# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Keith Murray' _publ_contact_author_email k.s.murray@sci.monash.edu.au _publ_contact_author_phone +61-3-9905-4512 _publ_contact_author_fax +61-3-9905-4597 loop_ _publ_author_name _publ_author_address S.K.Langley ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; N.F.Chilton ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.Moubaraki ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; K.S.Murray ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_section_title ; Structure and Magnetic Exchange in Hetero-metallic 3d-3d transition metal triethanolamine clusters ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; # Attachment '- 1 Mn4Co4finalSept29.CIF' #========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 838818' #TrackingRef '- 1 Mn4Co4finalSept29.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit consists of half the cluster, as well as a tetrafluoroborate counter ion, a disordered acetate anion and disordered solvent molecules. The "free" triethanolamine arm is found to be at partial occupancy (39%) with diethanolamine and a solvent MeOH (61%) molecules present when the arm is absent. Thermal (SIMU and DELU) and bond (DFIX) restraints are placed on this arm and MEOH molecule. The solvent acetate anions are disordered over two positions (set at 50:50) with bond (DFIX) and thermal (ISOR) restraints placed on these. A solvent MeOH is also found and is disordered over two sites (set at 50:50) as well as a water molecule. All non H-atoms are refined anisotropically. All H-atoms are placed in calculated positions, except for H5 which was found. The H atoms for the solvent water and one of the protonated triethanolamine arms could not be found. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.82 H100 B2 Co4 F8 Mn4 N6 O31' _chemical_formula_weight 1824.08 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9188(3) _cell_length_b 27.5788(6) _cell_length_c 12.3562(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.8490(10) _cell_angle_gamma 90.00 _cell_volume 3769.81(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8975 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 26.17 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1865 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 36130 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7682 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The structure was solved by direct methods. The asymmetric unit consists of half the cluster, as well as a tetrafluoroborate counter ion, a disordered acetate anion and disordered solvent molecules. The "free" triethanolamine arm is found to be at partial occupancy (39%) with diethanolamine and a solvent MeOH (61%) molecules present when the arm is absent. Thermal (SIMU and DELU) and bond (DFIX) restraints are placed on this arm and MEOH molecule. The solvent acetate anions are disordered over two positions (set at 50:50) with bond (DFIX) and thermal (ISOR) restraints placed on these. A solvent MeOH is also found and is disordered over two sites (set at 50:50) as well as a water molecule. All non H-atoms are refined anisotropically. All H-atoms are placed in calculated positions, except for H5 which was found. The H atoms for the solvent water and one of the protonated triethanolamine arms could not be found. ; _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^)+(0.1196P)^2^+16.8420P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7682 _refine_ls_number_parameters 534 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2436 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.045 _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 Co1 Co 0.28907(9) 0.16101(4) 0.48146(10) 0.0425(3) Uani 1 1 d . A . Co3 Co 0.00168(9) 0.13336(4) 0.38060(9) 0.0356(3) Uani 1 1 d . . . Mn1 Mn 0.08764(9) -0.02933(4) 0.58635(9) 0.0306(3) Uani 1 1 d . . . Mn2 Mn 0.17916(9) 0.06121(4) 0.53712(9) 0.0331(3) Uani 1 1 d . . . O1 O 0.2014(5) -0.0156(2) 0.7448(4) 0.0422(13) Uani 1 1 d . A . O2 O 0.2221(4) -0.0039(2) 0.5217(4) 0.0363(12) Uani 1 1 d . A . O3 O 0.0401(4) 0.03622(18) 0.5613(4) 0.0290(11) Uani 1 1 d . . . O4 O 0.2750(5) 0.0575(2) 0.7225(5) 0.0454(14) Uani 1 1 d . . . O5 O 0.0504(4) 0.07046(19) 0.3525(4) 0.0351(12) Uani 1 1 d . . . O6 O 0.1189(4) 0.12691(19) 0.5360(4) 0.0350(12) Uani 1 1 d . A . O7 O -0.1269(4) 0.09792(18) 0.3991(4) 0.0338(11) Uani 1 1 d . . . O8 O 0.3075(5) 0.0891(2) 0.5019(5) 0.0458(14) Uani 1 1 d . . . O9 O 0.1254(5) 0.1694(2) 0.3580(5) 0.0419(13) Uani 1 1 d . A . O11 O 0.2951(6) 0.2069(3) 0.6119(7) 0.073(3) Uani 1 1 d D . . O12 O 0.3745(5) 0.1915(2) 0.3801(6) 0.0545(16) Uani 1 1 d . . . N1 N -0.0639(6) 0.1886(3) 0.4389(6) 0.0470(17) Uani 1 1 d . A . H1 H -0.0628 0.2156 0.3969 0.056 Uiso 1 1 calc R . . N2 N -0.0846(6) 0.1403(3) 0.2135(6) 0.0490(18) Uani 0.410(19) 1 d PD A 1 N3 N 0.4829(6) 0.1552(3) 0.6014(7) 0.059(2) Uani 1 1 d . . . C1 C 0.2669(8) 0.0223(4) 0.7816(7) 0.049(2) Uani 1 1 d . A . C2 C 0.3408(11) 0.0229(4) 0.9124(8) 0.084(4) Uani 1 1 d . . . H2A H 0.4008 0.0480 0.9298 0.127 Uiso 1 1 calc R A . H2B H 0.3797 -0.0079 0.9358 0.127 Uiso 1 1 calc R . . H2C H 0.2883 0.0290 0.9539 0.127 Uiso 1 1 calc R . . C3 C 0.2343(9) -0.0201(3) 0.4164(8) 0.054(2) Uani 1 1 d . . . H3A H 0.1594 -0.0341 0.3658 0.081 Uiso 1 1 calc R A . H3B H 0.2973 -0.0439 0.4348 0.081 Uiso 1 1 calc R . . H3C H 0.2542 0.0070 0.3781 0.081 Uiso 1 1 calc R . . C4 C -0.1914(8) 0.1759(3) 0.4195(10) 0.067(3) Uani 1 1 d . . . H4A H -0.2423 0.1813 0.3384 0.081 Uiso 1 1 calc RD A . H4B H -0.2205 0.1963 0.4674 0.081 Uiso 1 1 calc R . . C5 C -0.1973(7) 0.1238(3) 0.4505(9) 0.051(2) Uani 1 1 d . A . H5A H -0.1647 0.1196 0.5345 0.062 Uiso 1 1 calc R . . H5B H -0.2802 0.1124 0.4200 0.062 Uiso 1 1 calc R . . C6 C 0.0169(7) 0.1962(3) 0.5632(8) 0.049(2) Uani 1 1 d . . . H6A H -0.0296 0.2094 0.6063 0.058 Uiso 1 1 calc R A . H6B H 0.0796 0.2194 0.5673 0.058 Uiso 1 1 calc R . . C7 C 0.0737(7) 0.1490(3) 0.6172(6) 0.0408(19) Uani 1 1 d . A . H7A H 0.1391 0.1547 0.6914 0.049 Uiso 1 1 calc R . . H7B H 0.0142 0.1281 0.6300 0.049 Uiso 1 1 calc R . . C8 C -0.0620(8) 0.0945(3) 0.1575(6) 0.050(2) Uani 1 1 d . . . H8A H -0.0538 0.1024 0.0843 0.060 Uiso 1 1 calc R A 1 H8B H -0.1304 0.0727 0.1409 0.060 Uiso 1 1 calc R A 1 C9 C 0.0528(8) 0.0693(3) 0.2382(6) 0.046(2) Uani 1 1 d . A . H9A H 0.0550 0.0360 0.2134 0.056 Uiso 1 1 calc R . . H9B H 0.1238 0.0860 0.2367 0.056 Uiso 1 1 calc R . . C10 C -0.0357(8) 0.1850(4) 0.1793(8) 0.056(2) Uani 1 1 d . . . H10A H -0.0690 0.2136 0.2020 0.067 Uiso 1 1 calc R A 1 H10B H -0.0572 0.1857 0.0954 0.067 Uiso 1 1 calc R A 1 C11 C 0.0995(8) 0.1840(4) 0.2405(7) 0.053(2) Uani 1 1 d . A . H11A H 0.1349 0.1613 0.2023 0.063 Uiso 1 1 calc R . . H11B H 0.1329 0.2159 0.2387 0.063 Uiso 1 1 calc R . . C14 C 0.4989(9) 0.1052(5) 0.6445(10) 0.079(4) Uani 1 1 d . A . H14A H 0.4723 0.1025 0.7096 0.094 Uiso 1 1 calc R . . H14B H 0.5839 0.0966 0.6722 0.094 Uiso 1 1 calc R . . C15 C 0.4284(8) 0.0710(4) 0.5508(10) 0.068(3) Uani 1 1 d . A . H15A H 0.4632 0.0691 0.4914 0.082 Uiso 1 1 calc R . . H15B H 0.4291 0.0388 0.5828 0.082 Uiso 1 1 calc R . . C16 C 0.5583(8) 0.1656(4) 0.5311(10) 0.071(3) Uani 1 1 d . A . H16A H 0.6382 0.1761 0.5818 0.085 Uiso 1 1 calc R . . H16B H 0.5670 0.1364 0.4911 0.085 Uiso 1 1 calc R . . C17 C 0.4991(8) 0.2039(4) 0.4449(10) 0.067(3) Uani 1 1 d . A . H17A H 0.5032 0.2345 0.4849 0.081 Uiso 1 1 calc R . . H17B H 0.5413 0.2077 0.3918 0.081 Uiso 1 1 calc R . . C18 C 0.5061(9) 0.1901(5) 0.6969(10) 0.084(4) Uani 1 1 d . A . H18A H 0.5292 0.2213 0.6751 0.100 Uiso 1 1 calc R . . H18B H 0.5711 0.1786 0.7662 0.100 Uiso 1 1 calc R . . C19 C 0.3919(10) 0.1950(6) 0.7198(10) 0.096(5) Uani 1 1 d . A . H19A H 0.3743 0.1647 0.7504 0.116 Uiso 1 1 calc R . . H19B H 0.4008 0.2203 0.7769 0.116 Uiso 1 1 calc R . . H5 H 0.297(14) 0.233(5) 0.592(14) 0.116 Uiso 1 1 d . . . F1S F -0.0347(7) 0.2887(3) 0.3612(12) 0.168(5) Uani 1 1 d . . . F2S F -0.2190(8) 0.2693(3) 0.2501(16) 0.219(8) Uani 1 1 d . . . F3S F -0.1494(9) 0.3389(4) 0.2311(8) 0.145(4) Uani 1 1 d . . . F4S F -0.1964(11) 0.3243(8) 0.3746(10) 0.237(9) Uani 1 1 d . . . O1S O 0.3368(11) 0.3010(3) 0.6600(10) 0.070(4) Uani 0.50 1 d PD B 6 O2S O 0.2485(12) 0.3190(5) 0.4565(9) 0.083(5) Uani 0.50 1 d PD B 6 O3S O 0.499(2) 0.3639(8) 0.692(3) 0.182(11) Uani 0.50 1 d PDU C 5 O4S O 0.5003(13) 0.4472(5) 0.7446(13) 0.077(4) Uani 0.50 1 d PD C 5 O7S O 0.1103(18) 0.4389(8) 0.4923(15) 0.116(7) Uani 0.50 1 d PD D 4 H7S H 0.1140 0.4682 0.4946 0.139 Uiso 0.50 1 d P E 4 O8S O -0.237(4) 0.4631(15) 0.372(4) 0.230(16) Uani 0.50 1 d PDU F 3 H8S H -0.2574 0.4407 0.3965 0.276 Uiso 0.50 1 d P G 3 C1S C 0.2856(16) 0.3216(5) 0.5653(9) 0.057(5) Uani 0.50 1 d PDU B 6 C2S C 0.2929(14) 0.3739(4) 0.5961(11) 0.044(4) Uani 0.50 1 d PD B 6 H2S1 H 0.3355 0.3776 0.6786 0.067 Uiso 0.50 1 calc PR B 6 H2S2 H 0.2127 0.3869 0.5746 0.067 Uiso 0.50 1 calc PR B 6 H2S3 H 0.3350 0.3910 0.5551 0.067 Uiso 0.50 1 calc PR B 6 C3S C 0.4899(14) 0.4017(5) 0.7425(15) 0.047(4) Uani 0.50 1 d PDU C 5 C4S C 0.386(2) 0.3940(11) 0.779(3) 0.116(10) Uani 0.50 1 d PDU C 5 H4S1 H 0.3376 0.3737 0.7264 0.173 Uiso 0.50 1 d P H 5 H4S2 H 0.3526 0.4271 0.7731 0.173 Uiso 0.50 1 d P I 5 H4S3 H 0.4188 0.3846 0.8566 0.173 Uiso 0.50 1 d P J 5 C7S C 0.036(2) 0.4257(8) 0.3788(16) 0.085(8) Uani 0.50 1 d PD D 4 H7S1 H -0.0460 0.4347 0.3650 0.127 Uiso 0.50 1 calc PR D 4 H7S2 H 0.0405 0.3912 0.3698 0.127 Uiso 0.50 1 calc PR D 4 H7S3 H 0.0625 0.4420 0.3239 0.127 Uiso 0.50 1 calc PR D 4 C8S C -0.108(4) 0.477(2) 0.430(5) 0.21(2) Uani 0.50 1 d PDU F 3 H8C H -0.0747 0.4648 0.5062 0.315 Uiso 0.50 1 d P K 3 H8D H -0.0904 0.5074 0.4176 0.315 Uiso 0.50 1 d P L 3 H8E H -0.0598 0.4550 0.3873 0.315 Uiso 0.50 1 d P M 3 B1S B -0.1464(12) 0.3062(6) 0.3071(14) 0.077(4) Uani 1 1 d . . . O1W O 0.3384(18) 0.3022(7) 0.5471(18) 0.099(6) Uani 0.50 1 d PU N 11 C12 C -0.2147(9) 0.1554(6) 0.1780(11) 0.092(11) Uani 0.410(19) 1 d PDU A 1 H12A H -0.2156 0.1888 0.2026 0.110 Uiso 0.410(19) 1 calc PRD A 1 H12B H -0.2505 0.1359 0.2220 0.110 Uiso 0.410(19) 1 calc PRD A 1 O13 O -0.413(2) 0.1662(10) 0.028(2) 0.099(9) Uani 0.410(19) 1 d P A 1 H13 H -0.4238 0.1662 0.0899 0.119 Uiso 0.410(19) 1 calc PRD A 1 C13 C -0.299(2) 0.1521(14) 0.0472(16) 0.096(12) Uani 0.410(19) 1 d PD A 1 H13A H -0.2662 0.1725 0.0018 0.115 Uiso 0.410(19) 1 calc PR A 1 H13B H -0.2995 0.1190 0.0208 0.115 Uiso 0.410(19) 1 calc PR A 1 O9S O -0.3362(11) 0.1340(6) 0.1248(13) 0.091(6) Uani 0.590(19) 1 d PDU A 2 H9S H -0.3880 0.1298 0.1527 0.109 Uiso 0.590(19) 1 calc PRD A 2 C9S C -0.394(3) 0.1383(14) -0.0025(15) 0.132(10) Uani 0.590(19) 1 d PDU A 2 H9S1 H -0.4765 0.1486 -0.0230 0.197 Uiso 0.590(19) 1 calc PR A 2 H9S2 H -0.3927 0.1074 -0.0378 0.197 Uiso 0.590(19) 1 calc PR A 2 H9S3 H -0.3514 0.1617 -0.0301 0.197 Uiso 0.590(19) 1 calc PR A 2 N2A N -0.0846(6) 0.1403(3) 0.2135(6) 0.0490(18) Uani 0.590(19) 1 d P A 2 H2A1 H -0.1652 0.1438 0.1974 0.059 Uiso 0.590(19) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0262(5) 0.0558(8) 0.0448(6) -0.0034(5) 0.0124(5) 0.0044(5) Co3 0.0255(5) 0.0472(7) 0.0304(5) 0.0029(4) 0.0062(4) 0.0046(4) Mn1 0.0212(5) 0.0455(7) 0.0210(5) 0.0017(4) 0.0033(4) 0.0075(5) Mn2 0.0199(5) 0.0491(7) 0.0290(6) 0.0019(5) 0.0075(4) 0.0079(5) O1 0.034(3) 0.055(4) 0.027(3) 0.001(2) 0.000(2) 0.004(3) O2 0.024(3) 0.048(3) 0.039(3) 0.002(2) 0.014(2) 0.008(2) O3 0.022(2) 0.043(3) 0.023(2) 0.001(2) 0.0086(19) 0.009(2) O4 0.035(3) 0.057(4) 0.035(3) -0.002(3) 0.002(2) 0.000(3) O5 0.033(3) 0.051(3) 0.023(2) -0.003(2) 0.011(2) 0.006(2) O6 0.030(3) 0.045(3) 0.030(3) -0.003(2) 0.011(2) 0.006(2) O7 0.020(2) 0.039(3) 0.039(3) -0.001(2) 0.007(2) 0.003(2) O8 0.026(3) 0.054(4) 0.058(4) 0.009(3) 0.016(3) 0.011(2) O9 0.030(3) 0.058(4) 0.037(3) 0.006(2) 0.012(2) 0.000(2) O11 0.041(4) 0.103(7) 0.079(5) -0.042(5) 0.026(4) -0.012(4) O12 0.029(3) 0.071(4) 0.065(4) 0.004(3) 0.019(3) -0.003(3) N1 0.030(3) 0.048(4) 0.060(5) -0.001(3) 0.014(3) 0.008(3) N2 0.041(4) 0.063(5) 0.038(4) 0.013(3) 0.008(3) 0.005(3) N3 0.022(3) 0.085(6) 0.064(5) 0.003(4) 0.008(3) -0.002(4) C1 0.042(5) 0.066(6) 0.026(4) 0.004(4) -0.001(3) 0.010(4) C2 0.089(8) 0.095(9) 0.034(5) 0.002(5) -0.019(5) -0.013(7) C3 0.068(6) 0.061(6) 0.050(5) 0.004(4) 0.041(5) 0.018(5) C4 0.026(4) 0.047(6) 0.129(10) -0.006(6) 0.029(5) 0.007(4) C5 0.024(4) 0.050(6) 0.082(7) -0.009(4) 0.021(4) 0.007(4) C6 0.034(4) 0.060(6) 0.058(5) -0.012(4) 0.025(4) 0.006(4) C7 0.033(4) 0.061(6) 0.030(4) -0.008(4) 0.013(3) 0.007(4) C8 0.056(5) 0.074(6) 0.019(4) 0.005(4) 0.012(4) -0.008(5) C9 0.057(5) 0.063(6) 0.024(4) 0.002(4) 0.021(4) -0.001(4) C10 0.046(5) 0.072(7) 0.040(5) 0.022(4) 0.005(4) 0.000(5) C11 0.059(6) 0.057(6) 0.041(5) 0.007(4) 0.017(4) -0.004(5) C14 0.036(5) 0.113(10) 0.077(8) 0.022(7) 0.009(5) 0.020(6) C15 0.034(5) 0.077(8) 0.102(9) 0.025(6) 0.034(5) 0.017(5) C16 0.032(5) 0.099(9) 0.086(8) 0.008(6) 0.028(5) 0.006(5) C17 0.027(4) 0.067(7) 0.106(9) 0.003(6) 0.021(5) -0.004(4) C18 0.036(5) 0.138(12) 0.070(7) -0.017(7) 0.012(5) -0.011(6) C19 0.060(7) 0.173(14) 0.055(7) -0.053(8) 0.020(6) -0.031(8) F1S 0.053(4) 0.095(6) 0.294(14) 0.060(7) -0.008(6) 0.013(4) F2S 0.064(5) 0.076(6) 0.44(2) 0.032(9) 0.005(9) 0.020(5) F3S 0.133(8) 0.181(10) 0.088(6) 0.052(6) 0.003(5) -0.043(7) F4S 0.120(9) 0.49(3) 0.092(8) -0.040(11) 0.034(7) 0.042(12) O1S 0.061(9) 0.105(12) 0.053(8) 0.012(8) 0.032(7) 0.022(8) O2S 0.044(8) 0.150(16) 0.047(8) 0.047(9) 0.009(6) 0.007(8) O3S 0.182(11) 0.182(11) 0.182(11) 0.0001(10) 0.068(4) -0.0001(10) O4S 0.060(9) 0.066(10) 0.079(10) 0.013(7) -0.003(7) -0.015(7) O7S 0.133(17) 0.145(19) 0.100(15) -0.002(13) 0.078(14) -0.028(14) O8S 0.235(18) 0.235(18) 0.223(18) 0.001(10) 0.088(11) 0.002(10) C1S 0.046(8) 0.075(10) 0.056(9) 0.005(7) 0.027(7) 0.005(7) C2S 0.031(8) 0.050(10) 0.034(8) 0.004(7) -0.008(6) -0.013(7) C3S 0.048(4) 0.047(4) 0.047(4) -0.0002(10) 0.0176(18) 0.0005(10) C4S 0.116(10) 0.115(10) 0.115(10) 0.0000(10) 0.043(4) 0.0001(10) C7S 0.105(19) 0.070(16) 0.059(14) 0.010(11) 0.008(13) -0.031(14) C8S 0.22(2) 0.21(2) 0.21(2) 0.016(10) 0.081(13) -0.006(10) B1S 0.056(8) 0.094(11) 0.084(10) 0.038(8) 0.031(7) 0.034(8) O1W 0.086(9) 0.095(9) 0.109(10) -0.003(8) 0.027(7) -0.011(7) C12 0.095(14) 0.093(13) 0.089(13) 0.008(9) 0.036(9) 0.009(9) O13 0.077(15) 0.14(2) 0.078(16) -0.001(14) 0.019(12) 0.027(14) C13 0.024(12) 0.15(3) 0.08(2) 0.02(2) -0.022(13) -0.013(16) O9S 0.036(7) 0.120(13) 0.098(10) 0.033(9) 0.004(7) 0.000(7) C9S 0.136(14) 0.142(14) 0.113(11) 0.008(9) 0.041(9) -0.002(10) N2A 0.041(4) 0.063(5) 0.038(4) 0.013(3) 0.008(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O9 1.993(5) . ? Co1 O8 2.001(6) . ? Co1 O11 2.030(7) . ? Co1 O12 2.065(6) . ? Co1 N3 2.238(7) . ? Co3 O9 1.883(5) . ? Co3 O5 1.902(5) . ? Co3 O7 1.902(5) . ? Co3 O6 1.916(5) . ? Co3 N2 1.943(7) . ? Co3 N1 1.968(7) . ? Co3 Mn2 3.0213(15) . ? Mn1 O3 1.886(5) . ? Mn1 O3 1.901(5) 3_556 ? Mn1 O7 1.941(5) 3_556 ? Mn1 O1 1.959(5) . ? Mn1 O2 2.156(5) . ? Mn1 O5 2.343(5) 3_556 ? Mn1 Mn1 2.867(2) 3_556 ? Mn1 Mn2 2.8792(17) . ? Mn1 Mn2 3.0987(15) 3_556 ? Mn2 O2 1.896(5) . ? Mn2 O8 1.902(5) . ? Mn2 O3 1.919(5) . ? Mn2 O6 1.947(5) . ? Mn2 O4 2.149(5) . ? Mn2 O5 2.240(5) . ? Mn2 Mn1 3.0987(15) 3_556 ? O1 C1 1.283(11) . ? O2 C3 1.433(9) . ? O3 Mn1 1.901(5) 3_556 ? O4 C1 1.239(10) . ? O5 C9 1.425(8) . ? O5 Mn1 2.343(5) 3_556 ? O6 C7 1.439(8) . ? O7 C5 1.418(9) . ? O7 Mn1 1.941(5) 3_556 ? O8 C15 1.429(10) . ? O9 C11 1.425(9) . ? O11 C19 1.440(15) . ? O11 H5 0.77(15) . ? O12 C17 1.442(10) . ? N1 C4 1.489(10) . ? N1 C6 1.493(11) . ? N1 H1 0.9100 . ? N2 C10 1.490(11) . ? N2 C12 1.505(5) . ? N2 C8 1.513(12) . ? N3 C18 1.466(14) . ? N3 C14 1.467(14) . ? N3 C16 1.492(12) . ? C1 C2 1.527(11) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.496(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.505(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.528(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.504(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C14 C15 1.487(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.481(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.496(14) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? F1S B1S 1.337(14) . ? F2S B1S 1.35(2) . ? F3S B1S 1.292(15) . ? F4S B1S 1.293(18) . ? O1S C1S 1.239(9) . ? O2S C1S 1.251(9) . ? O3S C3S 1.237(10) . ? O4S C3S 1.261(9) . ? O7S C7S 1.400(10) . ? O7S H7S 0.8082 . ? O8S C8S 1.480(10) . ? O8S H8S 0.7678 . ? C1S C2S 1.485(9) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S C4S 1.486(4) . ? C4S H4S1 0.8876 . ? C4S H4S2 0.9881 . ? C4S H4S3 0.9262 . ? C7S H7S1 0.9600 . ? C7S H7S2 0.9600 . ? C7S H7S3 0.9600 . ? C8S H8C 0.9437 . ? C8S H8D 0.8839 . ? C8S H8E 1.0973 . ? C12 C13 1.555(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O13 C13 1.35(4) . ? O13 H13 0.8200 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O9S C9S 1.469(10) . ? O9S H9S 0.8200 . ? C9S H9S1 0.9600 . ? C9S H9S2 0.9600 . ? C9S H9S3 0.9600 . ? 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 O9 Co1 O8 104.0(2) . . ? O9 Co1 O11 105.7(3) . . ? O8 Co1 O11 123.2(3) . . ? O9 Co1 O12 93.0(2) . . ? O8 Co1 O12 115.1(2) . . ? O11 Co1 O12 110.4(3) . . ? O9 Co1 N3 172.0(3) . . ? O8 Co1 N3 78.9(3) . . ? O11 Co1 N3 78.2(3) . . ? O12 Co1 N3 79.1(3) . . ? O9 Co3 O5 98.4(2) . . ? O9 Co3 O7 178.2(2) . . ? O5 Co3 O7 82.4(2) . . ? O9 Co3 O6 83.0(2) . . ? O5 Co3 O6 86.5(2) . . ? O7 Co3 O6 98.7(2) . . ? O9 Co3 N2 85.7(3) . . ? O5 Co3 N2 88.4(3) . . ? O7 Co3 N2 92.7(3) . . ? O6 Co3 N2 166.8(3) . . ? O9 Co3 N1 94.9(3) . . ? O5 Co3 N1 164.4(3) . . ? O7 Co3 N1 84.6(3) . . ? O6 Co3 N1 86.9(3) . . ? N2 Co3 N1 100.8(3) . . ? O9 Co3 Mn2 92.42(17) . . ? O5 Co3 Mn2 47.73(14) . . ? O7 Co3 Mn2 89.32(15) . . ? O6 Co3 Mn2 38.91(15) . . ? N2 Co3 Mn2 135.4(2) . . ? N1 Co3 Mn2 123.7(2) . . ? O3 Mn1 O3 81.6(2) . 3_556 ? O3 Mn1 O7 175.6(2) . 3_556 ? O3 Mn1 O7 94.0(2) 3_556 3_556 ? O3 Mn1 O1 91.9(2) . . ? O3 Mn1 O1 170.9(2) 3_556 . ? O7 Mn1 O1 92.4(2) 3_556 . ? O3 Mn1 O2 81.2(2) . . ? O3 Mn1 O2 96.72(19) 3_556 . ? O7 Mn1 O2 99.5(2) 3_556 . ? O1 Mn1 O2 88.5(2) . . ? O3 Mn1 O5 108.23(19) . 3_556 ? O3 Mn1 O5 81.56(18) 3_556 3_556 ? O7 Mn1 O5 70.88(19) 3_556 3_556 ? O1 Mn1 O5 94.5(2) . 3_556 ? O2 Mn1 O5 169.9(2) . 3_556 ? O3 Mn1 Mn1 41.01(14) . 3_556 ? O3 Mn1 Mn1 40.59(15) 3_556 3_556 ? O7 Mn1 Mn1 134.64(15) 3_556 3_556 ? O1 Mn1 Mn1 132.57(18) . 3_556 ? O2 Mn1 Mn1 88.68(14) . 3_556 ? O5 Mn1 Mn1 96.22(13) 3_556 3_556 ? O3 Mn1 Mn2 41.24(14) . . ? O3 Mn1 Mn2 96.60(16) 3_556 . ? O7 Mn1 Mn2 140.14(15) 3_556 . ? O1 Mn1 Mn2 82.41(18) . . ? O2 Mn1 Mn2 41.19(14) . . ? O5 Mn1 Mn2 148.73(13) 3_556 . ? Mn1 Mn1 Mn2 65.27(5) 3_556 . ? O3 Mn1 Mn2 90.03(15) . 3_556 ? O3 Mn1 Mn2 35.97(14) 3_556 3_556 ? O7 Mn1 Mn2 86.38(14) 3_556 3_556 ? O1 Mn1 Mn2 138.46(17) . 3_556 ? O2 Mn1 Mn2 132.67(14) . 3_556 ? O5 Mn1 Mn2 46.06(12) 3_556 3_556 ? Mn1 Mn1 Mn2 57.56(4) 3_556 3_556 ? Mn2 Mn1 Mn2 122.83(4) . 3_556 ? O2 Mn2 O8 95.2(2) . . ? O2 Mn2 O3 87.5(2) . . ? O8 Mn2 O3 175.0(2) . . ? O2 Mn2 O6 173.3(2) . . ? O8 Mn2 O6 87.0(2) . . ? O3 Mn2 O6 89.9(2) . . ? O2 Mn2 O4 90.3(2) . . ? O8 Mn2 O4 96.3(2) . . ? O3 Mn2 O4 87.9(2) . . ? O6 Mn2 O4 95.8(2) . . ? O2 Mn2 O5 96.5(2) . . ? O8 Mn2 O5 91.5(2) . . ? O3 Mn2 O5 83.99(19) . . ? O6 Mn2 O5 77.0(2) . . ? O4 Mn2 O5 169.2(2) . . ? O2 Mn2 Mn1 48.49(15) . . ? O8 Mn2 Mn1 143.08(18) . . ? O3 Mn2 Mn1 40.38(14) . . ? O6 Mn2 Mn1 129.86(16) . . ? O4 Mn2 Mn1 79.97(17) . . ? O5 Mn2 Mn1 98.28(14) . . ? O2 Mn2 Co3 135.25(16) . . ? O8 Mn2 Co3 91.06(17) . . ? O3 Mn2 Co3 84.07(14) . . ? O6 Mn2 Co3 38.19(14) . . ? O4 Mn2 Co3 133.01(17) . . ? O5 Mn2 Co3 38.93(13) . . ? Mn1 Mn2 Co3 118.45(4) . . ? O2 Mn2 Mn1 86.99(15) . 3_556 ? O8 Mn2 Mn1 140.15(18) . 3_556 ? O3 Mn2 Mn1 35.60(13) . 3_556 ? O6 Mn2 Mn1 87.26(15) . 3_556 ? O4 Mn2 Mn1 123.52(16) . 3_556 ? O5 Mn2 Mn1 48.87(13) . 3_556 ? Mn1 Mn2 Mn1 57.17(4) . 3_556 ? Co3 Mn2 Mn1 61.70(3) . 3_556 ? C1 O1 Mn1 128.0(5) . . ? C3 O2 Mn2 120.5(5) . . ? C3 O2 Mn1 125.1(5) . . ? Mn2 O2 Mn1 90.32(19) . . ? Mn1 O3 Mn1 98.4(2) . 3_556 ? Mn1 O3 Mn2 98.4(2) . . ? Mn1 O3 Mn2 108.4(2) 3_556 . ? C1 O4 Mn2 122.6(5) . . ? C9 O5 Co3 108.8(5) . . ? C9 O5 Mn2 138.5(5) . . ? Co3 O5 Mn2 93.3(2) . . ? C9 O5 Mn1 125.7(5) . 3_556 ? Co3 O5 Mn1 94.82(19) . 3_556 ? Mn2 O5 Mn1 85.07(17) . 3_556 ? C7 O6 Co3 109.7(4) . . ? C7 O6 Mn2 128.4(5) . . ? Co3 O6 Mn2 102.9(2) . . ? C5 O7 Co3 115.6(5) . . ? C5 O7 Mn1 127.7(5) . 3_556 ? Co3 O7 Mn1 109.5(2) . 3_556 ? C15 O8 Mn2 122.1(6) . . ? C15 O8 Co1 116.5(6) . . ? Mn2 O8 Co1 111.7(3) . . ? C11 O9 Co3 114.6(5) . . ? C11 O9 Co1 126.3(5) . . ? Co3 O9 Co1 115.0(3) . . ? C19 O11 Co1 111.8(7) . . ? C19 O11 H5 114(10) . . ? Co1 O11 H5 109(10) . . ? C17 O12 Co1 113.5(6) . . ? C4 N1 C6 115.3(7) . . ? C4 N1 Co3 106.2(5) . . ? C6 N1 Co3 107.1(5) . . ? C4 N1 H1 109.4 . . ? C6 N1 H1 109.4 . . ? Co3 N1 H1 109.4 . . ? C10 N2 C12 99.0(9) . . ? C10 N2 C8 113.9(7) . . ? C12 N2 C8 116.0(8) . . ? C10 N2 Co3 105.9(5) . . ? C12 N2 Co3 114.7(7) . . ? C8 N2 Co3 106.9(5) . . ? C18 N3 C14 111.4(10) . . ? C18 N3 C16 111.7(9) . . ? C14 N3 C16 111.5(8) . . ? C18 N3 Co1 109.0(6) . . ? C14 N3 Co1 105.6(6) . . ? C16 N3 Co1 107.3(6) . . ? O4 C1 O1 126.9(7) . . ? O4 C1 C2 118.3(9) . . ? O1 C1 C2 114.8(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 109.1(7) . . ? N1 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? N1 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O7 C5 C4 106.1(7) . . ? O7 C5 H5A 110.5 . . ? C4 C5 H5A 110.5 . . ? O7 C5 H5B 110.5 . . ? C4 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? N1 C6 C7 110.2(7) . . ? N1 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O6 C7 C6 106.3(6) . . ? O6 C7 H7A 110.5 . . ? C6 C7 H7A 110.5 . . ? O6 C7 H7B 110.5 . . ? C6 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? N2 C8 C9 110.5(6) . . ? N2 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O5 C9 C8 107.0(6) . . ? O5 C9 H9A 110.3 . . ? C8 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C8 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 107.5(7) . . ? N2 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? N2 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O9 C11 C10 107.6(7) . . ? O9 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? O9 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N3 C14 C15 110.8(9) . . ? N3 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O8 C15 C14 107.2(9) . . ? O8 C15 H15A 110.3 . . ? C14 C15 H15A 110.3 . . ? O8 C15 H15B 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C17 C16 N3 109.0(8) . . ? C17 C16 H16A 109.9 . . ? N3 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? N3 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O12 C17 C16 110.3(8) . . ? O12 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? O12 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N3 C18 C19 107.4(8) . . ? N3 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? N3 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? O11 C19 C18 108.5(9) . . ? O11 C19 H19A 110.0 . . ? C18 C19 H19A 110.0 . . ? O11 C19 H19B 110.0 . . ? C18 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C7S O7S H7S 107.6 . . ? C8S O8S H8S 116.7 . . ? O1S C1S O2S 147.2(13) . . ? O1S C1S C2S 104.1(8) . . ? O2S C1S C2S 107.2(9) . . ? C1S C2S H4S1 103.7 . . ? H2S2 C2S H4S1 102.7 . . ? H2S3 C2S H4S1 121.5 . . ? O3S C3S O4S 145(2) . . ? O3S C3S C4S 105.8(9) . . ? O4S C3S C4S 102.9(17) . . ? C3S C4S H4S1 104.5 . . ? C3S C4S H4S2 101.6 . . ? H4S1 C4S H4S2 113.3 . . ? C3S C4S H4S3 105.8 . . ? H4S1 C4S H4S3 119.6 . . ? H4S2 C4S H4S3 109.9 . . ? O7S C7S H8E 90.2 . . ? H7S2 C7S H8E 130.3 . . ? H7S3 C7S H8E 105.5 . . ? O8S C8S H8C 111.2 . . ? O8S C8S H8D 115.8 . . ? H8C C8S H8D 118.1 . . ? O8S C8S H8E 104.9 . . ? H8C C8S H8E 100.1 . . ? H8D C8S H8E 104.1 . . ? F3S B1S F4S 107.7(15) . . ? F3S B1S F1S 111.6(12) . . ? F4S B1S F1S 115.4(15) . . ? F3S B1S F2S 107.9(15) . . ? F4S B1S F2S 105.5(14) . . ? F1S B1S F2S 108.3(13) . . ? N2 C12 C13 118.8(13) . . ? N2 C12 H12A 107.6 . . ? C13 C12 H12A 107.6 . . ? N2 C12 H12B 107.6 . . ? C13 C12 H12B 107.6 . . ? H12A C12 H12B 107.1 . . ? O13 C13 C12 113(2) . . ? O13 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? O13 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C9S O9S H9S 109.5 . . ? O9S C9S H9S1 109.5 . . ? O9S C9S H9S2 109.5 . . ? H9S1 C9S H9S2 109.5 . . ? O9S C9S H9S3 109.5 . . ? H9S1 C9S H9S3 109.5 . . ? H9S2 C9S H9S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.310 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.139 # Attachment '- 2 Mn4Co2finalSept29.CIF' #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 838819' #TrackingRef '- 2 Mn4Co2finalSept29.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _publ_section_exptl_refinement ; The crystal was run on the Australian synchrotron in which We were restricted to a 360 degree phi scan. With just two possible space groups to choose from, P-1 was choosen to be the most likely space group from the statistics observed, followed by confirmation via ADDSYM analysis through platon. The structure was solved by direct methods. The asymmetric unit contains one half of the cluster as well as one molecule of MeOH and one nitrate ion. H atoms were included in calculated positions, except for some of the protonated hydroxyl arms of the tea ligands, which were found. All non-H atoms were refined anisotropically. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H86 Co2 Mn4 N4 O22, 2(C H4 O), 2(N O3)' _chemical_formula_sum 'C48 H94 Co2 Mn4 N6 O30' _chemical_formula_weight 1572.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4100(19) _cell_length_b 12.940(3) _cell_length_c 14.520(3) _cell_angle_alpha 101.81(3) _cell_angle_beta 104.55(3) _cell_angle_gamma 104.57(3) _cell_volume 1587.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16351 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 24.03 _exptl_crystal_description plate _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9345 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71054 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16351 _diffrn_reflns_av_R_equivalents 0.1267 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 24.03 _reflns_number_total 4594 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which We were restricted to a 360 degree phi scan. With just two possible space groups to choose from, P-1 was choosen to be the most likely space group from the statistics observed, followed by confirmation via ADDSYM analysis through platon. The structure was solved by direct methods. The asymmetric unit contains one half of the cluster as well as one molecule of MeOH and one nitrate ion. H atoms were included in calculated positions, except for some of the protonated hydroxyl arms of the tea ligands, which were found. All non-H atoms were refined anisotropically. ; _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^)+(0.0826P)^2^+2.3129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.170(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4594 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24922(5) 0.67042(4) 0.30160(3) 0.0083(2) Uani 1 1 d . . . Mn1 Mn 0.08221(6) 0.46061(4) 0.10920(4) 0.0089(3) Uani 1 1 d . . . Mn2 Mn 0.04016(6) 0.70907(4) 0.11552(4) 0.0070(3) Uani 1 1 d . . . O1 O -0.1152(3) 0.3881(2) -0.03592(19) 0.0099(6) Uani 1 1 d . . . O2 O 0.1310(3) 0.3336(2) 0.1856(2) 0.0210(7) Uani 1 1 d . . . O3 O 0.0420(3) 0.5938(2) 0.2155(2) 0.0108(6) Uani 1 1 d . . . O4 O 0.1478(3) 0.3739(2) -0.01240(19) 0.0131(6) Uani 1 1 d . . . O5 O 0.3041(3) 0.5738(2) 0.21224(19) 0.0116(6) Uani 1 1 d . . . O6 O 0.2403(3) 0.7672(2) 0.22085(18) 0.0099(6) Uani 1 1 d . . . O7 O 0.7641(3) 0.7870(2) 0.5563(2) 0.0273(7) Uani 1 1 d . . . H7 H 0.7224 0.7625 0.5957 0.033 Uiso 1 1 calc R . . O8 O -0.0585(3) 0.7881(2) 0.19134(19) 0.0130(6) Uani 1 1 d . . . O9 O 0.1049(3) 0.8518(2) 0.06307(19) 0.0141(6) Uani 1 1 d . . . O10 O 0.1879(3) 0.7670(2) 0.3905(2) 0.0121(6) Uani 1 1 d . . . O11 O 0.2557(3) 0.5684(2) 0.37833(19) 0.0145(6) Uani 1 1 d . . . N1 N -0.1489(3) 0.3784(2) 0.1490(2) 0.0132(7) Uani 1 1 d . . . N2 N 0.4739(3) 0.7540(2) 0.3612(2) 0.0113(7) Uani 1 1 d . . . C1 C -0.2678(4) 0.3493(3) -0.0289(3) 0.0123(8) Uani 1 1 d . . . H1A H -0.3371 0.2928 -0.0917 0.015 Uiso 1 1 calc R . . H1B H -0.3094 0.4124 -0.0189 0.015 Uiso 1 1 calc R . . C2 C -0.2653(4) 0.2989(3) 0.0563(3) 0.0156(8) Uani 1 1 d . . . H2A H -0.3690 0.2806 0.0648 0.019 Uiso 1 1 calc R . . H2B H -0.2393 0.2291 0.0417 0.019 Uiso 1 1 calc R . . C3 C 0.0041(4) 0.2595(3) 0.2026(3) 0.0182(9) Uani 1 1 d . . . H3A H 0.0441 0.2320 0.2594 0.022 Uiso 1 1 calc R . . H3B H -0.0513 0.1946 0.1432 0.022 Uiso 1 1 calc R . . C4 C -0.1063(5) 0.3215(3) 0.2247(3) 0.0180(8) Uani 1 1 d . . . H4A H -0.2010 0.2682 0.2264 0.022 Uiso 1 1 calc R . . H4B H -0.0565 0.3771 0.2908 0.022 Uiso 1 1 calc R . . C5 C -0.2094(4) 0.4678(3) 0.1861(3) 0.0138(8) Uani 1 1 d . . . H5A H -0.2843 0.4399 0.2196 0.017 Uiso 1 1 calc R . . H5B H -0.2643 0.4900 0.1296 0.017 Uiso 1 1 calc R . . C6 C -0.0781(4) 0.5679(3) 0.2584(3) 0.0126(8) Uani 1 1 d . . . H6A H -0.1158 0.6324 0.2727 0.015 Uiso 1 1 calc R . . H6B H -0.0380 0.5512 0.3216 0.015 Uiso 1 1 calc R . . C7 C 0.2846(4) 0.3420(3) 0.0022(3) 0.0194(9) Uani 1 1 d . . . H7A H 0.2628 0.2682 0.0131 0.029 Uiso 1 1 calc R . . H7B H 0.3670 0.3964 0.0602 0.029 Uiso 1 1 calc R . . H7C H 0.3179 0.3397 -0.0567 0.029 Uiso 1 1 calc R . . C8 C 0.4641(4) 0.5884(3) 0.2389(3) 0.0183(9) Uani 1 1 d . . . H8A H 0.5076 0.6204 0.1918 0.022 Uiso 1 1 calc R . . H8B H 0.4804 0.5151 0.2350 0.022 Uiso 1 1 calc R . . C9 C 0.5474(4) 0.6653(3) 0.3437(3) 0.0206(9) Uani 1 1 d . . . H9A H 0.5405 0.6222 0.3924 0.025 Uiso 1 1 calc R . . H9B H 0.6582 0.6995 0.3521 0.025 Uiso 1 1 calc R . . C10 C 0.5079(4) 0.8366(3) 0.3032(3) 0.0196(9) Uani 1 1 d . . . H10A H 0.5950 0.9037 0.3463 0.024 Uiso 1 1 calc R . . H10B H 0.5376 0.8029 0.2463 0.024 Uiso 1 1 calc R . . C11 C 0.3647(4) 0.8681(3) 0.2664(3) 0.0159(8) Uani 1 1 d . . . H11A H 0.3459 0.9146 0.3225 0.019 Uiso 1 1 calc R . . H11B H 0.3767 0.9107 0.2180 0.019 Uiso 1 1 calc R . . C12 C 0.5231(5) 0.8162(3) 0.4700(3) 0.0204(9) Uani 1 1 d . . . H12A H 0.4770 0.7649 0.5045 0.024 Uiso 1 1 calc R . . H12B H 0.4786 0.8780 0.4763 0.024 Uiso 1 1 calc R . . C13 C 0.6974(4) 0.8648(4) 0.5241(3) 0.0218(9) Uani 1 1 d . . . H13A H 0.7493 0.8946 0.4792 0.026 Uiso 1 1 calc R . . H13B H 0.7169 0.9279 0.5825 0.026 Uiso 1 1 calc R . . C14 C 0.1927(5) 1.0432(3) 0.0748(3) 0.0198(9) Uani 1 1 d . . . H14A H 0.3056 1.0635 0.1021 0.030 Uiso 1 1 calc R . . H14B H 0.1603 1.1076 0.0972 0.030 Uiso 1 1 calc R . . H14C H 0.1612 1.0201 0.0021 0.030 Uiso 1 1 calc R . . C15 C 0.1181(4) 0.9495(3) 0.1098(3) 0.0144(8) Uani 1 1 d . . . C16 C 0.0655(4) 0.9738(3) 0.1930(3) 0.0167(8) Uani 1 1 d . . . H16 H 0.0912 1.0500 0.2281 0.020 Uiso 1 1 calc R . . C17 C -0.0198(4) 0.8955(3) 0.2267(3) 0.0138(8) Uani 1 1 d . . . C18 C -0.0814(4) 0.9340(3) 0.3086(3) 0.0195(9) Uani 1 1 d . . . H18A H -0.1858 0.9370 0.2800 0.029 Uiso 1 1 calc R . . H18B H -0.0131 1.0083 0.3504 0.029 Uiso 1 1 calc R . . H18C H -0.0855 0.8818 0.3489 0.029 Uiso 1 1 calc R . . C19 C 0.1194(5) 0.8403(3) 0.5294(3) 0.0209(9) Uani 1 1 d . . . H19A H 0.1275 0.9031 0.5009 0.031 Uiso 1 1 calc R . . H19B H 0.1876 0.8664 0.5985 0.031 Uiso 1 1 calc R . . H19C H 0.0120 0.8084 0.5273 0.031 Uiso 1 1 calc R . . C20 C 0.1669(4) 0.7528(3) 0.4706(3) 0.0128(8) Uani 1 1 d . . . C21 C 0.1855(4) 0.6637(3) 0.5089(3) 0.0179(8) Uani 1 1 d . . . H21 H 0.1664 0.6618 0.5698 0.022 Uiso 1 1 calc R . . C22 C 0.2303(4) 0.5784(3) 0.4619(3) 0.0160(8) Uani 1 1 d . . . C23 C 0.2527(5) 0.4886(4) 0.5102(3) 0.0270(10) Uani 1 1 d . . . H23A H 0.1918 0.4154 0.4629 0.040 Uiso 1 1 calc R . . H23B H 0.2183 0.4975 0.5688 0.040 Uiso 1 1 calc R . . H23C H 0.3627 0.4946 0.5303 0.040 Uiso 1 1 calc R . . H2 H 0.209(6) 0.347(4) 0.237(4) 0.032 Uiso 1 1 d . . . O1S O 0.3780(4) 0.3116(3) 0.3227(3) 0.0369(8) Uani 1 1 d . . . O2S O 0.4557(4) 0.1658(3) 0.3036(2) 0.0329(8) Uani 1 1 d . . . O3S O 0.5050(4) 0.2817(3) 0.2190(3) 0.0455(10) Uani 1 1 d . . . O4S O 0.6489(4) 0.0588(3) 0.2333(3) 0.0340(8) Uani 1 1 d . . . H4S H 0.5861 0.0915 0.2452 0.041 Uiso 1 1 calc R . . N1S N 0.4470(4) 0.2534(3) 0.2815(3) 0.0275(9) Uani 1 1 d . . . C1S C 0.6092(6) 0.0127(5) 0.1299(4) 0.0381(12) Uani 1 1 d . . . H1S1 H 0.6012 0.0708 0.0967 0.057 Uiso 1 1 calc R . . H1S2 H 0.5094 -0.0471 0.1055 0.057 Uiso 1 1 calc R . . H1S3 H 0.6892 -0.0177 0.1155 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0096(3) 0.0082(4) 0.0090(4) 0.0027(2) 0.0047(2) 0.0040(2) Mn1 0.0123(4) 0.0070(4) 0.0086(4) 0.0011(3) 0.0046(2) 0.0048(2) Mn2 0.0092(4) 0.0061(4) 0.0067(4) 0.0002(3) 0.0037(2) 0.0041(2) O1 0.0128(13) 0.0088(12) 0.0102(13) 0.0022(11) 0.0070(10) 0.0042(10) O2 0.0164(14) 0.0238(15) 0.0263(16) 0.0129(13) 0.0062(12) 0.0082(12) O3 0.0085(12) 0.0118(13) 0.0140(14) 0.0046(11) 0.0070(10) 0.0026(10) O4 0.0101(13) 0.0137(13) 0.0138(14) -0.0004(11) 0.0008(10) 0.0073(10) O5 0.0093(13) 0.0130(13) 0.0142(14) 0.0017(11) 0.0059(10) 0.0062(10) O6 0.0113(12) 0.0081(12) 0.0095(13) 0.0025(10) 0.0034(10) 0.0016(10) O7 0.0205(15) 0.0295(17) 0.0338(18) 0.0111(14) 0.0078(13) 0.0105(13) O8 0.0168(13) 0.0130(14) 0.0139(13) 0.0031(11) 0.0083(11) 0.0100(11) O9 0.0195(14) 0.0137(14) 0.0124(13) 0.0040(11) 0.0070(11) 0.0086(11) O10 0.0116(13) 0.0113(13) 0.0148(15) 0.0014(11) 0.0067(11) 0.0052(10) O11 0.0164(14) 0.0139(13) 0.0141(14) 0.0027(11) 0.0051(11) 0.0070(11) N1 0.0156(16) 0.0119(15) 0.0134(16) 0.0032(13) 0.0065(13) 0.0053(13) N2 0.0133(15) 0.0128(15) 0.0110(16) 0.0062(13) 0.0057(12) 0.0058(13) C1 0.0094(17) 0.0160(18) 0.0123(19) 0.0030(16) 0.0071(14) 0.0024(15) C2 0.0141(18) 0.0149(19) 0.016(2) 0.0022(16) 0.0069(15) 0.0017(15) C3 0.023(2) 0.0126(19) 0.022(2) 0.0084(17) 0.0078(17) 0.0068(16) C4 0.025(2) 0.0165(19) 0.016(2) 0.0067(16) 0.0099(16) 0.0071(16) C5 0.0152(18) 0.0141(18) 0.016(2) 0.0048(16) 0.0102(15) 0.0057(15) C6 0.0135(18) 0.0139(18) 0.0146(19) 0.0043(16) 0.0098(15) 0.0058(15) C7 0.0174(19) 0.024(2) 0.021(2) 0.0032(18) 0.0071(16) 0.0154(17) C8 0.0119(19) 0.022(2) 0.022(2) 0.0015(18) 0.0056(16) 0.0108(16) C9 0.016(2) 0.018(2) 0.025(2) 0.0003(18) 0.0043(17) 0.0076(16) C10 0.018(2) 0.019(2) 0.023(2) 0.0105(17) 0.0081(17) 0.0027(16) C11 0.0166(19) 0.0125(19) 0.017(2) 0.0057(16) 0.0041(16) 0.0027(15) C12 0.019(2) 0.022(2) 0.018(2) 0.0007(18) 0.0059(17) 0.0073(17) C13 0.015(2) 0.026(2) 0.018(2) 0.0019(18) 0.0022(16) 0.0030(17) C14 0.023(2) 0.0143(19) 0.022(2) 0.0070(17) 0.0064(17) 0.0058(16) C15 0.0127(18) 0.0152(19) 0.0122(19) 0.0031(16) -0.0018(14) 0.0055(15) C16 0.0187(19) 0.0091(18) 0.023(2) 0.0032(16) 0.0065(16) 0.0068(15) C17 0.0117(18) 0.0130(19) 0.016(2) -0.0005(16) 0.0013(15) 0.0090(15) C18 0.0185(19) 0.017(2) 0.022(2) -0.0005(17) 0.0080(16) 0.0072(16) C19 0.026(2) 0.023(2) 0.015(2) 0.0002(17) 0.0104(17) 0.0107(17) C20 0.0073(17) 0.0160(19) 0.0102(19) -0.0005(16) 0.0022(14) -0.0005(14) C21 0.020(2) 0.025(2) 0.0113(19) 0.0067(17) 0.0088(16) 0.0051(16) C22 0.0122(18) 0.020(2) 0.015(2) 0.0054(17) 0.0031(15) 0.0029(15) C23 0.037(2) 0.030(2) 0.025(2) 0.020(2) 0.015(2) 0.015(2) O1S 0.0339(18) 0.045(2) 0.045(2) 0.0190(17) 0.0187(16) 0.0240(16) O2S 0.0395(19) 0.0343(18) 0.0261(17) 0.0101(15) 0.0092(14) 0.0139(15) O3S 0.046(2) 0.052(2) 0.053(2) 0.029(2) 0.0328(19) 0.0111(18) O4S 0.0306(18) 0.0356(19) 0.0376(19) 0.0150(16) 0.0090(15) 0.0120(15) N1S 0.0181(18) 0.033(2) 0.027(2) 0.0077(18) 0.0044(16) 0.0040(16) C1S 0.041(3) 0.048(3) 0.033(3) 0.017(3) 0.020(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 1.874(2) . ? Co1 O6 1.885(3) . ? Co1 O11 1.897(3) . ? Co1 O10 1.908(2) . ? Co1 O3 1.909(3) . ? Co1 N2 1.984(3) . ? Mn1 O5 2.176(3) . ? Mn1 O4 2.201(3) . ? Mn1 O2 2.239(3) . ? Mn1 O3 2.242(3) . ? Mn1 O1 2.262(3) . ? Mn1 O1 2.402(3) 2_565 ? Mn1 N1 2.431(3) . ? Mn2 O4 1.892(3) 2_565 ? Mn2 O8 1.910(2) . ? Mn2 O1 1.918(2) 2_565 ? Mn2 O6 1.955(3) . ? Mn2 O9 2.146(3) . ? Mn2 O3 2.284(3) . ? O1 C1 1.434(4) . ? O1 Mn2 1.918(2) 2_565 ? O1 Mn1 2.402(3) 2_565 ? O2 C3 1.440(5) . ? O2 H2 0.86(6) . ? O3 C6 1.424(4) . ? O4 C7 1.427(4) . ? O4 Mn2 1.892(3) 2_565 ? O5 C8 1.409(4) . ? O6 C11 1.415(5) . ? O7 C13 1.410(5) . ? O7 H7 0.8400 . ? O8 C17 1.299(5) . ? O9 C15 1.266(5) . ? O10 C20 1.268(5) . ? O11 C22 1.282(5) . ? N1 C4 1.473(5) . ? N1 C5 1.477(5) . ? N1 C2 1.481(5) . ? N2 C9 1.493(5) . ? N2 C10 1.510(5) . ? N2 C12 1.512(5) . ? C1 C2 1.510(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.519(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.519(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.507(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.528(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.491(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.424(6) . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C18 1.498(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.505(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.408(6) . ? C21 C22 1.389(6) . ? C21 H21 0.9500 . ? C22 C23 1.506(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O1S N1S 1.267(5) . ? O2S N1S 1.256(5) . ? O3S N1S 1.241(5) . ? O4S C1S 1.411(6) . ? O4S H4S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O6 91.94(11) . . ? O5 Co1 O11 86.17(11) . . ? O6 Co1 O11 177.78(10) . . ? O5 Co1 O10 178.51(10) . . ? O6 Co1 O10 87.86(11) . . ? O11 Co1 O10 94.00(12) . . ? O5 Co1 O3 84.96(11) . . ? O6 Co1 O3 82.59(11) . . ? O11 Co1 O3 96.07(12) . . ? O10 Co1 O3 93.55(11) . . ? O5 Co1 N2 86.49(12) . . ? O6 Co1 N2 86.96(12) . . ? O11 Co1 N2 94.09(12) . . ? O10 Co1 N2 94.98(12) . . ? O3 Co1 N2 166.24(13) . . ? O5 Mn1 O4 102.87(10) . . ? O5 Mn1 O2 86.20(11) . . ? O4 Mn1 O2 87.13(10) . . ? O5 Mn1 O3 70.62(10) . . ? O4 Mn1 O3 162.14(10) . . ? O2 Mn1 O3 108.52(11) . . ? O5 Mn1 O1 156.20(10) . . ? O4 Mn1 O1 67.23(9) . . ? O2 Mn1 O1 113.80(11) . . ? O3 Mn1 O1 111.88(10) . . ? O5 Mn1 O1 79.63(10) . 2_565 ? O4 Mn1 O1 85.42(9) . 2_565 ? O2 Mn1 O1 162.09(10) . 2_565 ? O3 Mn1 O1 77.11(9) . 2_565 ? O1 Mn1 O1 78.06(10) . 2_565 ? O5 Mn1 N1 127.30(10) . . ? O4 Mn1 N1 123.12(10) . . ? O2 Mn1 N1 73.04(10) . . ? O3 Mn1 N1 71.25(10) . . ? O1 Mn1 N1 73.30(10) . . ? O1 Mn1 N1 124.46(10) 2_565 . ? O4 Mn2 O8 93.24(11) 2_565 . ? O4 Mn2 O1 80.88(11) 2_565 2_565 ? O8 Mn2 O1 172.09(11) . 2_565 ? O4 Mn2 O6 169.07(11) 2_565 . ? O8 Mn2 O6 93.96(11) . . ? O1 Mn2 O6 91.14(11) 2_565 . ? O4 Mn2 O9 99.12(11) 2_565 . ? O8 Mn2 O9 87.80(11) . . ? O1 Mn2 O9 98.31(11) 2_565 . ? O6 Mn2 O9 89.37(10) . . ? O4 Mn2 O3 99.98(11) 2_565 . ? O8 Mn2 O3 89.09(11) . . ? O1 Mn2 O3 86.73(10) 2_565 . ? O6 Mn2 O3 71.94(10) . . ? O9 Mn2 O3 160.79(10) . . ? C1 O1 Mn2 120.5(2) . 2_565 ? C1 O1 Mn1 116.4(2) . . ? Mn2 O1 Mn1 102.68(11) 2_565 . ? C1 O1 Mn1 112.7(2) . 2_565 ? Mn2 O1 Mn1 99.92(11) 2_565 2_565 ? Mn1 O1 Mn1 101.94(10) . 2_565 ? C3 O2 Mn1 118.2(2) . . ? C3 O2 H2 105(4) . . ? Mn1 O2 H2 124(4) . . ? C6 O3 Co1 118.6(2) . . ? C6 O3 Mn1 121.2(2) . . ? Co1 O3 Mn1 100.21(11) . . ? C6 O3 Mn2 120.7(2) . . ? Co1 O3 Mn2 96.18(11) . . ? Mn1 O3 Mn2 94.45(10) . . ? C7 O4 Mn2 123.5(2) . 2_565 ? C7 O4 Mn1 123.8(2) . . ? Mn2 O4 Mn1 105.87(12) 2_565 . ? C8 O5 Co1 114.1(2) . . ? C8 O5 Mn1 141.6(2) . . ? Co1 O5 Mn1 103.76(11) . . ? C11 O6 Co1 110.2(2) . . ? C11 O6 Mn2 139.0(2) . . ? Co1 O6 Mn2 109.19(12) . . ? C13 O7 H7 109.5 . . ? C17 O8 Mn2 126.6(2) . . ? C15 O9 Mn2 123.6(2) . . ? C20 O10 Co1 125.5(2) . . ? C22 O11 Co1 126.1(2) . . ? C4 N1 C5 111.1(3) . . ? C4 N1 C2 111.3(3) . . ? C5 N1 C2 109.6(3) . . ? C4 N1 Mn1 108.2(2) . . ? C5 N1 Mn1 108.8(2) . . ? C2 N1 Mn1 107.7(2) . . ? C9 N2 C10 112.5(3) . . ? C9 N2 C12 112.0(3) . . ? C10 N2 C12 109.1(3) . . ? C9 N2 Co1 103.0(2) . . ? C10 N2 Co1 105.9(2) . . ? C12 N2 Co1 114.2(2) . . ? O1 C1 C2 110.9(3) . . ? O1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C1 109.9(3) . . ? N1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 109.3(3) . . ? O2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N1 C4 C3 111.1(3) . . ? N1 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 110.4(3) . . ? N1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O3 C6 C5 108.7(3) . . ? O3 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O3 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O4 C7 H7A 109.5 . . ? O4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 C9 110.6(3) . . ? O5 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? O5 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N2 C9 C8 109.0(3) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 N2 108.7(3) . . ? C11 C10 H10A 110.0 . . ? N2 C10 H10A 110.0 . . ? C11 C10 H10B 110.0 . . ? N2 C10 H10B 110.0 . . ? H10A C10 H10B 108.3 . . ? O6 C11 C10 106.5(3) . . ? O6 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? O6 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? N2 C12 C13 116.4(3) . . ? N2 C12 H12A 108.2 . . ? C13 C12 H12A 108.2 . . ? N2 C12 H12B 108.2 . . ? C13 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? O7 C13 C12 113.7(3) . . ? O7 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? O7 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O9 C15 C16 123.4(4) . . ? O9 C15 C14 117.6(3) . . ? C16 C15 C14 119.0(3) . . ? C17 C16 C15 125.2(3) . . ? C17 C16 H16 117.4 . . ? C15 C16 H16 117.4 . . ? O8 C17 C16 125.8(3) . . ? O8 C17 C18 115.1(3) . . ? C16 C17 C18 119.0(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O10 C20 C21 125.9(3) . . ? O10 C20 C19 116.3(3) . . ? C21 C20 C19 117.9(4) . . ? C22 C21 C20 123.3(4) . . ? C22 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? O11 C22 C21 125.3(4) . . ? O11 C22 C23 115.1(3) . . ? C21 C22 C23 119.6(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1S O4S H4S 109.5 . . ? O3S N1S O2S 119.8(4) . . ? O3S N1S O1S 120.6(4) . . ? O2S N1S O1S 119.6(4) . . ? O4S C1S H1S1 109.5 . . ? O4S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O4S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O1S 0.84 1.95 2.782(5) 173.3 2_666 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 24.03 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.817 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.140 # Attachment '- 3_Mn2Ni4final.CIF' #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 838820' #TrackingRef '- 3_Mn2Ni4final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H80 Mn2 N6 Ni4 O28' _chemical_formula_weight 1486.01 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2228(3) _cell_length_b 10.7616(4) _cell_length_c 14.1200(4) _cell_angle_alpha 95.028(2) _cell_angle_beta 108.896(2) _cell_angle_gamma 90.062(2) _cell_volume 1463.31(8) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 30.1 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 6550 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6550 _reflns_number_gt 5577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The structure was solved by patterson methods. The asymmetric unit contains one half of the cluster as well a molecule of MeCN. The oxygen atoms attached to C30 on one of the "free" teaH arms are disordered over three sites. These oxygen atoms are refined freely on three seperate free variables using the SUMP command, with their bond lengths being restrained using the DFIX command. All H atoms were placed in calculated positions, except for the hydrogen atoms found on the protonated teaH2 arms, which were found. All non-H atoms were refined anisotropically. ; _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^)+(0.0407P)^2^+19.6588P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6550 _refine_ls_number_parameters 409 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.60886(8) 0.42594(7) 0.57933(6) 0.01631(19) Uani 1 1 d . . . Ni2 Ni 0.72909(8) 0.80762(7) 0.84209(6) 0.01774(19) Uani 1 1 d . . . Mn1 Mn 0.67999(9) 0.70344(8) 0.61986(6) 0.0142(2) Uani 1 1 d . . . O1 O 0.4941(4) 0.3993(4) 0.4237(3) 0.0147(8) Uani 1 1 d . . . O2 O 0.7383(5) 0.4300(4) 0.7288(3) 0.0230(9) Uani 1 1 d . . . O4 O 0.7313(4) 0.5597(4) 0.5552(3) 0.0164(8) Uani 1 1 d . . . O5 O 0.7261(4) 0.6309(4) 0.7710(3) 0.0200(9) Uani 1 1 d . . . O6 O 0.6372(5) 0.8113(4) 0.4927(3) 0.0259(10) Uani 1 1 d . . . O7 O 0.5163(5) 0.6734(4) 0.3676(3) 0.0241(10) Uani 1 1 d . . . O8 O 0.8696(4) 0.7710(4) 0.6607(3) 0.0218(9) Uani 1 1 d . . . O9 O 0.9129(5) 0.8483(4) 0.8217(3) 0.0233(10) Uani 1 1 d . . . O10 O 0.6185(4) 0.8295(4) 0.6948(3) 0.0172(8) Uani 1 1 d . . . O11 O 0.5452(5) 0.7774(5) 0.8703(4) 0.0234(10) Uani 1 1 d . . . O12 O 0.8394(5) 0.7852(5) 0.9872(3) 0.0263(10) Uani 1 1 d . . . O13 O 0.6744(6) 0.7720(7) 1.0579(4) 0.0447(15) Uani 1 1 d . . . O14 O 0.7022(8) 1.2388(7) 1.0060(6) 0.063(2) Uani 1 1 d . . . H14 H 0.6241 1.2112 0.9685 0.076 Uiso 1 1 calc R . . N1 N 0.7506(5) 0.3090(5) 0.5355(4) 0.0172(10) Uani 1 1 d . . . N2 N 0.6889(6) 0.9983(5) 0.8621(4) 0.0225(11) Uani 1 1 d . . . C1 C 0.5960(6) 0.3803(6) 0.3738(4) 0.0181(12) Uani 1 1 d . . . H1A H 0.6468 0.4599 0.3774 0.022 Uiso 1 1 calc R . . H1B H 0.5500 0.3513 0.3020 0.022 Uiso 1 1 calc R . . C3 C 0.6956(6) 0.2842(6) 0.4242(5) 0.0215(13) Uani 1 1 d . . . H3A H 0.6480 0.2010 0.4069 0.026 Uiso 1 1 calc R . . H3B H 0.7740 0.2816 0.3975 0.026 Uiso 1 1 calc R . . C10 C 0.8813(6) 0.3869(6) 0.5696(5) 0.0209(13) Uani 1 1 d . . . H10A H 0.9473 0.3493 0.5381 0.025 Uiso 1 1 calc R . . H10B H 0.9236 0.3871 0.6434 0.025 Uiso 1 1 calc R . . C11 C 0.9460(6) 0.8225(6) 0.7452(5) 0.0196(12) Uani 1 1 d . . . C12 C 0.8566(6) 0.5206(6) 0.5427(5) 0.0200(12) Uani 1 1 d . . . H12A H 0.9339 0.5759 0.5866 0.024 Uiso 1 1 calc R . . H12B H 0.8523 0.5256 0.4721 0.024 Uiso 1 1 calc R . . C14 C 0.7728(7) 0.5232(6) 0.7905(5) 0.0212(13) Uani 1 1 d . . . C16 C 0.6090(7) 0.7582(6) 0.4052(5) 0.0216(13) Uani 1 1 d . . . C17 C 0.5591(7) 1.0050(7) 0.8886(5) 0.0257(14) Uani 1 1 d . . . H17A H 0.5071 1.0782 0.8603 0.031 Uiso 1 1 calc R . . H17B H 0.5831 1.0172 0.9626 0.031 Uiso 1 1 calc R . . C19 C 0.7681(7) 0.1928(6) 0.5847(6) 0.0281(15) Uani 1 1 d . A . H19A H 0.6767 0.1489 0.5638 0.034 Uiso 1 1 calc R . . H19B H 0.7950 0.2154 0.6581 0.034 Uiso 1 1 calc R . . C20 C 0.4668(7) 0.8875(7) 0.8490(5) 0.0259(14) Uani 1 1 d . . . H20A H 0.3933 0.8879 0.8806 0.031 Uiso 1 1 calc R . . H20B H 0.4218 0.8872 0.7754 0.031 Uiso 1 1 calc R . . C22 C 0.6767(8) 1.0441(6) 0.7638(5) 0.0278(14) Uani 1 1 d . . . H22A H 0.7703 1.0555 0.7589 0.033 Uiso 1 1 calc R . . H22B H 0.6330 1.1264 0.7595 0.033 Uiso 1 1 calc R . . C23 C 0.7976(7) 0.7764(7) 1.0616(5) 0.0271(14) Uani 1 1 d . . . C24 C 0.8070(8) 1.0650(7) 0.9429(6) 0.0304(15) Uani 1 1 d . . . H24A H 0.8928 1.0455 0.9272 0.036 Uiso 1 1 calc R . . H24B H 0.8150 1.0296 1.0068 0.036 Uiso 1 1 calc R . . C25 C 0.5912(7) 0.9542(6) 0.6759(5) 0.0227(13) Uani 1 1 d . . . H25A H 0.4916 0.9685 0.6636 0.027 Uiso 1 1 calc R . . H25B H 0.6125 0.9710 0.6145 0.027 Uiso 1 1 calc R . . C26 C 1.0919(7) 0.8561(7) 0.7496(6) 0.0293(15) Uani 1 1 d . . . H26A H 1.1307 0.9228 0.8036 0.044 Uiso 1 1 calc R . . H26B H 1.0902 0.8848 0.6853 0.044 Uiso 1 1 calc R . . H26C H 1.1491 0.7826 0.7630 0.044 Uiso 1 1 calc R . . C27 C 0.6915(9) 0.7935(8) 0.3406(6) 0.0382(18) Uani 1 1 d . . . H27A H 0.7252 0.8804 0.3598 0.057 Uiso 1 1 calc R . . H27B H 0.6329 0.7844 0.2699 0.057 Uiso 1 1 calc R . . H27C H 0.7704 0.7388 0.3498 0.057 Uiso 1 1 calc R . . C28 C 0.9069(8) 0.7754(8) 1.1639(5) 0.0365(18) Uani 1 1 d . . . H28A H 0.8891 0.8412 1.2104 0.055 Uiso 1 1 calc R . . H28B H 0.9984 0.7902 1.1580 0.055 Uiso 1 1 calc R . . H28C H 0.9038 0.6942 1.1897 0.055 Uiso 1 1 calc R . . C29 C 0.8018(9) 1.2060(7) 0.9605(7) 0.0379(18) Uani 1 1 d . . . H29A H 0.8937 1.2400 1.0041 0.046 Uiso 1 1 calc R . . H29B H 0.7792 1.2429 0.8955 0.046 Uiso 1 1 calc R . . C30 C 0.8695(9) 0.1026(7) 0.5664(8) 0.055(3) Uani 1 1 d D . . C31 C 0.8769(10) 0.5104(8) 0.8913(6) 0.050(3) Uani 1 1 d . . . H31A H 0.9234 0.4310 0.8897 0.075 Uiso 1 1 calc R . . H31B H 0.8302 0.5123 0.9420 0.075 Uiso 1 1 calc R . . H31C H 0.9455 0.5795 0.9082 0.075 Uiso 1 1 calc R . . O3A O 1.0042(14) 0.135(2) 0.5793(18) 0.045(8) Uani 0.259(17) 1 d PD A 1 H3A1 H 1.0440 0.0728 0.5627 0.053 Uiso 0.259(17) 1 calc PR A 1 O3B O 0.8220(13) 0.0160(10) 0.4875(9) 0.039(4) Uani 0.464(17) 1 d PD A 2 H3B1 H 0.7425 0.0344 0.4517 0.047 Uiso 0.464(17) 1 calc PR A 2 O3C O 0.891(3) -0.0167(16) 0.594(2) 0.078(12) Uani 0.284(19) 1 d PD A 3 H3C H 0.8156 -0.0576 0.5740 0.094 Uiso 0.284(19) 1 calc PR A 3 N1S N 0.7683(18) 0.4584(12) 1.1822(18) 0.167(10) Uani 1 1 d . . . C1S C 0.658(2) 0.4936(11) 1.1577(13) 0.092(5) Uani 1 1 d . . . C2S C 0.5186(15) 0.5439(12) 1.1374(9) 0.075(4) Uani 1 1 d . . . H2A H 0.4975 0.5570 1.2004 0.112 Uiso 1 1 calc R . . H2B H 0.4504 0.4848 1.0902 0.112 Uiso 1 1 calc R . . H2C H 0.5153 0.6237 1.1082 0.112 Uiso 1 1 calc R . . H22 H 0.574(9) 0.784(9) 0.920(7) 0.03(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0159(4) 0.0162(4) 0.0152(4) -0.0011(3) 0.0035(3) 0.0007(3) Ni2 0.0162(4) 0.0206(4) 0.0161(4) -0.0034(3) 0.0061(3) -0.0019(3) Mn1 0.0142(4) 0.0137(4) 0.0143(4) -0.0018(3) 0.0048(3) -0.0004(3) O1 0.0153(19) 0.0158(19) 0.0137(18) -0.0027(15) 0.0069(16) -0.0029(15) O2 0.023(2) 0.018(2) 0.022(2) -0.0006(17) -0.0009(18) -0.0007(17) O4 0.014(2) 0.016(2) 0.019(2) -0.0017(16) 0.0074(16) -0.0010(16) O5 0.020(2) 0.020(2) 0.017(2) 0.0001(17) 0.0032(17) 0.0020(17) O6 0.039(3) 0.017(2) 0.020(2) 0.0018(17) 0.007(2) 0.0022(19) O7 0.025(2) 0.024(2) 0.019(2) -0.0009(18) 0.0033(18) 0.0007(19) O8 0.018(2) 0.024(2) 0.023(2) -0.0074(18) 0.0076(18) -0.0059(17) O9 0.018(2) 0.029(2) 0.022(2) -0.0067(18) 0.0079(18) -0.0014(18) O10 0.019(2) 0.014(2) 0.019(2) -0.0018(16) 0.0076(17) -0.0005(16) O11 0.023(2) 0.028(3) 0.020(2) -0.001(2) 0.009(2) -0.0059(19) O12 0.026(2) 0.036(3) 0.016(2) -0.0024(19) 0.0074(18) 0.000(2) O13 0.030(3) 0.081(5) 0.028(3) 0.017(3) 0.012(2) 0.002(3) O14 0.054(4) 0.058(4) 0.079(5) -0.012(4) 0.028(4) -0.004(3) N1 0.013(2) 0.013(2) 0.024(3) 0.0001(19) 0.004(2) 0.0016(18) N2 0.025(3) 0.026(3) 0.015(2) -0.006(2) 0.007(2) -0.001(2) C1 0.015(3) 0.023(3) 0.017(3) -0.004(2) 0.007(2) -0.004(2) C3 0.017(3) 0.026(3) 0.022(3) -0.006(2) 0.009(2) 0.002(2) C10 0.011(3) 0.022(3) 0.026(3) -0.003(2) 0.003(2) -0.001(2) C11 0.017(3) 0.020(3) 0.021(3) -0.003(2) 0.007(2) 0.001(2) C12 0.013(3) 0.022(3) 0.026(3) -0.002(2) 0.010(2) 0.000(2) C14 0.021(3) 0.021(3) 0.018(3) 0.004(2) 0.001(2) -0.001(2) C16 0.026(3) 0.018(3) 0.023(3) 0.005(2) 0.009(3) 0.005(2) C17 0.023(3) 0.029(3) 0.028(3) -0.005(3) 0.014(3) -0.001(3) C19 0.023(3) 0.019(3) 0.040(4) 0.008(3) 0.007(3) 0.001(3) C20 0.017(3) 0.035(4) 0.026(3) -0.003(3) 0.010(3) 0.000(3) C22 0.034(4) 0.022(3) 0.029(3) 0.001(3) 0.013(3) 0.000(3) C23 0.030(4) 0.034(4) 0.019(3) 0.002(3) 0.009(3) 0.004(3) C24 0.029(4) 0.031(4) 0.030(4) -0.009(3) 0.010(3) -0.001(3) C25 0.026(3) 0.015(3) 0.026(3) 0.004(2) 0.006(3) 0.004(2) C26 0.017(3) 0.038(4) 0.032(4) -0.012(3) 0.010(3) -0.007(3) C27 0.044(5) 0.037(4) 0.044(4) 0.006(3) 0.027(4) -0.002(3) C28 0.037(4) 0.050(5) 0.020(3) 0.001(3) 0.007(3) 0.004(4) C29 0.047(5) 0.029(4) 0.044(4) -0.005(3) 0.026(4) -0.005(3) C30 0.029(4) 0.025(4) 0.108(9) 0.005(5) 0.019(5) 0.010(3) C31 0.063(6) 0.029(4) 0.031(4) 0.001(3) -0.022(4) 0.007(4) O3A 0.043(14) 0.035(13) 0.054(15) -0.006(10) 0.017(11) 0.016(10) O3B 0.042(7) 0.028(6) 0.047(8) -0.013(5) 0.017(6) 0.001(5) O3C 0.041(15) 0.09(2) 0.11(3) 0.045(19) 0.021(15) 0.001(14) N1S 0.157(14) 0.061(7) 0.38(3) 0.075(12) 0.209(19) 0.043(9) C1S 0.153(15) 0.044(6) 0.127(12) 0.000(7) 0.114(12) -0.003(8) C2S 0.109(11) 0.070(8) 0.051(6) 0.005(6) 0.035(7) -0.009(7) _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 Ni1 O7 2.025(5) 2_666 ? Ni1 O4 2.028(4) . ? Ni1 O2 2.093(4) . ? Ni1 O1 2.123(4) . ? Ni1 N1 2.125(5) . ? Ni1 O1 2.153(4) 2_666 ? Ni2 O12 2.029(5) . ? Ni2 O9 2.043(5) . ? Ni2 O10 2.054(4) . ? Ni2 O5 2.066(4) . ? Ni2 O11 2.074(5) . ? Ni2 N2 2.106(6) . ? Mn1 O10 1.881(4) . ? Mn1 O4 1.889(4) . ? Mn1 O8 1.954(4) . ? Mn1 O1 1.984(4) 2_666 ? Mn1 O6 2.149(5) . ? Mn1 O5 2.243(4) . ? O1 C1 1.440(7) . ? O1 Mn1 1.984(4) 2_666 ? O1 Ni1 2.153(4) 2_666 ? O2 C14 1.240(8) . ? O4 C12 1.408(7) . ? O5 C14 1.272(8) . ? O6 C16 1.258(8) . ? O7 C16 1.264(8) . ? O7 Ni1 2.025(5) 2_666 ? O8 C11 1.273(7) . ? O9 C11 1.242(8) . ? O10 C25 1.402(7) . ? O11 C20 1.430(8) . ? O11 H22 0.66(9) . ? O12 C23 1.267(8) . ? O13 C23 1.244(9) . ? O14 C29 1.400(10) . ? O14 H14 0.8400 . ? N1 C19 1.465(8) . ? N1 C3 1.487(8) . ? N1 C10 1.493(7) . ? N2 C22 1.482(9) . ? N2 C17 1.490(8) . ? N2 C24 1.495(9) . ? C1 C3 1.509(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C10 C12 1.521(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C26 1.514(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C31 1.494(9) . ? C16 C27 1.499(10) . ? C17 C20 1.528(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C30 1.488(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C25 1.525(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.514(10) . ? C24 C29 1.520(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O3B 1.347(9) . ? C30 O3A 1.370(10) . ? C30 O3C 1.372(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O3A H3A1 0.8400 . ? O3B H3B1 0.8400 . ? O3C H3C 0.8400 . ? N1S C1S 1.15(2) . ? C1S C2S 1.47(2) . ? C2S H2A 0.9800 . ? C2S H2B 0.9800 . ? C2S H2C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ni1 O4 164.86(17) 2_666 . ? O7 Ni1 O2 81.99(18) 2_666 . ? O4 Ni1 O2 89.67(18) . . ? O7 Ni1 O1 98.77(17) 2_666 . ? O4 Ni1 O1 91.30(16) . . ? O2 Ni1 O1 171.69(17) . . ? O7 Ni1 N1 111.18(19) 2_666 . ? O4 Ni1 N1 81.14(18) . . ? O2 Ni1 N1 89.10(19) . . ? O1 Ni1 N1 82.90(18) . . ? O7 Ni1 O1 97.69(17) 2_666 2_666 ? O4 Ni1 O1 71.79(16) . 2_666 ? O2 Ni1 O1 102.99(16) . 2_666 ? O1 Ni1 O1 85.14(16) . 2_666 ? N1 Ni1 O1 150.08(18) . 2_666 ? O12 Ni2 O9 87.29(19) . . ? O12 Ni2 O10 179.57(19) . . ? O9 Ni2 O10 92.40(18) . . ? O12 Ni2 O5 102.70(19) . . ? O9 Ni2 O5 89.97(18) . . ? O10 Ni2 O5 76.99(17) . . ? O12 Ni2 O11 90.8(2) . . ? O9 Ni2 O11 175.90(19) . . ? O10 Ni2 O11 89.54(19) . . ? O5 Ni2 O11 93.98(19) . . ? O12 Ni2 N2 97.7(2) . . ? O9 Ni2 N2 91.7(2) . . ? O10 Ni2 N2 82.59(18) . . ? O5 Ni2 N2 159.57(19) . . ? O11 Ni2 N2 85.0(2) . . ? O10 Mn1 O4 171.25(19) . . ? O10 Mn1 O8 94.78(18) . . ? O4 Mn1 O8 90.33(18) . . ? O10 Mn1 O1 95.68(18) . 2_666 ? O4 Mn1 O1 78.58(17) . 2_666 ? O8 Mn1 O1 167.97(18) . 2_666 ? O10 Mn1 O6 92.26(18) . . ? O4 Mn1 O6 95.11(18) . . ? O8 Mn1 O6 86.9(2) . . ? O1 Mn1 O6 98.56(18) 2_666 . ? O10 Mn1 O5 76.37(17) . . ? O4 Mn1 O5 96.64(17) . . ? O8 Mn1 O5 89.28(18) . . ? O1 Mn1 O5 87.42(16) 2_666 . ? O6 Mn1 O5 167.68(17) . . ? C1 O1 Mn1 121.0(3) . 2_666 ? C1 O1 Ni1 105.2(3) . . ? Mn1 O1 Ni1 118.71(19) 2_666 . ? C1 O1 Ni1 120.3(3) . 2_666 ? Mn1 O1 Ni1 94.21(17) 2_666 2_666 ? Ni1 O1 Ni1 94.86(15) . 2_666 ? C14 O2 Ni1 126.5(4) . . ? C12 O4 Mn1 133.7(4) . . ? C12 O4 Ni1 116.6(4) . . ? Mn1 O4 Ni1 101.45(19) . . ? C14 O5 Ni2 140.1(4) . . ? C14 O5 Mn1 123.6(4) . . ? Ni2 O5 Mn1 92.59(17) . . ? C16 O6 Mn1 120.5(4) . . ? C16 O7 Ni1 134.9(4) . 2_666 ? C11 O8 Mn1 130.2(4) . . ? C11 O9 Ni2 127.7(4) . . ? C25 O10 Mn1 129.1(4) . . ? C25 O10 Ni2 113.6(4) . . ? Mn1 O10 Ni2 104.7(2) . . ? C20 O11 Ni2 107.2(4) . . ? C20 O11 H22 103(8) . . ? Ni2 O11 H22 95(8) . . ? C23 O12 Ni2 129.5(5) . . ? C29 O14 H14 109.5 . . ? C19 N1 C3 111.4(5) . . ? C19 N1 C10 111.4(5) . . ? C3 N1 C10 112.1(5) . . ? C19 N1 Ni1 111.2(4) . . ? C3 N1 Ni1 107.1(3) . . ? C10 N1 Ni1 103.2(4) . . ? C22 N2 C17 114.2(5) . . ? C22 N2 C24 109.9(6) . . ? C17 N2 C24 111.3(5) . . ? C22 N2 Ni2 103.6(4) . . ? C17 N2 Ni2 106.7(4) . . ? C24 N2 Ni2 110.7(4) . . ? O1 C1 C3 109.1(5) . . ? O1 C1 H1A 109.9 . . ? C3 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C3 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N1 C3 C1 113.5(5) . . ? N1 C3 H3A 108.9 . . ? C1 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N1 C10 C12 112.1(5) . . ? N1 C10 H10A 109.2 . . ? C12 C10 H10A 109.2 . . ? N1 C10 H10B 109.2 . . ? C12 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O9 C11 O8 127.0(6) . . ? O9 C11 C26 118.2(6) . . ? O8 C11 C26 114.8(5) . . ? O4 C12 C10 109.4(5) . . ? O4 C12 H12A 109.8 . . ? C10 C12 H12A 109.8 . . ? O4 C12 H12B 109.8 . . ? C10 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? O2 C14 O5 122.9(6) . . ? O2 C14 C31 119.0(6) . . ? O5 C14 C31 118.0(6) . . ? O6 C16 O7 124.3(6) . . ? O6 C16 C27 119.0(6) . . ? O7 C16 C27 116.6(6) . . ? N2 C17 C20 112.4(5) . . ? N2 C17 H17A 109.1 . . ? C20 C17 H17A 109.1 . . ? N2 C17 H17B 109.1 . . ? C20 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N1 C19 C30 118.3(7) . . ? N1 C19 H19A 107.7 . . ? C30 C19 H19A 107.7 . . ? N1 C19 H19B 107.7 . . ? C30 C19 H19B 107.7 . . ? H19A C19 H19B 107.1 . . ? O11 C20 C17 111.1(5) . . ? O11 C20 H20A 109.4 . . ? C17 C20 H20A 109.4 . . ? O11 C20 H20B 109.4 . . ? C17 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N2 C22 C25 112.1(5) . . ? N2 C22 H22A 109.2 . . ? C25 C22 H22A 109.2 . . ? N2 C22 H22B 109.2 . . ? C25 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O13 C23 O12 125.4(6) . . ? O13 C23 C28 117.4(6) . . ? O12 C23 C28 117.2(6) . . ? N2 C24 C29 117.9(6) . . ? N2 C24 H24A 107.8 . . ? C29 C24 H24A 107.8 . . ? N2 C24 H24B 107.8 . . ? C29 C24 H24B 107.8 . . ? H24A C24 H24B 107.2 . . ? O10 C25 C22 111.6(5) . . ? O10 C25 H25A 109.3 . . ? C22 C25 H25A 109.3 . . ? O10 C25 H25B 109.3 . . ? C22 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C11 C26 H26A 109.5 . . ? C11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C16 C27 H27A 109.5 . . ? C16 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C16 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O14 C29 C24 110.6(7) . . ? O14 C29 H29A 109.5 . . ? C24 C29 H29A 109.5 . . ? O14 C29 H29B 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? O3B C30 O3A 109.7(13) . . ? O3B C30 O3C 67.7(15) . . ? O3A C30 O3C 97.7(15) . . ? O3B C30 C19 116.9(8) . . ? O3A C30 C19 123.3(11) . . ? O3C C30 C19 128.4(15) . . ? C14 C31 H31A 109.5 . . ? C14 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C14 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 O3A H3A1 109.5 . . ? C30 O3B H3B1 109.5 . . ? C30 O3C H3C 109.5 . . ? N1S C1S C2S 173.9(19) . . ? C1S C2S H2A 109.5 . . ? C1S C2S H2B 109.5 . . ? H2A C2S H2B 109.5 . . ? C1S C2S H2C 109.5 . . ? H2A C2S H2C 109.5 . . ? H2B C2S H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.465 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.170 # Attachment '- 4_Mn2Co2final.CIF' #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 838821' #TrackingRef '- 4_Mn2Co2final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H56 Co2 Mn2 N2 O18, 2(C H4 O)' _chemical_formula_sum 'C40 H64 Co2 Mn2 N2 O20' _chemical_formula_weight 1120.67 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1764(3) _cell_length_b 11.4785(3) _cell_length_c 19.1645(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.1580(10) _cell_angle_gamma 90.00 _cell_volume 2373.04(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8766 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.21 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.372 _exptl_absorpt_correction_T_max 0.598 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 32852 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.65 _reflns_number_total 7280 _reflns_number_gt 6852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The compound was solved by direct methods. The asymmetric unit contains half the cluster as well as one solvent MeOH molecule. All non-hydrogen atoms are refined anisotropically and the hydrogen atoms are placed in calculated positions, exept for H1 which was found. ; _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^)+(0.0199P)^2^+1.7059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7280 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.619725(18) 0.921035(16) 0.018627(9) 0.01067(5) Uani 1 1 d . . . Mn2 Mn 0.35830(2) 0.800291(18) -0.048183(11) 0.01171(5) Uani 1 1 d . . . O1 O 0.72933(10) 1.05016(9) -0.00368(5) 0.0154(2) Uani 1 1 d . . . O2 O 0.69107(10) 0.81323(9) -0.04448(5) 0.0157(2) Uani 1 1 d . . . O3 O 0.55879(9) 1.05882(8) 0.07159(5) 0.01205(18) Uani 1 1 d . . . O4 O 0.49450(10) 0.80551(9) 0.03384(5) 0.0142(2) Uani 1 1 d . . . O5 O 1.04713(11) 0.82050(12) 0.21786(7) 0.0282(3) Uani 1 1 d . . . H5 H 1.0649 0.8897 0.2169 0.034 Uiso 1 1 calc R . . O6 O 0.47572(11) 0.69947(9) -0.10641(6) 0.0181(2) Uani 1 1 d . . . O7 O 0.29769(10) 0.66805(9) -0.01367(5) 0.0157(2) Uani 1 1 d . . . O8 O 0.22425(10) 0.80682(9) -0.13223(6) 0.0177(2) Uani 1 1 d . . . O9 O 0.05506(11) 0.75517(10) -0.21449(6) 0.0215(2) Uani 1 1 d . . . N1 N 0.70967(11) 0.86717(10) 0.12750(6) 0.0128(2) Uani 1 1 d . . . C1 C 0.87254(18) 1.15609(15) -0.05082(11) 0.0286(4) Uani 1 1 d . . . H1A H 0.8160 1.2206 -0.0607 0.043 Uiso 1 1 calc R . . H1B H 0.9122 1.1483 -0.0894 0.043 Uiso 1 1 calc R . . H1C H 0.9341 1.1695 -0.0062 0.043 Uiso 1 1 calc R . . C2 C 0.80275(14) 1.04645(13) -0.04499(8) 0.0166(3) Uani 1 1 d . . . C3 C 0.82108(15) 0.94810(14) -0.08376(8) 0.0198(3) Uani 1 1 d . . . H3 H 0.8760 0.9554 -0.1125 0.024 Uiso 1 1 calc R . . C4 C 0.76431(13) 0.83949(13) -0.08326(7) 0.0148(3) Uani 1 1 d . . . C5 C 0.78868(16) 0.74494(14) -0.13195(8) 0.0205(3) Uani 1 1 d . . . H5A H 0.8118 0.6747 -0.1045 0.031 Uiso 1 1 calc R . . H5B H 0.8547 0.7685 -0.1523 0.031 Uiso 1 1 calc R . . H5C H 0.7151 0.7312 -0.1701 0.031 Uiso 1 1 calc R . . C6 C 0.55991(14) 1.02230(12) 0.14320(7) 0.0147(3) Uani 1 1 d . . . H6A H 0.4877 0.9743 0.1413 0.018 Uiso 1 1 calc R . . H6B H 0.5554 1.0902 0.1726 0.018 Uiso 1 1 calc R . . C7 C 0.67719(14) 0.95331(13) 0.17792(7) 0.0152(3) Uani 1 1 d . . . H7A H 0.7457 1.0071 0.1943 0.018 Uiso 1 1 calc R . . H7B H 0.6655 0.9125 0.2200 0.018 Uiso 1 1 calc R . . C8 C 0.65827(14) 0.74891(12) 0.13335(8) 0.0153(3) Uani 1 1 d . . . H8A H 0.6767 0.7263 0.1838 0.018 Uiso 1 1 calc R . . H8B H 0.6973 0.6930 0.1083 0.018 Uiso 1 1 calc R . . C9 C 0.51906(14) 0.74690(12) 0.10086(7) 0.0146(3) Uani 1 1 d . . . H9A H 0.4896 0.6672 0.0939 0.018 Uiso 1 1 calc R . . H9B H 0.4772 0.7856 0.1328 0.018 Uiso 1 1 calc R . . C10 C 0.84556(13) 0.86112(14) 0.13793(8) 0.0164(3) Uani 1 1 d . . . H10A H 0.8763 0.9392 0.1340 0.020 Uiso 1 1 calc R . . H10B H 0.8621 0.8152 0.0990 0.020 Uiso 1 1 calc R . . C11 C 0.91808(15) 0.80895(15) 0.20972(8) 0.0221(3) Uani 1 1 d . . . H11A H 0.8956 0.8484 0.2492 0.027 Uiso 1 1 calc R . . H11B H 0.8971 0.7272 0.2115 0.027 Uiso 1 1 calc R . . C12 C 0.47980(17) 0.57521(13) -0.10392(9) 0.0235(3) Uani 1 1 d . . . H12A H 0.5157 0.5502 -0.0551 0.035 Uiso 1 1 calc R . . H12B H 0.5293 0.5471 -0.1345 0.035 Uiso 1 1 calc R . . H12C H 0.3972 0.5448 -0.1205 0.035 Uiso 1 1 calc R . . C13 C 0.20604(13) 0.59915(12) -0.04938(8) 0.0139(3) Uani 1 1 d . . . C14 C 0.18712(15) 0.49545(13) -0.01472(8) 0.0183(3) Uani 1 1 d . . . H14 H 0.2372 0.4788 0.0312 0.022 Uiso 1 1 calc R . . C15 C 0.09553(15) 0.41807(14) -0.04773(9) 0.0216(3) Uani 1 1 d . . . H15 H 0.0842 0.3501 -0.0238 0.026 Uiso 1 1 calc R . . C16 C 0.01966(15) 0.44053(14) -0.11653(9) 0.0221(3) Uani 1 1 d . . . H16 H -0.0409 0.3874 -0.1391 0.026 Uiso 1 1 calc R . . C17 C 0.03573(14) 0.54267(13) -0.15055(8) 0.0186(3) Uani 1 1 d . . . H17 H -0.0156 0.5585 -0.1962 0.022 Uiso 1 1 calc R . . C18 C 0.12772(13) 0.62383(12) -0.11813(7) 0.0142(3) Uani 1 1 d . . . C19 C 0.13468(14) 0.73376(13) -0.15755(7) 0.0150(3) Uani 1 1 d . . . H1 H 0.542(2) 0.722(2) -0.0901(13) 0.039(7) Uiso 1 1 d . . . O1S O -0.08073(12) 0.94845(11) -0.25311(8) 0.0315(3) Uani 1 1 d . . . H1S H -0.0330 0.8930 -0.2431 0.038 Uiso 1 1 calc R . . C1S C -0.19684(17) 0.90963(18) -0.29607(11) 0.0330(4) Uani 1 1 d . . . H1S1 H -0.2205 0.8398 -0.2755 0.049 Uiso 1 1 calc R . . H1S2 H -0.1907 0.8938 -0.3442 0.049 Uiso 1 1 calc R . . H1S3 H -0.2581 0.9689 -0.2976 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01219(9) 0.00974(9) 0.01033(8) -0.00014(6) 0.00339(6) -0.00156(7) Mn2 0.01277(10) 0.00997(10) 0.01158(9) 0.00008(7) 0.00175(7) -0.00291(7) O1 0.0168(5) 0.0135(5) 0.0181(5) -0.0013(4) 0.0086(4) -0.0034(4) O2 0.0175(5) 0.0146(5) 0.0166(5) -0.0011(4) 0.0072(4) -0.0016(4) O3 0.0147(5) 0.0111(4) 0.0107(4) 0.0007(3) 0.0038(3) -0.0015(4) O4 0.0149(5) 0.0140(5) 0.0124(4) 0.0030(4) 0.0009(4) -0.0045(4) O5 0.0165(6) 0.0315(7) 0.0319(6) -0.0001(5) -0.0020(5) 0.0018(5) O6 0.0196(6) 0.0135(5) 0.0214(5) -0.0035(4) 0.0059(4) -0.0012(4) O7 0.0167(5) 0.0135(5) 0.0148(4) 0.0013(4) 0.0007(4) -0.0064(4) O8 0.0182(5) 0.0147(5) 0.0170(5) 0.0022(4) -0.0007(4) -0.0049(4) O9 0.0198(5) 0.0223(6) 0.0181(5) 0.0014(4) -0.0025(4) -0.0019(4) N1 0.0130(5) 0.0118(5) 0.0131(5) 0.0000(4) 0.0027(4) -0.0009(4) C1 0.0315(9) 0.0212(8) 0.0414(10) -0.0043(7) 0.0245(8) -0.0097(7) C2 0.0156(7) 0.0164(7) 0.0195(6) 0.0013(5) 0.0072(5) -0.0023(5) C3 0.0209(7) 0.0194(7) 0.0233(7) -0.0020(6) 0.0137(6) -0.0027(6) C4 0.0138(6) 0.0166(6) 0.0141(6) 0.0005(5) 0.0036(5) 0.0018(5) C5 0.0250(8) 0.0186(7) 0.0209(7) -0.0026(6) 0.0115(6) 0.0006(6) C6 0.0189(7) 0.0137(6) 0.0132(6) 0.0004(5) 0.0069(5) 0.0001(5) C7 0.0203(7) 0.0146(6) 0.0104(5) 0.0001(5) 0.0033(5) -0.0002(5) C8 0.0162(7) 0.0126(6) 0.0156(6) 0.0023(5) 0.0016(5) -0.0006(5) C9 0.0170(7) 0.0128(6) 0.0137(6) 0.0030(5) 0.0035(5) -0.0030(5) C10 0.0127(6) 0.0209(7) 0.0147(6) 0.0003(5) 0.0018(5) -0.0008(5) C11 0.0169(7) 0.0279(8) 0.0186(7) 0.0025(6) -0.0009(5) 0.0021(6) C12 0.0288(9) 0.0141(7) 0.0293(8) -0.0012(6) 0.0109(7) 0.0002(6) C13 0.0129(6) 0.0118(6) 0.0175(6) -0.0028(5) 0.0052(5) -0.0023(5) C14 0.0186(7) 0.0147(6) 0.0204(7) 0.0014(5) 0.0031(5) -0.0033(5) C15 0.0206(8) 0.0141(7) 0.0297(8) 0.0007(6) 0.0057(6) -0.0048(6) C16 0.0169(7) 0.0168(7) 0.0300(8) -0.0041(6) 0.0017(6) -0.0059(6) C17 0.0148(7) 0.0179(7) 0.0211(7) -0.0037(5) 0.0008(5) -0.0020(6) C18 0.0130(6) 0.0135(6) 0.0163(6) -0.0020(5) 0.0041(5) -0.0011(5) C19 0.0149(6) 0.0154(6) 0.0147(6) -0.0024(5) 0.0040(5) 0.0001(5) O1S 0.0223(6) 0.0257(6) 0.0413(7) 0.0033(6) -0.0012(5) -0.0002(5) C1S 0.0239(9) 0.0366(10) 0.0346(9) 0.0075(8) 0.0007(7) -0.0019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.0039(10) . ? Co1 O2 2.0332(10) . ? Co1 O1 2.0381(10) . ? Co1 O3 2.0873(10) . ? Co1 N1 2.1563(11) . ? Co1 O3 2.2846(10) 3_675 ? Mn2 O7 1.8533(10) . ? Mn2 O4 1.8816(10) . ? Mn2 O8 1.8929(10) . ? Mn2 O3 1.9729(10) 3_675 ? Mn2 O6 2.2523(11) . ? Mn2 O1 2.3244(11) 3_675 ? O1 C2 1.2814(18) . ? O1 Mn2 2.3244(11) 3_675 ? O2 C4 1.2774(18) . ? O3 C6 1.4320(16) . ? O3 Mn2 1.9729(10) 3_675 ? O3 Co1 2.2846(10) 3_675 ? O4 C9 1.4118(16) . ? O5 C11 1.416(2) . ? O5 H5 0.8200 . ? O6 C12 1.4274(18) . ? O6 H1 0.77(2) . ? O7 C13 1.3328(16) . ? O8 C19 1.2988(17) . ? O9 C19 1.2391(17) . ? N1 C10 1.4808(19) . ? N1 C8 1.4896(18) . ? N1 C7 1.4921(18) . ? C1 C2 1.500(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.396(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9300 . ? C4 C5 1.502(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.527(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.517(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.525(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.406(2) . ? C13 C18 1.4069(19) . ? C14 C15 1.378(2) . ? C14 H14 0.9300 . ? C15 C16 1.393(2) . ? C15 H15 0.9300 . ? C16 C17 1.376(2) . ? C16 H16 0.9300 . ? C17 C18 1.406(2) . ? C17 H17 0.9300 . ? C18 C19 1.483(2) . ? O1S C1S 1.415(2) . ? O1S H1S 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O2 94.66(4) . . ? O4 Co1 O1 173.07(4) . . ? O2 Co1 O1 88.12(4) . . ? O4 Co1 O3 95.83(4) . . ? O2 Co1 O3 168.22(4) . . ? O1 Co1 O3 80.87(4) . . ? O4 Co1 N1 80.57(4) . . ? O2 Co1 N1 104.18(4) . . ? O1 Co1 N1 104.94(4) . . ? O3 Co1 N1 82.85(4) . . ? O4 Co1 O3 70.86(4) . 3_675 ? O2 Co1 O3 90.70(4) . 3_675 ? O1 Co1 O3 102.80(4) . 3_675 ? O3 Co1 O3 87.70(4) . 3_675 ? N1 Co1 O3 148.79(4) . 3_675 ? O7 Mn2 O4 91.11(4) . . ? O7 Mn2 O8 93.11(4) . . ? O4 Mn2 O8 175.64(5) . . ? O7 Mn2 O3 171.78(4) . 3_675 ? O4 Mn2 O3 80.70(4) . 3_675 ? O8 Mn2 O3 95.07(4) . 3_675 ? O7 Mn2 O6 94.05(5) . . ? O4 Mn2 O6 88.93(4) . . ? O8 Mn2 O6 91.88(5) . . ? O3 Mn2 O6 86.53(4) 3_675 . ? O7 Mn2 O1 102.60(4) . 3_675 ? O4 Mn2 O1 87.63(4) . 3_675 ? O8 Mn2 O1 90.37(4) . 3_675 ? O3 Mn2 O1 76.55(4) 3_675 3_675 ? O6 Mn2 O1 163.05(4) . 3_675 ? C2 O1 Co1 128.50(9) . . ? C2 O1 Mn2 134.29(9) . 3_675 ? Co1 O1 Mn2 95.96(4) . 3_675 ? C4 O2 Co1 127.82(9) . . ? C6 O3 Mn2 124.82(8) . 3_675 ? C6 O3 Co1 108.79(8) . . ? Mn2 O3 Co1 106.15(5) 3_675 . ? C6 O3 Co1 122.82(8) . 3_675 ? Mn2 O3 Co1 96.55(4) 3_675 3_675 ? Co1 O3 Co1 92.30(4) . 3_675 ? C9 O4 Mn2 131.85(9) . . ? C9 O4 Co1 118.08(8) . . ? Mn2 O4 Co1 110.04(5) . . ? C11 O5 H5 109.5 . . ? C12 O6 Mn2 120.96(10) . . ? C12 O6 H1 107.7(18) . . ? Mn2 O6 H1 104.5(18) . . ? C13 O7 Mn2 127.33(9) . . ? C19 O8 Mn2 130.81(9) . . ? C10 N1 C8 110.44(11) . . ? C10 N1 C7 111.00(11) . . ? C8 N1 C7 113.03(11) . . ? C10 N1 Co1 110.26(8) . . ? C8 N1 Co1 104.04(8) . . ? C7 N1 Co1 107.81(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.24(14) . . ? O1 C2 C1 116.59(13) . . ? C3 C2 C1 119.17(14) . . ? C2 C3 C4 125.93(14) . . ? C2 C3 H3 117.0 . . ? C4 C3 H3 117.0 . . ? O2 C4 C3 125.08(13) . . ? O2 C4 C5 116.04(13) . . ? C3 C4 C5 118.88(13) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 C7 111.15(11) . . ? O3 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? O3 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N1 C7 C6 112.83(11) . . ? N1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 110.93(11) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? O4 C9 C8 107.49(11) . . ? O4 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O4 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N1 C10 C11 115.13(12) . . ? N1 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N1 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? O5 C11 C10 110.39(13) . . ? O5 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? O5 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 C14 116.75(12) . . ? O7 C13 C18 124.60(13) . . ? C14 C13 C18 118.65(13) . . ? C15 C14 C13 120.95(14) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.72(15) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 118.93(14) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 121.76(14) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 118.97(13) . . ? C17 C18 C19 117.93(13) . . ? C13 C18 C19 123.07(12) . . ? O9 C19 O8 120.45(14) . . ? O9 C19 C18 119.74(13) . . ? O8 C19 C18 119.81(12) . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O1S 0.82 1.97 2.7383(19) 154.7 3_675 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.65 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.438 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.062 # Attachment '- 5_Mn2Fe2final.CIF' #========================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 838822' #TrackingRef '- 5_Mn2Fe2final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H62 Fe2 Mn2 N10 O14, 2(C H4 O), C H2 Cl2, 2(N O3)' _chemical_formula_sum 'C51 H72 Cl2 Fe2 Mn2 N12 O22' _chemical_formula_weight 1497.69 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1669(3) _cell_length_b 20.2693(6) _cell_length_c 13.4861(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.5940(10) _cell_angle_gamma 90.00 _cell_volume 3315.18(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9765 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.56 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 45005 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.58 _reflns_number_total 10117 _reflns_number_gt 8575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The asymmetric unit contains half the cluster as well as a nitrate, methanol and half a DCM molecule. Bond restraints (DFIX) were placed on the DCM molecule. All non-hydrogen atoms are refined anisotropically. All of the hydrogen atoms are placed in calculated positions, except for the H-atoms on the singly protonated teaH ligand and on the terminal MeOH which were found. ; _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^)+(0.0560P)^2^+4.5513P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10117 _refine_ls_number_parameters 432 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.21027(3) 0.048375(18) 0.06025(3) 0.01795(9) Uani 1 1 d . . . Mn1 Mn 0.05735(3) -0.082334(19) -0.01032(3) 0.01747(9) Uani 1 1 d . . . O1 O 0.04591(18) -0.19210(10) -0.03453(16) 0.0281(4) Uani 1 1 d . . . O2 O 0.19482(14) -0.04555(9) 0.07909(13) 0.0198(3) Uani 1 1 d . . . O3 O -0.08875(13) -0.03868(9) 0.04593(12) 0.0180(3) Uani 1 1 d . . . O4 O 0.33222(14) 0.04121(10) -0.02448(14) 0.0243(4) Uani 1 1 d . . . O5 O 0.22349(14) 0.14888(10) 0.04641(14) 0.0237(4) Uani 1 1 d . . . O6 O 0.30180(14) 0.05804(10) 0.18671(14) 0.0246(4) Uani 1 1 d . . . O7 O 0.07107(13) 0.07263(9) 0.13969(13) 0.0189(3) Uani 1 1 d . . . N1 N 0.04526(17) -0.13458(11) 0.14897(16) 0.0210(4) Uani 1 1 d . . . N2 N -0.16345(17) 0.09955(11) 0.13998(16) 0.0210(4) Uani 1 1 d . . . N3 N -0.01753(17) 0.12069(12) 0.26481(16) 0.0232(4) Uani 1 1 d . . . H3 H -0.0050 0.1417 0.3200 0.028 Uiso 1 1 calc R . . N4 N 0.3100(2) 0.24687(12) 0.03438(19) 0.0288(5) Uani 1 1 d . . . H4 H 0.3672 0.2668 0.0155 0.035 Uiso 1 1 calc R . . N5 N 0.2164(2) 0.34556(14) 0.0346(2) 0.0373(6) Uani 1 1 d . . . C1 C 0.0155(3) -0.23280(14) 0.0452(2) 0.0300(6) Uani 1 1 d . . . H1A H 0.0402 -0.2777 0.0356 0.036 Uiso 1 1 calc R . . H1B H -0.0641 -0.2333 0.0466 0.036 Uiso 1 1 calc R . . C2 C 0.0681(2) -0.20576(14) 0.1421(2) 0.0278(6) Uani 1 1 d . . . H2A H 0.0390 -0.2286 0.1974 0.033 Uiso 1 1 calc R . . H2B H 0.1472 -0.2130 0.1455 0.033 Uiso 1 1 calc R . . C3 C 0.1276(2) -0.10177(14) 0.21843(19) 0.0224(5) Uani 1 1 d . . . H3A H 0.1490 -0.1310 0.2736 0.027 Uiso 1 1 calc R . . H3B H 0.0961 -0.0622 0.2449 0.027 Uiso 1 1 calc R . . C4 C 0.2281(2) -0.08403(13) 0.16417(19) 0.0218(5) Uani 1 1 d . . . H4A H 0.2800 -0.0593 0.2081 0.026 Uiso 1 1 calc R . . H4B H 0.2643 -0.1239 0.1441 0.026 Uiso 1 1 calc R . . C5 C -0.2734(2) 0.09883(15) 0.1158(2) 0.0262(6) Uani 1 1 d . . . H5 H -0.2981 0.0877 0.0509 0.031 Uiso 1 1 calc R . . C6 C -0.3511(2) 0.11352(18) 0.1815(2) 0.0346(7) Uani 1 1 d . . . H6 H -0.4259 0.1132 0.1612 0.041 Uiso 1 1 calc R . . C7 C -0.1039(2) -0.05278(14) 0.14806(18) 0.0215(5) Uani 1 1 d . . . H7A H -0.1810 -0.0471 0.1596 0.026 Uiso 1 1 calc R . . H7B H -0.0613 -0.0218 0.1903 0.026 Uiso 1 1 calc R . . C8 C -0.0685(2) -0.12235(14) 0.1755(2) 0.0234(5) Uani 1 1 d . . . H8A H -0.0722 -0.1289 0.2465 0.028 Uiso 1 1 calc R . . H8B H -0.1183 -0.1535 0.1408 0.028 Uiso 1 1 calc R . . C9 C 0.4892(2) 0.06132(17) -0.1109(2) 0.0338(7) Uani 1 1 d . . . H9A H 0.5366 0.0320 -0.0712 0.051 Uiso 1 1 calc R . . H9B H 0.5315 0.0979 -0.1322 0.051 Uiso 1 1 calc R . . H9C H 0.4568 0.0381 -0.1680 0.051 Uiso 1 1 calc R . . C10 C 0.3998(2) 0.08623(14) -0.0502(2) 0.0243(5) Uani 1 1 d . . . C11 C 0.3945(2) 0.15164(15) -0.0273(2) 0.0283(6) Uani 1 1 d . . . H11 H 0.4517 0.1789 -0.0440 0.034 Uiso 1 1 calc R . . C12 C 0.3059(2) 0.18058(14) 0.0210(2) 0.0240(5) Uani 1 1 d . . . C13 C 0.2307(2) 0.28633(15) 0.0759(2) 0.0277(6) Uani 1 1 d . . . C14 C 0.1743(3) 0.26521(16) 0.1559(2) 0.0325(6) Uani 1 1 d . . . H14 H 0.1884 0.2241 0.1849 0.039 Uiso 1 1 calc R . . C15 C 0.1408(3) 0.38558(19) 0.0702(3) 0.0446(8) Uani 1 1 d . . . H15 H 0.1301 0.4271 0.0418 0.054 Uiso 1 1 calc R . . C16 C 0.0787(3) 0.3678(2) 0.1466(3) 0.0471(9) Uani 1 1 d . . . H16 H 0.0254 0.3962 0.1679 0.057 Uiso 1 1 calc R . . C17 C 0.0969(3) 0.30713(18) 0.1911(3) 0.0414(8) Uani 1 1 d . . . H17 H 0.0574 0.2946 0.2443 0.050 Uiso 1 1 calc R . . C18 C 0.3739(2) 0.09865(19) 0.3422(2) 0.0381(8) Uani 1 1 d . . . H18A H 0.4077 0.0571 0.3605 0.057 Uiso 1 1 calc R . . H18B H 0.3482 0.1193 0.4001 0.057 Uiso 1 1 calc R . . H18C H 0.4270 0.1267 0.3143 0.057 Uiso 1 1 calc R . . C19 C 0.2776(2) 0.08730(14) 0.2661(2) 0.0243(5) Uani 1 1 d . . . C20 C 0.1744(2) 0.10818(14) 0.28773(19) 0.0243(5) Uani 1 1 d . . . H20 H 0.1689 0.1298 0.3479 0.029 Uiso 1 1 calc R . . C21 C 0.0758(2) 0.09926(13) 0.22532(19) 0.0197(5) Uani 1 1 d . . . C22 C -0.1298(2) 0.11542(13) 0.23349(19) 0.0218(5) Uani 1 1 d . . . C23 C -0.2027(2) 0.12958(16) 0.3057(2) 0.0299(6) Uani 1 1 d . . . H23 H -0.1763 0.1394 0.3706 0.036 Uiso 1 1 calc R . . C24 C -0.3140(2) 0.12877(18) 0.2787(2) 0.0358(7) Uani 1 1 d . . . H24 H -0.3641 0.1384 0.3252 0.043 Uiso 1 1 calc R . . H1 H 0.087(3) -0.2112(19) -0.069(3) 0.041(11) Uiso 1 1 d . . . Cl1S Cl -0.2990(7) -0.0341(3) 0.4037(4) 0.180(2) Uani 0.50 1 d PU . . Cl2S Cl -0.0580(7) -0.0253(3) 0.4279(6) 0.211(3) Uani 0.50 1 d PDU . . O1S O 0.49767(19) 0.30697(14) -0.05210(19) 0.0474(7) Uani 1 1 d . . . O2S O 0.5659(3) 0.28514(17) 0.0978(2) 0.0638(8) Uani 1 1 d . . . O3S O 0.6701(3) 0.2910(3) -0.0211(3) 0.128(2) Uani 1 1 d U . . O4S O -0.1753(2) 0.26730(15) 0.1350(2) 0.0523(7) Uani 1 1 d . . . H4S H -0.2301 0.2769 0.0985 0.063 Uiso 1 1 calc R . . N1S N 0.5790(2) 0.29478(18) 0.0087(3) 0.0536(9) Uani 1 1 d . . . C1S C -0.1871(3) 0.2911(2) 0.2308(3) 0.0481(9) Uani 1 1 d . . . H1S1 H -0.1320 0.2715 0.2766 0.072 Uiso 1 1 calc R . . H1S2 H -0.2591 0.2800 0.2501 0.072 Uiso 1 1 calc R . . H1S3 H -0.1784 0.3382 0.2315 0.072 Uiso 1 1 calc R . . C2S C -0.1778(10) -0.0102(6) 0.4704(9) 0.102(5) Uani 0.50 1 d PD . . H2S1 H -0.1822 0.0371 0.4805 0.122 Uiso 0.50 1 calc PR . . H2S2 H -0.1772 -0.0305 0.5355 0.122 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00922(15) 0.02509(19) 0.01984(17) -0.00038(13) 0.00299(12) -0.00037(13) Mn1 0.01060(16) 0.02483(19) 0.01712(18) -0.00025(14) 0.00205(12) 0.00147(13) O1 0.0309(10) 0.0272(10) 0.0268(10) 0.0005(8) 0.0066(8) 0.0028(8) O2 0.0125(7) 0.0273(9) 0.0196(8) 0.0033(7) 0.0012(6) 0.0008(7) O3 0.0107(7) 0.0269(9) 0.0167(8) 0.0011(7) 0.0034(6) 0.0005(6) O4 0.0130(8) 0.0322(10) 0.0288(10) 0.0005(8) 0.0083(7) -0.0003(7) O5 0.0147(8) 0.0274(9) 0.0294(10) -0.0014(8) 0.0049(7) -0.0041(7) O6 0.0133(8) 0.0347(10) 0.0256(9) -0.0046(8) -0.0009(7) 0.0007(7) O7 0.0114(7) 0.0269(9) 0.0187(8) -0.0021(7) 0.0025(6) 0.0007(7) N1 0.0158(9) 0.0242(11) 0.0230(10) 0.0030(8) 0.0009(8) 0.0005(8) N2 0.0141(9) 0.0275(11) 0.0215(10) -0.0018(8) 0.0032(7) 0.0010(8) N3 0.0150(9) 0.0349(12) 0.0200(10) -0.0060(9) 0.0024(8) 0.0007(9) N4 0.0230(11) 0.0311(12) 0.0328(13) 0.0006(10) 0.0062(9) -0.0079(9) N5 0.0476(16) 0.0372(14) 0.0270(13) 0.0005(11) 0.0027(11) 0.0019(12) C1 0.0331(15) 0.0249(13) 0.0317(14) 0.0014(11) 0.0001(11) -0.0019(11) C2 0.0266(13) 0.0262(13) 0.0299(14) 0.0043(11) -0.0017(11) 0.0007(11) C3 0.0180(11) 0.0287(13) 0.0204(12) 0.0029(10) 0.0003(9) -0.0004(10) C4 0.0154(11) 0.0280(13) 0.0216(12) 0.0026(10) -0.0007(9) 0.0015(9) C5 0.0145(11) 0.0389(15) 0.0254(13) -0.0072(11) 0.0021(9) 0.0035(10) C6 0.0140(11) 0.0542(19) 0.0360(16) -0.0092(14) 0.0045(11) 0.0037(12) C7 0.0150(10) 0.0329(13) 0.0173(11) 0.0033(10) 0.0053(8) 0.0015(10) C8 0.0144(11) 0.0314(13) 0.0247(12) 0.0047(10) 0.0032(9) -0.0022(10) C9 0.0193(12) 0.0458(17) 0.0381(16) 0.0081(13) 0.0146(11) 0.0054(12) C10 0.0123(10) 0.0365(14) 0.0242(12) 0.0065(11) 0.0024(9) 0.0011(10) C11 0.0150(11) 0.0373(15) 0.0333(14) 0.0057(12) 0.0066(10) -0.0045(11) C12 0.0182(11) 0.0323(14) 0.0213(12) 0.0020(10) 0.0005(9) -0.0033(10) C13 0.0258(13) 0.0314(14) 0.0254(13) -0.0020(11) -0.0011(10) -0.0059(11) C14 0.0320(15) 0.0339(15) 0.0320(15) -0.0066(12) 0.0052(12) -0.0109(12) C15 0.058(2) 0.0421(19) 0.0328(17) -0.0043(14) -0.0057(15) 0.0119(17) C16 0.0408(19) 0.057(2) 0.043(2) -0.0206(17) -0.0001(15) 0.0073(17) C17 0.0358(17) 0.049(2) 0.0405(18) -0.0162(15) 0.0090(14) -0.0107(15) C18 0.0173(12) 0.061(2) 0.0348(16) -0.0153(15) -0.0038(11) -0.0002(13) C19 0.0168(11) 0.0303(13) 0.0255(13) -0.0015(10) -0.0011(9) -0.0033(10) C20 0.0188(11) 0.0349(14) 0.0190(12) -0.0039(10) 0.0003(9) -0.0011(10) C21 0.0149(10) 0.0250(12) 0.0197(11) 0.0011(9) 0.0036(8) -0.0010(9) C22 0.0141(10) 0.0284(13) 0.0233(12) -0.0026(10) 0.0037(9) 0.0016(9) C23 0.0193(12) 0.0468(17) 0.0241(13) -0.0083(12) 0.0053(10) 0.0009(12) C24 0.0185(12) 0.059(2) 0.0317(15) -0.0104(14) 0.0101(11) 0.0013(13) Cl1S 0.290(7) 0.116(3) 0.125(4) -0.009(3) -0.029(4) -0.043(4) Cl2S 0.259(7) 0.152(4) 0.234(6) 0.056(4) 0.101(5) 0.056(5) O1S 0.0274(11) 0.0691(17) 0.0439(14) 0.0297(12) -0.0083(10) -0.0137(11) O2S 0.070(2) 0.080(2) 0.0379(15) 0.0117(14) -0.0156(13) -0.0106(17) O3S 0.0387(17) 0.233(5) 0.112(3) 0.117(3) 0.0085(19) 0.015(2) O4S 0.0351(13) 0.0734(19) 0.0468(15) -0.0215(14) -0.0058(11) 0.0230(13) N1S 0.0307(15) 0.070(2) 0.057(2) 0.0363(17) -0.0107(13) -0.0173(15) C1S 0.0398(19) 0.054(2) 0.052(2) -0.0166(18) 0.0079(16) 0.0067(17) C2S 0.152(12) 0.084(8) 0.076(7) 0.061(7) 0.046(8) 0.027(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.9318(19) . ? Fe1 O4 1.9493(18) . ? Fe1 O6 1.9706(18) . ? Fe1 O3 1.9838(17) 3 ? Fe1 O5 2.053(2) . ? Fe1 O7 2.1328(17) . ? Mn1 O2 2.1177(17) . ? Mn1 O3 2.1758(17) . ? Mn1 O1 2.251(2) . ? Mn1 O7 2.2554(17) 3 ? Mn1 N2 2.282(2) 3 ? Mn1 N1 2.410(2) . ? O1 C1 1.427(4) . ? O1 H1 0.81(4) . ? O2 C4 1.419(3) . ? O3 C7 1.433(3) . ? O3 Fe1 1.9838(17) 3 ? O4 C10 1.294(3) . ? O5 C12 1.262(3) . ? O6 C19 1.279(3) . ? O7 C21 1.272(3) . ? O7 Mn1 2.2554(17) 3 ? N1 C2 1.474(4) . ? N1 C3 1.474(3) . ? N1 C8 1.478(3) . ? N2 C22 1.334(3) . ? N2 C5 1.351(3) . ? N2 Mn1 2.282(2) 3 ? N3 C21 1.363(3) . ? N3 C22 1.401(3) . ? N3 H3 0.8600 . ? N4 C12 1.356(4) . ? N4 C13 1.404(4) . ? N4 H4 0.8600 . ? N5 C13 1.329(4) . ? N5 C15 1.343(5) . ? C1 C2 1.511(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.517(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.379(4) . ? C5 H5 0.9300 . ? C6 C24 1.386(4) . ? C6 H6 0.9300 . ? C7 C8 1.512(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.501(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.364(4) . ? C11 C12 1.429(4) . ? C11 H11 0.9300 . ? C13 C14 1.392(4) . ? C14 C17 1.381(5) . ? C14 H14 0.9300 . ? C15 C16 1.374(6) . ? C15 H15 0.9300 . ? C16 C17 1.379(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.511(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.378(4) . ? C20 C21 1.421(3) . ? C20 H20 0.9300 . ? C22 C23 1.398(4) . ? C23 C24 1.375(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? Cl1S C2S 1.735(15) . ? Cl2S C2S 1.636(8) . ? O1S N1S 1.258(4) . ? O2S N1S 1.240(4) . ? O3S N1S 1.212(5) . ? O4S C1S 1.398(4) . ? O4S H4S 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? 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 O2 Fe1 O4 95.19(8) . . ? O2 Fe1 O6 92.20(8) . . ? O4 Fe1 O6 96.36(8) . . ? O2 Fe1 O3 85.56(7) . 3 ? O4 Fe1 O3 97.34(8) . 3 ? O6 Fe1 O3 166.26(7) . 3 ? O2 Fe1 O5 177.32(8) . . ? O4 Fe1 O5 87.24(8) . . ? O6 Fe1 O5 86.39(8) . . ? O3 Fe1 O5 95.28(7) 3 . ? O2 Fe1 O7 94.10(7) . . ? O4 Fe1 O7 169.73(8) . . ? O6 Fe1 O7 87.64(7) . . ? O3 Fe1 O7 79.02(7) 3 . ? O5 Fe1 O7 83.57(7) . . ? O2 Mn1 O3 106.76(7) . . ? O2 Mn1 O1 117.86(7) . . ? O3 Mn1 O1 114.18(7) . . ? O2 Mn1 O7 151.21(7) . 3 ? O3 Mn1 O7 72.52(6) . 3 ? O1 Mn1 O7 86.73(7) . 3 ? O2 Mn1 N2 91.19(7) . 3 ? O3 Mn1 N2 149.03(7) . 3 ? O1 Mn1 N2 76.70(8) . 3 ? O7 Mn1 N2 79.63(7) 3 3 ? O2 Mn1 N1 75.46(7) . . ? O3 Mn1 N1 76.00(7) . . ? O1 Mn1 N1 71.80(8) . . ? O7 Mn1 N1 129.78(7) 3 . ? N2 Mn1 N1 133.98(8) 3 . ? O2 Mn1 O3 81.91(5) . 4_566 ? O3 Mn1 O3 28.46(5) . 4_566 ? O1 Mn1 O3 140.75(6) . 4_566 ? O7 Mn1 O3 87.73(5) 3 4_566 ? N2 Mn1 O3 139.94(6) 3 4_566 ? N1 Mn1 O3 82.41(5) . 4_566 ? C1 O1 Mn1 118.61(17) . . ? C1 O1 H1 112(3) . . ? Mn1 O1 H1 122(3) . . ? C4 O2 Fe1 128.57(16) . . ? C4 O2 Mn1 115.34(15) . . ? Fe1 O2 Mn1 110.66(8) . . ? C7 O3 Fe1 121.88(14) . 3 ? C7 O3 Mn1 115.20(14) . . ? Fe1 O3 Mn1 106.89(8) 3 . ? C10 O4 Fe1 129.36(18) . . ? C12 O5 Fe1 126.86(18) . . ? C19 O6 Fe1 128.23(17) . . ? C21 O7 Fe1 125.03(15) . . ? C21 O7 Mn1 130.05(16) . 3 ? Fe1 O7 Mn1 99.23(7) . 3 ? C2 N1 C3 111.1(2) . . ? C2 N1 C8 111.4(2) . . ? C3 N1 C8 111.9(2) . . ? C2 N1 Mn1 110.39(16) . . ? C3 N1 Mn1 106.34(15) . . ? C8 N1 Mn1 105.52(15) . . ? C22 N2 C5 117.0(2) . . ? C22 N2 Mn1 127.70(17) . 3 ? C5 N2 Mn1 115.02(17) . 3 ? C21 N3 C22 132.9(2) . . ? C21 N3 H3 113.6 . . ? C22 N3 H3 113.6 . . ? C12 N4 C13 126.7(2) . . ? C12 N4 H4 116.6 . . ? C13 N4 H4 116.6 . . ? C13 N5 C15 117.8(3) . . ? O1 C1 C2 108.9(2) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C1 109.9(2) . . ? N1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C4 109.5(2) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O2 C4 C3 109.36(19) . . ? O2 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O2 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? N2 C5 C6 124.0(3) . . ? N2 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C5 C6 C24 117.9(3) . . ? C5 C6 H6 121.1 . . ? C24 C6 H6 121.1 . . ? O3 C7 C8 111.4(2) . . ? O3 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O3 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N1 C8 C7 110.6(2) . . ? N1 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 125.6(2) . . ? O4 C10 C9 114.4(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 123.6(2) . . ? C10 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? O5 C12 N4 119.3(2) . . ? O5 C12 C11 124.0(3) . . ? N4 C12 C11 116.5(2) . . ? N5 C13 C14 123.1(3) . . ? N5 C13 N4 114.8(3) . . ? C14 C13 N4 122.1(3) . . ? C17 C14 C13 118.0(3) . . ? C17 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N5 C15 C16 122.9(3) . . ? N5 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 118.8(3) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C14 119.3(3) . . ? C16 C17 H17 120.3 . . ? C14 C17 H17 120.3 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C19 C20 126.4(2) . . ? O6 C19 C18 114.9(2) . . ? C20 C19 C18 118.7(3) . . ? C19 C20 C21 125.2(2) . . ? C19 C20 H20 117.4 . . ? C21 C20 H20 117.4 . . ? O7 C21 N3 120.8(2) . . ? O7 C21 C20 124.5(2) . . ? N3 C21 C20 114.7(2) . . ? N2 C22 C23 122.9(2) . . ? N2 C22 N3 121.4(2) . . ? C23 C22 N3 115.6(2) . . ? C24 C23 C22 118.7(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C6 119.5(3) . . ? C23 C24 H24 120.3 . . ? C6 C24 H24 120.3 . . ? C1S O4S H4S 109.5 . . ? O3S N1S O2S 120.3(3) . . ? O3S N1S O1S 119.2(4) . . ? O2S N1S O1S 120.5(3) . . ? O4S C1S H1S1 109.5 . . ? O4S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O4S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? Cl2S C2S Cl1S 120.7(9) . . ? Cl2S C2S H2S1 107.1 . . ? Cl1S C2S H2S1 107.1 . . ? Cl2S C2S H2S2 107.1 . . ? Cl1S C2S H2S2 107.1 . . ? H2S1 C2S H2S2 106.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O1S 0.86 2.01 2.865(3) 170.7 4_566 O4S H4S O3S 0.82 1.96 2.751(5) 161.5 1_455 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.310 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.097 # Attachment '- 6 Mn3Co2finalSept29.CIF' #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 838823' #TrackingRef '- 6 Mn3Co2finalSept29.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _publ_section_exptl_refinement ; The asymmetric unit contains the cluster as well as nitrate and disordered tetrafluoroborate counter ions with three solvent MeOH molecules. The O-atom of the free tea arm is disordered over two positions. One of the solvent MeOH molecules has had its bond length restrained using the DFIX command. All non-hydrogen atoms are refined anisotropically and the hydrogen atoms are placed in calculated positions, except for H-atom of one of the protonated teaH ligands, which was found. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H70 B Co2 F6 Mn3 N9 O18' _chemical_formula_weight 1492.64 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5301(3) _cell_length_b 17.9740(4) _cell_length_c 48.5907(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11816.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8767 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 24.12 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6120 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.607 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 48652 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9972 _reflns_number_gt 8314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The asymmetric unit contains the cluster as well as nitrate and disordered tetrafluoroborate counter ions with three solvent MeOH molecules. The O-atom of the free tea arm is disordered over two positions. One of the solvent MeOH molecules has had its bond length restrained using the DFIX command. All non-hydrogen atoms are refined anisotropically and the hydrogen atoms are placed in calculated positions, except for H-atom of one of the protonated teaH ligands, which was found. ; _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^)+(0.0397P)^2^+108.6529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9972 _refine_ls_number_parameters 850 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.00939(7) 0.31676(5) 0.159664(19) 0.0232(2) Uani 1 1 d . . . Co2 Co 0.31405(8) 0.18915(6) 0.07217(2) 0.0324(3) Uani 1 1 d . . . Mn1 Mn 0.12714(8) 0.22268(6) 0.11262(2) 0.0250(3) Uani 1 1 d . . . Mn2 Mn 0.21882(8) 0.25682(6) 0.17352(2) 0.0252(3) Uani 1 1 d . . . Mn3 Mn 0.35454(8) 0.20072(6) 0.13480(2) 0.0287(3) Uani 1 1 d . . . F7 F 0.1880(3) 0.2352(2) 0.21002(8) 0.0341(10) Uani 1 1 d . . . F11 F 0.4516(3) 0.1281(2) 0.13517(9) 0.0385(11) Uani 1 1 d . . . O1 O 0.0465(4) 0.3212(3) 0.12240(10) 0.0260(11) Uani 1 1 d . . . O2 O 0.1342(3) 0.3449(3) 0.17320(9) 0.0254(11) Uani 1 1 d . . . O4 O 0.0687(3) 0.2194(2) 0.15775(9) 0.0226(10) Uani 1 1 d . . . O5 O -0.0034(4) 0.2022(3) 0.08329(11) 0.0373(13) Uani 1 1 d D . . O6 O 0.2606(4) 0.1400(3) 0.10402(9) 0.0292(12) Uani 1 1 d . . . O8 O 0.3476(4) 0.3258(3) 0.18586(10) 0.0309(12) Uani 1 1 d . . . O9 O 0.4513(4) 0.2776(3) 0.15483(11) 0.0370(13) Uani 1 1 d . . . O10 O 0.2499(4) 0.2658(3) 0.13701(9) 0.0262(11) Uani 1 1 d . . . O12 O 0.2057(4) 0.2536(3) 0.07644(10) 0.0325(12) Uani 1 1 d . . . O13 O 0.3953(4) 0.2361(3) 0.09830(10) 0.0321(12) Uani 1 1 d . . . O14 O 0.2966(4) 0.1664(3) 0.16949(10) 0.0329(12) Uani 1 1 d . . . N1 N -0.0379(4) 0.3059(3) 0.19734(12) 0.0264(14) Uani 1 1 d . . . N2 N -0.1239(4) 0.2834(3) 0.15030(12) 0.0258(13) Uani 1 1 d . . . N3 N -0.0182(4) 0.4249(3) 0.15621(12) 0.0272(14) Uani 1 1 d . B . N4 N 0.0689(5) 0.1014(3) 0.11978(13) 0.0323(15) Uani 1 1 d . . . N5 N 0.6354(6) 0.5031(5) 0.18312(18) 0.061(2) Uani 1 1 d . . . N6 N 0.3651(5) 0.2622(4) 0.04595(13) 0.0380(16) Uani 1 1 d . . . H6A H 0.3901 0.2387 0.0309 0.046 Uiso 1 1 calc R . . N7 N 0.4178(5) 0.1164(4) 0.06576(13) 0.0381(17) Uani 1 1 d . . . N8 N 0.2421(6) 0.1313(4) 0.04476(13) 0.0415(17) Uani 1 1 d . . . C1 C 0.0084(6) 0.3202(4) 0.22081(15) 0.0327(18) Uani 1 1 d . . . H1 H 0.0731 0.3376 0.2203 0.039 Uiso 1 1 calc R . . C2 C -0.0367(6) 0.3101(5) 0.24603(16) 0.0374(19) Uani 1 1 d . . . H2 H -0.0015 0.3187 0.2622 0.045 Uiso 1 1 calc R . . C3 C -0.1329(6) 0.2874(4) 0.24731(16) 0.0371(19) Uani 1 1 d . . . H3 H -0.1638 0.2817 0.2643 0.045 Uiso 1 1 calc R . . C4 C -0.1843(6) 0.2728(4) 0.22321(15) 0.0316(18) Uani 1 1 d . . . C5 C -0.2848(6) 0.2488(5) 0.22177(17) 0.039(2) Uani 1 1 d . . . H5 H -0.3206 0.2428 0.2380 0.047 Uiso 1 1 calc R . . C6 C -0.3288(6) 0.2347(5) 0.19757(18) 0.041(2) Uani 1 1 d . . . H6 H -0.3939 0.2182 0.1973 0.049 Uiso 1 1 calc R . . C7 C -0.2768(5) 0.2445(4) 0.17206(16) 0.0314(17) Uani 1 1 d . . . C8 C -0.3161(6) 0.2301(4) 0.14594(17) 0.0365(19) Uani 1 1 d . . . H8 H -0.3802 0.2121 0.1441 0.044 Uiso 1 1 calc R . . C9 C -0.2592(6) 0.2429(5) 0.12293(16) 0.0380(19) Uani 1 1 d . . . H9 H -0.2847 0.2336 0.1055 0.046 Uiso 1 1 calc R . . C10 C -0.1626(5) 0.2699(4) 0.12595(15) 0.0300(17) Uani 1 1 d . . . H10 H -0.1247 0.2786 0.1103 0.036 Uiso 1 1 calc R . . C11 C -0.1795(5) 0.2703(4) 0.17294(15) 0.0267(16) Uani 1 1 d . . . C12 C -0.1330(5) 0.2832(4) 0.19863(14) 0.0269(16) Uani 1 1 d . . . C13 C 0.1630(5) 0.4139(4) 0.16212(16) 0.0298(17) Uani 1 1 d . . . H13A H 0.1810 0.4086 0.1429 0.036 Uiso 1 1 calc R . . H13B H 0.2191 0.4339 0.1721 0.036 Uiso 1 1 calc R . . C14 C 0.0738(6) 0.4645(4) 0.16513(16) 0.0331(18) Uani 1 1 d . . . H14A H 0.0672 0.4798 0.1842 0.040 Uiso 1 1 calc R . . H14B H 0.0830 0.5087 0.1540 0.040 Uiso 1 1 calc R . . C15 C 0.0320(6) 0.3906(4) 0.10910(16) 0.0349(19) Uani 1 1 d . . . H15A H 0.0056 0.3827 0.0908 0.042 Uiso 1 1 calc R . . H15B H 0.0944 0.4167 0.1075 0.042 Uiso 1 1 calc R . . C16 C -0.0406(6) 0.4367(4) 0.12622(15) 0.0328(18) Uani 1 1 d . . . H16A H -0.0340 0.4890 0.1216 0.039 Uiso 1 1 calc R . . H16B H -0.1079 0.4214 0.1223 0.039 Uiso 1 1 calc R . . C17 C -0.1025(7) 0.4554(5) 0.1725(2) 0.052(2) Uani 1 1 d . . . H17A H -0.0872 0.4493 0.1919 0.063 Uiso 1 1 calc R A 1 H17B H -0.1604 0.4252 0.1686 0.063 Uiso 1 1 calc R A 1 C18 C -0.1303(8) 0.5377(5) 0.1676(2) 0.061(3) Uani 0.577(15) 1 d P B 1 H18A H -0.0709 0.5667 0.1644 0.073 Uiso 0.577(15) 1 calc PR B 1 H18B H -0.1719 0.5417 0.1514 0.073 Uiso 0.577(15) 1 calc PR B 1 C19 C 0.0748(7) 0.0890(4) 0.14987(16) 0.0374(19) Uani 1 1 d . . . H19A H 0.1437 0.0847 0.1552 0.045 Uiso 1 1 calc R . . H19B H 0.0424 0.0424 0.1543 0.045 Uiso 1 1 calc R . . C20 C 0.0275(6) 0.1508(4) 0.16637(15) 0.0291(17) Uani 1 1 d . . . H20A H -0.0434 0.1510 0.1634 0.035 Uiso 1 1 calc R . . H20B H 0.0398 0.1433 0.1858 0.035 Uiso 1 1 calc R . . C21 C 0.1315(7) 0.0477(5) 0.10497(18) 0.044(2) Uani 1 1 d . . . H21A H 0.1142 0.0484 0.0856 0.053 Uiso 1 1 calc R . . H21B H 0.1184 -0.0019 0.1119 0.053 Uiso 1 1 calc R . . C22 C 0.2407(6) 0.0643(4) 0.10797(16) 0.0334(18) Uani 1 1 d . . . H22A H 0.2625 0.0496 0.1262 0.040 Uiso 1 1 calc R . . H22B H 0.2776 0.0353 0.0946 0.040 Uiso 1 1 calc R . . C23 C -0.0336(7) 0.0961(5) 0.11000(18) 0.046(2) Uani 1 1 d . . . H23A H -0.0767 0.1207 0.1231 0.055 Uiso 1 1 calc R . . H23B H -0.0527 0.0441 0.1093 0.055 Uiso 1 1 calc R . . C24 C -0.0486(7) 0.1301(5) 0.08225(16) 0.039(2) Uani 1 1 d . . . H24A H -0.0177 0.0998 0.0681 0.047 Uiso 1 1 calc R . . H24B H -0.1185 0.1345 0.0782 0.047 Uiso 1 1 calc R . . C25 C 0.3553(8) 0.1399(5) 0.19225(18) 0.057(3) Uani 1 1 d . . . H25A H 0.3473 0.1727 0.2077 0.085 Uiso 1 1 calc R . . H25B H 0.4236 0.1385 0.1870 0.085 Uiso 1 1 calc R . . H25C H 0.3341 0.0907 0.1972 0.085 Uiso 1 1 calc R . . C26 C 0.4251(6) 0.3263(4) 0.17174(15) 0.0284(17) Uani 1 1 d . . . C27 C 0.4970(6) 0.3894(4) 0.17575(16) 0.0326(18) Uani 1 1 d . . . C28 C 0.4912(7) 0.4365(5) 0.19801(18) 0.044(2) Uani 1 1 d . . . H28 H 0.4401 0.4320 0.2107 0.053 Uiso 1 1 calc R . . C29 C 0.5636(7) 0.4912(6) 0.2011(2) 0.056(3) Uani 1 1 d . . . H29 H 0.5613 0.5211 0.2167 0.067 Uiso 1 1 calc R . . C30 C 0.6358(7) 0.4588(6) 0.1604(2) 0.056(3) Uani 1 1 d . . . H30 H 0.6833 0.4676 0.1470 0.067 Uiso 1 1 calc R . . C31 C 0.5703(6) 0.4023(5) 0.15623(19) 0.044(2) Uani 1 1 d . . . H31 H 0.5746 0.3727 0.1406 0.053 Uiso 1 1 calc R . . C32 C 0.4436(9) 0.3044(6) 0.0600(2) 0.064(3) Uani 1 1 d . . . H32A H 0.4469 0.3543 0.0525 0.077 Uiso 1 1 calc R . . H32B H 0.5069 0.2804 0.0569 0.077 Uiso 1 1 calc R . . C33 C 0.4232(9) 0.3081(5) 0.0906(2) 0.061(3) Uani 1 1 d . . . H33A H 0.4820 0.3236 0.1005 0.073 Uiso 1 1 calc R . . H33B H 0.3705 0.3433 0.0944 0.073 Uiso 1 1 calc R . . C34 C 0.2811(7) 0.3100(6) 0.03798(19) 0.057(3) Uani 1 1 d . . . H34A H 0.2440 0.2864 0.0233 0.069 Uiso 1 1 calc R . . H34B H 0.3054 0.3574 0.0313 0.069 Uiso 1 1 calc R . . C35 C 0.2143(7) 0.3222(5) 0.06266(18) 0.052(3) Uani 1 1 d . . . H35A H 0.2426 0.3593 0.0748 0.062 Uiso 1 1 calc R . . H35B H 0.1498 0.3394 0.0567 0.062 Uiso 1 1 calc R . . C36 C 0.5067(7) 0.1115(5) 0.07665(19) 0.049(2) Uani 1 1 d . . . H36 H 0.5263 0.1468 0.0895 0.058 Uiso 1 1 calc R . . C37 C 0.5733(8) 0.0541(6) 0.06938(19) 0.060(3) Uani 1 1 d . . . H37 H 0.6361 0.0527 0.0771 0.072 Uiso 1 1 calc R . . C38 C 0.5448(9) 0.0010(6) 0.0510(2) 0.065(3) Uani 1 1 d . . . H38 H 0.5875 -0.0378 0.0467 0.077 Uiso 1 1 calc R . . C39 C 0.4508(9) 0.0048(5) 0.0386(2) 0.058(3) Uani 1 1 d . . . C40 C 0.4129(11) -0.0451(5) 0.0179(2) 0.067(4) Uani 1 1 d . . . H40 H 0.4515 -0.0849 0.0122 0.080 Uiso 1 1 calc R . . C41 C 0.3240(11) -0.0355(6) 0.0070(2) 0.071(4) Uani 1 1 d . . . H41 H 0.3030 -0.0683 -0.0066 0.085 Uiso 1 1 calc R . . C42 C 0.2593(9) 0.0230(5) 0.01513(19) 0.058(3) Uani 1 1 d . . . C43 C 0.1639(9) 0.0378(7) 0.0044(2) 0.074(4) Uani 1 1 d . . . H43 H 0.1372 0.0082 -0.0094 0.089 Uiso 1 1 calc R . . C44 C 0.1125(9) 0.0961(7) 0.0147(2) 0.075(4) Uani 1 1 d . . . H44 H 0.0488 0.1050 0.0083 0.090 Uiso 1 1 calc R . . C45 C 0.1520(7) 0.1430(6) 0.03465(18) 0.057(3) Uani 1 1 d . . . H45 H 0.1151 0.1832 0.0410 0.068 Uiso 1 1 calc R . . C46 C 0.2947(7) 0.0726(5) 0.03549(17) 0.044(2) Uani 1 1 d . . . C47 C 0.3899(7) 0.0638(4) 0.04686(17) 0.041(2) Uani 1 1 d . . . F1' F 0.609(5) 0.452(3) 0.0648(9) 0.20(3) Uani 0.37(2) 1 d P C 4 F2' F 0.658(5) 0.383(3) 0.0911(11) 0.24(3) Uani 0.37(2) 1 d P C 4 F3' F 0.723(4) 0.402(3) 0.0547(6) 0.21(2) Uani 0.37(2) 1 d P C 4 F1S F 0.7325(6) 0.4803(7) 0.09944(19) 0.150(4) Uani 1 1 d . C . F2S F 0.7670(12) 0.3920(8) 0.0720(6) 0.137(9) Uani 0.63(2) 1 d P C 3 F3S F 0.6967(8) 0.4999(7) 0.0591(2) 0.069(4) Uani 0.63(2) 1 d P C 3 F4S F 0.6049(13) 0.4218(12) 0.0847(5) 0.107(8) Uani 0.63(2) 1 d P C 3 O1S O 0.4669(9) 0.1960(5) -0.04365(18) 0.116(4) Uani 1 1 d . . . O2S O 0.4321(7) 0.2881(4) -0.0150(2) 0.100(3) Uani 1 1 d . . . O3S O 0.4222(8) 0.1745(5) -0.00102(19) 0.112(4) Uani 1 1 d . . . O4S O 0.6768(11) 0.2453(7) 0.0590(2) 0.140(4) Uani 1 1 d . . . H4S H 0.7062 0.2845 0.0617 0.168 Uiso 1 1 calc R . . O6S O 0.3146(14) 0.0029(10) 0.2387(4) 0.208(7) Uani 1 1 d . . . H6S H 0.3691 0.0025 0.2461 0.249 Uiso 1 1 calc R . . O7S O 0.1429(12) 0.0988(9) 0.2321(3) 0.170(5) Uani 1 1 d DU . . H7S H 0.1847 0.0671 0.2355 0.205 Uiso 1 1 calc R . . N1S N 0.4447(8) 0.2206(5) -0.0200(2) 0.081(3) Uani 1 1 d . . . C1S C 0.6939(15) 0.2218(11) 0.0333(3) 0.150(8) Uani 1 1 d . . . H1S1 H 0.7159 0.2629 0.0223 0.224 Uiso 1 1 calc R . . H1S2 H 0.6341 0.2018 0.0257 0.224 Uiso 1 1 calc R . . H1S3 H 0.7440 0.1840 0.0336 0.224 Uiso 1 1 calc R . . C5S C 0.2668(16) -0.0554(9) 0.2456(4) 0.160(9) Uani 1 1 d . . . H5S1 H 0.3053 -0.0850 0.2579 0.240 Uiso 1 1 d . . . H5S2 H 0.2495 -0.0833 0.2296 0.240 Uiso 1 1 d . . . H5S3 H 0.2062 -0.0404 0.2550 0.240 Uiso 1 1 d . . . C8S C 0.0620(16) 0.0945(14) 0.2527(4) 0.198(10) Uani 1 1 d DU . . H8S1 H 0.0801 0.1225 0.2688 0.296 Uiso 1 1 calc R . . H8S2 H 0.0512 0.0435 0.2578 0.296 Uiso 1 1 calc R . . H8S3 H 0.0024 0.1147 0.2450 0.296 Uiso 1 1 calc R . . B1S B 0.6941(12) 0.4440(10) 0.0777(4) 0.075(4) Uani 1 1 d . . . H5X H -0.017(8) 0.227(5) 0.0679(13) 0.090 Uiso 1 1 d D . . O15 O -0.1795(10) 0.5650(7) 0.1901(3) 0.075(5) Uani 0.577(15) 1 d P B 1 H15 H -0.2301 0.5408 0.1926 0.090 Uiso 0.577(15) 1 calc PR B 1 O16 O -0.0637(14) 0.5867(10) 0.1764(3) 0.082(7) Uani 0.423(15) 1 d P B 2 H16 H -0.0303 0.6011 0.1634 0.098 Uiso 0.423(15) 1 calc PRD B 2 C18A C -0.1303(8) 0.5377(5) 0.1676(2) 0.061(3) Uani 0.42 1 d P B 2 H18C H -0.1404 0.5452 0.1480 0.073 Uiso 0.423(15) 1 calc PR B 2 H18D H -0.1926 0.5477 0.1768 0.073 Uiso 0.423(15) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0233(5) 0.0248(5) 0.0215(5) 0.0026(4) 0.0011(4) -0.0002(4) Co2 0.0367(6) 0.0350(6) 0.0256(6) 0.0034(5) 0.0065(5) 0.0081(5) Mn1 0.0286(6) 0.0271(6) 0.0194(5) 0.0011(5) 0.0002(5) 0.0022(5) Mn2 0.0271(6) 0.0273(6) 0.0211(6) 0.0030(5) -0.0011(5) 0.0032(5) Mn3 0.0294(6) 0.0293(6) 0.0274(6) 0.0035(5) 0.0002(5) 0.0074(5) F7 0.037(2) 0.043(3) 0.022(2) 0.0013(19) -0.0037(19) 0.002(2) F11 0.039(3) 0.039(3) 0.038(3) 0.006(2) 0.000(2) 0.013(2) O1 0.027(3) 0.026(3) 0.024(3) 0.005(2) 0.003(2) 0.005(2) O2 0.026(3) 0.025(3) 0.024(3) 0.003(2) -0.002(2) -0.002(2) O4 0.026(3) 0.022(2) 0.019(2) 0.004(2) 0.001(2) 0.002(2) O5 0.042(3) 0.042(3) 0.028(3) 0.001(2) -0.005(3) -0.004(3) O6 0.039(3) 0.027(3) 0.021(3) 0.001(2) 0.008(2) 0.006(2) O8 0.026(3) 0.039(3) 0.027(3) -0.001(2) -0.001(2) -0.001(2) O9 0.027(3) 0.042(3) 0.042(3) -0.005(3) -0.004(2) 0.005(2) O10 0.028(3) 0.033(3) 0.017(2) 0.005(2) 0.000(2) 0.005(2) O12 0.035(3) 0.037(3) 0.025(3) 0.004(2) 0.002(2) 0.009(2) O13 0.032(3) 0.032(3) 0.032(3) 0.004(2) 0.008(2) 0.004(2) O14 0.043(3) 0.030(3) 0.026(3) 0.003(2) -0.005(2) 0.010(2) N1 0.028(3) 0.023(3) 0.028(3) 0.000(3) 0.000(3) -0.004(3) N2 0.026(3) 0.025(3) 0.026(3) 0.002(3) 0.003(3) 0.004(3) N3 0.025(3) 0.033(3) 0.024(3) 0.002(3) 0.002(3) 0.004(3) N4 0.036(4) 0.031(3) 0.030(4) -0.003(3) 0.001(3) -0.001(3) N5 0.041(5) 0.083(6) 0.060(5) 0.017(5) -0.004(4) -0.024(4) N6 0.044(4) 0.039(4) 0.031(4) 0.005(3) 0.008(3) 0.010(3) N7 0.047(4) 0.037(4) 0.030(4) 0.010(3) 0.013(3) 0.009(3) N8 0.051(5) 0.046(4) 0.027(4) -0.006(3) 0.015(3) -0.001(4) C1 0.035(4) 0.039(4) 0.025(4) -0.001(3) -0.003(3) -0.005(4) C2 0.043(5) 0.049(5) 0.021(4) -0.007(4) 0.001(4) 0.001(4) C3 0.042(5) 0.044(5) 0.025(4) -0.002(4) 0.013(4) 0.002(4) C4 0.037(4) 0.031(4) 0.027(4) 0.003(3) 0.009(3) 0.001(3) C5 0.038(5) 0.046(5) 0.033(5) 0.000(4) 0.011(4) -0.005(4) C6 0.029(4) 0.045(5) 0.048(5) 0.001(4) 0.010(4) -0.006(4) C7 0.027(4) 0.033(4) 0.033(4) -0.002(3) 0.001(3) -0.003(3) C8 0.026(4) 0.039(5) 0.045(5) -0.006(4) -0.002(4) 0.003(3) C9 0.031(4) 0.050(5) 0.032(4) -0.004(4) -0.009(4) 0.005(4) C10 0.030(4) 0.039(4) 0.021(4) -0.002(3) 0.000(3) 0.006(3) C11 0.025(4) 0.022(4) 0.033(4) -0.002(3) 0.004(3) 0.002(3) C12 0.030(4) 0.027(4) 0.024(4) -0.001(3) 0.003(3) -0.001(3) C13 0.030(4) 0.025(4) 0.035(4) 0.006(3) 0.002(3) -0.006(3) C14 0.032(4) 0.032(4) 0.035(5) 0.008(3) 0.002(4) -0.002(3) C15 0.047(5) 0.030(4) 0.027(4) 0.008(3) 0.002(4) 0.005(4) C16 0.043(5) 0.029(4) 0.026(4) 0.005(3) -0.001(4) 0.008(4) C17 0.040(5) 0.047(5) 0.069(7) 0.003(5) -0.011(5) -0.002(4) C18 0.048(6) 0.047(6) 0.089(8) -0.004(6) 0.009(6) -0.001(5) C19 0.049(5) 0.026(4) 0.037(5) 0.004(4) -0.004(4) -0.003(4) C20 0.031(4) 0.028(4) 0.028(4) 0.008(3) 0.003(3) 0.000(3) C21 0.058(6) 0.031(4) 0.043(5) -0.004(4) 0.006(4) -0.001(4) C22 0.045(5) 0.026(4) 0.030(4) -0.002(3) 0.000(4) 0.013(4) C23 0.048(6) 0.043(5) 0.047(5) -0.001(4) -0.008(4) -0.011(4) C24 0.044(5) 0.044(5) 0.029(4) 0.001(4) -0.003(4) -0.004(4) C25 0.079(7) 0.058(6) 0.034(5) 0.007(4) -0.008(5) 0.030(6) C26 0.028(4) 0.030(4) 0.027(4) 0.007(3) -0.010(3) 0.005(3) C27 0.030(4) 0.032(4) 0.036(4) 0.008(4) -0.009(4) 0.004(3) C28 0.041(5) 0.051(5) 0.040(5) 0.007(4) -0.003(4) -0.002(4) C29 0.053(6) 0.067(7) 0.047(6) 0.011(5) -0.005(5) -0.019(5) C30 0.038(5) 0.075(7) 0.055(6) 0.003(5) -0.005(5) -0.005(5) C31 0.032(5) 0.050(5) 0.051(6) 0.007(4) -0.006(4) 0.007(4) C32 0.078(8) 0.065(7) 0.051(6) 0.025(5) 0.002(6) -0.020(6) C33 0.086(8) 0.040(5) 0.057(6) 0.011(5) -0.012(6) -0.023(5) C34 0.059(6) 0.069(7) 0.043(5) 0.031(5) 0.013(5) 0.031(5) C35 0.065(6) 0.047(5) 0.043(5) 0.026(4) 0.016(5) 0.022(5) C36 0.046(6) 0.058(6) 0.041(5) 0.016(4) 0.020(4) 0.019(5) C37 0.061(6) 0.082(8) 0.036(5) 0.030(5) 0.027(5) 0.040(6) C38 0.089(9) 0.058(7) 0.046(6) 0.032(5) 0.046(6) 0.039(6) C39 0.095(9) 0.036(5) 0.045(6) 0.017(4) 0.044(6) 0.021(5) C40 0.120(11) 0.029(5) 0.052(7) -0.003(5) 0.058(7) 0.001(6) C41 0.117(11) 0.045(6) 0.051(7) -0.011(5) 0.053(7) -0.024(7) C42 0.091(8) 0.045(6) 0.039(5) -0.011(4) 0.042(6) -0.017(5) C43 0.080(9) 0.092(9) 0.051(7) -0.029(6) 0.018(6) -0.035(7) C44 0.060(7) 0.118(10) 0.048(6) -0.036(7) 0.014(5) -0.022(7) C45 0.050(6) 0.086(8) 0.035(5) -0.020(5) 0.005(5) 0.000(5) C46 0.061(6) 0.043(5) 0.030(5) 0.003(4) 0.027(4) -0.009(4) C47 0.063(6) 0.030(4) 0.032(5) 0.005(4) 0.026(4) 0.007(4) F1' 0.27(6) 0.21(5) 0.14(3) -0.11(3) -0.05(4) 0.04(4) F2' 0.30(7) 0.14(4) 0.27(5) 0.08(3) 0.06(5) -0.04(4) F3' 0.27(5) 0.26(5) 0.09(2) -0.03(2) 0.03(3) 0.12(4) F1S 0.067(6) 0.265(14) 0.117(7) 0.000(8) 0.013(5) -0.012(7) F2S 0.085(11) 0.060(8) 0.27(3) 0.002(12) 0.071(14) 0.013(7) F3S 0.063(7) 0.090(9) 0.055(6) 0.006(6) -0.009(5) -0.003(6) F4S 0.074(11) 0.098(13) 0.150(18) -0.047(13) 0.054(12) -0.050(9) O1S 0.201(11) 0.071(6) 0.075(6) 0.008(5) 0.091(7) 0.014(6) O2S 0.115(7) 0.057(5) 0.128(8) 0.007(5) 0.066(6) 0.003(5) O3S 0.157(9) 0.083(6) 0.096(7) 0.044(5) 0.065(7) 0.024(6) O4S 0.169(12) 0.145(12) 0.107(9) 0.002(8) -0.015(8) -0.020(9) O6S 0.223(19) 0.183(14) 0.216(17) 0.086(13) -0.064(15) -0.046(14) O7S 0.182(9) 0.156(9) 0.174(9) 0.001(7) -0.031(8) -0.015(7) N1S 0.117(9) 0.058(6) 0.068(7) 0.013(5) 0.024(6) 0.039(6) C1S 0.194(19) 0.186(19) 0.068(10) -0.040(11) 0.054(11) 0.042(15) C5S 0.19(2) 0.090(11) 0.20(2) 0.052(13) -0.065(16) -0.088(13) C8S 0.201(13) 0.210(13) 0.182(12) -0.036(9) -0.002(9) -0.011(9) B1S 0.059(9) 0.082(11) 0.085(11) -0.020(10) 0.001(9) -0.006(8) O15 0.062(9) 0.078(10) 0.086(10) -0.025(8) 0.027(7) -0.018(7) O16 0.060(12) 0.067(13) 0.118(17) -0.007(12) -0.005(11) -0.013(10) C18A 0.048(6) 0.047(6) 0.089(8) -0.004(6) 0.009(6) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.881(5) . ? Co1 O2 1.882(5) . ? Co1 O4 1.927(5) . ? Co1 N1 1.949(6) . ? Co1 N2 1.954(6) . ? Co1 N3 1.986(6) . ? Co1 Mn2 3.1053(14) . ? Co2 O13 1.880(5) . ? Co2 O12 1.880(5) . ? Co2 O6 1.923(5) . ? Co2 N7 1.944(7) . ? Co2 N8 1.951(7) . ? Co2 N6 1.955(6) . ? Co2 Mn3 3.0993(15) . ? Mn1 O12 2.128(5) . ? Mn1 O1 2.134(5) . ? Mn1 O10 2.183(5) . ? Mn1 O5 2.299(5) . ? Mn1 O4 2.332(5) . ? Mn1 N4 2.344(6) . ? Mn1 O6 2.376(5) . ? Mn2 O10 1.830(4) . ? Mn2 F7 1.863(4) . ? Mn2 O14 1.946(5) . ? Mn2 O2 1.954(5) . ? Mn2 O8 2.221(5) . ? Mn2 O4 2.272(5) . ? Mn2 Mn3 2.8159(16) . ? Mn3 O10 1.839(5) . ? Mn3 F11 1.853(4) . ? Mn3 O14 1.959(5) . ? Mn3 O13 1.963(5) . ? Mn3 O9 2.138(5) . ? Mn3 O6 2.246(5) . ? O1 C15 1.418(8) . ? O2 C13 1.407(8) . ? O4 C20 1.417(8) . ? O5 C24 1.434(10) . ? O5 H5X 0.888(10) . ? O6 C22 1.400(9) . ? O8 C26 1.253(9) . ? O9 C26 1.251(9) . ? O12 C35 1.409(9) . ? O13 C33 1.401(10) . ? O14 C25 1.443(9) . ? N1 C1 1.326(9) . ? N1 C12 1.351(9) . ? N2 C10 1.316(9) . ? N2 C11 1.353(9) . ? N3 C17 1.493(11) . ? N3 C14 1.498(9) . ? N3 C16 1.503(9) . ? N4 C23 1.470(11) . ? N4 C21 1.472(10) . ? N4 C19 1.481(10) . ? N5 C29 1.323(12) . ? N5 C30 1.360(13) . ? N6 C32 1.473(12) . ? N6 C34 1.477(10) . ? N6 H6A 0.9100 . ? N7 C36 1.317(11) . ? N7 C47 1.370(11) . ? N8 C45 1.330(12) . ? N8 C46 1.350(11) . ? C1 C2 1.381(11) . ? C1 H1 0.9300 . ? C2 C3 1.365(11) . ? C2 H2 0.9300 . ? C3 C4 1.387(11) . ? C3 H3 0.9300 . ? C4 C12 1.394(10) . ? C4 C5 1.428(11) . ? C5 C6 1.342(11) . ? C5 H5 0.9300 . ? C6 C7 1.436(11) . ? C6 H6 0.9300 . ? C7 C11 1.396(10) . ? C7 C8 1.400(11) . ? C8 C9 1.377(11) . ? C8 H8 0.9300 . ? C9 C10 1.403(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.417(10) . ? C13 C14 1.518(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.531(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.545(13) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O15 1.369(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.511(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.515(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.495(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.506(11) . ? C27 C28 1.376(12) . ? C27 C31 1.392(12) . ? C28 C29 1.397(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.364(13) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.510(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.517(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.413(12) . ? C36 H36 0.9300 . ? C37 C38 1.362(15) . ? C37 H37 0.9300 . ? C38 C39 1.409(16) . ? C38 H38 0.9300 . ? C39 C47 1.402(12) . ? C39 C40 1.440(16) . ? C40 C41 1.326(17) . ? C40 H40 0.9300 . ? C41 C42 1.423(15) . ? C41 H41 0.9300 . ? C42 C46 1.416(13) . ? C42 C43 1.416(16) . ? C43 C44 1.353(16) . ? C43 H43 0.9300 . ? C44 C45 1.391(13) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.410(13) . ? F1' B1S 1.32(5) . ? F2' B1S 1.37(4) . ? F3' B1S 1.41(4) . ? F1S B1S 1.345(18) . ? F2S B1S 1.39(2) . ? F3S B1S 1.35(2) . ? F4S B1S 1.31(2) . ? O1S N1S 1.266(11) . ? O2S N1S 1.249(11) . ? O3S N1S 1.279(11) . ? O4S C1S 1.340(15) . ? O4S H4S 0.8200 . ? O6S C5S 1.277(18) . ? O6S H6S 0.8200 . ? O7S C8S 1.488(10) . ? O7S H7S 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C5S H5S1 0.9538 . ? C5S H5S2 0.9537 . ? C5S H5S3 0.9758 . ? C8S H8S1 0.9600 . ? C8S H8S2 0.9600 . ? C8S H8S3 0.9600 . ? O15 H15 0.8200 . ? O16 H16 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 94.9(2) . . ? O1 Co1 O4 83.18(19) . . ? O2 Co1 O4 83.5(2) . . ? O1 Co1 N1 175.0(2) . . ? O2 Co1 N1 89.6(2) . . ? O4 Co1 N1 95.2(2) . . ? O1 Co1 N2 92.0(2) . . ? O2 Co1 N2 172.8(2) . . ? O4 Co1 N2 95.4(2) . . ? N1 Co1 N2 83.4(2) . . ? O1 Co1 N3 85.8(2) . . ? O2 Co1 N3 86.3(2) . . ? O4 Co1 N3 164.3(2) . . ? N1 Co1 N3 96.6(2) . . ? N2 Co1 N3 96.1(2) . . ? O1 Co1 Mn2 88.85(15) . . ? O2 Co1 Mn2 36.74(14) . . ? O4 Co1 Mn2 46.79(14) . . ? N1 Co1 Mn2 93.53(18) . . ? N2 Co1 Mn2 141.83(17) . . ? N3 Co1 Mn2 121.96(18) . . ? O13 Co2 O12 96.0(2) . . ? O13 Co2 O6 83.3(2) . . ? O12 Co2 O6 84.3(2) . . ? O13 Co2 N7 89.3(3) . . ? O12 Co2 N7 174.5(3) . . ? O6 Co2 N7 95.2(2) . . ? O13 Co2 N8 173.1(3) . . ? O12 Co2 N8 90.8(3) . . ? O6 Co2 N8 96.7(3) . . ? N7 Co2 N8 83.8(3) . . ? O13 Co2 N6 86.1(3) . . ? O12 Co2 N6 86.2(2) . . ? O6 Co2 N6 164.9(3) . . ? N7 Co2 N6 95.3(3) . . ? N8 Co2 N6 95.2(3) . . ? O13 Co2 Mn3 37.16(15) . . ? O12 Co2 Mn3 89.32(15) . . ? O6 Co2 Mn3 46.15(16) . . ? N7 Co2 Mn3 94.3(2) . . ? N8 Co2 Mn3 142.6(2) . . ? N6 Co2 Mn3 122.1(2) . . ? O12 Mn1 O1 102.87(19) . . ? O12 Mn1 O10 88.63(19) . . ? O1 Mn1 O10 88.50(19) . . ? O12 Mn1 O5 85.0(2) . . ? O1 Mn1 O5 83.0(2) . . ? O10 Mn1 O5 167.96(19) . . ? O12 Mn1 O4 162.33(19) . . ? O1 Mn1 O4 68.78(17) . . ? O10 Mn1 O4 75.89(17) . . ? O5 Mn1 O4 108.58(18) . . ? O12 Mn1 N4 122.2(2) . . ? O1 Mn1 N4 124.6(2) . . ? O10 Mn1 N4 120.3(2) . . ? O5 Mn1 N4 71.7(2) . . ? O4 Mn1 N4 73.94(19) . . ? O12 Mn1 O6 68.80(18) . . ? O1 Mn1 O6 161.27(19) . . ? O10 Mn1 O6 74.87(18) . . ? O5 Mn1 O6 112.01(19) . . ? O4 Mn1 O6 114.05(16) . . ? N4 Mn1 O6 72.5(2) . . ? O10 Mn2 F7 173.0(2) . . ? O10 Mn2 O14 81.4(2) . . ? F7 Mn2 O14 92.4(2) . . ? O10 Mn2 O2 93.2(2) . . ? F7 Mn2 O2 92.63(19) . . ? O14 Mn2 O2 173.1(2) . . ? O10 Mn2 O8 91.8(2) . . ? F7 Mn2 O8 92.02(19) . . ? O14 Mn2 O8 94.0(2) . . ? O2 Mn2 O8 90.53(19) . . ? O10 Mn2 O4 84.53(19) . . ? F7 Mn2 O4 93.40(18) . . ? O14 Mn2 O4 101.7(2) . . ? O2 Mn2 O4 73.36(18) . . ? O8 Mn2 O4 163.21(18) . . ? O10 Mn2 Mn3 39.99(15) . . ? F7 Mn2 Mn3 135.00(14) . . ? O14 Mn2 Mn3 44.03(15) . . ? O2 Mn2 Mn3 131.83(14) . . ? O8 Mn2 Mn3 82.44(14) . . ? O4 Mn2 Mn3 104.58(12) . . ? O10 Mn2 Co1 88.24(15) . . ? F7 Mn2 Co1 94.29(14) . . ? O14 Mn2 Co1 139.58(16) . . ? O2 Mn2 Co1 35.19(14) . . ? O8 Mn2 Co1 125.51(14) . . ? O4 Mn2 Co1 38.18(11) . . ? Mn3 Mn2 Co1 125.06(5) . . ? O10 Mn3 F11 173.4(2) . . ? O10 Mn3 O14 80.9(2) . . ? F11 Mn3 O14 93.1(2) . . ? O10 Mn3 O13 93.6(2) . . ? F11 Mn3 O13 92.2(2) . . ? O14 Mn3 O13 172.7(2) . . ? O10 Mn3 O9 91.9(2) . . ? F11 Mn3 O9 91.0(2) . . ? O14 Mn3 O9 93.3(2) . . ? O13 Mn3 O9 91.7(2) . . ? O10 Mn3 O6 85.0(2) . . ? F11 Mn3 O6 93.73(19) . . ? O14 Mn3 O6 101.2(2) . . ? O13 Mn3 O6 73.4(2) . . ? O9 Mn3 O6 164.6(2) . . ? O10 Mn3 Mn2 39.77(14) . . ? F11 Mn3 Mn2 135.10(14) . . ? O14 Mn3 Mn2 43.66(15) . . ? O13 Mn3 Mn2 132.13(15) . . ? O9 Mn3 Mn2 82.15(15) . . ? O6 Mn3 Mn2 104.48(13) . . ? O10 Mn3 Co2 87.93(14) . . ? F11 Mn3 Co2 95.03(14) . . ? O14 Mn3 Co2 138.86(16) . . ? O13 Mn3 Co2 35.34(16) . . ? O9 Mn3 Co2 126.78(16) . . ? O6 Mn3 Co2 38.13(12) . . ? Mn2 Mn3 Co2 124.39(5) . . ? C15 O1 Co1 116.1(4) . . ? C15 O1 Mn1 134.4(4) . . ? Co1 O1 Mn1 108.4(2) . . ? C13 O2 Co1 110.6(4) . . ? C13 O2 Mn2 123.7(4) . . ? Co1 O2 Mn2 108.1(2) . . ? C20 O4 Co1 127.8(4) . . ? C20 O4 Mn2 120.6(4) . . ? Co1 O4 Mn2 95.03(19) . . ? C20 O4 Mn1 115.6(4) . . ? Co1 O4 Mn1 99.43(18) . . ? Mn2 O4 Mn1 90.39(17) . . ? C24 O5 Mn1 119.6(5) . . ? C24 O5 H5X 110(7) . . ? Mn1 O5 H5X 127(8) . . ? C22 O6 Co2 129.0(4) . . ? C22 O6 Mn3 119.3(4) . . ? Co2 O6 Mn3 95.7(2) . . ? C22 O6 Mn1 116.0(4) . . ? Co2 O6 Mn1 98.0(2) . . ? Mn3 O6 Mn1 90.49(17) . . ? C26 O8 Mn2 120.9(5) . . ? C26 O9 Mn3 125.3(5) . . ? Mn2 O10 Mn3 100.2(2) . . ? Mn2 O10 Mn1 108.7(2) . . ? Mn3 O10 Mn1 109.2(2) . . ? C35 O12 Co2 115.0(5) . . ? C35 O12 Mn1 131.5(5) . . ? Co2 O12 Mn1 108.7(2) . . ? C33 O13 Co2 113.0(5) . . ? C33 O13 Mn3 128.2(5) . . ? Co2 O13 Mn3 107.5(2) . . ? C25 O14 Mn2 119.8(5) . . ? C25 O14 Mn3 122.9(5) . . ? Mn2 O14 Mn3 92.3(2) . . ? C1 N1 C12 117.9(6) . . ? C1 N1 Co1 129.3(5) . . ? C12 N1 Co1 112.7(5) . . ? C10 N2 C11 118.5(6) . . ? C10 N2 Co1 129.2(5) . . ? C11 N2 Co1 112.2(5) . . ? C17 N3 C14 107.9(6) . . ? C17 N3 C16 107.9(6) . . ? C14 N3 C16 112.4(6) . . ? C17 N3 Co1 117.3(5) . . ? C14 N3 Co1 106.5(4) . . ? C16 N3 Co1 104.9(4) . . ? C23 N4 C21 110.0(7) . . ? C23 N4 C19 111.1(6) . . ? C21 N4 C19 110.7(6) . . ? C23 N4 Mn1 109.2(5) . . ? C21 N4 Mn1 110.1(5) . . ? C19 N4 Mn1 105.6(4) . . ? C29 N5 C30 116.3(9) . . ? C32 N6 C34 112.2(8) . . ? C32 N6 Co2 107.3(5) . . ? C34 N6 Co2 106.8(5) . . ? C32 N6 H6A 110.1 . . ? C34 N6 H6A 110.1 . . ? Co2 N6 H6A 110.1 . . ? C36 N7 C47 118.3(8) . . ? C36 N7 Co2 129.8(6) . . ? C47 N7 Co2 111.9(6) . . ? C45 N8 C46 119.0(8) . . ? C45 N8 Co2 128.6(6) . . ? C46 N8 Co2 112.4(6) . . ? N1 C1 C2 121.9(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.0(8) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.8(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C12 116.6(7) . . ? C3 C4 C5 125.2(7) . . ? C12 C4 C5 118.2(7) . . ? C6 C5 C4 121.5(8) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.1(8) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C11 C7 C8 116.5(7) . . ? C11 C7 C6 118.4(7) . . ? C8 C7 C6 125.0(7) . . ? C9 C8 C7 119.5(7) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.6(7) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 121.9(7) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N2 C11 C7 123.9(7) . . ? N2 C11 C12 116.2(6) . . ? C7 C11 C12 120.0(7) . . ? N1 C12 C4 123.7(7) . . ? N1 C12 C11 115.5(6) . . ? C4 C12 C11 120.8(7) . . ? O2 C13 C14 105.7(6) . . ? O2 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O2 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? N3 C14 C13 110.4(6) . . ? N3 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? N3 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O1 C15 C16 108.5(6) . . ? O1 C15 H15A 110.0 . . ? C16 C15 H15A 110.0 . . ? O1 C15 H15B 110.0 . . ? C16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? N3 C16 C15 108.7(6) . . ? N3 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? N3 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N3 C17 C18 117.1(8) . . ? N3 C17 H17A 108.0 . . ? C18 C17 H17A 108.0 . . ? N3 C17 H17B 108.0 . . ? C18 C17 H17B 108.0 . . ? H17A C17 H17B 107.3 . . ? O15 C18 C17 109.8(10) . . ? O15 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O15 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N4 C19 C20 113.0(6) . . ? N4 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N4 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? O4 C20 C19 108.5(6) . . ? O4 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? O4 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? N4 C21 C22 112.6(7) . . ? N4 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? N4 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? O6 C22 C21 111.5(6) . . ? O6 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? O6 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? N4 C23 C24 113.1(7) . . ? N4 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? N4 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O5 C24 C23 106.3(6) . . ? O5 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O5 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O14 C25 H25A 109.5 . . ? O14 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O14 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O9 C26 O8 126.2(7) . . ? O9 C26 C27 115.4(7) . . ? O8 C26 C27 118.4(7) . . ? C28 C27 C31 118.3(8) . . ? C28 C27 C26 121.9(7) . . ? C31 C27 C26 119.8(7) . . ? C27 C28 C29 118.5(9) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? N5 C29 C28 124.0(10) . . ? N5 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? N5 C30 C31 123.8(9) . . ? N5 C30 H30 118.1 . . ? C31 C30 H30 118.1 . . ? C30 C31 C27 119.0(9) . . ? C30 C31 H31 120.5 . . ? C27 C31 H31 120.5 . . ? N6 C32 C33 110.3(8) . . ? N6 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? N6 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O13 C33 C32 105.8(8) . . ? O13 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O13 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? N6 C34 C35 109.6(7) . . ? N6 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? N6 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? O12 C35 C34 107.3(7) . . ? O12 C35 H35A 110.2 . . ? C34 C35 H35A 110.2 . . ? O12 C35 H35B 110.2 . . ? C34 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? N7 C36 C37 122.0(10) . . ? N7 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C38 C37 C36 119.7(10) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 120.1(9) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C47 C39 C38 116.4(10) . . ? C47 C39 C40 117.4(11) . . ? C38 C39 C40 126.2(10) . . ? C41 C40 C39 121.5(10) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C40 C41 C42 122.9(11) . . ? C40 C41 H41 118.6 . . ? C42 C41 H41 118.6 . . ? C46 C42 C43 116.5(9) . . ? C46 C42 C41 116.8(12) . . ? C43 C42 C41 126.7(11) . . ? C44 C43 C42 118.6(10) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C45 121.9(12) . . ? C43 C44 H44 119.0 . . ? C45 C44 H44 119.0 . . ? N8 C45 C44 120.8(10) . . ? N8 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? N8 C46 C47 116.0(8) . . ? N8 C46 C42 123.1(10) . . ? C47 C46 C42 120.8(9) . . ? N7 C47 C39 123.5(10) . . ? N7 C47 C46 115.9(7) . . ? C39 C47 C46 120.6(9) . . ? C1S O4S H4S 109.5 . . ? C5S O6S H6S 109.5 . . ? C8S O7S H7S 109.5 . . ? O2S N1S O1S 123.3(10) . . ? O2S N1S O3S 117.1(10) . . ? O1S N1S O3S 119.0(10) . . ? O4S C1S H1S1 109.5 . . ? O4S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O4S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O6S C5S H5S1 110.2 . . ? O6S C5S H5S2 110.1 . . ? H5S1 C5S H5S2 110.5 . . ? O6S C5S H5S3 108.7 . . ? H5S1 C5S H5S3 108.7 . . ? H5S2 C5S H5S3 108.7 . . ? O7S C8S H8S1 109.5 . . ? O7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? O7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? F4S B1S F1' 50(2) . . ? F4S B1S F1S 107.4(16) . . ? F1' B1S F1S 131(2) . . ? F4S B1S F3S 115(2) . . ? F1' B1S F3S 68(3) . . ? F1S B1S F3S 98.8(13) . . ? F4S B1S F2' 46(3) . . ? F1' B1S F2' 90(3) . . ? F1S B1S F2' 99(3) . . ? F3S B1S F2' 158(3) . . ? F4S B1S F2S 120.0(17) . . ? F1' B1S F2S 127(2) . . ? F1S B1S F2S 102.1(17) . . ? F3S B1S F2S 110.2(16) . . ? F2' B1S F2S 79(3) . . ? F4S B1S F3' 107(3) . . ? F1' B1S F3' 86(3) . . ? F1S B1S F3' 141(3) . . ? F3S B1S F3' 82(2) . . ? F2' B1S F3' 93(3) . . ? C18 O15 H15 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.244 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.114 # Attachment '- 7 Mn3Co2(acac)finalSept29.CIF' #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 838824' #TrackingRef '- 7 Mn3Co2(acac)finalSept29.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' #========================================================================== _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the cluster as well as nitrate counter ions and solvent DCM molecules. One of the solvent DCM molecules is disordered and is modelled over two positions, each at half occupancy. Bond and thermal restraints (DFIX and ISOR) are placed on these molecules. All non H-atoms are refined anisotropically. All H-atoms are placed in calculated positions, except for some of the H-atoms found on the tea arms which were found. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H75 Co2 Mn3 N4 O19, 0.5(C2 H4 Cl4), 2(C H2 Cl2), 2(N O3)' _chemical_formula_sum 'C42 H81 Cl6 Co2 Mn3 N6 O25' _chemical_formula_weight 1565.51 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2545(4) _cell_length_b 15.5313(5) _cell_length_c 17.7000(6) _cell_angle_alpha 89.130(2) _cell_angle_beta 70.950(2) _cell_angle_gamma 83.650(2) _cell_volume 3164.00(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.12 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _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 47014 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.59 _reflns_number_total 18804 _reflns_number_gt 11730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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. The structure was solved by direct methods. The asymmetric unit contains the cluster as well as nitrate counter ions and solvent DCM molecules. One of the solvent DCM molecules is disordered and is modelled over two positions, each at half occupancy. Bond and thermal restraints (DFIX and ISOR) are placed on these molecules. All non H-atoms are refined anisotropically. All H-atoms are placed in calculated positions, except for some of the H-atoms found on the tea arms which were found. ; _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^)+(0.0787P)^2^+2.2579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18804 _refine_ls_number_parameters 807 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.32737(4) 1.32520(3) 0.39910(3) 0.02539(12) Uani 1 1 d . . . Co2 Co 0.32383(4) 0.93677(3) 0.31075(3) 0.02222(11) Uani 1 1 d . . . Mn1 Mn 0.25685(4) 1.28344(3) 0.24417(3) 0.02674(13) Uani 1 1 d . . . Mn2 Mn 0.27161(4) 1.08184(3) 0.20120(3) 0.02501(13) Uani 1 1 d . . . Mn3 Mn 0.37362(4) 1.12626(3) 0.34698(3) 0.02171(12) Uani 1 1 d . . . O1 O 0.3526(3) 1.40353(18) 0.20645(19) 0.0417(7) Uani 1 1 d D . . O2 O 0.3413(2) 1.18294(15) 0.15202(15) 0.0266(5) Uani 1 1 d . . . O3 O 0.0606(2) 1.30731(19) 0.2678(2) 0.0426(7) Uani 1 1 d D . . O4 O 0.2272(2) 1.15637(15) 0.29330(15) 0.0223(5) Uani 1 1 d . . . O5 O 0.1129(2) 1.10541(17) 0.17465(17) 0.0369(6) Uani 1 1 d . . . O6 O 0.3348(2) 1.01255(18) 0.10644(17) 0.0384(6) Uani 1 1 d . . . O7 O 0.2103(2) 0.98576(15) 0.26846(15) 0.0268(5) Uani 1 1 d . . . O8 O 0.41229(19) 1.02382(14) 0.25039(15) 0.0250(5) Uani 1 1 d . . . O9 O 0.2042(2) 1.34174(17) 0.35819(17) 0.0336(6) Uani 1 1 d . . . O10 O 0.2902(2) 1.21703(15) 0.43992(15) 0.0276(5) Uani 1 1 d . . . O11 O 0.4547(2) 1.30763(15) 0.43963(16) 0.0287(6) Uani 1 1 d . . . O12 O 0.1790(4) 1.4222(4) 0.6857(3) 0.1100(19) Uani 1 1 d . . . H12 H 0.1132 1.4211 0.7174 0.132 Uiso 1 1 calc R . . O13 O 0.3701(2) 1.43381(16) 0.35324(17) 0.0319(6) Uani 1 1 d . . . O14 O 0.4691(2) 1.0572(2) 0.42949(17) 0.0315(6) Uani 1 1 d . . . O15 O 0.43861(19) 0.89458(15) 0.35731(16) 0.0285(6) Uani 1 1 d . . . O16 O 0.3774(2) 0.85378(15) 0.22509(15) 0.0294(5) Uani 1 1 d . . . O17 O 0.1912(3) 0.63158(17) 0.4210(2) 0.0443(7) Uani 1 1 d . . . H17 H 0.1779 0.6164 0.3810 0.053 Uiso 1 1 calc R . . O18 O 0.27581(19) 1.01874(15) 0.39417(15) 0.0240(5) Uani 1 1 d . . . O19 O 0.40650(19) 1.26110(15) 0.30032(15) 0.0254(5) Uani 1 1 d . . . N1 N 0.2223(3) 1.3394(2) 0.1246(2) 0.0397(8) Uani 1 1 d . . . N2 N 0.2149(2) 1.37563(19) 0.5011(2) 0.0289(7) Uani 1 1 d . . . N3 N 0.5768(2) 1.11797(18) 0.27454(18) 0.0258(6) Uani 1 1 d . . . N4 N 0.2018(2) 0.86763(17) 0.37743(17) 0.0228(6) Uani 1 1 d . . . C1 C 0.2978(4) 1.4084(3) 0.0921(3) 0.0488(12) Uani 1 1 d . . . H1A H 0.2655 1.4451 0.0580 0.059 Uiso 1 1 calc R . . H1B H 0.3743 1.3825 0.0599 0.059 Uiso 1 1 calc R . . C2 C 0.3082(4) 1.4620(3) 0.1580(3) 0.0474(11) Uani 1 1 d . . . H2A H 0.3607 1.5054 0.1366 0.057 Uiso 1 1 calc R . . H2B H 0.2329 1.4911 0.1890 0.057 Uiso 1 1 calc R . . C3 C 0.0986(4) 1.3750(3) 0.1451(3) 0.0515(12) Uani 1 1 d . . . H3A H 0.0782 1.3805 0.0965 0.062 Uiso 1 1 calc R . . H3B H 0.0878 1.4325 0.1690 0.062 Uiso 1 1 calc R . . C4 C 0.0198(4) 1.3187(3) 0.2018(3) 0.0482(11) Uani 1 1 d . . . H4A H -0.0596 1.3462 0.2189 0.058 Uiso 1 1 calc R . . H4B H 0.0223 1.2633 0.1764 0.058 Uiso 1 1 calc R . . C5 C 0.2514(4) 1.2649(3) 0.0680(3) 0.0434(10) Uani 1 1 d . . . H5A H 0.2667 1.2859 0.0140 0.052 Uiso 1 1 calc R . . H5B H 0.1857 1.2315 0.0800 0.052 Uiso 1 1 calc R . . C6 C 0.3569(3) 1.2070(3) 0.0725(2) 0.0347(9) Uani 1 1 d . . . H6A H 0.3687 1.1555 0.0392 0.042 Uiso 1 1 calc R . . H6B H 0.4253 1.2374 0.0526 0.042 Uiso 1 1 calc R . . C7 C -0.0369(4) 1.0776(3) 0.1269(3) 0.0551(13) Uani 1 1 d . . . H7A H -0.0881 1.0555 0.1747 0.083 Uiso 1 1 calc R . . H7B H -0.0442 1.0495 0.0811 0.083 Uiso 1 1 calc R . . H7C H -0.0571 1.1389 0.1248 0.083 Uiso 1 1 calc R . . C8 C 0.0863(4) 1.0603(3) 0.1267(3) 0.0408(10) Uani 1 1 d . . . C9 C 0.1633(4) 0.9954(3) 0.0754(3) 0.0457(11) Uani 1 1 d . . . H9 H 0.1336 0.9635 0.0441 0.055 Uiso 1 1 calc R . . C10 C 0.2796(4) 0.9751(3) 0.0677(3) 0.0446(11) Uani 1 1 d . . . C11 C 0.3536(5) 0.9050(3) 0.0123(3) 0.0609(14) Uani 1 1 d . . . H11A H 0.4201 0.9280 -0.0242 0.091 Uiso 1 1 calc R . . H11B H 0.3097 0.8819 -0.0172 0.091 Uiso 1 1 calc R . . H11C H 0.3789 0.8598 0.0424 0.091 Uiso 1 1 calc R . . C12 C 0.1357(3) 0.9244(2) 0.2664(3) 0.0347(9) Uani 1 1 d . . . H12A H 0.1758 0.8795 0.2265 0.042 Uiso 1 1 calc R . . H12B H 0.0689 0.9517 0.2536 0.042 Uiso 1 1 calc R . . C13 C 0.0983(3) 0.8868(2) 0.3488(2) 0.0286(8) Uani 1 1 d . . . H13A H 0.0637 0.8339 0.3474 0.034 Uiso 1 1 calc R . . H13B H 0.0403 0.9276 0.3856 0.034 Uiso 1 1 calc R . . C14 C 0.1756(3) 0.9035(2) 0.4600(2) 0.0270(7) Uani 1 1 d . . . H14A H 0.2340 0.8789 0.4827 0.032 Uiso 1 1 calc R . . H14B H 0.1004 0.8890 0.4939 0.032 Uiso 1 1 calc R . . C15 C 0.1754(3) 1.0011(2) 0.4553(2) 0.0287(8) Uani 1 1 d . . . H15A H 0.1069 1.0270 0.4439 0.034 Uiso 1 1 calc R . . H15B H 0.1746 1.0250 0.5058 0.034 Uiso 1 1 calc R . . C16 C 0.2382(3) 0.7729(2) 0.3739(2) 0.0286(8) Uani 1 1 d . . . H16A H 0.3140 0.7636 0.3806 0.034 Uiso 1 1 calc R . . H16B H 0.2464 0.7509 0.3211 0.034 Uiso 1 1 calc R . . C17 C 0.1557(3) 0.7201(2) 0.4359(3) 0.0337(9) Uani 1 1 d . . . H17A H 0.1549 0.7356 0.4890 0.040 Uiso 1 1 calc R . . H17B H 0.0775 0.7333 0.4338 0.040 Uiso 1 1 calc R . . C18 C 0.4800(5) 0.7327(3) 0.1456(3) 0.0542(13) Uani 1 1 d . . . H18A H 0.4091 0.7089 0.1504 0.081 Uiso 1 1 calc R . . H18B H 0.5392 0.6867 0.1454 0.081 Uiso 1 1 calc R . . H18C H 0.5042 0.7637 0.0967 0.081 Uiso 1 1 calc R . . C19 C 0.4606(3) 0.7935(2) 0.2150(3) 0.0379(10) Uani 1 1 d . . . C20 C 0.5304(3) 0.7806(3) 0.2637(3) 0.0401(10) Uani 1 1 d . . . H20 H 0.5898 0.7350 0.2502 0.048 Uiso 1 1 calc R . . C21 C 0.5175(3) 0.8308(2) 0.3301(3) 0.0358(9) Uani 1 1 d . . . C22 C 0.5981(3) 0.8119(3) 0.3783(3) 0.0489(12) Uani 1 1 d . . . H22A H 0.6336 0.8630 0.3822 0.073 Uiso 1 1 calc R . . H22B H 0.6572 0.7660 0.3525 0.073 Uiso 1 1 calc R . . H22C H 0.5547 0.7947 0.4309 0.073 Uiso 1 1 calc R . . C23 C 0.5290(3) 1.0034(2) 0.1988(2) 0.0270(7) Uani 1 1 d . . . H23A H 0.5298 0.9873 0.1459 0.032 Uiso 1 1 calc R . . H23B H 0.5669 0.9550 0.2196 0.032 Uiso 1 1 calc R . . C24 C 0.5924(3) 1.0828(2) 0.1946(2) 0.0261(7) Uani 1 1 d . . . H24A H 0.6745 1.0675 0.1666 0.031 Uiso 1 1 calc R . . H24B H 0.5635 1.1269 0.1644 0.031 Uiso 1 1 calc R . . C25 C 0.6443(3) 1.0614(3) 0.3155(2) 0.0333(9) Uani 1 1 d . . . H25A H 0.7230 1.0768 0.3000 0.040 Uiso 1 1 calc R . . H25B H 0.6478 1.0016 0.2990 0.040 Uiso 1 1 calc R . . C26 C 0.5899(3) 1.0702(3) 0.4046(2) 0.0329(9) Uani 1 1 d . . . H26A H 0.6306 1.0280 0.4298 0.040 Uiso 1 1 calc R . . H26B H 0.5976 1.1275 0.4219 0.040 Uiso 1 1 calc R . . C27 C 0.6100(3) 1.2068(2) 0.2695(2) 0.0296(8) Uani 1 1 d . . . H27A H 0.6847 1.2083 0.2282 0.036 Uiso 1 1 calc R . . H27B H 0.6180 1.2232 0.3199 0.036 Uiso 1 1 calc R . . C28 C 0.5211(3) 1.2713(2) 0.2507(2) 0.0275(8) Uani 1 1 d . . . H28A H 0.5380 1.3296 0.2580 0.033 Uiso 1 1 calc R . . H28B H 0.5268 1.2638 0.1952 0.033 Uiso 1 1 calc R . . C29 C 0.6257(4) 1.3284(3) 0.4661(3) 0.0455(11) Uani 1 1 d . . . H29A H 0.5996 1.2844 0.5045 0.068 Uiso 1 1 calc R . . H29B H 0.6432 1.3764 0.4920 0.068 Uiso 1 1 calc R . . H29C H 0.6942 1.3050 0.4242 0.068 Uiso 1 1 calc R . . C30 C 0.5320(3) 1.3585(2) 0.4313(2) 0.0313(8) Uani 1 1 d . . . C31 C 0.5360(3) 1.4377(3) 0.3927(3) 0.0379(9) Uani 1 1 d . . . H31 H 0.5949 1.4708 0.3925 0.045 Uiso 1 1 calc R . . C32 C 0.4587(3) 1.4703(2) 0.3548(3) 0.0331(9) Uani 1 1 d . . . C33 C 0.4743(4) 1.5537(3) 0.3115(3) 0.0462(11) Uani 1 1 d . . . H33A H 0.4930 1.5426 0.2552 0.069 Uiso 1 1 calc R . . H33B H 0.5363 1.5797 0.3209 0.069 Uiso 1 1 calc R . . H33C H 0.4037 1.5922 0.3305 0.069 Uiso 1 1 calc R . . C34 C 0.1893(3) 1.2209(2) 0.5042(2) 0.0355(9) Uani 1 1 d . . . H34A H 0.1903 1.1701 0.5366 0.043 Uiso 1 1 calc R . . H34B H 0.1228 1.2225 0.4857 0.043 Uiso 1 1 calc R . . C35 C 0.1803(4) 1.3010(2) 0.5528(3) 0.0410(10) Uani 1 1 d . . . H35A H 0.1009 1.3142 0.5880 0.049 Uiso 1 1 calc R . . H35B H 0.2299 1.2908 0.5857 0.049 Uiso 1 1 calc R . . C36 C 0.1167(4) 1.4201(3) 0.4794(3) 0.0517(12) Uani 1 1 d . . . H36A H 0.0467 1.4239 0.5256 0.062 Uiso 1 1 calc R . . H36B H 0.1327 1.4786 0.4631 0.062 Uiso 1 1 calc R . . C37 C 0.0985(4) 1.3736(3) 0.4146(3) 0.0530(13) Uani 1 1 d . . . H37A H 0.0540 1.3257 0.4362 0.064 Uiso 1 1 calc R . . H37B H 0.0542 1.4121 0.3890 0.064 Uiso 1 1 calc R . . C38 C 0.2581(4) 1.4402(4) 0.5427(4) 0.0678(17) Uani 1 1 d . . . H38A H 0.2796 1.4882 0.5071 0.081 Uiso 1 1 calc R . . H38B H 0.3282 1.4134 0.5513 0.081 Uiso 1 1 calc R . . C39 C 0.1750(5) 1.4768(4) 0.6223(4) 0.078(2) Uani 1 1 d . . . H39A H 0.1949 1.5333 0.6321 0.094 Uiso 1 1 calc R . . H39B H 0.0965 1.4842 0.6199 0.094 Uiso 1 1 calc R . . H1 H 0.343(6) 1.419(4) 0.2568(14) 0.094 Uiso 1 1 d D . . H3 H 0.037(5) 1.259(2) 0.294(3) 0.094 Uiso 1 1 d D . . H4 H 0.162(5) 1.150(4) 0.326(4) 0.078(19) Uiso 1 1 d . . . H22 H 0.460(3) 1.014(3) 0.424(2) 0.021(11) Uiso 1 1 d . . . Cl5' Cl 0.2473(8) 1.5520(5) 0.8538(7) 0.248(5) Uani 0.50 1 d PD A 2 Cl6' Cl 0.1996(5) 1.3733(3) 0.8845(3) 0.1321(18) Uani 0.50 1 d PD A 2 C3' C 0.2762(7) 1.4518(6) 0.8811(6) 0.062(3) Uani 0.50 1 d PDU A 2 H3'1 H 0.3539 1.4317 0.8463 0.074 Uiso 0.50 1 calc PR A 2 H3'2 H 0.2816 1.4570 0.9343 0.074 Uiso 0.50 1 calc PR A 2 Cl1S Cl 0.12052(15) 1.14402(16) -0.24620(13) 0.1068(7) Uani 1 1 d . . . Cl2S Cl 0.1596(2) 1.14623(15) -0.09410(15) 0.1228(8) Uani 1 1 d . . . Cl3S Cl 0.63366(17) 1.35696(16) 0.02148(15) 0.1206(8) Uani 1 1 d . . . Cl4S Cl 0.8474(2) 1.26529(19) 0.03092(18) 0.1502(11) Uani 1 1 d . . . Cl5S Cl 0.2757(13) 1.4786(12) 0.8734(12) 0.384(10) Uani 0.50 1 d PDU B 1 Cl6S Cl 0.0383(6) 1.4413(5) 0.9515(3) 0.183(3) Uani 0.50 1 d PD . 1 O1S O 0.1774(5) 0.6834(3) 0.2159(3) 0.1033(18) Uani 1 1 d . . . O2S O 0.0804(3) 0.6030(3) 0.3094(2) 0.0712(11) Uani 1 1 d . . . O3S O 0.0350(5) 0.6256(3) 0.2014(3) 0.1001(16) Uani 1 1 d . . . O4S O -0.0113(2) 1.17634(19) 0.37219(17) 0.0403(7) Uani 1 1 d . . . O5S O -0.1488(3) 1.1913(2) 0.3201(2) 0.0587(9) Uani 1 1 d . . . O6S O -0.0941(3) 1.0639(2) 0.35510(19) 0.0479(8) Uani 1 1 d . . . N1S N 0.0971(5) 0.6392(3) 0.2420(3) 0.0690(14) Uani 1 1 d . . . N2S N -0.0860(3) 1.1432(2) 0.3485(2) 0.0384(8) Uani 1 1 d . . . C1S C 0.0869(13) 1.1921(7) -0.1563(6) 0.206(7) Uani 1 1 d . . . H1S1 H 0.0042 1.1920 -0.1293 0.247 Uiso 1 1 calc R . . H1S2 H 0.1023 1.2521 -0.1642 0.247 Uiso 1 1 calc R . . C2S C 0.7821(7) 1.3363(6) -0.0235(5) 0.129(4) Uani 1 1 d . . . H2S1 H 0.8161 1.3905 -0.0294 0.155 Uiso 1 1 calc R . . H2S2 H 0.7982 1.3115 -0.0765 0.155 Uiso 1 1 calc R . . C3S C 0.1446(9) 1.4733(7) 0.8653(6) 0.076(4) Uani 0.50 1 d PD B 1 H3S1 H 0.1528 1.4329 0.8220 0.092 Uiso 0.50 1 calc PR B 1 H3S2 H 0.1169 1.5298 0.8504 0.092 Uiso 0.50 1 calc PR B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0190(2) 0.0212(2) 0.0355(3) 0.0044(2) -0.0079(2) -0.00385(17) Co2 0.0180(2) 0.0206(2) 0.0247(3) 0.00646(18) -0.00334(18) -0.00029(16) Mn1 0.0243(3) 0.0256(3) 0.0321(3) 0.0099(2) -0.0118(2) -0.0039(2) Mn2 0.0239(2) 0.0235(3) 0.0252(3) 0.0072(2) -0.0058(2) -0.0004(2) Mn3 0.0168(2) 0.0215(3) 0.0259(3) 0.0067(2) -0.0061(2) -0.00193(18) O1 0.0421(16) 0.0345(15) 0.0497(19) 0.0174(14) -0.0173(15) -0.0047(12) O2 0.0280(12) 0.0281(13) 0.0224(13) 0.0110(10) -0.0073(10) -0.0023(10) O3 0.0335(14) 0.0422(17) 0.058(2) 0.0145(15) -0.0241(15) -0.0039(12) O4 0.0189(11) 0.0228(12) 0.0241(14) 0.0034(10) -0.0055(10) -0.0024(9) O5 0.0417(15) 0.0340(15) 0.0425(18) 0.0066(13) -0.0240(14) -0.0052(12) O6 0.0424(16) 0.0415(16) 0.0280(16) 0.0037(12) -0.0076(13) -0.0032(13) O7 0.0254(12) 0.0266(12) 0.0284(14) 0.0081(10) -0.0091(11) -0.0026(10) O8 0.0186(11) 0.0226(12) 0.0285(14) 0.0080(10) -0.0014(10) -0.0003(9) O9 0.0192(11) 0.0357(14) 0.0449(17) 0.0029(12) -0.0108(11) 0.0016(10) O10 0.0236(11) 0.0220(12) 0.0334(15) 0.0009(10) -0.0025(11) -0.0070(9) O11 0.0247(12) 0.0266(13) 0.0366(16) 0.0029(11) -0.0119(11) -0.0047(10) O12 0.075(3) 0.179(6) 0.077(4) -0.060(4) -0.029(3) 0.002(3) O13 0.0265(12) 0.0245(13) 0.0453(17) 0.0079(11) -0.0121(12) -0.0055(10) O14 0.0278(13) 0.0353(16) 0.0329(16) 0.0123(13) -0.0117(12) -0.0057(12) O15 0.0185(11) 0.0286(13) 0.0346(15) 0.0125(11) -0.0052(10) 0.0005(10) O16 0.0283(12) 0.0241(12) 0.0288(15) 0.0039(10) -0.0007(11) -0.0006(10) O17 0.0426(16) 0.0244(14) 0.059(2) 0.0092(13) -0.0078(15) -0.0048(12) O18 0.0199(11) 0.0231(12) 0.0265(14) 0.0070(10) -0.0040(10) -0.0047(9) O19 0.0185(11) 0.0242(12) 0.0316(14) 0.0056(10) -0.0054(10) -0.0034(9) N1 0.0394(18) 0.0353(18) 0.048(2) 0.0150(16) -0.0200(17) -0.0022(15) N2 0.0232(14) 0.0235(15) 0.0387(19) 0.0019(13) -0.0082(13) -0.0029(11) N3 0.0186(13) 0.0263(15) 0.0325(18) 0.0109(13) -0.0083(12) -0.0034(11) N4 0.0180(12) 0.0213(14) 0.0259(16) 0.0044(12) -0.0033(11) -0.0016(10) C1 0.055(3) 0.040(2) 0.054(3) 0.027(2) -0.021(2) -0.009(2) C2 0.054(3) 0.032(2) 0.056(3) 0.014(2) -0.021(2) 0.0015(19) C3 0.042(2) 0.049(3) 0.065(3) 0.022(2) -0.025(2) 0.006(2) C4 0.037(2) 0.057(3) 0.056(3) 0.013(2) -0.024(2) 0.002(2) C5 0.051(3) 0.048(3) 0.035(3) 0.017(2) -0.018(2) -0.011(2) C6 0.040(2) 0.033(2) 0.028(2) 0.0133(16) -0.0068(17) -0.0064(16) C7 0.049(3) 0.066(3) 0.062(3) 0.009(3) -0.032(3) -0.015(2) C8 0.048(2) 0.042(2) 0.043(3) 0.014(2) -0.027(2) -0.0150(19) C9 0.063(3) 0.047(3) 0.035(3) 0.004(2) -0.024(2) -0.013(2) C10 0.064(3) 0.038(2) 0.033(2) 0.0133(19) -0.015(2) -0.013(2) C11 0.084(4) 0.056(3) 0.035(3) -0.003(2) -0.012(3) 0.003(3) C12 0.035(2) 0.032(2) 0.040(2) 0.0080(17) -0.0149(18) -0.0096(16) C13 0.0221(16) 0.0263(18) 0.038(2) 0.0083(15) -0.0102(15) -0.0041(13) C14 0.0266(16) 0.0275(18) 0.025(2) 0.0087(15) -0.0045(14) -0.0063(14) C15 0.0269(17) 0.0271(18) 0.027(2) 0.0026(15) -0.0004(15) -0.0059(14) C16 0.0246(16) 0.0219(17) 0.034(2) 0.0079(15) -0.0027(15) -0.0035(13) C17 0.0271(17) 0.0242(18) 0.044(2) 0.0085(16) -0.0040(17) -0.0037(14) C18 0.068(3) 0.033(2) 0.041(3) 0.001(2) 0.005(2) 0.009(2) C19 0.034(2) 0.0242(19) 0.038(2) 0.0084(16) 0.0096(17) 0.0001(15) C20 0.0288(19) 0.0264(19) 0.052(3) 0.0135(19) 0.0018(18) 0.0058(15) C21 0.0218(16) 0.030(2) 0.046(3) 0.0196(18) -0.0003(17) 0.0011(15) C22 0.0251(19) 0.051(3) 0.066(3) 0.026(2) -0.013(2) 0.0055(18) C23 0.0183(15) 0.0237(17) 0.033(2) 0.0055(15) -0.0013(14) 0.0015(13) C24 0.0192(15) 0.0289(18) 0.0253(19) 0.0095(15) -0.0008(14) -0.0028(13) C25 0.0213(16) 0.038(2) 0.041(2) 0.0139(18) -0.0118(16) -0.0024(15) C26 0.0253(17) 0.042(2) 0.036(2) 0.0137(18) -0.0156(16) -0.0066(15) C27 0.0210(15) 0.0311(19) 0.035(2) 0.0092(16) -0.0060(15) -0.0055(14) C28 0.0204(15) 0.0270(18) 0.033(2) 0.0098(15) -0.0063(15) -0.0043(13) C29 0.039(2) 0.046(2) 0.064(3) 0.007(2) -0.031(2) -0.0121(19) C30 0.0283(18) 0.034(2) 0.034(2) -0.0012(16) -0.0128(16) -0.0062(15) C31 0.0308(19) 0.034(2) 0.052(3) 0.0047(19) -0.0152(19) -0.0126(16) C32 0.0279(18) 0.0229(18) 0.043(2) 0.0016(16) -0.0030(17) -0.0050(14) C33 0.044(2) 0.026(2) 0.067(3) 0.015(2) -0.015(2) -0.0103(17) C34 0.0328(19) 0.0250(18) 0.036(2) 0.0072(16) 0.0056(17) -0.0019(15) C35 0.056(3) 0.028(2) 0.033(2) 0.0063(17) -0.010(2) 0.0069(18) C36 0.047(3) 0.052(3) 0.048(3) 0.007(2) -0.014(2) 0.025(2) C37 0.029(2) 0.074(3) 0.054(3) 0.002(3) -0.018(2) 0.018(2) C38 0.039(2) 0.067(3) 0.083(4) -0.042(3) 0.007(3) -0.023(2) C39 0.041(3) 0.093(5) 0.091(5) -0.051(4) 0.000(3) -0.025(3) Cl5' 0.180(7) 0.167(7) 0.374(15) -0.077(9) -0.049(8) -0.045(6) Cl6' 0.152(4) 0.133(4) 0.127(4) 0.022(3) -0.080(4) 0.026(3) C3' 0.023(3) 0.129(8) 0.018(4) -0.003(5) -0.004(3) 0.044(5) Cl1S 0.0631(10) 0.1613(19) 0.0992(15) -0.0055(13) -0.0217(10) -0.0405(11) Cl2S 0.158(2) 0.1055(16) 0.1143(18) -0.0152(13) -0.0660(16) 0.0121(15) Cl3S 0.0702(11) 0.1398(19) 0.141(2) 0.0381(16) -0.0193(12) -0.0179(12) Cl4S 0.135(2) 0.157(2) 0.151(2) 0.0646(19) -0.0525(18) 0.0266(18) Cl5S 0.395(13) 0.390(13) 0.332(12) 0.032(9) -0.098(9) 0.033(9) Cl6S 0.184(6) 0.276(8) 0.121(4) 0.097(5) -0.087(5) -0.054(6) O1S 0.129(4) 0.079(3) 0.083(3) -0.009(2) 0.009(3) -0.065(3) O2S 0.071(3) 0.076(3) 0.056(3) -0.004(2) 0.000(2) -0.027(2) O3S 0.105(4) 0.106(4) 0.108(4) 0.032(3) -0.057(3) -0.026(3) O4S 0.0281(13) 0.0561(18) 0.0361(17) 0.0014(14) -0.0071(12) -0.0131(13) O5S 0.0506(19) 0.060(2) 0.076(3) 0.0143(18) -0.0354(19) -0.0021(16) O6S 0.0537(19) 0.0441(18) 0.050(2) 0.0069(15) -0.0202(16) -0.0129(14) N1S 0.076(3) 0.043(2) 0.068(4) -0.006(2) 0.007(3) -0.014(2) N2S 0.0275(16) 0.046(2) 0.042(2) 0.0037(16) -0.0111(15) -0.0063(14) C1S 0.37(2) 0.124(8) 0.088(7) -0.018(6) -0.073(10) 0.116(10) C2S 0.096(6) 0.157(8) 0.108(7) 0.071(6) -0.010(5) 0.013(6) C3S 0.103(10) 0.057(7) 0.096(10) 0.001(6) -0.076(9) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O10 1.863(2) . ? Co1 O9 1.868(2) . ? Co1 O11 1.912(2) . ? Co1 O13 1.912(2) . ? Co1 O19 1.929(3) . ? Co1 N2 1.988(3) . ? Co2 O18 1.863(3) . ? Co2 O7 1.872(2) . ? Co2 O16 1.901(3) . ? Co2 O15 1.904(2) . ? Co2 O8 1.915(2) . ? Co2 N4 1.986(3) . ? Mn1 O9 2.094(3) . ? Mn1 O4 2.164(2) . ? Mn1 O2 2.188(3) . ? Mn1 O1 2.288(3) . ? Mn1 O3 2.291(3) . ? Mn1 O19 2.347(2) . ? Mn1 N1 2.421(3) . ? Mn2 O6 1.896(3) . ? Mn2 O4 1.906(3) . ? Mn2 O2 1.929(2) . ? Mn2 O7 1.954(2) . ? Mn2 O5 2.138(3) . ? Mn2 O8 2.270(2) . ? Mn3 O10 2.096(3) . ? Mn3 O18 2.161(2) . ? Mn3 O8 2.251(3) . ? Mn3 O19 2.269(2) . ? Mn3 O4 2.292(2) . ? Mn3 O14 2.333(3) . ? Mn3 N3 2.390(3) . ? O1 C2 1.425(5) . ? O1 H1 0.891(10) . ? O2 C6 1.407(4) . ? O3 C4 1.415(5) . ? O3 H3 0.895(10) . ? O4 H4 0.83(6) . ? O5 C8 1.252(5) . ? O6 C10 1.292(5) . ? O7 C12 1.399(4) . ? O8 C23 1.427(4) . ? O9 C37 1.396(5) . ? O10 C34 1.376(4) . ? O11 C30 1.271(4) . ? O12 C39 1.408(9) . ? O12 H12 0.8200 . ? O13 C32 1.287(4) . ? O14 C26 1.437(4) . ? O14 H22 0.71(4) . ? O15 C21 1.284(4) . ? O16 C19 1.274(5) . ? O17 C17 1.398(4) . ? O17 H17 0.8200 . ? O18 C15 1.399(4) . ? O19 C28 1.417(4) . ? N1 C5 1.476(6) . ? N1 C1 1.480(5) . ? N1 C3 1.482(5) . ? N2 C36 1.477(5) . ? N2 C35 1.478(5) . ? N2 C38 1.490(5) . ? N3 C24 1.470(5) . ? N3 C27 1.474(4) . ? N3 C25 1.480(4) . ? N4 C16 1.486(4) . ? N4 C14 1.492(5) . ? N4 C13 1.512(4) . ? C1 C2 1.489(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.494(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.514(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.502(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.410(7) . ? C9 C10 1.387(7) . ? C9 H9 0.9300 . ? C10 C11 1.484(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.509(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.516(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.526(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.500(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.398(6) . ? C20 C21 1.376(6) . ? C20 H20 0.9300 . ? C21 C22 1.505(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.517(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.500(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.511(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.501(5) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.395(5) . ? C31 C32 1.379(5) . ? C31 H31 0.9300 . ? C32 C33 1.494(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.496(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.454(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.518(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? Cl5' C3' 1.658(9) . ? Cl6' C3' 1.608(8) . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? Cl1S C1S 1.673(10) . ? Cl2S C1S 1.730(10) . ? Cl3S C2S 1.726(8) . ? Cl4S C2S 1.749(7) . ? Cl5S C3S 1.670(9) . ? Cl6S C3S 1.759(9) . ? Cl6S Cl6S 2.412(16) 2_587 ? O1S N1S 1.223(6) . ? O2S N1S 1.275(6) . ? O3S N1S 1.240(7) . ? O4S N2S 1.281(4) . ? O5S N2S 1.232(4) . ? O6S N2S 1.247(4) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? 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 O10 Co1 O9 93.73(11) . . ? O10 Co1 O11 86.31(10) . . ? O9 Co1 O11 179.24(12) . . ? O10 Co1 O13 177.58(12) . . ? O9 Co1 O13 86.49(11) . . ? O11 Co1 O13 93.45(10) . . ? O10 Co1 O19 84.25(10) . . ? O9 Co1 O19 84.00(11) . . ? O11 Co1 O19 95.25(10) . . ? O13 Co1 O19 93.38(11) . . ? O10 Co1 N2 86.86(11) . . ? O9 Co1 N2 86.33(12) . . ? O11 Co1 N2 94.43(12) . . ? O13 Co1 N2 95.56(12) . . ? O19 Co1 N2 166.39(10) . . ? O18 Co2 O7 91.44(11) . . ? O18 Co2 O16 178.32(10) . . ? O7 Co2 O16 89.69(11) . . ? O18 Co2 O15 84.87(11) . . ? O7 Co2 O15 175.99(11) . . ? O16 Co2 O15 93.97(11) . . ? O18 Co2 O8 85.05(10) . . ? O7 Co2 O8 83.67(10) . . ? O16 Co2 O8 93.83(10) . . ? O15 Co2 O8 94.42(10) . . ? O18 Co2 N4 87.42(11) . . ? O7 Co2 N4 85.77(11) . . ? O16 Co2 N4 93.91(11) . . ? O15 Co2 N4 95.62(10) . . ? O8 Co2 N4 166.86(11) . . ? O9 Mn1 O4 92.08(10) . . ? O9 Mn1 O2 156.55(9) . . ? O4 Mn1 O2 69.75(9) . . ? O9 Mn1 O1 83.64(11) . . ? O4 Mn1 O1 157.11(10) . . ? O2 Mn1 O1 107.17(10) . . ? O9 Mn1 O3 80.31(11) . . ? O4 Mn1 O3 86.81(9) . . ? O2 Mn1 O3 112.15(10) . . ? O1 Mn1 O3 114.41(10) . . ? O9 Mn1 O19 69.53(9) . . ? O4 Mn1 O19 80.20(8) . . ? O2 Mn1 O19 92.16(9) . . ? O1 Mn1 O19 77.23(9) . . ? O3 Mn1 O19 146.48(10) . . ? O9 Mn1 N1 128.44(11) . . ? O4 Mn1 N1 126.80(11) . . ? O2 Mn1 N1 75.02(11) . . ? O1 Mn1 N1 71.31(11) . . ? O3 Mn1 N1 71.01(11) . . ? O19 Mn1 N1 140.25(10) . . ? O6 Mn2 O4 172.69(11) . . ? O6 Mn2 O2 93.90(11) . . ? O4 Mn2 O2 80.90(10) . . ? O6 Mn2 O7 94.34(11) . . ? O4 Mn2 O7 90.18(11) . . ? O2 Mn2 O7 168.85(10) . . ? O6 Mn2 O5 88.66(12) . . ? O4 Mn2 O5 97.12(11) . . ? O2 Mn2 O5 98.01(10) . . ? O7 Mn2 O5 89.68(10) . . ? O6 Mn2 O8 92.03(11) . . ? O4 Mn2 O8 83.78(9) . . ? O2 Mn2 O8 99.20(9) . . ? O7 Mn2 O8 73.01(9) . . ? O5 Mn2 O8 162.68(9) . . ? O10 Mn3 O18 98.87(9) . . ? O10 Mn3 O8 164.12(8) . . ? O18 Mn3 O8 70.73(9) . . ? O10 Mn3 O19 71.18(9) . . ? O18 Mn3 O19 157.87(8) . . ? O8 Mn3 O19 114.01(9) . . ? O10 Mn3 O4 90.67(9) . . ? O18 Mn3 O4 81.20(8) . . ? O8 Mn3 O4 76.15(8) . . ? O19 Mn3 O4 79.26(8) . . ? O10 Mn3 O14 88.33(11) . . ? O18 Mn3 O14 75.85(9) . . ? O8 Mn3 O14 100.23(10) . . ? O19 Mn3 O14 122.22(9) . . ? O4 Mn3 O14 156.58(9) . . ? O10 Mn3 N3 122.62(10) . . ? O18 Mn3 N3 126.51(9) . . ? O8 Mn3 N3 72.94(9) . . ? O19 Mn3 N3 74.11(9) . . ? O4 Mn3 N3 125.54(10) . . ? O14 Mn3 N3 73.52(10) . . ? C2 O1 Mn1 115.2(2) . . ? C2 O1 H1 120(4) . . ? Mn1 O1 H1 93(4) . . ? C6 O2 Mn2 125.0(2) . . ? C6 O2 Mn1 116.3(2) . . ? Mn2 O2 Mn1 102.06(11) . . ? C4 O3 Mn1 118.7(3) . . ? C4 O3 H3 110(4) . . ? Mn1 O3 H3 101(4) . . ? Mn2 O4 Mn1 103.72(11) . . ? Mn2 O4 Mn3 104.31(10) . . ? Mn1 O4 Mn3 102.65(9) . . ? Mn2 O4 H4 114(4) . . ? Mn1 O4 H4 118(4) . . ? Mn3 O4 H4 112(4) . . ? C8 O5 Mn2 124.2(3) . . ? C10 O6 Mn2 128.0(3) . . ? C12 O7 Co2 110.0(2) . . ? C12 O7 Mn2 134.9(2) . . ? Co2 O7 Mn2 108.17(11) . . ? C23 O8 Co2 121.71(19) . . ? C23 O8 Mn3 119.2(2) . . ? Co2 O8 Mn3 99.49(10) . . ? C23 O8 Mn2 120.7(2) . . ? Co2 O8 Mn2 95.15(9) . . ? Mn3 O8 Mn2 94.64(9) . . ? C37 O9 Co1 113.8(3) . . ? C37 O9 Mn1 135.9(3) . . ? Co1 O9 Mn1 108.93(12) . . ? C34 O10 Co1 113.5(2) . . ? C34 O10 Mn3 134.0(2) . . ? Co1 O10 Mn3 106.47(12) . . ? C30 O11 Co1 125.8(2) . . ? C39 O12 H12 109.5 . . ? C32 O13 Co1 126.0(2) . . ? C26 O14 Mn3 112.3(2) . . ? C26 O14 H22 113(3) . . ? Mn3 O14 H22 99(3) . . ? C21 O15 Co2 125.5(3) . . ? C19 O16 Co2 125.8(3) . . ? C17 O17 H17 109.5 . . ? C15 O18 Co2 113.3(2) . . ? C15 O18 Mn3 139.9(2) . . ? Co2 O18 Mn3 104.48(11) . . ? C28 O19 Co1 124.1(2) . . ? C28 O19 Mn3 116.42(19) . . ? Co1 O19 Mn3 97.94(10) . . ? C28 O19 Mn1 118.0(2) . . ? Co1 O19 Mn1 97.50(9) . . ? Mn3 O19 Mn1 97.85(8) . . ? C5 N1 C1 111.1(4) . . ? C5 N1 C3 111.6(3) . . ? C1 N1 C3 109.9(3) . . ? C5 N1 Mn1 105.7(2) . . ? C1 N1 Mn1 109.5(2) . . ? C3 N1 Mn1 109.0(3) . . ? C36 N2 C35 111.8(3) . . ? C36 N2 C38 107.8(4) . . ? C35 N2 C38 110.6(4) . . ? C36 N2 Co1 105.3(3) . . ? C35 N2 Co1 105.5(2) . . ? C38 N2 Co1 115.9(2) . . ? C24 N3 C27 110.8(3) . . ? C24 N3 C25 111.0(3) . . ? C27 N3 C25 110.6(3) . . ? C24 N3 Mn3 106.34(19) . . ? C27 N3 Mn3 107.4(2) . . ? C25 N3 Mn3 110.6(2) . . ? C16 N4 C14 110.9(3) . . ? C16 N4 C13 110.5(3) . . ? C14 N4 C13 110.9(3) . . ? C16 N4 Co2 114.2(2) . . ? C14 N4 Co2 103.69(19) . . ? C13 N4 Co2 106.48(19) . . ? N1 C1 C2 110.7(4) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 106.1(3) . . ? O1 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O1 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? N1 C3 C4 111.8(3) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 106.3(4) . . ? O3 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O3 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? N1 C5 C6 111.5(3) . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? O2 C6 C5 110.3(3) . . ? O2 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O2 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 C9 124.1(4) . . ? O5 C8 C7 115.9(4) . . ? C9 C8 C7 120.0(4) . . ? C10 C9 C8 125.6(4) . . ? C10 C9 H9 117.2 . . ? C8 C9 H9 117.2 . . ? O6 C10 C9 125.5(4) . . ? O6 C10 C11 113.0(4) . . ? C9 C10 C11 121.5(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O7 C12 C13 105.9(3) . . ? O7 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? O7 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C12 C13 N4 110.0(3) . . ? C12 C13 H13A 109.7 . . ? N4 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? N4 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N4 C14 C15 108.3(3) . . ? N4 C14 H14A 110.0 . . ? C15 C14 H14A 110.0 . . ? N4 C14 H14B 110.0 . . ? C15 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? O18 C15 C14 107.9(3) . . ? O18 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? O18 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N4 C16 C17 115.2(3) . . ? N4 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? N4 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? O17 C17 C16 110.1(3) . . ? O17 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? O17 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O16 C19 C20 124.9(4) . . ? O16 C19 C18 115.2(4) . . ? C20 C19 C18 119.9(4) . . ? C21 C20 C19 124.5(4) . . ? C21 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? O15 C21 C20 125.2(4) . . ? O15 C21 C22 114.4(4) . . ? C20 C21 C22 120.4(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O8 C23 C24 108.1(3) . . ? O8 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O8 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N3 C24 C23 111.9(3) . . ? N3 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? N3 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N3 C25 C26 111.0(3) . . ? N3 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N3 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? O14 C26 C25 111.3(3) . . ? O14 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? O14 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? N3 C27 C28 111.8(3) . . ? N3 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? N3 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? O19 C28 C27 111.9(3) . . ? O19 C28 H28A 109.2 . . ? C27 C28 H28A 109.2 . . ? O19 C28 H28B 109.2 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O11 C30 C31 125.5(3) . . ? O11 C30 C29 115.5(3) . . ? C31 C30 C29 119.1(3) . . ? C32 C31 C30 124.5(3) . . ? C32 C31 H31 117.8 . . ? C30 C31 H31 117.8 . . ? O13 C32 C31 124.7(3) . . ? O13 C32 C33 115.0(4) . . ? C31 C32 C33 120.3(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O10 C34 C35 108.5(3) . . ? O10 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? O10 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? N2 C35 C34 111.3(3) . . ? N2 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? N2 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C37 C36 N2 110.7(4) . . ? C37 C36 H36A 109.5 . . ? N2 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? N2 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? O9 C37 C36 111.1(4) . . ? O9 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? O9 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N2 C38 C39 116.6(4) . . ? N2 C38 H38A 108.1 . . ? C39 C38 H38A 108.1 . . ? N2 C38 H38B 108.1 . . ? C39 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? O12 C39 C38 111.7(6) . . ? O12 C39 H39A 109.3 . . ? C38 C39 H39A 109.3 . . ? O12 C39 H39B 109.3 . . ? C38 C39 H39B 109.3 . . ? H39A C39 H39B 107.9 . . ? Cl6' C3' Cl5' 125.7(6) . . ? Cl6' C3' H3'1 105.9 . . ? Cl5' C3' H3'1 105.9 . . ? Cl6' C3' H3'2 105.9 . . ? Cl5' C3' H3'2 105.9 . . ? H3'1 C3' H3'2 106.2 . . ? C3S Cl6S Cl6S 111.6(6) . 2_587 ? O1S N1S O3S 120.3(6) . . ? O1S N1S O2S 120.2(6) . . ? O3S N1S O2S 119.4(5) . . ? O5S N2S O6S 121.8(3) . . ? O5S N2S O4S 118.5(3) . . ? O6S N2S O4S 119.7(3) . . ? Cl1S C1S Cl2S 116.0(6) . . ? Cl1S C1S H1S1 108.3 . . ? Cl2S C1S H1S1 108.3 . . ? Cl1S C1S H1S2 108.3 . . ? Cl2S C1S H1S2 108.3 . . ? H1S1 C1S H1S2 107.4 . . ? Cl3S C2S Cl4S 112.7(4) . . ? Cl3S C2S H2S1 109.0 . . ? Cl4S C2S H2S1 109.0 . . ? Cl3S C2S H2S2 109.0 . . ? Cl4S C2S H2S2 109.0 . . ? H2S1 C2S H2S2 107.8 . . ? Cl5S C3S Cl6S 115.7(9) . . ? Cl5S C3S H3S1 108.4 . . ? Cl6S C3S H3S1 108.4 . . ? Cl5S C3S H3S2 108.4 . . ? Cl6S C3S H3S2 108.4 . . ? H3S1 C3S H3S2 107.4 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.308 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.108