.63545(12) 0.0502(10) Uani 1 1 d . . . C1 C 0.1481(7) 0.1517(11) 0.4615(8) 0.038(6) Uiso 1 1 d D . . C2 C 0.0992(8) 0.0491(8) 0.4695(7) 0.032(5) Uiso 1 1 d D . . C3 C 0.1049(7) 0.2654(9) 0.4646(6) 0.038(5) Uiso 1 1 d D . . C4 C 0.1366(8) 0.1398(11) 0.5375(6) 0.040(6) Uiso 1 1 d D . . C5 C 0.0587(8) 0.1339(11) 0.3951(6) 0.038(5) Uiso 1 1 d D . . C6 C 0.0501(10) 0.2125(13) 0.5107(9) 0.068(7) Uiso 1 1 d D . . C7 C 0.0167(6) 0.0956(9) 0.4630(7) 0.033(4) Uiso 1 1 d D . . C8 C 0.0109(7) 0.2200(10) 0.4249(7) 0.042(5) Uiso 1 1 d D . . C9 C 0.3625(6) 0.1495(9) 0.4477(6) 0.020(4) Uiso 1 1 d D . . C10 C 0.4132(8) 0.0416(9) 0.4431(7) 0.038(5) Uiso 1 1 d D . . C11 C 0.4034(6) 0.2554(7) 0.4327(5) 0.020(3) Uiso 1 1 d D . . C12 C 0.3756(8) 0.1487(11) 0.3748(7) 0.042(6) Uiso 1 1 d D . . C13 C 0.4519(7) 0.1395(9) 0.5088(5) 0.023(4) Uiso 1 1 d D . . C14 C 0.4566(8) 0.1874(11) 0.3889(7) 0.048(5) Uiso 1 1 d D . . C15 C 0.4966(6) 0.0844(11) 0.4541(9) 0.061(7) Uiso 1 1 d D . . C16 C 0.4952(6) 0.2176(9) 0.4746(6) 0.034(4) Uiso 1 1 d D . . C17 C 0.2190(7) 0.0158(9) 0.3812(6) 0.030(5) Uiso 1 1 d D . . C18 C 0.2242(8) 0.0151(10) 0.3019(7) 0.045(6) Uiso 1 1 d D . . C19 C 0.1647(6) -0.0909(9) 0.3801(5) 0.022(4) Uiso 1 1 d D . . C20 C 0.1373(6) 0.0059(9) 0.3130(6) 0.026(4) Uiso 1 1 d D . . C21 C 0.2696(7) -0.0961(11) 0.3807(7) 0.036(5) Uiso 1 1 d D . . C22 C 0.2316(8) -0.1175(10) 0.2929(7) 0.035(5) Uiso 1 1 d D . . C23 C 0.1355(11) -0.0980(15) 0.2723(10) 0.085(8) Uiso 1 1 d D . . C24 C 0.1921(10) -0.1808(12) 0.3372(9) 0.072(7) Uiso 1 1 d D . . C25 C 0.2056(6) 0.2546(8) 0.3738(5) 0.020(4) Uiso 1 1 d D . . C26 C 0.1653(8) 0.3738(11) 0.3781(6) 0.037(5) Uiso 1 1 d D . . C27 C 0.1192(8) 0.2513(10) 0.3090(7) 0.041(6) Uiso 1 1 d D . . C28 C 0.2475(6) 0.3666(10) 0.3626(7) 0.038(5) Uiso 1 1 d D . . C29 C 0.2212(6) 0.2644(8) 0.3006(6) 0.021(4) Uiso 1 1 d D . . C30 C 0.1392(10) 0.3192(15) 0.2494(7) 0.067(8) Uiso 1 1 d D . . C31 C 0.1918(11) 0.4299(15) 0.3009(10) 0.077(8) Uiso 1 1 d D . . C32 C 0.0999(8) 0.3812(13) 0.2911(9) 0.069(7) Uiso 1 1 d D . . C33 C 0.2914(6) 0.0210(8) 0.5333(5) 0.016(4) Uiso 1 1 d D . . C34 C 0.2839(7) 0.0271(9) 0.6090(6) 0.025(4) Uiso 1 1 d D . . C35 C 0.3820(8) 0.0113(11) 0.5999(8) 0.049(6) Uiso 1 1 d D . . C36 C 0.3453(7) -0.0866(10) 0.5359(6) 0.031(5) Uiso 1 1 d D . . C37 C 0.2429(6) -0.0897(10) 0.5327(6) 0.026(4) Uiso 1 1 d D . . C38 C 0.2736(9) -0.1048(11) 0.6174(8) 0.050(6) Uiso 1 1 d D . . C39 C 0.3581(8) -0.0606(12) 0.6538(7) 0.058(6) Uiso 1 1 d D . . C40 C 0.3325(12) -0.1625(15) 0.5867(11) 0.087(9) Uiso 1 1 d D . . C41 C 0.3007(7) 0.2623(9) 0.5323(6) 0.034(5) Uiso 1 1 d D . . C42 C 0.3470(7) 0.3792(10) 0.5252(5) 0.028(4) Uiso 1 1 d D . . C43 C 0.3883(8) 0.2519(10) 0.5971(7) 0.037(5) Uiso 1 1 d D . . C44 C 0.2607(6) 0.3748(11) 0.5384(6) 0.038(5) Uiso 1 1 d D . . C45 C 0.2944(8) 0.2679(13) 0.6074(8) 0.056(7) Uiso 1 1 d D . . C46 C 0.3729(8) 0.3342(11) 0.6580(6) 0.041(5) Uiso 1 1 d D . . C47 C 0.3249(12) 0.4453(9) 0.6032(11) 0.104(12) Uiso 1 1 d D . . C48 C 0.4055(7) 0.3949(10) 0.6065(7) 0.037(5) Uiso 1 1 d D . . C201 C 0.5054(14) -0.110(3) 0.4994(19) 0.19(2) Uiso 1 1 d D . . C202 C 0.3936(9) -0.1090(12) 0.3592(8) 0.051(6) Uiso 1 1 d . . . C203 C 0.372(3) -0.284(4) 0.423(2) 0.28(3) Uiso 1 1 d . . . C204 C 0.061(2) 0.082(3) 0.1956(17) 0.180(19) Uiso 1 1 d . . . C205 C -0.0268(9) 0.2415(13) 0.3018(8) 0.057(6) Uiso 1 1 d . . . C206 C -0.067(2) 0.030(3) 0.2810(18) 0.20(2) Uiso 1 1 d . . . C207 C 0.0065(8) -0.1063(12) 0.4157(7) 0.047(5) Uiso 1 1 d . . . C208 C 0.1262(11) -0.1237(15) 0.5558(10) 0.070(8) Uiso 1 1 d . . . C209 C 0.1096(15) -0.282(2) 0.4448(14) 0.138(14) Uiso 1 1 d . . . C210 C 0.5060(16) -0.0171(17) 0.6033(12) 0.149(15) Uiso 1 1 d D . . C211 C 0.4418(11) 0.1327(15) 0.6978(10) 0.090(9) Uiso 1 1 d . . . C212 C 0.5262(12) 0.2539(16) 0.6049(10) 0.087(9) Uiso 1 1 d . . . C213 C 0.2867(15) 0.548(2) 0.4118(13) 0.105(12) Uiso 1 1 d . . . C214 C 0.3644(9) 0.3992(13) 0.3390(8) 0.059(6) Uiso 1 1 d . . . C215 C 0.4714(11) 0.4132(15) 0.5124(9) 0.070(8) Uiso 1 1 d . . . C216 C 0.2185(12) 0.5548(16) 0.5014(10) 0.079(9) Uiso 1 1 d . . . C217 C 0.1461(19) 0.420(2) 0.5646(10) 0.159(19) Uiso 1 1 d D . . C218 C 0.0425(11) 0.4185(15) 0.3879(10) 0.073(8) Uiso 1 1 d . . . C219 C 0.1814(10) 0.1912(14) 0.1916(9) 0.068(7) Uiso 1 1 d . . . C220 C 0.3365(10) 0.0044(14) 0.2646(9) 0.076(7) Uiso 1 1 d . . . C221 C 0.3685(10) 0.2348(15) 0.2612(9) 0.075(7) Uiso 1 1 d . . . C222 C 0.3404(13) 0.1651(17) 0.7190(11) 0.096(10) Uiso 1 1 d . . . C223 C 0.1999(9) 0.0208(13) 0.6729(8) 0.063(6) Uiso 1 1 d . . . C224 C 0.1439(17) 0.222(4) 0.654(3) 0.30(4) Uiso 1 1 d D . . O803 O 0.4855(15) -0.196(2) 0.5908(13) 0.216(16) Uiso 1 1 d . . . C810 C 0.1403(14) 0.5761(19) 0.3486(14) 0.114(12) Uiso 1 1 d . . . C813 C 0.2396(18) 0.392(3) 0.2167(16) 0.157(16) Uiso 1 1 d . . . C814 C 0.2972(11) -0.2783(15) 0.4827(10) 0.086(8) Uiso 1 1 d . . . O805 O 0.3846(12) 0.5777(15) 0.5284(10) 0.155(10) Uiso 1 1 d . . . N1 N 0.1858(6) 0.1476(8) 0.4570(6) 0.029(4) Uiso 1 1 d D . . N2 N 0.1102(7) -0.0092(8) 0.4655(6) 0.036(4) Uiso 1 1 d D . . N3 N 0.1206(7) 0.3229(9) 0.4675(7) 0.053(5) Uiso 1 1 d D . . N4 N 0.1683(7) 0.1457(10) 0.5743(6) 0.049(5) Uiso 1 1 d D . . N5 N 0.0509(6) 0.1249(8) 0.3571(5) 0.033(4) Uiso 1 1 d D . . N6 N 0.0345(11) 0.2572(15) 0.5266(10) 0.132(11) Uiso 1 1 d D . . N7 N -0.0159(7) 0.0609(10) 0.4645(7) 0.061(5) Uiso 1 1 d D . . N8 N -0.0223(7) 0.2560(10) 0.4000(6) 0.061(5) Uiso 1 1 d D . . N9 N 0.3238(5) 0.1429(7) 0.4499(5) 0.021(3) Uiso 1 1 d D . . N10 N 0.4009(7) -0.0165(8) 0.4446(6) 0.040(5) Uiso 1 1 d D . . N11 N 0.3891(6) 0.3137(7) 0.4325(5) 0.034(4) Uiso 1 1 d D . . N12 N 0.3434(7) 0.1395(10) 0.3389(6) 0.049(5) Uiso 1 1 d D . . N13 N 0.4594(7) 0.1249(9) 0.5461(5) 0.042(5) Uiso 1 1 d D . . N14 N 0.4698(7) 0.2134(10) 0.3627(6) 0.063(5) Uiso 1 1 d D . . N15 N 0.5340(7) 0.0537(14) 0.4587(10) 0.120(11) Uiso 1 1 d D . . N16 N 0.5304(5) 0.2541(8) 0.4944(5) 0.037(4) Uiso 1 1 d D . . N17 N 0.2320(6) 0.0617(7) 0.4074(5) 0.026(4) Uiso 1 1 d D . . N18 N 0.2427(6) 0.0616(8) 0.2902(5) 0.029(4) Uiso 1 1 d D . . N19 N 0.1483(6) -0.1022(8) 0.4069(5) 0.033(4) Uiso 1 1 d D . . N20 N 0.1028(6) 0.0431(9) 0.3049(6) 0.042(5) Uiso 1 1 d D . . N21 N 0.3109(7) -0.1106(10) 0.4059(6) 0.045(5) Uiso 1 1 d D . . N22 N 0.2568(10) -0.1374(14) 0.2747(9) 0.091(9) Uiso 1 1 d D . . N23 N 0.1064(15) -0.094(2) 0.2341(11) 0.198(17) Uiso 1 1 d D . . N24 N 0.1915(9) -0.2417(11) 0.3443(8) 0.087(7) Uiso 1 1 d D . . N25 N 0.2278(6) 0.2162(8) 0.4033(5) 0.035(4) Uiso 1 1 d D . . N26 N 0.1613(7) 0.3943(10) 0.4105(6) 0.047(5) Uiso 1 1 d D . . N27 N 0.0897(7) 0.2064(9) 0.3053(6) 0.042(5) Uiso 1 1 d D . . N28 N 0.2882(5) 0.3874(8) 0.3868(5) 0.030(4) Uiso 1 1 d D . . N29 N 0.2426(6) 0.2200(8) 0.2908(6) 0.045(5) Uiso 1 1 d D . . N30 N 0.1188(8) 0.3137(12) 0.2096(7) 0.072(6) Uiso 1 1 d D . . N31 N 0.2110(18) 0.467(2) 0.2831(16) 0.23(2) Uiso 1 1 d D . . N32 N 0.0602(8) 0.4090(11) 0.2777(7) 0.072(6) Uiso 1 1 d D . . N33 N 0.2801(6) 0.0659(7) 0.5065(5) 0.028(4) Uiso 1 1 d D . . N34 N 0.2640(8) 0.0751(10) 0.6178(7) 0.061(6) Uiso 1 1 d D . . N35 N 0.4138(6) 0.0518(8) 0.6045(5) 0.035(4) Uiso 1 1 d D . . N36 N 0.3604(6) -0.0993(8) 0.5087(5) 0.031(4) Uiso 1 1 d D . . N37 N 0.2023(5) -0.1029(8) 0.5056(5) 0.027(4) Uiso 1 1 d D . . N38 N 0.2577(8) -0.1407(10) 0.6381(7) 0.056(6) Uiso 1 1 d D . . N39 N 0.3803(9) -0.0677(12) 0.6933(7) 0.085(7) Uiso 1 1 d D . . N40 N 0.3472(13) -0.2207(16) 0.5942(11) 0.147(12) Uiso 1 1 d D . . N41 N 0.2847(5) 0.2185(7) 0.5047(4) 0.018(3) Uiso 1 1 d D . . N42 N 0.3475(7) 0.3947(9) 0.4904(5) 0.045(5) Uiso 1 1 d D . . N43 N 0.4190(7) 0.2065(10) 0.6090(7) 0.055(6) Uiso 1 1 d D . . N44 N 0.2209(6) 0.3881(9) 0.5103(6) 0.049(5) Uiso 1 1 d D . . N45 N 0.2663(6) 0.2357(8) 0.6177(5) 0.033(4) Uiso 1 1 d D . . N46 N 0.3958(8) 0.3337(11) 0.6971(6) 0.071(6) Uiso 1 1 d D . . N47 N 0.3140(8) 0.4981(7) 0.6162(7) 0.082(6) Uiso 1 1 d D . . N48 N 0.4414(10) 0.4319(14) 0.6177(10) 0.123(10) Uiso 1 1 d D . . O1 O 0.4621(6) -0.1286(8) 0.5062(5) 0.046(4) Uiso 1 1 d D . . O2 O 0.4081(6) -0.1468(7) 0.4025(5) 0.041(4) Uiso 1 1 d . . . O3 O 0.3777(6) -0.2271(8) 0.4624(5) 0.049(4) Uiso 1 1 d . . . O4 O 0.0270(7) 0.1071(9) 0.2209(6) 0.062(5) Uiso 1 1 d . . . O5 O -0.0217(7) 0.1818(10) 0.2713(6) 0.073(5) Uiso 1 1 d . . . O6 O -0.0086(7) 0.0307(9) 0.2802(6) 0.060(5) Uiso 1 1 d . . . O7 O 0.0522(6) -0.1339(8) 0.4126(5) 0.049(4) Uiso 1 1 d . . . O8 O 0.1022(8) -0.1440(9) 0.5090(7) 0.065(6) Uiso 1 1 d . . . O9 O 0.1384(7) -0.2252(10) 0.4534(6) 0.067(5) Uiso 1 1 d . . . O10 O 0.5229(8) 0.0399(10) 0.6346(6) 0.071(6) Uiso 1 1 d D . . O11 O 0.4870(6) 0.1242(8) 0.6861(5) 0.051(4) Uiso 1 1 d . . . O12 O 0.5298(6) 0.1950(8) 0.6329(5) 0.051(4) Uiso 1 1 d . . . O13 O 0.3385(6) 0.5205(8) 0.4320(5) 0.050(4) Uiso 1 1 d . . . O14 O 0.3749(5) 0.4415(7) 0.3761(5) 0.047(4) Uiso 1 1 d . . . O15 O 0.4331(7) 0.4507(9) 0.4744(6) 0.067(5) Uiso 1 1 d . . . O16 O 0.1712(6) 0.5250(8) 0.4653(5) 0.057(4) Uiso 1 1 d . . . O17 O 0.1317(7) 0.4548(10) 0.5223(6) 0.077(5) Uiso 1 1 d D . . O18 O 0.0784(7) 0.4545(9) 0.4252(6) 0.065(5) Uiso 1 1 d . . . O19 O 0.2225(7) 0.1466(8) 0.2047(6) 0.059(5) Uiso 1 1 d . . . O20 O 0.3198(7) 0.0716(10) 0.2466(6) 0.066(5) Uiso 1 1 d . . . O21 O 0.3159(6) 0.2175(9) 0.2480(5) 0.065(4) Uiso 1 1 d . . . O22 O 0.2805(6) 0.1564(8) 0.7019(6) 0.054(4) Uiso 1 1 d . . . O23 O 0.1875(7) 0.0836(10) 0.6584(6) 0.073(5) Uiso 1 1 d . . . O24 O 0.1887(6) 0.2424(8) 0.6499(5) 0.058(4) Uiso 1 1 d D . . O800 O 0.3588(6) 0.5711(8) 0.3365(5) 0.067(4) Uiso 1 1 d . . . O801 O 0.1231(19) 0.619(3) 0.5745(17) 0.125(16) Uiso 0.50 1 d P . . O810 O 0.1573(14) 0.590(2) 0.3825(13) 0.194(15) Uiso 1 1 d . . . O811 O 0.2521(8) 0.6014(12) 0.2827(7) 0.111(7) Uiso 1 1 d . . . O813 O 0.2665(13) 0.3313(17) 0.1942(12) 0.181(13) Uiso 1 1 d . . . O814 O 0.2581(15) -0.2558(15) 0.4432(12) 0.184(12) Uiso 1 1 d . . . O815 O 0.0514(19) 0.069(3) 0.6033(17) 0.137(17) Uiso 0.50 1 d P . . O817 O 0.5363(16) -0.062(2) 0.7033(14) 0.109(13) Uiso 0.50 1 d P . . O900 O 0.2762(9) 0.6568(11) 0.6087(8) 0.114(7) Uiso 1 1 d . . . O804 O 0.2427(12) 0.3588(15) 0.6954(11) 0.156(11) Uiso 1 1 d . . . O806 O 0.0215(7) -0.2038(10) 0.3323(7) 0.021(4) Uiso 0.50 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 Re1 0.0284(9) 0.0385(9) 0.0666(12) -0.0245(8) 0.0293(8) -0.0156(7) Re2 0.0263(9) 0.0350(8) 0.0498(10) -0.0020(7) 0.0234(7) -0.0003(6) Re3 0.0339(9) 0.0499(9) 0.0233(8) -0.0151(7) 0.0104(7) -0.0074(7) Re4 0.0315(9) 0.0239(7) 0.0557(11) 0.0097(7) 0.0081(7) -0.0001(6) Re5 0.0375(10) 0.0427(9) 0.0249(8) -0.0037(6) 0.0099(7) -0.0155(7) Re6 0.0416(11) 0.0365(9) 0.0542(11) -0.0212(8) 0.0239(8) -0.0180(7) Mo1 0.0284(9) 0.0385(9) 0.0666(12) -0.0245(8) 0.0293(8) -0.0156(7) Mo2 0.0263(9) 0.0350(8) 0.0498(10) -0.0020(7) 0.0234(7) -0.0003(6) Mo3 0.0339(9) 0.0499(9) 0.0233(8) -0.0151(7) 0.0104(7) -0.0074(7) Mo4 0.0315(9) 0.0239(7) 0.0557(11) 0.0097(7) 0.0081(7) -0.0001(6) Mo5 0.0375(10) 0.0427(9) 0.0249(8) -0.0037(6) 0.0099(7) -0.0155(7) Mo6 0.0416(11) 0.0365(9) 0.0542(11) -0.0212(8) 0.0239(8) -0.0180(7) Co7 0.0176(7) 0.0207(8) 0.0236(9) -0.0067(13) 0.0111(7) -0.0090(15) Co8 0.0316(17) 0.0325(15) 0.0372(18) -0.0066(12) 0.0160(14) 0.0032(12) Co9 0.0300(18) 0.0374(17) 0.046(2) 0.0140(14) -0.0021(15) -0.0084(13) Co10 0.0305(17) 0.0298(15) 0.0337(17) -0.0141(12) 0.0151(13) -0.0203(12) Co11 0.0245(17) 0.0529(19) 0.0355(19) -0.0124(14) 0.0018(14) -0.0132(13) Co12 0.0288(16) 0.0263(14) 0.0559(19) -0.0025(13) 0.0204(14) -0.0065(12) Co13 0.0295(18) 0.0353(18) 0.132(3) -0.0409(19) 0.040(2) -0.0052(14) Co14 0.050(2) 0.071(2) 0.0308(18) 0.0068(15) 0.0247(16) 0.0059(17) Co15 0.066(2) 0.059(2) 0.047(2) -0.0298(16) 0.0449(18) -0.0292(17) _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 Re1 C7 2.079(15) . ? Re1 C2 2.103(15) . ? Re1 C1 2.108(19) . ? Re1 C6 2.17(2) . ? Re1 C5 2.194(16) . ? Re1 C3 2.200(16) . ? Re1 C8 2.208(17) . ? Re1 C4 2.217(18) . ? Re2 C13 2.039(15) . ? Re2 C12 2.083(18) . ? Re2 C16 2.087(14) . ? Re2 C11 2.094(12) . ? Re2 C9 2.132(15) . ? Re2 C15 2.138(8) . ? Re2 C10 2.159(16) . ? Re2 C14 2.171(17) . ? Re3 C23 2.07(3) . ? Re3 C20 2.074(15) . ? Re3 C18 2.114(15) . ? Re3 C22 2.12(2) . ? Re3 C21 2.130(17) . ? Re3 C17 2.133(15) . ? Re3 C24 2.18(2) . ? Re3 C19 2.198(14) . ? Re4 C31 2.09(3) . ? Re4 C28 2.099(15) . ? Re4 C27 2.108(17) . ? Re4 C30 2.11(2) . ? Re4 C26 2.119(16) . ? Re4 C25 2.139(14) . ? Re4 C32 2.16(2) . ? Re4 C29 2.160(14) . ? Re5 C40 2.00(3) . ? Re5 C33 2.092(13) . ? Re5 C36 2.100(15) . ? Re5 C39 2.10(2) . ? Re5 C37 2.127(14) . ? Re5 C38 2.139(19) . ? Re5 C34 2.193(15) . ? Re5 C35 2.212(17) . ? Re6 C45 2.121(17) . ? Re6 C41 2.121(14) . ? Re6 C48 2.123(19) . ? Re6 C43 2.150(17) . ? Re6 C47 2.158(8) . ? Re6 C46 2.164(19) . ? Re6 C44 2.172(16) . ? Re6 C42 2.203(16) . ? Co7 N9 2.045(15) . ? Co7 N17 2.057(14) . ? Co7 N1 2.058(18) . ? Co7 N41 2.059(13) . ? Co7 N25 2.065(14) . ? Co7 N33 2.082(13) . ? Co8 O3 2.046(16) . ? Co8 N10 2.063(16) . ? Co8 N21 2.096(17) . ? Co8 O2 2.135(16) . ? Co8 O1 2.144(16) . ? Co8 N36 2.158(14) . ? Co9 N5 2.006(16) . ? Co9 O5 2.059(19) . ? Co9 O6 2.095(17) . ? Co9 N27 2.121(16) . ? Co9 N20 2.159(15) . ? Co9 O4 2.165(17) . ? Co10 N19 2.041(14) . ? Co10 O7 2.070(16) . ? Co10 O9 2.071(19) . ? Co10 O8 2.08(2) . ? Co10 N37 2.100(14) . ? Co10 N2 2.126(15) . ? Co11 N35 2.008(16) . ? Co11 O11 2.066(16) . ? Co11 N43 2.073(18) . ? Co11 O12 2.094(16) . ? Co11 O10 2.118(19) . ? Co11 N13 2.189(16) . ? Co12 O13 2.050(15) . ? Co12 N42 2.050(16) . ? Co12 O15 2.057(18) . ? Co12 N28 2.091(14) . ? Co12 N11 2.112(13) . ? Co12 O14 2.126(15) . ? Co13 N3 1.995(16) . ? Co13 O18 2.032(18) . ? Co13 N44 2.056(16) . ? Co13 N26 2.091(16) . ? Co13 O16 2.093(16) . ? Co13 O17 2.11(2) . ? Co14 O21 2.042(16) . ? Co14 N29 2.052(15) . ? Co14 N18 2.131(14) . ? Co14 O20 2.134(19) . ? Co14 N12 2.144(18) . ? Co14 O19 2.149(17) . ? Co15 N4 2.009(18) . ? Co15 N34 2.055(16) . ? Co15 O22 2.056(17) . ? Co15 O23 2.09(2) . ? Co15 N45 2.111(15) . ? Co15 O24 2.145(16) . ? C1 N1 1.160(9) . ? C2 N2 1.165(9) . ? C3 N3 1.163(9) . ? C4 N4 1.165(9) . ? C5 N5 1.164(9) . ? C6 N6 1.172(10) . ? C7 N7 1.165(9) . ? C8 N8 1.177(9) . ? C9 N9 1.159(9) . ? C10 N10 1.158(9) . ? C11 N11 1.171(9) . ? C12 N12 1.160(9) . ? C13 N13 1.164(9) . ? C14 N14 1.167(9) . ? C15 N15 1.182(8) . ? C16 N16 1.174(9) . ? C17 N17 1.156(9) . ? C18 N18 1.168(9) . ? C19 N19 1.165(9) . ? C20 N20 1.157(9) . ? C21 N21 1.164(9) . ? C22 N22 1.173(10) . ? C23 N23 1.169(10) . ? C24 N24 1.171(10) . ? C25 N25 1.155(9) . ? C26 N26 1.164(9) . ? C27 N27 1.172(9) . ? C28 N28 1.177(9) . ? C29 N29 1.159(9) . ? C30 N30 1.173(10) . ? C31 N31 1.177(10) . ? C32 N32 1.172(10) . ? C33 N33 1.154(9) . ? C34 N34 1.167(9) . ? C35 N35 1.157(9) . ? C36 N36 1.155(9) . ? C37 N37 1.163(9) . ? C38 N38 1.171(9) . ? C39 N39 1.173(10) . ? C40 N40 1.162(10) . ? C41 N41 1.158(9) . ? C42 N42 1.168(9) . ? C43 N43 1.175(9) . ? C44 N44 1.158(9) . ? C45 N45 1.168(9) . ? C46 N46 1.156(9) . ? C47 N47 1.1701(10) . ? C48 N48 1.177(10) . ? C201 O1 1.405(10) . ? C202 O2 1.46(3) . ? C203 O3 1.62(7) . ? C204 O4 1.58(5) . ? C205 O5 1.54(3) . ? C206 O6 1.71(6) . ? C207 O7 1.46(2) . ? C208 O8 1.43(3) . ? C209 O9 1.31(4) . ? C210 O10 1.414(10) . ? C211 O11 1.52(3) . ? C212 O12 1.41(3) . ? C213 O13 1.46(4) . ? C214 O14 1.36(3) . ? C215 O15 1.45(3) . ? C216 O16 1.49(3) . ? C217 O17 1.408(10) . ? C218 O18 1.40(3) . ? C219 O19 1.37(3) . ? C220 O20 1.39(3) . ? C221 O21 1.44(3) . ? C222 O22 1.60(4) . ? C223 O23 1.27(3) . ? C224 O24 1.402(10) . ? C810 O810 1.03(4) . ? C813 O813 1.71(5) . ? C814 O814 1.37(4) . ? 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 C7 Re1 C2 72.5(8) . . ? C7 Re1 C1 143.1(8) . . ? C2 Re1 C1 71.8(8) . . ? C7 Re1 C6 76.4(9) . . ? C2 Re1 C6 128.6(9) . . ? C1 Re1 C6 135.4(9) . . ? C7 Re1 C5 89.3(8) . . ? C2 Re1 C5 78.2(8) . . ? C1 Re1 C5 74.5(8) . . ? C6 Re1 C5 141.2(9) . . ? C7 Re1 C3 144.6(7) . . ? C2 Re1 C3 142.7(8) . . ? C1 Re1 C3 71.0(8) . . ? C6 Re1 C3 78.8(9) . . ? C5 Re1 C3 94.6(7) . . ? C7 Re1 C8 75.2(8) . . ? C2 Re1 C8 135.1(8) . . ? C1 Re1 C8 127.1(8) . . ? C6 Re1 C8 70.4(9) . . ? C5 Re1 C8 71.2(8) . . ? C3 Re1 C8 73.0(7) . . ? C7 Re1 C4 104.8(8) . . ? C2 Re1 C4 75.0(8) . . ? C1 Re1 C4 74.6(9) . . ? C6 Re1 C4 74.7(9) . . ? C5 Re1 C4 144.0(8) . . ? C3 Re1 C4 92.4(7) . . ? C8 Re1 C4 144.1(8) . . ? C13 Re2 C12 147.5(8) . . ? C13 Re2 C16 73.5(7) . . ? C12 Re2 C16 134.2(8) . . ? C13 Re2 C11 99.1(6) . . ? C12 Re2 C11 78.0(7) . . ? C16 Re2 C11 74.5(7) . . ? C13 Re2 C9 74.5(7) . . ? C12 Re2 C9 73.9(8) . . ? C16 Re2 C9 128.1(7) . . ? C11 Re2 C9 71.4(6) . . ? C13 Re2 C15 83.6(8) . . ? C12 Re2 C15 116.1(9) . . ? C16 Re2 C15 75.8(9) . . ? C11 Re2 C15 148.0(8) . . ? C9 Re2 C15 138.5(8) . . ? C13 Re2 C10 79.2(7) . . ? C12 Re2 C10 84.2(8) . . ? C16 Re2 C10 137.2(8) . . ? C11 Re2 C10 143.1(8) . . ? C9 Re2 C10 72.7(8) . . ? C15 Re2 C10 68.8(9) . . ? C13 Re2 C14 146.5(8) . . ? C12 Re2 C14 65.8(9) . . ? C16 Re2 C14 74.5(8) . . ? C11 Re2 C14 81.9(7) . . ? C9 Re2 C14 135.4(7) . . ? C15 Re2 C14 78.9(9) . . ? C10 Re2 C14 119.5(8) . . ? C23 Re3 C20 68.9(9) . . ? C23 Re3 C18 98.2(10) . . ? C20 Re3 C18 80.0(8) . . ? C23 Re3 C22 76.8(10) . . ? C20 Re3 C22 132.6(7) . . ? C18 Re3 C22 73.4(8) . . ? C23 Re3 C21 144.6(10) . . ? C20 Re3 C21 146.2(8) . . ? C18 Re3 C21 95.0(8) . . ? C22 Re3 C21 75.7(8) . . ? C23 Re3 C17 141.0(10) . . ? C20 Re3 C17 72.2(7) . . ? C18 Re3 C17 76.4(8) . . ? C22 Re3 C17 134.7(8) . . ? C21 Re3 C17 74.1(8) . . ? C23 Re3 C24 74.7(10) . . ? C20 Re3 C24 126.7(9) . . ? C18 Re3 C24 143.8(10) . . ? C22 Re3 C24 70.4(9) . . ? C21 Re3 C24 75.3(9) . . ? C17 Re3 C24 130.9(9) . . ? C23 Re3 C19 98.1(9) . . ? C20 Re3 C19 77.9(7) . . ? C18 Re3 C19 145.5(8) . . ? C22 Re3 C19 140.1(7) . . ? C21 Re3 C19 89.0(7) . . ? C17 Re3 C19 71.8(7) . . ? C24 Re3 C19 70.2(9) . . ? C31 Re4 C28 66.8(10) . . ? C31 Re4 C27 147.6(10) . . ? C28 Re4 C27 145.6(8) . . ? C31 Re4 C30 80.2(11) . . ? C28 Re4 C30 129.2(10) . . ? C27 Re4 C30 75.0(10) . . ? C31 Re4 C26 94.3(10) . . ? C28 Re4 C26 77.2(8) . . ? C27 Re4 C26 94.2(8) . . ? C30 Re4 C26 145.2(10) . . ? C31 Re4 C25 140.0(9) . . ? C28 Re4 C25 73.3(7) . . ? C27 Re4 C25 72.3(7) . . ? C30 Re4 C25 130.3(9) . . ? C26 Re4 C25 73.9(7) . . ? C31 Re4 C32 79.2(11) . . ? C28 Re4 C32 135.0(9) . . ? C27 Re4 C32 72.4(9) . . ? C30 Re4 C32 68.3(11) . . ? C26 Re4 C32 76.9(9) . . ? C25 Re4 C32 131.6(9) . . ? C31 Re4 C29 98.9(10) . . ? C28 Re4 C29 76.9(7) . . ? C27 Re4 C29 92.7(8) . . ? C30 Re4 C29 71.1(9) . . ? C26 Re4 C29 143.3(7) . . ? C25 Re4 C29 74.1(6) . . ? C32 Re4 C29 139.1(8) . . ? C40 Re5 C33 138.0(10) . . ? C40 Re5 C36 68.9(10) . . ? C33 Re5 C36 74.4(7) . . ? C40 Re5 C39 84.2(11) . . ? C33 Re5 C39 134.4(7) . . ? C36 Re5 C39 123.3(8) . . ? C40 Re5 C37 85.7(10) . . ? C33 Re5 C37 72.9(7) . . ? C36 Re5 C37 87.6(8) . . ? C39 Re5 C37 140.5(8) . . ? C40 Re5 C38 75.7(11) . . ? C33 Re5 C38 127.6(8) . . ? C36 Re5 C38 140.4(8) . . ? C39 Re5 C38 68.3(9) . . ? C37 Re5 C38 72.2(8) . . ? C40 Re5 C34 145.7(10) . . ? C33 Re5 C34 72.8(6) . . ? C36 Re5 C34 145.4(7) . . ? C39 Re5 C34 75.0(8) . . ? C37 Re5 C34 93.2(7) . . ? C38 Re5 C34 71.4(8) . . ? C40 Re5 C35 113.5(11) . . ? C33 Re5 C35 74.8(8) . . ? C36 Re5 C35 75.4(8) . . ? C39 Re5 C35 71.3(9) . . ? C37 Re5 C35 146.6(8) . . ? C38 Re5 C35 137.3(9) . . ? C34 Re5 C35 85.5(8) . . ? C45 Re6 C41 72.5(9) . . ? C45 Re6 C48 142.4(9) . . ? C41 Re6 C48 132.8(8) . . ? C45 Re6 C43 85.2(9) . . ? C41 Re6 C43 72.9(8) . . ? C48 Re6 C43 79.4(8) . . ? C45 Re6 C47 108.3(11) . . ? C41 Re6 C47 140.7(10) . . ? C48 Re6 C47 70.8(10) . . ? C43 Re6 C47 145.8(11) . . ? C45 Re6 C46 71.7(9) . . ? C41 Re6 C46 134.5(8) . . ? C48 Re6 C46 71.4(8) . . ? C43 Re6 C46 76.9(8) . . ? C47 Re6 C46 78.0(10) . . ? C45 Re6 C44 83.4(9) . . ? C41 Re6 C44 69.9(8) . . ? C48 Re6 C44 127.9(8) . . ? C43 Re6 C44 142.8(8) . . ? C47 Re6 C44 71.2(10) . . ? C46 Re6 C44 131.5(8) . . ? C45 Re6 C42 146.1(8) . . ? C41 Re6 C42 75.0(7) . . ? C48 Re6 C42 69.9(7) . . ? C43 Re6 C42 94.6(7) . . ? C47 Re6 C42 90.7(10) . . ? C46 Re6 C42 141.3(8) . . ? C44 Re6 C42 76.4(7) . . ? N9 Co7 N17 88.9(6) . . ? N9 Co7 N1 175.7(6) . . ? N17 Co7 N1 91.9(7) . . ? N9 Co7 N41 87.8(6) . . ? N17 Co7 N41 175.7(6) . . ? N1 Co7 N41 91.5(6) . . ? N9 Co7 N25 89.8(7) . . ? N17 Co7 N25 89.8(7) . . ? N1 Co7 N25 86.0(7) . . ? N41 Co7 N25 93.0(4) . . ? N9 Co7 N33 93.0(6) . . ? N17 Co7 N33 89.4(4) . . ? N1 Co7 N33 91.2(7) . . ? N41 Co7 N33 87.9(6) . . ? N25 Co7 N33 177.1(7) . . ? O3 Co8 N10 171.2(7) . . ? O3 Co8 N21 92.4(7) . . ? N10 Co8 N21 90.9(7) . . ? O3 Co8 O2 86.4(6) . . ? N10 Co8 O2 85.5(7) . . ? N21 Co8 O2 88.1(7) . . ? O3 Co8 O1 88.3(6) . . ? N10 Co8 O1 88.4(7) . . ? N21 Co8 O1 179.2(7) . . ? O2 Co8 O1 91.6(6) . . ? O3 Co8 N36 90.4(6) . . ? N10 Co8 N36 97.7(7) . . ? N21 Co8 N36 90.7(7) . . ? O2 Co8 N36 176.6(6) . . ? O1 Co8 N36 89.6(6) . . ? N5 Co9 O5 90.8(7) . . ? N5 Co9 O6 92.0(7) . . ? O5 Co9 O6 87.3(7) . . ? N5 Co9 N27 86.2(7) . . ? O5 Co9 N27 90.9(7) . . ? O6 Co9 N27 177.4(7) . . ? N5 Co9 N20 95.8(7) . . ? O5 Co9 N20 172.7(7) . . ? O6 Co9 N20 89.4(7) . . ? N27 Co9 N20 92.6(7) . . ? N5 Co9 O4 177.4(7) . . ? O5 Co9 O4 87.4(7) . . ? O6 Co9 O4 86.0(7) . . ? N27 Co9 O4 95.7(7) . . ? N20 Co9 O4 85.9(7) . . ? N19 Co10 O7 90.7(7) . . ? N19 Co10 O9 87.2(7) . . ? O7 Co10 O9 87.4(7) . . ? N19 Co10 O8 174.1(7) . . ? O7 Co10 O8 86.4(7) . . ? O9 Co10 O8 87.4(7) . . ? N19 Co10 N37 89.2(7) . . ? O7 Co10 N37 179.1(6) . . ? O9 Co10 N37 91.7(7) . . ? O8 Co10 N37 93.6(7) . . ? N19 Co10 N2 96.0(7) . . ? O7 Co10 N2 90.2(6) . . ? O9 Co10 N2 176.0(7) . . ? O8 Co10 N2 89.2(7) . . ? N37 Co10 N2 90.7(6) . . ? N35 Co11 O11 92.3(7) . . ? N35 Co11 N43 91.1(7) . . ? O11 Co11 N43 88.9(7) . . ? N35 Co11 O12 176.9(7) . . ? O11 Co11 O12 85.9(6) . . ? N43 Co11 O12 91.3(7) . . ? N35 Co11 O10 89.3(7) . . ? O11 Co11 O10 83.7(7) . . ? N43 Co11 O10 172.5(8) . . ? O12 Co11 O10 88.0(7) . . ? N35 Co11 N13 92.8(7) . . ? O11 Co11 N13 173.7(7) . . ? N43 Co11 N13 94.6(8) . . ? O12 Co11 N13 88.8(7) . . ? O10 Co11 N13 92.8(7) . . ? O13 Co12 N42 92.8(7) . . ? O13 Co12 O15 86.9(6) . . ? N42 Co12 O15 91.0(7) . . ? O13 Co12 N28 91.1(6) . . ? N42 Co12 N28 95.2(7) . . ? O15 Co12 N28 173.5(7) . . ? O13 Co12 N11 173.3(6) . . ? N42 Co12 N11 93.1(7) . . ? O15 Co12 N11 89.8(7) . . ? N28 Co12 N11 91.4(6) . . ? O13 Co12 O14 86.2(6) . . ? N42 Co12 O14 178.8(7) . . ? O15 Co12 O14 88.2(6) . . ? N28 Co12 O14 85.5(6) . . ? N11 Co12 O14 87.8(6) . . ? N3 Co13 O18 89.9(8) . . ? N3 Co13 N44 92.1(7) . . ? O18 Co13 N44 177.8(8) . . ? N3 Co13 N26 90.2(8) . . ? O18 Co13 N26 88.1(7) . . ? N44 Co13 N26 91.0(8) . . ? N3 Co13 O16 174.8(8) . . ? O18 Co13 O16 84.9(7) . . ? N44 Co13 O16 93.1(7) . . ? N26 Co13 O16 90.5(7) . . ? N3 Co13 O17 93.2(8) . . ? O18 Co13 O17 87.2(7) . . ? N44 Co13 O17 93.6(7) . . ? N26 Co13 O17 174.2(8) . . ? O16 Co13 O17 85.8(7) . . ? O21 Co14 N29 93.2(7) . . ? O21 Co14 N18 172.9(6) . . ? N29 Co14 N18 90.8(7) . . ? O21 Co14 O20 82.2(7) . . ? N29 Co14 O20 173.5(7) . . ? N18 Co14 O20 93.2(6) . . ? O21 Co14 N12 94.5(7) . . ? N29 Co14 N12 94.2(7) . . ? N18 Co14 N12 91.1(7) . . ? O20 Co14 N12 90.8(7) . . ? O21 Co14 O19 84.2(6) . . ? N29 Co14 O19 88.6(7) . . ? N18 Co14 O19 90.0(6) . . ? O20 Co14 O19 86.3(7) . . ? N12 Co14 O19 177.0(8) . . ? N4 Co15 N34 89.4(8) . . ? N4 Co15 O22 171.1(8) . . ? N34 Co15 O22 92.7(8) . . ? N4 Co15 O23 85.7(8) . . ? N34 Co15 O23 93.1(8) . . ? O22 Co15 O23 85.6(7) . . ? N4 Co15 N45 97.3(7) . . ? N34 Co15 N45 93.0(8) . . ? O22 Co15 N45 91.1(6) . . ? O23 Co15 N45 173.2(7) . . ? N4 Co15 O24 88.6(7) . . ? N34 Co15 O24 176.1(8) . . ? O22 Co15 O24 89.7(6) . . ? O23 Co15 O24 90.1(7) . . ? N45 Co15 O24 83.9(6) . . ? N1 C1 Re1 178(2) . . ? N2 C2 Re1 171.8(18) . . ? N3 C3 Re1 173.8(18) . . ? N4 C4 Re1 166.3(19) . . ? N5 C5 Re1 175.4(18) . . ? N6 C6 Re1 162(3) . . ? N7 C7 Re1 174.4(19) . . ? N8 C8 Re1 173.4(19) . . ? N9 C9 Re2 174.6(16) . . ? N10 C10 Re2 177(2) . . ? N11 C11 Re2 173.6(14) . . ? N12 C12 Re2 173(2) . . ? N13 C13 Re2 171.6(16) . . ? N14 C14 Re2 173.0(19) . . ? N15 C15 Re2 171(3) . . ? N16 C16 Re2 178.7(17) . . ? N17 C17 Re3 177.1(18) . . ? N18 C18 Re3 173.3(19) . . ? N19 C19 Re3 178.0(16) . . ? N20 C20 Re3 174.9(17) . . ? N21 C21 Re3 175(2) . . ? N22 C22 Re3 169(2) . . ? N23 C23 Re3 156(3) . . ? N24 C24 Re3 175(2) . . ? N25 C25 Re4 172.5(16) . . ? N26 C26 Re4 177.3(19) . . ? N27 C27 Re4 175.9(19) . . ? N28 C28 Re4 177.8(19) . . ? N29 C29 Re4 169.9(16) . . ? N30 C30 Re4 178(3) . . ? N31 C31 Re4 154(4) . . ? N32 C32 Re4 176(2) . . ? N33 C33 Re5 177.5(15) . . ? N34 C34 Re5 172.3(18) . . ? N35 C35 Re5 173(2) . . ? N36 C36 Re5 176.8(18) . . ? N37 C37 Re5 176.4(17) . . ? N38 C38 Re5 166(2) . . ? N39 C39 Re5 174(2) . . ? N40 C40 Re5 172(3) . . ? N41 C41 Re6 175.2(17) . . ? N42 C42 Re6 170.8(17) . . ? N43 C43 Re6 172.6(19) . . ? N44 C44 Re6 172.0(19) . . ? N45 C45 Re6 171(2) . . ? N46 C46 Re6 175(2) . . ? N47 C47 Re6 169(3) . . ? N48 C48 Re6 174(2) . . ? C1 N1 Co7 175.1(17) . . ? C2 N2 Co10 176.8(18) . . ? C3 N3 Co13 175.2(19) . . ? C4 N4 Co15 175(2) . . ? C5 N5 Co9 175.1(16) . . ? C9 N9 Co7 174.3(14) . . ? C10 N10 Co8 173.0(18) . . ? C11 N11 Co12 176.8(15) . . ? C12 N12 Co14 168.9(18) . . ? C13 N13 Co11 166.6(16) . . ? C17 N17 Co7 178.9(18) . . ? C18 N18 Co14 175.9(17) . . ? C19 N19 Co10 173.8(16) . . ? C20 N20 Co9 177.0(17) . . ? C21 N21 Co8 170.7(18) . . ? C25 N25 Co7 170.4(16) . . ? C26 N26 Co13 173.0(18) . . ? C27 N27 Co9 170.8(18) . . ? C28 N28 Co12 174.7(16) . . ? C29 N29 Co14 178.0(17) . . ? C33 N33 Co7 175.9(16) . . ? C34 N34 Co15 176(2) . . ? C35 N35 Co11 175.7(18) . . ? C36 N36 Co8 177.2(16) . . ? C37 N37 Co10 174.3(16) . . ? C41 N41 Co7 179.0(17) . . ? C42 N42 Co12 170.4(17) . . ? C43 N43 Co11 169.3(19) . . ? C44 N44 Co13 171.5(18) . . ? C45 N45 Co15 165.0(17) . . ? C201 O1 Co8 125(3) . . ? C202 O2 Co8 126.3(13) . . ? C203 O3 Co8 123(3) . . ? C204 O4 Co9 133(2) . . ? C205 O5 Co9 122.3(14) . . ? C206 O6 Co9 128(2) . . ? C207 O7 Co10 126.7(13) . . ? C208 O8 Co10 125.9(17) . . ? C209 O9 Co10 134(2) . . ? C210 O10 Co11 112(2) . . ? C211 O11 Co11 114.5(14) . . ? C212 O12 Co11 121.2(16) . . ? C213 O13 Co12 127.4(17) . . ? C214 O14 Co12 126.1(14) . . ? C215 O15 Co12 127.2(16) . . ? C216 O16 Co13 121.6(15) . . ? C217 O17 Co13 126(2) . . ? C218 O18 Co13 127.4(16) . . ? C219 O19 Co14 123.4(15) . . ? C220 O20 Co14 124.2(16) . . ? C221 O21 Co14 131.5(15) . . ? C222 O22 Co15 126.7(16) . . ? C223 O23 Co15 127.9(17) . . ? C224 O24 Co15 113(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.455 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.221 # Attachment '4b.cif' data_df39i _database_code_depnum_ccdc_archive 'CCDC 292905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common na _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72.50 H110 Mn9 Mo3.12 N48 O30.50 Re2.88' _chemical_formula_weight 3471.28 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 29.385(4) _cell_length_b 18.742(3) _cell_length_c 32.641(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.837(3) _cell_angle_gamma 90.00 _cell_volume 16314(4) _cell_formula_units_Z 4 _cell_measurement_temperature 179 _cell_measurement_reflns_used 4282 _cell_measurement_theta_min 4.329 _cell_measurement_theta_max 38.711 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6348 _exptl_absorpt_coefficient_mu 3.089 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 179 _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 'Bruker SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28158 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.1093 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 20.86 _reflns_number_total 12827 _reflns_number_gt 9137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.53(3) _refine_ls_number_reflns 12827 _refine_ls_number_parameters 769 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.2925 _refine_ls_wR_factor_gt 0.2647 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.212 _refine_ls_shift/su_max 0.435 _refine_ls_shift/su_mean 0.008 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 Re1 Re 2.27581(8) -1.85130(12) 2.54518(8) 0.0405(6) Uani 0.48 1 d PD . . Re2 Re 2.63446(10) -1.84522(13) 2.52441(9) 0.0594(8) Uani 0.48 1 d PD . . Re3 Re 2.51296(9) -2.07860(13) 2.65723(7) 0.0467(7) Uani 0.48 1 d PD . . Re4 Re 2.39622(9) -2.06491(15) 2.40345(7) 0.0566(8) Uani 0.48 1 d PD . . Re5 Re 2.53670(10) -1.67186(14) 2.67424(10) 0.0657(9) Uani 0.48 1 d PD . . Re6 Re 2.37751(11) -1.65678(16) 2.40789(11) 0.0865(12) Uani 0.48 1 d PD . . Mo1 Mo 2.27581(8) -1.85130(12) 2.54518(8) 0.0405(6) Uani 0.52 1 d P . . Mo2 Mo 2.63446(10) -1.84522(13) 2.52441(9) 0.0594(8) Uani 0.52 1 d P . . Mo3 Mo 2.51296(9) -2.07860(13) 2.65723(7) 0.0467(7) Uani 0.52 1 d P . . Mo4 Mo 2.39622(9) -2.06491(15) 2.40345(7) 0.0566(8) Uani 0.52 1 d P . . Mo5 Mo 2.53670(10) -1.67186(14) 2.67424(10) 0.0657(9) Uani 0.52 1 d P . . Mo6 Mo 2.37751(11) -1.65678(16) 2.40789(11) 0.0865(12) Uani 0.52 1 d P . . Mn7 Mn 2.4556(3) -1.86203(19) 2.5346(2) 0.0306(10) Uani 1 1 d . . . Mn8 Mn 2.3243(2) -2.1286(3) 2.5303(2) 0.0489(18) Uani 1 1 d . . . Mn9 Mn 2.5843(2) -2.1242(3) 2.5302(2) 0.0394(16) Uani 1 1 d . . . Mn10 Mn 2.2423(3) -1.8764(5) 2.3687(3) 0.078(3) Uani 1 1 d D . . Mn11 Mn 2.6682(3) -1.8918(4) 2.6993(2) 0.0588(19) Uani 1 1 d . . . Mn12 Mn 2.4260(3) -1.8621(5) 2.7145(2) 0.089(3) Uani 1 1 d . . . Mn13 Mn 2.4868(4) -1.8449(6) 2.3550(3) 0.127(5) Uani 1 1 d D . . Mn14 Mn 2.3507(3) -1.5846(4) 2.5584(3) 0.078(2) Uani 1 1 d . . . Mn15 Mn 2.5653(3) -1.5751(4) 2.5314(4) 0.109(4) Uani 1 1 d D . . C1 C 2.3440(12) -1.8575(17) 2.5410(11) 0.034(9) Uiso 1 1 d D . . C2 C 2.3343(14) -1.8552(18) 2.6163(11) 0.038(9) Uiso 1 1 d D . . C3 C 2.2950(15) -1.9609(16) 2.5455(13) 0.048(11) Uiso 1 1 d D . . C4 C 2.3058(13) -1.7469(15) 2.5550(11) 0.042(9) Uiso 1 1 d D . . C5 C 2.2584(15) -1.8561(19) 2.4776(10) 0.046(11) Uiso 1 1 d D . . C6 C 2.2105(10) -1.7887(18) 2.5103(11) 0.059(11) Uiso 1 1 d D . . C7 C 2.2481(18) -1.818(2) 2.5923(14) 0.088(15) Uiso 1 1 d D . . C8 C 2.2125(18) -1.921(3) 2.5322(18) 0.13(3) Uiso 1 1 d D . . C9 C 2.5659(13) -1.8438(18) 2.5303(12) 0.042(10) Uiso 1 1 d D . . C10 C 2.6991(15) -1.786(3) 2.5683(15) 0.111(19) Uiso 1 1 d D . . C11 C 2.6165(14) -1.9515(16) 2.5249(11) 0.037(9) Uiso 1 1 d D . . C12 C 2.610(2) -1.731(2) 2.5314(17) 0.094(16) Uiso 1 1 d D . . C13 C 2.5796(15) -1.866(2) 2.4557(11) 0.064(13) Uiso 1 1 d D . . C14 C 2.6637(19) -1.780(2) 2.4869(15) 0.100(16) Uiso 1 1 d D . . C15 C 2.6541(14) -1.8734(18) 2.5926(10) 0.043(10) Uiso 1 1 d D . . C16 C 2.6951(11) -1.912(2) 2.5262(12) 0.061(12) Uiso 1 1 d D . . C17 C 2.525(2) -2.1909(10) 2.6602(19) 0.105(18) Uiso 1 1 d D . . C18 C 2.4885(14) -1.9925(15) 2.6049(11) 0.040(9) Uiso 1 1 d D . . C19 C 2.5708(16) -2.006(2) 2.6747(16) 0.079(15) Uiso 1 1 d D . . C20 C 2.4787(12) -2.1328(16) 2.6936(10) 0.038(9) Uiso 1 1 d D . . C21 C 2.5442(10) -2.1009(13) 2.6119(8) 0.009(6) Uiso 1 1 d D . . C22 C 2.4423(10) -2.1056(14) 2.6099(9) 0.016(7) Uiso 1 1 d D . . C23 C 2.4875(13) -2.0000(16) 2.6851(11) 0.037(9) Uiso 1 1 d D . . C24 C 2.5774(18) -2.121(4) 2.7124(13) 0.16(3) Uiso 1 1 d D . . C25 C 2.3678(19) -2.087(2) 2.4485(15) 0.083(15) Uiso 1 1 d D . . C26 C 2.4175(11) -1.9903(13) 2.4484(9) 0.015(7) Uiso 1 1 d D . . C27 C 2.4367(16) -2.106(2) 2.3675(14) 0.081(14) Uiso 1 1 d D . . C28 C 2.3304(12) -2.0005(17) 2.3859(11) 0.034(9) Uiso 1 1 d D . . C29 C 2.3486(13) -2.068(2) 2.3335(6) 0.065(11) Uiso 1 1 d D . . C30 C 2.386(2) -2.1784(11) 2.4007(18) 0.11(2) Uiso 1 1 d D . . C31 C 2.4690(13) -2.091(2) 2.4549(13) 0.073(14) Uiso 1 1 d D . . C32 C 2.4299(14) -1.9767(17) 2.3772(12) 0.047(9) Uiso 1 1 d D . . C33 C 2.6099(10) -1.626(2) 2.7037(15) 0.086(14) Uiso 1 1 d D . . C34 C 2.5093(13) -1.7459(17) 2.6226(10) 0.042(10) Uiso 1 1 d D . . C35 C 2.4831(16) -1.741(2) 2.6906(14) 0.070(12) Uiso 1 1 d D . . C36 C 2.5487(15) -1.6267(18) 2.6211(11) 0.053(10) Uiso 1 1 d D . . C37 C 2.5903(15) -1.7583(19) 2.6879(14) 0.069(12) Uiso 1 1 d D . . C38 C 2.518(2) -1.5751(17) 2.6981(17) 0.107(17) Uiso 1 1 d D . . C39 C 2.4683(15) -1.641(2) 2.6345(13) 0.069(12) Uiso 1 1 d D . . C40 C 2.5676(17) -1.680(2) 2.7461(6) 0.082(14) Uiso 1 1 d D . . C41 C 2.4073(14) -1.7334(17) 2.4560(11) 0.049(10) Uiso 1 1 d D . . C42 C 2.339(3) -1.668(4) 2.3369(8) 0.18(3) Uiso 1 1 d D . . C43 C 2.3088(11) -1.598(2) 2.3859(14) 0.074(13) Uiso 1 1 d D . . C44 C 2.3648(19) -1.619(2) 2.4661(14) 0.077(13) Uiso 1 1 d D . . C45 C 2.3251(14) -1.7383(19) 2.3927(12) 0.052(10) Uiso 1 1 d D . . C46 C 2.4543(16) -1.623(2) 2.4502(14) 0.082(14) Uiso 1 1 d D . . C47 C 2.391(2) -1.5491(14) 2.3938(19) 0.111(18) Uiso 1 1 d D . . C48 C 2.4190(14) -1.7128(19) 2.3842(13) 0.059(11) Uiso 1 1 d D . . C201 C 2.199(2) -2.115(3) 2.490(2) 0.064(19) Uiso 0.70 1 d P . . C202 C 2.311(3) -2.102(4) 2.626(3) 0.15(3) Uiso 1 1 d . . . C203 C 2.332(4) -2.306(6) 2.552(4) 0.25(5) Uiso 1 1 d . . . C204 C 2.5844(19) -2.129(2) 2.4307(17) 0.080(14) Uiso 1 1 d . . . C205 C 2.600(2) -2.291(3) 2.5481(17) 0.098(16) Uiso 1 1 d . . . C206 C 2.688(2) -2.080(3) 2.616(2) 0.121(19) Uiso 1 1 d . . . C208 C 2.5371(19) -1.844(2) 2.7965(16) 0.085(14) Uiso 1 1 d . . . C209 C 2.179(3) -1.741(3) 2.384(2) 0.12(2) Uiso 1 1 d . . . C210 C 2.210(4) -2.027(5) 2.382(3) 0.24(4) Uiso 1 1 d . . . C211 C 2.708(8) -1.859(8) 2.807(5) 0.52(13) Uiso 1 1 d D . . C213 C 2.729(3) -1.769(3) 2.691(2) 0.16(3) Uiso 1 1 d D . . C214 C 2.374(3) -2.008(4) 2.727(2) 0.14(2) Uiso 1 1 d . . . C215 C 2.335(2) -1.766(3) 2.7269(17) 0.101(16) Uiso 1 1 d . . . C216 C 2.5158(15) -1.973(2) 2.3216(13) 0.057(11) Uiso 1 1 d . . . C218 C 2.381(3) -1.792(3) 2.270(2) 0.13(2) Uiso 1 1 d . . . C219 C 2.250(3) -1.558(4) 2.465(3) 0.15(3) Uiso 1 1 d . . . C220 C 2.344(2) -1.605(3) 2.651(2) 0.12(2) Uiso 1 1 d . . . C221 C 2.425(4) -1.464(5) 2.580(3) 0.20(4) Uiso 1 1 d . . . C222 C 2.671(3) -1.591(3) 2.589(2) 0.13(2) Uiso 1 1 d . . . C223 C 2.498(3) -1.438(3) 2.495(2) 0.26(5) Uiso 1 1 d D . . C224 C 2.576(2) -1.574(3) 2.4415(19) 0.098(17) Uiso 1 1 d . . . C803 C 2.571(3) -1.424(4) 2.652(3) 0.16(3) Uiso 1 1 d . . . N1 N 2.3822(12) -1.8603(15) 2.5377(10) 0.042(8) Uiso 1 1 d D . . N2 N 2.3641(15) -1.884(2) 2.6479(13) 0.105(15) Uiso 1 1 d D . . N3 N 2.3088(12) -2.0186(15) 2.5433(10) 0.043(8) Uiso 1 1 d D . . N4 N 2.3223(12) -1.6888(15) 2.5605(10) 0.059(9) Uiso 1 1 d D . . N5 N 2.2529(14) -1.8741(17) 2.4415(10) 0.057(10) Uiso 1 1 d D . . N6 N 2.1774(8) -1.7494(12) 2.4903(8) 0.045(7) Uiso 1 1 d D . . N7 N 2.2292(18) -1.812(2) 2.6175(14) 0.131(16) Uiso 1 1 d D . . N8 N 2.1852(17) -1.952(3) 2.5437(18) 0.15(2) Uiso 1 1 d D . . N9 N 2.5275(13) -1.8524(16) 2.5322(11) 0.053(9) Uiso 1 1 d D . . N10 N 2.731(2) -1.751(4) 2.594(2) 0.23(3) Uiso 1 1 d D . . N11 N 2.6034(13) -2.0106(15) 2.5231(10) 0.050(9) Uiso 1 1 d D . . N12 N 2.6012(19) -1.672(2) 2.5373(16) 0.116(15) Uiso 1 1 d D . . N13 N 2.5476(12) -1.8573(15) 2.4195(10) 0.051(8) Uiso 1 1 d D . . N14 N 2.6723(18) -1.744(2) 2.4615(13) 0.122(16) Uiso 1 1 d D . . N15 N 2.6609(14) -1.8791(18) 2.6303(10) 0.062(10) Uiso 1 1 d D . . N16 N 2.7325(13) -1.945(3) 2.5435(16) 0.141(19) Uiso 1 1 d D . . N17 N 2.521(3) -2.2533(11) 2.658(3) 0.23(3) Uiso 1 1 d D . . N18 N 2.4760(11) -1.9433(13) 2.5808(9) 0.035(7) Uiso 1 1 d D . . N19 N 2.6018(12) -1.9627(16) 2.6819(10) 0.047(8) Uiso 1 1 d D . . N20 N 2.4562(13) -2.1547(17) 2.7131(11) 0.071(10) Uiso 1 1 d D . . N21 N 2.5615(12) -2.1107(15) 2.5860(9) 0.046(8) Uiso 1 1 d D . . N22 N 2.4005(11) -2.1098(19) 2.5835(11) 0.069(11) Uiso 1 1 d D . . N23 N 2.4698(13) -1.9561(17) 2.6994(11) 0.070(10) Uiso 1 1 d D . . N24 N 2.6065(19) -2.139(3) 2.7484(11) 0.18(2) Uiso 1 1 d D . . N25 N 2.3539(11) -2.1088(15) 2.4750(10) 0.040(8) Uiso 1 1 d D . . N26 N 2.4259(13) -1.9463(15) 2.4760(10) 0.057(10) Uiso 1 1 d D . . N27 N 2.4631(13) -2.1343(19) 2.3539(13) 0.092(13) Uiso 1 1 d D . . N28 N 2.2946(12) -1.9663(17) 2.3783(11) 0.059(10) Uiso 1 1 d D . . N29 N 2.3235(17) -2.075(3) 2.2947(7) 0.134(17) Uiso 1 1 d D . . N31 N 2.5048(10) -2.1172(14) 2.4823(9) 0.032(7) Uiso 1 1 d D . . N32 N 2.4457(14) -1.9233(18) 2.3696(12) 0.078(11) Uiso 1 1 d D . . N33 N 2.6452(10) -1.5886(17) 2.7147(12) 0.089(12) Uiso 1 1 d D . . N34 N 2.4872(12) -1.7825(15) 2.5916(9) 0.046(9) Uiso 1 1 d D . . N35 N 2.4610(12) -1.7856(17) 2.7001(10) 0.063(9) Uiso 1 1 d D . . N36 N 2.5513(13) -1.6023(16) 2.5893(10) 0.061(9) Uiso 1 1 d D . . N37 N 2.6180(11) -1.8056(15) 2.6922(9) 0.049(8) Uiso 1 1 d D . . N38 N 2.500(2) -1.5220(18) 2.7023(18) 0.15(2) Uiso 1 1 d D . . N39 N 2.4322(15) -1.613(2) 2.6075(13) 0.091(12) Uiso 1 1 d D . . N40 N 2.5877(14) -1.693(2) 2.7846(6) 0.092(12) Uiso 1 1 d D . . N41 N 2.4261(12) -1.7807(16) 2.4809(10) 0.052(9) Uiso 1 1 d D . . N42 N 2.323(2) -1.658(3) 2.2976(9) 0.15(2) Uiso 1 1 d D . . N43 N 2.2786(17) -1.556(3) 2.385(2) 0.18(2) Uiso 1 1 d D . . N44 N 2.3629(16) -1.607(2) 2.5006(13) 0.094(12) Uiso 1 1 d D . . N45 N 2.2934(14) -1.7810(19) 2.3837(12) 0.083(11) Uiso 1 1 d D . . N46 N 2.4899(13) -1.6062(18) 2.4824(12) 0.071(10) Uiso 1 1 d D . . N47 N 2.406(2) -1.4914(15) 2.392(2) 0.16(2) Uiso 1 1 d D . . N48 N 2.4442(12) -1.7521(17) 2.3748(11) 0.065(9) Uiso 1 1 d D . . O1 O 2.2474(11) -2.1378(14) 2.4773(10) 0.066(9) Uiso 1 1 d . . . O2 O 2.2999(16) -2.1532(18) 2.5855(13) 0.100(12) Uiso 1 1 d . . . O3 O 2.3343(17) -2.242(2) 2.5313(14) 0.128(15) Uiso 1 1 d . . . O4 O 2.6081(12) -2.1495(14) 2.4775(10) 0.065(9) Uiso 1 1 d . . . O5 O 2.5768(13) -2.2374(18) 2.5399(10) 0.083(10) Uiso 1 1 d . . . O6 O 2.6634(12) -2.1358(14) 2.5807(10) 0.064(8) Uiso 1 1 d . . . O7 O 2.2283(12) -1.8812(16) 2.2987(10) 0.084(10) Uiso 1 1 d D . . O8 O 2.4874(11) -1.8660(14) 2.7846(9) 0.070(8) Uiso 1 1 d . . . O9 O 2.1856(15) -1.787(2) 2.3532(13) 0.119(13) Uiso 1 1 d . . . O10 O 2.1857(14) -1.9603(18) 2.3522(11) 0.096(11) Uiso 1 1 d . . . O11 O 2.6850(12) -1.9128(16) 2.7751(10) 0.084(9) Uiso 1 1 d D . . O12 O 2.7189(14) -1.9804(18) 2.7097(11) 0.098(11) Uiso 1 1 d D . . O13 O 2.7333(13) -1.8243(17) 2.7225(11) 0.093(10) Uiso 1 1 d D . . O14 O 2.3914(14) -1.9416(19) 2.7456(11) 0.099(11) Uiso 1 1 d . . . O15 O 2.3873(13) -1.7948(17) 2.7391(11) 0.098(10) Uiso 1 1 d . . . O16 O 2.5289(16) -1.911(2) 2.3302(13) 0.128(14) Uiso 1 1 d . . . C217 C 2.493(7) -1.707(11) 2.304(6) 0.58(16) Uiso 0.90 1 d PD . . O18 O 2.4348(13) -1.8267(16) 2.2846(10) 0.091(10) Uiso 1 1 d . . . O19 O 2.2759(12) -1.5476(16) 2.5119(10) 0.086(9) Uiso 1 1 d . . . O20 O 2.3347(13) -1.5528(17) 2.6152(11) 0.086(10) Uiso 1 1 d . . . O21 O 2.3712(13) -1.4731(16) 2.5568(11) 0.090(9) Uiso 1 1 d . . . O22 O 2.6366(18) -1.533(2) 2.5743(15) 0.140(15) Uiso 1 1 d . . . O23 O 2.5364(13) -1.4676(16) 2.5357(10) 0.093(9) Uiso 1 1 d D . . O24 O 2.5910(14) -1.5347(18) 2.4829(13) 0.115(11) Uiso 1 1 d . . . O800 O 1.9340(17) -1.846(2) 2.3789(14) 0.138(14) Uiso 1 1 d . . . O801 O 2.6917(17) -1.208(2) 2.6602(14) 0.046(12) Uiso 0.50 1 d P . . O803 O 2.549(2) -1.403(2) 2.6128(18) 0.168(18) Uiso 1 1 d . . . O804 O 2.036(2) -1.800(3) 2.4427(17) 0.067(15) Uiso 0.50 1 d P . . O805 O 2.245(3) -2.237(4) 2.376(2) 0.11(2) Uiso 0.50 1 d P . . O806 O 2.436(3) -2.265(3) 2.515(2) 0.10(2) Uiso 0.50 1 d P . . O807 O 1.949(3) -1.850(3) 2.285(2) 0.090(19) Uiso 0.50 1 d P . . O810 O 2.137(4) -2.086(5) 2.274(3) 0.16(3) Uiso 0.50 1 d P . . O811 O 2.057(3) -1.935(3) 2.403(2) 0.093(19) Uiso 0.50 1 d P . . O812 O 2.340(4) -2.329(5) 2.648(3) 0.16(3) Uiso 0.50 1 d P . . O817 O 2.458(2) -1.400(3) 2.7151(18) 0.075(16) Uiso 0.50 1 d P . . C312 C 2.764(2) -1.963(4) 2.705(2) 0.05(2) Uiso 0.50 1 d PD . . C301 C 2.201(3) -2.085(5) 2.480(3) 0.00(2) Uiso 0.30 1 d P . . C307 C 2.265(2) -1.893(4) 2.2824(18) 0.20(3) Uiso 1 1 d D . . N30 N 2.385(3) -2.2371(15) 2.414(2) 0.20(3) Uiso 1 1 d D . . O17 O 2.5245(16) -1.755(2) 2.3368(13) 0.118(12) Uiso 1 1 d D . . C317 C 2.562(8) -1.714(11) 2.370(2) 0.04(9) Uiso 0.10 1 d PD . . 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 Re1 0.0211(14) 0.0457(14) 0.0631(15) -0.0167(12) 0.0258(12) -0.0099(11) Re2 0.0387(18) 0.0576(16) 0.101(2) 0.0230(15) 0.0483(16) 0.0081(13) Re3 0.0282(15) 0.0826(17) 0.0264(13) 0.0241(11) 0.0087(11) -0.0010(12) Re4 0.0322(16) 0.112(2) 0.0196(12) -0.0177(12) 0.0053(11) 0.0224(14) Re5 0.0375(17) 0.0575(16) 0.104(2) -0.0525(15) 0.0310(15) -0.0222(12) Re6 0.052(2) 0.094(2) 0.129(3) 0.084(2) 0.0529(19) 0.0410(16) Mo1 0.0211(14) 0.0457(14) 0.0631(15) -0.0167(12) 0.0258(12) -0.0099(11) Mo2 0.0387(18) 0.0576(16) 0.101(2) 0.0230(15) 0.0483(16) 0.0081(13) Mo3 0.0282(15) 0.0826(17) 0.0264(13) 0.0241(11) 0.0087(11) -0.0010(12) Mo4 0.0322(16) 0.112(2) 0.0196(12) -0.0177(12) 0.0053(11) 0.0224(14) Mo5 0.0375(17) 0.0575(16) 0.104(2) -0.0525(15) 0.0310(15) -0.0222(12) Mo6 0.052(2) 0.094(2) 0.129(3) 0.084(2) 0.0529(19) 0.0410(16) Mn7 0.019(2) 0.035(2) 0.041(3) -0.005(3) 0.016(2) 0.006(3) Mn8 0.026(4) 0.057(4) 0.058(4) -0.003(3) 0.013(3) -0.014(3) Mn9 0.034(4) 0.033(3) 0.042(4) -0.004(3) 0.007(3) 0.011(3) Mn10 0.034(5) 0.120(6) 0.069(5) 0.053(4) 0.012(4) 0.030(4) Mn11 0.036(5) 0.071(4) 0.056(4) -0.020(3) 0.006(3) -0.003(3) Mn12 0.040(5) 0.208(9) 0.028(4) -0.041(4) 0.023(4) -0.016(5) Mn13 0.079(7) 0.249(12) 0.077(6) 0.096(7) 0.057(6) 0.087(7) Mn14 0.040(5) 0.055(4) 0.154(7) -0.010(4) 0.055(5) 0.003(3) Mn15 0.059(6) 0.053(5) 0.235(11) 0.051(6) 0.080(7) 0.007(4) _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 Re1 C5 2.05(3) . ? Re1 C1 2.07(3) . ? Re1 C7 2.114(17) . ? Re1 C4 2.11(3) . ? Re1 C6 2.125(15) . ? Re1 C3 2.13(3) . ? Re1 C8 2.162(19) . ? Re1 C2 2.24(3) . ? Re2 C11 2.06(3) . ? Re2 C9 2.10(3) . ? Re2 C15 2.12(3) . ? Re2 C10 2.142(18) . ? Re2 C14 2.152(17) . ? Re2 C16 2.161(17) . ? Re2 C13 2.18(3) . ? Re2 C12 2.30(5) . ? Re3 C23 2.03(3) . ? Re3 C19 2.06(3) . ? Re3 C22 2.06(3) . ? Re3 C21 2.09(2) . ? Re3 C20 2.110(15) . ? Re3 C17 2.128(18) . ? Re3 C24 2.146(18) . ? Re3 C18 2.24(3) . ? Re4 C26 1.93(2) . ? Re4 C25 2.01(3) . ? Re4 C29 2.119(16) . ? Re4 C27 2.134(16) . ? Re4 C28 2.14(3) . ? Re4 C31 2.15(3) . ? Re4 C30 2.146(18) . ? Re4 C32 2.27(3) . ? Re5 C39 1.97(4) . ? Re5 C34 2.07(3) . ? Re5 C36 2.09(3) . ? Re5 C38 2.129(18) . ? Re5 C33 2.135(17) . ? Re5 C40 2.136(16) . ? Re5 C37 2.17(3) . ? Re5 C35 2.27(3) . ? Re6 C48 1.99(3) . ? Re6 C41 2.03(3) . ? Re6 C45 2.08(3) . ? Re6 C42 2.12(2) . ? Re6 C43 2.142(17) . ? Re6 C47 2.145(18) . ? Re6 C46 2.18(4) . ? Re6 C44 2.20(4) . ? Mn7 N18 2.05(2) . ? Mn7 N9 2.15(4) . ? Mn7 N1 2.20(3) . ? Mn7 N41 2.21(3) . ? Mn7 N34 2.26(3) . ? Mn7 N26 2.35(3) . ? Mn8 O3 2.14(5) . ? Mn8 N3 2.19(3) . ? Mn8 O1 2.20(3) . ? Mn8 N22 2.21(3) . ? Mn8 O2 2.25(4) . ? Mn8 N25 2.34(3) . ? Mn9 O4 2.16(3) . ? Mn9 O5 2.17(3) . ? Mn9 N31 2.20(3) . ? Mn9 N21 2.21(2) . ? Mn9 O6 2.22(3) . ? Mn9 N11 2.24(3) . ? Mn10 O7 2.15(3) . ? Mn10 O10 2.18(4) . ? Mn10 N28 2.21(3) . ? Mn10 N45 2.25(4) . ? Mn10 O9 2.26(4) . ? Mn10 N5 2.26(3) . ? Mn11 N37 2.13(3) . ? Mn11 O13 2.15(3) . ? Mn11 O12 2.16(4) . ? Mn11 N15 2.19(3) . ? Mn11 N19 2.23(3) . ? Mn11 O11 2.34(3) . ? Mn12 N35 1.94(3) . ? Mn12 O15 2.07(3) . ? Mn12 N2 2.21(4) . ? Mn12 O8 2.24(3) . ? Mn12 O14 2.27(4) . ? Mn12 N23 2.35(3) . ? Mn13 N32 2.08(3) . ? Mn13 N13 2.13(3) . ? Mn13 O16 2.14(4) . ? Mn13 O18 2.19(3) . ? Mn13 O17 2.23(4) . ? Mn13 N48 2.38(3) . ? Mn14 N44 2.10(4) . ? Mn14 N4 2.14(3) . ? Mn14 O20 2.18(3) . ? Mn14 O21 2.18(3) . ? Mn14 O19 2.20(3) . ? Mn14 N39 2.31(4) . ? Mn15 N12 2.06(5) . ? Mn15 O22 2.13(5) . ? Mn15 N36 2.16(3) . ? Mn15 O24 2.16(4) . ? Mn15 N46 2.20(4) . ? Mn15 O23 2.21(3) . ? C1 N1 1.173(10) . ? C2 N2 1.170(10) . ? C3 N3 1.168(10) . ? C4 N4 1.173(10) . ? C5 N5 1.167(10) . ? C6 N6 1.176(10) . ? C7 N7 1.174(10) . ? C8 N8 1.177(10) . ? C9 N9 1.170(10) . ? C10 N10 1.173(10) . ? C11 N11 1.167(10) . ? C12 N12 1.178(10) . ? C13 N13 1.169(10) . ? C14 N14 1.175(10) . ? C15 N15 1.166(10) . ? C16 N16 1.178(10) . ? C17 N17 1.173(10) . ? C18 N18 1.166(10) . ? C19 N19 1.172(10) . ? C20 N20 1.171(10) . ? C21 N21 1.169(10) . ? C22 N22 1.171(10) . ? C23 N23 1.170(10) . ? C24 N24 1.175(10) . ? C25 N25 1.176(10) . ? C26 N26 1.169(10) . ? C27 N27 1.172(10) . ? C28 N28 1.166(10) . ? C29 N29 1.174(10) . ? C30 N30 1.183(10) . ? C31 N31 1.170(10) . ? C32 N32 1.172(10) . ? C33 N33 1.174(10) . ? C34 N34 1.170(10) . ? C35 N35 1.175(10) . ? C36 N36 1.166(10) . ? C37 N37 1.172(10) . ? C38 N38 1.171(10) . ? C39 N39 1.183(10) . ? C40 N40 1.170(10) . ? C41 N41 1.172(10) . ? C42 N42 1.18(4) . ? C43 N43 1.177(10) . ? C44 N44 1.176(10) . ? C45 N45 1.167(10) . ? C46 N46 1.175(10) . ? C47 N47 1.173(10) . ? C48 N48 1.174(10) . ? C201 C301 0.68(9) . ? C201 O1 1.68(7) . ? C202 O2 1.55(8) . ? C203 O3 1.40(11) . ? C204 O4 1.44(5) . ? C205 O5 1.18(5) . ? C206 O6 1.50(6) . ? C208 O8 1.41(5) . ? C209 O9 1.42(6) . ? C210 O10 1.56(10) . ? C211 O11 1.41(3) . ? C213 O13 1.43(3) . ? C214 O14 1.37(7) . ? C215 O15 1.51(6) . ? C216 O16 1.22(5) . ? C218 O18 1.58(7) . ? C219 O19 1.41(8) . ? C220 O20 1.47(6) . ? C221 O21 1.44(10) . ? C222 O22 1.42(7) . ? C223 O23 1.45(3) . ? C224 O24 1.43(6) . ? C803 O803 1.24(8) . ? O1 C301 1.72(9) . ? O7 C307 1.41(3) . ? O12 C312 1.42(3) . ? C217 O17 1.41(2) . ? O17 C317 1.400(11) . ? 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 C5 Re1 C1 74.7(14) . . ? C5 Re1 C7 143.1(18) . . ? C1 Re1 C7 138.1(17) . . ? C5 Re1 C4 95.9(14) . . ? C1 Re1 C4 73.1(13) . . ? C7 Re1 C4 83.2(16) . . ? C5 Re1 C6 71.7(15) . . ? C1 Re1 C6 132.7(14) . . ? C7 Re1 C6 72.0(17) . . ? C4 Re1 C6 78.2(15) . . ? C5 Re1 C3 84.8(14) . . ? C1 Re1 C3 71.6(14) . . ? C7 Re1 C3 117.5(17) . . ? C4 Re1 C3 143.1(15) . . ? C6 Re1 C3 135.5(16) . . ? C5 Re1 C8 87.6(18) . . ? C1 Re1 C8 137(2) . . ? C7 Re1 C8 76(2) . . ? C4 Re1 C8 149(2) . . ? C6 Re1 C8 74(2) . . ? C3 Re1 C8 68(2) . . ? C5 Re1 C2 148.5(14) . . ? C1 Re1 C2 73.9(13) . . ? C7 Re1 C2 67.5(17) . . ? C4 Re1 C2 77.5(13) . . ? C6 Re1 C2 134.5(14) . . ? C3 Re1 C2 82.9(14) . . ? C8 Re1 C2 114.0(18) . . ? C11 Re2 C9 75.7(14) . . ? C11 Re2 C15 73.0(14) . . ? C9 Re2 C15 75.9(14) . . ? C11 Re2 C10 130.6(19) . . ? C9 Re2 C10 123.1(19) . . ? C15 Re2 C10 69.6(19) . . ? C11 Re2 C14 136.2(17) . . ? C9 Re2 C14 132.1(17) . . ? C15 Re2 C14 137.9(18) . . ? C10 Re2 C14 68(2) . . ? C11 Re2 C16 69.4(16) . . ? C9 Re2 C16 144.6(15) . . ? C15 Re2 C16 88.1(14) . . ? C10 Re2 C16 78(2) . . ? C14 Re2 C16 80.1(18) . . ? C11 Re2 C13 75.8(15) . . ? C9 Re2 C13 76.8(16) . . ? C15 Re2 C13 142.7(16) . . ? C10 Re2 C13 148(2) . . ? C14 Re2 C13 79.4(18) . . ? C16 Re2 C13 99.8(15) . . ? C11 Re2 C12 143.6(17) . . ? C9 Re2 C12 68.0(16) . . ? C15 Re2 C12 94.9(16) . . ? C10 Re2 C12 71(2) . . ? C14 Re2 C12 75.0(19) . . ? C16 Re2 C12 145.9(18) . . ? C13 Re2 C12 98.1(17) . . ? C23 Re3 C19 79.3(17) . . ? C23 Re3 C22 94.0(12) . . ? C19 Re3 C22 145.4(16) . . ? C23 Re3 C21 144.9(12) . . ? C19 Re3 C21 76.7(15) . . ? C22 Re3 C21 91.4(11) . . ? C23 Re3 C20 75.2(13) . . ? C19 Re3 C20 134.0(17) . . ? C22 Re3 C20 74.7(12) . . ? C21 Re3 C20 139.3(12) . . ? C23 Re3 C17 141.1(18) . . ? C19 Re3 C17 123(2) . . ? C22 Re3 C17 83.3(18) . . ? C21 Re3 C17 74.0(17) . . ? C20 Re3 C17 66.6(18) . . ? C23 Re3 C24 105(2) . . ? C19 Re3 C24 71(2) . . ? C22 Re3 C24 142(2) . . ? C21 Re3 C24 91.4(19) . . ? C20 Re3 C24 79(2) . . ? C17 Re3 C24 62(2) . . ? C23 Re3 C18 76.1(12) . . ? C19 Re3 C18 72.5(17) . . ? C22 Re3 C18 72.9(12) . . ? C21 Re3 C18 72.5(11) . . ? C20 Re3 C18 134.5(13) . . ? C17 Re3 C18 137.9(17) . . ? C24 Re3 C18 143(2) . . ? C26 Re4 C25 72.2(16) . . ? C26 Re4 C29 133.9(14) . . ? C25 Re4 C29 119.6(19) . . ? C26 Re4 C27 126.9(16) . . ? C25 Re4 C27 145.7(19) . . ? C29 Re4 C27 70.5(17) . . ? C26 Re4 C28 76.3(12) . . ? C25 Re4 C28 73.0(17) . . ? C29 Re4 C28 67.2(14) . . ? C27 Re4 C28 134.7(15) . . ? C26 Re4 C31 70.7(15) . . ? C25 Re4 C31 88.0(19) . . ? C29 Re4 C31 145.8(16) . . ? C27 Re4 C31 75.4(18) . . ? C28 Re4 C31 145.7(15) . . ? C26 Re4 C30 138.1(16) . . ? C25 Re4 C30 74(2) . . ? C29 Re4 C30 85.0(19) . . ? C27 Re4 C30 74(2) . . ? C28 Re4 C30 117(2) . . ? C31 Re4 C30 84(2) . . ? C26 Re4 C32 72.9(12) . . ? C25 Re4 C32 143.5(16) . . ? C29 Re4 C32 78.8(14) . . ? C27 Re4 C32 67.8(15) . . ? C28 Re4 C32 88.6(13) . . ? C31 Re4 C32 90.5(16) . . ? C30 Re4 C32 141.7(17) . . ? C39 Re5 C34 73.8(16) . . ? C39 Re5 C36 79.3(17) . . ? C34 Re5 C36 74.8(14) . . ? C39 Re5 C38 69.3(19) . . ? C34 Re5 C38 143.0(18) . . ? C36 Re5 C38 96.6(18) . . ? C39 Re5 C33 137.4(18) . . ? C34 Re5 C33 127.7(16) . . ? C36 Re5 C33 73.9(17) . . ? C38 Re5 C33 82(2) . . ? C39 Re5 C40 126.2(18) . . ? C34 Re5 C40 133.5(16) . . ? C36 Re5 C40 143.0(18) . . ? C38 Re5 C40 73.4(19) . . ? C33 Re5 C40 69.5(19) . . ? C39 Re5 C37 143.9(17) . . ? C34 Re5 C37 70.5(15) . . ? C36 Re5 C37 96.5(15) . . ? C38 Re5 C37 146.3(18) . . ? C33 Re5 C37 72.6(17) . . ? C40 Re5 C37 77.6(17) . . ? C39 Re5 C35 72.9(17) . . ? C34 Re5 C35 74.8(14) . . ? C36 Re5 C35 143.4(16) . . ? C38 Re5 C35 95.4(19) . . ? C33 Re5 C35 142.3(17) . . ? C40 Re5 C35 73.6(17) . . ? C37 Re5 C35 92.3(16) . . ? C48 Re6 C41 78.1(15) . . ? C48 Re6 C45 91.9(16) . . ? C41 Re6 C45 72.5(15) . . ? C48 Re6 C42 70(3) . . ? C41 Re6 C42 129(2) . . ? C45 Re6 C42 70(2) . . ? C48 Re6 C43 141.7(16) . . ? C41 Re6 C43 131.3(16) . . ? C45 Re6 C43 78.4(16) . . ? C42 Re6 C43 72(3) . . ? C48 Re6 C47 102.3(19) . . ? C41 Re6 C47 140.5(19) . . ? C45 Re6 C47 145.9(19) . . ? C42 Re6 C47 86(3) . . ? C43 Re6 C47 71(2) . . ? C48 Re6 C46 76.1(17) . . ? C41 Re6 C46 73.7(16) . . ? C45 Re6 C46 145.9(16) . . ? C42 Re6 C46 131(3) . . ? C43 Re6 C46 129.9(18) . . ? C47 Re6 C46 68(2) . . ? C48 Re6 C44 148.8(17) . . ? C41 Re6 C44 74.4(16) . . ? C45 Re6 C44 93.6(16) . . ? C42 Re6 C44 140(3) . . ? C43 Re6 C44 69.4(17) . . ? C47 Re6 C44 90(2) . . ? C46 Re6 C44 82.3(18) . . ? N18 Mn7 N9 95.8(12) . . ? N18 Mn7 N1 88.1(11) . . ? N9 Mn7 N1 174.3(9) . . ? N18 Mn7 N41 173.9(12) . . ? N9 Mn7 N41 88.7(12) . . ? N1 Mn7 N41 87.7(12) . . ? N18 Mn7 N34 89.6(11) . . ? N9 Mn7 N34 84.5(12) . . ? N1 Mn7 N34 91.5(11) . . ? N41 Mn7 N34 95.0(9) . . ? N18 Mn7 N26 89.6(9) . . ? N9 Mn7 N26 93.5(12) . . ? N1 Mn7 N26 90.6(12) . . ? N41 Mn7 N26 86.0(12) . . ? N34 Mn7 N26 177.8(12) . . ? O3 Mn8 N3 165.6(14) . . ? O3 Mn8 O1 91.4(14) . . ? N3 Mn8 O1 89.8(11) . . ? O3 Mn8 N22 93.4(16) . . ? N3 Mn8 N22 85.6(13) . . ? O1 Mn8 N22 175.3(13) . . ? O3 Mn8 O2 82.7(14) . . ? N3 Mn8 O2 82.8(12) . . ? O1 Mn8 O2 92.6(13) . . ? N22 Mn8 O2 87.9(14) . . ? O3 Mn8 N25 94.3(13) . . ? N3 Mn8 N25 100.1(11) . . ? O1 Mn8 N25 89.9(11) . . ? N22 Mn8 N25 89.9(13) . . ? O2 Mn8 N25 176.2(13) . . ? O4 Mn9 O5 89.4(11) . . ? O4 Mn9 N31 92.8(11) . . ? O5 Mn9 N31 91.1(12) . . ? O4 Mn9 N21 173.8(11) . . ? O5 Mn9 N21 84.6(11) . . ? N31 Mn9 N21 88.8(11) . . ? O4 Mn9 O6 89.0(11) . . ? O5 Mn9 O6 86.3(12) . . ? N31 Mn9 O6 176.8(11) . . ? N21 Mn9 O6 89.1(11) . . ? O4 Mn9 N11 87.0(11) . . ? O5 Mn9 N11 172.1(13) . . ? N31 Mn9 N11 96.2(11) . . ? N21 Mn9 N11 98.7(11) . . ? O6 Mn9 N11 86.6(12) . . ? O7 Mn10 O10 85.5(12) . . ? O7 Mn10 N28 86.0(12) . . ? O10 Mn10 N28 84.2(13) . . ? O7 Mn10 N45 94.4(13) . . ? O10 Mn10 N45 173.5(14) . . ? N28 Mn10 N45 102.3(14) . . ? O7 Mn10 O9 89.9(13) . . ? O10 Mn10 O9 93.6(14) . . ? N28 Mn10 O9 175.5(14) . . ? N45 Mn10 O9 79.9(14) . . ? O7 Mn10 N5 176.9(13) . . ? O10 Mn10 N5 91.6(12) . . ? N28 Mn10 N5 94.9(12) . . ? N45 Mn10 N5 88.3(13) . . ? O9 Mn10 N5 89.1(13) . . ? N37 Mn11 O13 93.7(12) . . ? N37 Mn11 O12 177.2(12) . . ? O13 Mn11 O12 86.8(13) . . ? N37 Mn11 N15 92.3(12) . . ? O13 Mn11 N15 89.2(13) . . ? O12 Mn11 N15 90.4(13) . . ? N37 Mn11 N19 86.2(12) . . ? O13 Mn11 N19 174.8(12) . . ? O12 Mn11 N19 93.1(13) . . ? N15 Mn11 N19 96.0(13) . . ? N37 Mn11 O11 94.1(11) . . ? O13 Mn11 O11 88.0(12) . . ? O12 Mn11 O11 83.1(12) . . ? N15 Mn11 O11 173.1(13) . . ? N19 Mn11 O11 86.8(11) . . ? N35 Mn12 O15 94.4(14) . . ? N35 Mn12 N2 101.6(15) . . ? O15 Mn12 N2 97.9(15) . . ? N35 Mn12 O8 89.5(12) . . ? O15 Mn12 O8 87.8(12) . . ? N2 Mn12 O8 167.0(14) . . ? N35 Mn12 O14 168.4(13) . . ? O15 Mn12 O14 78.8(13) . . ? N2 Mn12 O14 88.7(15) . . ? O8 Mn12 O14 80.9(12) . . ? N35 Mn12 N23 96.3(13) . . ? O15 Mn12 N23 167.0(13) . . ? N2 Mn12 N23 87.1(14) . . ? O8 Mn12 N23 85.1(11) . . ? O14 Mn12 N23 89.4(13) . . ? N32 Mn13 N13 91.3(13) . . ? N32 Mn13 O16 99.3(16) . . ? N13 Mn13 O16 86.2(14) . . ? N32 Mn13 O18 97.7(14) . . ? N13 Mn13 O18 169.6(13) . . ? O16 Mn13 O18 87.3(14) . . ? N32 Mn13 O17 174.8(16) . . ? N13 Mn13 O17 92.4(14) . . ? O16 Mn13 O17 84.6(15) . . ? O18 Mn13 O17 79.0(14) . . ? N32 Mn13 N48 91.8(14) . . ? N13 Mn13 N48 97.4(12) . . ? O16 Mn13 N48 168.3(14) . . ? O18 Mn13 N48 87.5(12) . . ? O17 Mn13 N48 84.1(13) . . ? N44 Mn14 N4 93.8(14) . . ? N44 Mn14 O20 174.6(15) . . ? N4 Mn14 O20 89.8(12) . . ? N44 Mn14 O21 90.7(14) . . ? N4 Mn14 O21 172.7(12) . . ? O20 Mn14 O21 85.3(12) . . ? N44 Mn14 O19 86.6(14) . . ? N4 Mn14 O19 91.1(12) . . ? O20 Mn14 O19 89.4(12) . . ? O21 Mn14 O19 83.5(12) . . ? N44 Mn14 N39 93.5(16) . . ? N4 Mn14 N39 94.3(14) . . ? O20 Mn14 N39 90.2(14) . . ? O21 Mn14 N39 91.2(14) . . ? O19 Mn14 N39 174.6(14) . . ? N12 Mn15 O22 86.7(19) . . ? N12 Mn15 N36 89.4(15) . . ? O22 Mn15 N36 90.5(15) . . ? N12 Mn15 O24 92.9(16) . . ? O22 Mn15 O24 78.4(16) . . ? N36 Mn15 O24 168.5(15) . . ? N12 Mn15 N46 99.0(17) . . ? O22 Mn15 N46 172.7(16) . . ? N36 Mn15 N46 94.1(13) . . ? O24 Mn15 N46 96.6(14) . . ? N12 Mn15 O23 170.9(17) . . ? O22 Mn15 O23 85.1(15) . . ? N36 Mn15 O23 86.7(12) . . ? O24 Mn15 O23 89.3(13) . . ? N46 Mn15 O23 89.5(13) . . ? N1 C1 Re1 178(3) . . ? N2 C2 Re1 154(4) . . ? N3 C3 Re1 172(3) . . ? N4 C4 Re1 180(3) . . ? N5 C5 Re1 165(3) . . ? N6 C6 Re1 173(4) . . ? N7 C7 Re1 168(5) . . ? N8 C8 Re1 152(4) . . ? N9 C9 Re2 171(3) . . ? N10 C10 Re2 172(7) . . ? N11 C11 Re2 176(4) . . ? N12 C12 Re2 175(5) . . ? N13 C13 Re2 161(4) . . ? N14 C14 Re2 170(5) . . ? N15 C15 Re2 169(3) . . ? N16 C16 Re2 156(4) . . ? N17 C17 Re3 168(6) . . ? N18 C18 Re3 174(3) . . ? N19 C19 Re3 175(4) . . ? N20 C20 Re3 171(3) . . ? N21 C21 Re3 177(2) . . ? N22 C22 Re3 169(3) . . ? N23 C23 Re3 176(3) . . ? N24 C24 Re3 164(6) . . ? N25 C25 Re4 171(4) . . ? N26 C26 Re4 173(3) . . ? N27 C27 Re4 169(4) . . ? N28 C28 Re4 177(3) . . ? N29 C29 Re4 175(4) . . ? N30 C30 Re4 159(5) . . ? N31 C31 Re4 167(4) . . ? N32 C32 Re4 167(3) . . ? N33 C33 Re5 166(4) . . ? N34 C34 Re5 170(3) . . ? N35 C35 Re5 169(4) . . ? N36 C36 Re5 175(4) . . ? N37 C37 Re5 175(3) . . ? N38 C38 Re5 166(5) . . ? N39 C39 Re5 167(4) . . ? N40 C40 Re5 170(4) . . ? N41 C41 Re6 173(3) . . ? N42 C42 Re6 163(7) . . ? N43 C43 Re6 161(5) . . ? N44 C44 Re6 171(4) . . ? N45 C45 Re6 176(4) . . ? N46 C46 Re6 160(4) . . ? N47 C47 Re6 169(6) . . ? N48 C48 Re6 171(3) . . ? C301 C201 O1 82(10) . . ? C1 N1 Mn7 177(3) . . ? C2 N2 Mn12 141(4) . . ? C3 N3 Mn8 172(3) . . ? C4 N4 Mn14 170(3) . . ? C5 N5 Mn10 164(3) . . ? C9 N9 Mn7 177(3) . . ? C11 N11 Mn9 172(3) . . ? C12 N12 Mn15 162(5) . . ? C13 N13 Mn13 177(3) . . ? C15 N15 Mn11 176(4) . . ? C18 N18 Mn7 175(3) . . ? C19 N19 Mn11 172(4) . . ? C21 N21 Mn9 172(3) . . ? C22 N22 Mn8 173(3) . . ? C23 N23 Mn12 170(3) . . ? C25 N25 Mn8 169(3) . . ? C26 N26 Mn7 171(3) . . ? C28 N28 Mn10 164(3) . . ? C31 N31 Mn9 156(3) . . ? C32 N32 Mn13 166(3) . . ? C34 N34 Mn7 171(3) . . ? C35 N35 Mn12 177(3) . . ? C36 N36 Mn15 169(3) . . ? C37 N37 Mn11 180(4) . . ? C39 N39 Mn14 164(4) . . ? C41 N41 Mn7 171(3) . . ? C44 N44 Mn14 174(4) . . ? C45 N45 Mn10 171(4) . . ? C46 N46 Mn15 166(4) . . ? C48 N48 Mn13 172(3) . . ? C201 O1 C301 23(3) . . ? C201 O1 Mn8 119(3) . . ? C301 O1 Mn8 120(3) . . ? C202 O2 Mn8 122(3) . . ? C203 O3 Mn8 146(6) . . ? C204 O4 Mn9 127(3) . . ? C205 O5 Mn9 141(4) . . ? C206 O6 Mn9 121(3) . . ? C307 O7 Mn10 125(3) . . ? C208 O8 Mn12 125(3) . . ? C209 O9 Mn10 127(3) . . ? C210 O10 Mn10 109(5) . . ? C211 O11 Mn11 119(9) . . ? C312 O12 Mn11 114(4) . . ? C213 O13 Mn11 112(4) . . ? C214 O14 Mn12 123(3) . . ? C215 O15 Mn12 141(3) . . ? C216 O16 Mn13 118(3) . . ? C218 O18 Mn13 124(3) . . ? C219 O19 Mn14 129(4) . . ? C220 O20 Mn14 117(3) . . ? C221 O21 Mn14 111(4) . . ? C222 O22 Mn15 107(4) . . ? C223 O23 Mn15 118(3) . . ? C224 O24 Mn15 116(3) . . ? C201 C301 O1 75(10) . . ? C317 O17 C217 107(10) . . ? C317 O17 Mn13 122(3) . . ? C217 O17 Mn13 116(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.86 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.267 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.237