# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ng, Gary K.-Y.' 'Ziller, Joseph' 'Borovik, Andrew' _publ_contact_author_name 'Borovik, Andrew' _publ_contact_author_email aborovik@uci.edu _publ_section_title ; Preparation and structures of dinuclear complexes containing MII-OH centers ; # Attachment '- 09092011.cif' data_asb180 _database_code_depnum_ccdc_archive 'CCDC 847961' #TrackingRef '- 09092011.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77.50 H105 B Co2 N12 O2.50' _chemical_formula_weight 1373.41 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4546(9) _cell_length_b 15.3395(10) _cell_length_c 19.6642(13) _cell_angle_alpha 99.2803(9) _cell_angle_beta 96.3614(9) _cell_angle_gamma 104.0454(9) _cell_volume 3837.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.76 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1466 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8938 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41752 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15634 _reflns_number_gt 10834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.6703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15634 _refine_ls_number_parameters 881 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.57206(3) 0.35715(2) 0.308719(17) 0.02466(9) Uani 1 1 d . . . Co2 Co 0.25446(3) 0.22190(2) 0.223173(18) 0.02495(9) Uani 1 1 d . . . O1 O 0.53687(14) 0.34237(12) 0.20851(9) 0.0307(4) Uani 1 1 d . . . H1 H 0.4731 0.3172 0.1963 0.046 Uiso 1 1 calc R . . O2 O 0.35586(14) 0.17845(12) 0.17365(9) 0.0316(4) Uani 1 1 d . . . H2 H 0.4154 0.2017 0.1969 0.047 Uiso 1 1 calc R . . N1 N 0.62135(16) 0.37877(14) 0.42159(11) 0.0272(5) Uani 1 1 d . . . N2 N 0.66532(16) 0.49333(14) 0.33364(11) 0.0301(5) Uani 1 1 d . . . N3 N 0.65321(15) 0.25730(14) 0.31705(11) 0.0256(5) Uani 1 1 d . . . N4 N 0.43525(16) 0.33347(14) 0.34653(10) 0.0254(5) Uani 1 1 d . . . N5 N 0.6002(2) 0.53054(17) 0.23198(13) 0.0414(6) Uani 1 1 d . . . H5 H 0.573(2) 0.469(2) 0.2159(14) 0.037(8) Uiso 1 1 d . . . N6 N 0.67546(18) 0.23668(15) 0.20139(11) 0.0306(5) Uani 1 1 d . . . H6 H 0.631(2) 0.271(2) 0.1953(15) 0.042(8) Uiso 1 1 d . . . N7 N 0.13330(16) 0.26441(14) 0.27559(11) 0.0282(5) Uani 1 1 d . . . N8 N 0.19903(17) 0.29913(14) 0.15584(11) 0.0319(5) Uani 1 1 d . . . N9 N 0.14629(16) 0.09545(14) 0.22195(11) 0.0273(5) Uani 1 1 d . . . N10 N 0.33257(15) 0.29578(14) 0.31822(11) 0.0256(5) Uani 1 1 d . . . N11 N 0.2732(2) 0.24311(17) 0.06436(13) 0.0425(6) Uani 1 1 d . . . H11 H 0.305(2) 0.217(2) 0.0964(16) 0.050(9) Uiso 1 1 d . . . N12 N 0.26051(19) 0.00839(16) 0.19735(13) 0.0338(6) Uani 1 1 d . . . H12 H 0.297(2) 0.0538(19) 0.1889(14) 0.028(8) Uiso 1 1 d . . . C1 C 0.7239(2) 0.44580(19) 0.43838(14) 0.0321(6) Uani 1 1 d . . . H1A H 0.7783 0.4141 0.4288 0.038 Uiso 1 1 calc R . . H1B H 0.7374 0.4740 0.4886 0.038 Uiso 1 1 calc R . . C2 C 0.7286(2) 0.51879(18) 0.39594(14) 0.0308(6) Uani 1 1 d . . . C3 C 0.7941(2) 0.60507(19) 0.41897(15) 0.0372(7) Uani 1 1 d . . . H3A H 0.8368 0.6207 0.4633 0.045 Uiso 1 1 calc R . . C4 C 0.7969(2) 0.6689(2) 0.37637(17) 0.0425(7) Uani 1 1 d . . . H4A H 0.8430 0.7285 0.3908 0.051 Uiso 1 1 calc R . . C5 C 0.7338(2) 0.64626(19) 0.31411(16) 0.0417(7) Uani 1 1 d . . . H5A H 0.7349 0.6901 0.2850 0.050 Uiso 1 1 calc R . . C6 C 0.6661(2) 0.55694(19) 0.29247(15) 0.0346(6) Uani 1 1 d . . . C7 C 0.5813(3) 0.5929(2) 0.18692(16) 0.0453(8) Uani 1 1 d . . . H7A H 0.6392 0.6062 0.1599 0.054 Uiso 1 1 calc R . . H7B H 0.5796 0.6514 0.2160 0.054 Uiso 1 1 calc R . . C8 C 0.4796(3) 0.5538(2) 0.13661(15) 0.0408(7) Uani 1 1 d . . . C9 C 0.4830(3) 0.4678(2) 0.08601(15) 0.0495(8) Uani 1 1 d . . . H9A H 0.4913 0.4202 0.1123 0.074 Uiso 1 1 calc R . . H9B H 0.5415 0.4827 0.0606 0.074 Uiso 1 1 calc R . . H9C H 0.4182 0.4454 0.0528 0.074 Uiso 1 1 calc R . . C10 C 0.4665(3) 0.6263(2) 0.09382(18) 0.0642(11) Uani 1 1 d . . . H10A H 0.4024 0.6026 0.0601 0.096 Uiso 1 1 calc R . . H10B H 0.5258 0.6410 0.0689 0.096 Uiso 1 1 calc R . . H10C H 0.4630 0.6818 0.1250 0.096 Uiso 1 1 calc R . . C11 C 0.3889(3) 0.5299(3) 0.17590(18) 0.0616(10) Uani 1 1 d . . . H11A H 0.3983 0.4831 0.2027 0.092 Uiso 1 1 calc R . . H11B H 0.3243 0.5064 0.1426 0.092 Uiso 1 1 calc R . . H11C H 0.3856 0.5849 0.2078 0.092 Uiso 1 1 calc R . . C12 C 0.6244(2) 0.28862(18) 0.43680(14) 0.0312(6) Uani 1 1 d . . . H12A H 0.5533 0.2521 0.4381 0.037 Uiso 1 1 calc R . . H12B H 0.6665 0.2966 0.4831 0.037 Uiso 1 1 calc R . . C13 C 0.67093(19) 0.23870(18) 0.38159(14) 0.0290(6) Uani 1 1 d . . . C14 C 0.7272(2) 0.17849(18) 0.39679(15) 0.0337(6) Uani 1 1 d . . . H14A H 0.7391 0.1677 0.4428 0.040 Uiso 1 1 calc R . . C15 C 0.7659(2) 0.13405(19) 0.34275(15) 0.0370(7) Uani 1 1 d . . . H15A H 0.8043 0.0916 0.3516 0.044 Uiso 1 1 calc R . . C16 C 0.7491(2) 0.15106(18) 0.27671(15) 0.0331(6) Uani 1 1 d . . . H16A H 0.7754 0.1204 0.2397 0.040 Uiso 1 1 calc R . . C17 C 0.69239(19) 0.21464(17) 0.26433(14) 0.0280(6) Uani 1 1 d . . . C18 C 0.7271(2) 0.2079(2) 0.14427(15) 0.0406(7) Uani 1 1 d . . . H18A H 0.7008 0.1407 0.1284 0.049 Uiso 1 1 calc R . . H18B H 0.8023 0.2220 0.1613 0.049 Uiso 1 1 calc R . . C19 C 0.7109(3) 0.2541(2) 0.08241(16) 0.0479(8) Uani 1 1 d . . . C20 C 0.7474(3) 0.3579(2) 0.10432(19) 0.0622(10) Uani 1 1 d . . . H20A H 0.8203 0.3760 0.1264 0.093 Uiso 1 1 calc R . . H20B H 0.7050 0.3789 0.1375 0.093 Uiso 1 1 calc R . . H20C H 0.7406 0.3858 0.0631 0.093 Uiso 1 1 calc R . . C21 C 0.5943(3) 0.2250(3) 0.05061(17) 0.0601(10) Uani 1 1 d . . . H21A H 0.5541 0.2471 0.0850 0.090 Uiso 1 1 calc R . . H21B H 0.5705 0.1580 0.0378 0.090 Uiso 1 1 calc R . . H21C H 0.5846 0.2514 0.0090 0.090 Uiso 1 1 calc R . . C22 C 0.7731(3) 0.2208(3) 0.02833(19) 0.0697(11) Uani 1 1 d . . . H22A H 0.8469 0.2394 0.0482 0.105 Uiso 1 1 calc R . . H22B H 0.7628 0.2476 -0.0130 0.105 Uiso 1 1 calc R . . H22C H 0.7497 0.1538 0.0151 0.105 Uiso 1 1 calc R . . C23 C 0.54351(19) 0.41458(19) 0.45578(13) 0.0300(6) Uani 1 1 d . . . H23A H 0.5575 0.4814 0.4575 0.036 Uiso 1 1 calc R . . H23B H 0.5464 0.4037 0.5042 0.036 Uiso 1 1 calc R . . C24 C 0.4389(2) 0.36624(17) 0.41462(13) 0.0277(6) Uani 1 1 d . . . C25 C 0.3401(2) 0.35065(17) 0.43198(14) 0.0302(6) Uani 1 1 d . . . H25A H 0.3206 0.3665 0.4764 0.036 Uiso 1 1 calc R . . C26 C 0.27604(19) 0.30644(17) 0.36950(13) 0.0272(6) Uani 1 1 d . . . C27 C 0.1611(2) 0.26902(18) 0.35100(14) 0.0315(6) Uani 1 1 d . . . H27A H 0.1394 0.2072 0.3621 0.038 Uiso 1 1 calc R . . H27B H 0.1258 0.3093 0.3779 0.038 Uiso 1 1 calc R . . C28 C 0.1345(2) 0.35509(17) 0.25946(14) 0.0323(6) Uani 1 1 d . . . H28A H 0.1946 0.4019 0.2886 0.039 Uiso 1 1 calc R . . H28B H 0.0705 0.3714 0.2703 0.039 Uiso 1 1 calc R . . C29 C 0.1418(2) 0.35361(18) 0.18385(15) 0.0340(6) Uani 1 1 d . . . C30 C 0.0956(2) 0.4058(2) 0.14628(17) 0.0435(8) Uani 1 1 d . . . H30A H 0.0564 0.4434 0.1673 0.052 Uiso 1 1 calc R . . C31 C 0.1082(3) 0.4018(2) 0.07696(17) 0.0518(9) Uani 1 1 d . . . H31A H 0.0773 0.4370 0.0498 0.062 Uiso 1 1 calc R . . C32 C 0.1649(3) 0.3471(2) 0.04740(16) 0.0484(8) Uani 1 1 d . . . H32A H 0.1723 0.3435 -0.0004 0.058 Uiso 1 1 calc R . . C33 C 0.2124(2) 0.29616(19) 0.08807(15) 0.0380(7) Uani 1 1 d . . . C34 C 0.2942(3) 0.2251(2) -0.00649(16) 0.0515(8) Uani 1 1 d . . . H34A H 0.3698 0.2333 -0.0051 0.062 Uiso 1 1 calc R . . H34B H 0.2747 0.2711 -0.0314 0.062 Uiso 1 1 calc R . . C35 C 0.2375(3) 0.1301(3) -0.04779(18) 0.0589(10) Uani 1 1 d . . . C36 C 0.1208(3) 0.1155(3) -0.0515(2) 0.0739(11) Uani 1 1 d . . . H36A H 0.1037 0.1236 -0.0041 0.111 Uiso 1 1 calc R . . H36B H 0.0850 0.0533 -0.0768 0.111 Uiso 1 1 calc R . . H36C H 0.0987 0.1602 -0.0758 0.111 Uiso 1 1 calc R . . C37 C 0.2672(4) 0.1242(3) -0.12127(19) 0.0892(15) Uani 1 1 d . . . H37A H 0.3428 0.1369 -0.1179 0.134 Uiso 1 1 calc R . . H37B H 0.2431 0.1693 -0.1440 0.134 Uiso 1 1 calc R . . H37C H 0.2347 0.0625 -0.1488 0.134 Uiso 1 1 calc R . . C38 C 0.2723(4) 0.0585(3) -0.0137(2) 0.0938(16) Uani 1 1 d . . . H38A H 0.2523 0.0613 0.0328 0.141 Uiso 1 1 calc R . . H38B H 0.3479 0.0704 -0.0096 0.141 Uiso 1 1 calc R . . H38C H 0.2394 -0.0024 -0.0423 0.141 Uiso 1 1 calc R . . C39 C 0.0355(2) 0.19510(18) 0.24641(15) 0.0337(6) Uani 1 1 d . . . H39A H 0.0092 0.2047 0.1999 0.040 Uiso 1 1 calc R . . H39B H -0.0170 0.2007 0.2772 0.040 Uiso 1 1 calc R . . C40 C 0.05320(19) 0.10059(17) 0.23990(14) 0.0291(6) Uani 1 1 d . . . C41 C -0.0206(2) 0.02751(19) 0.24995(15) 0.0353(6) Uani 1 1 d . . . H41A H -0.0840 0.0346 0.2639 0.042 Uiso 1 1 calc R . . C42 C 0.0001(2) -0.05819(19) 0.23911(15) 0.0373(7) Uani 1 1 d . . . H42A H -0.0501 -0.1106 0.2452 0.045 Uiso 1 1 calc R . . C43 C 0.0917(2) -0.06700(18) 0.21984(14) 0.0328(6) Uani 1 1 d . . . H43A H 0.1049 -0.1256 0.2112 0.039 Uiso 1 1 calc R . . C44 C 0.1670(2) 0.01182(17) 0.21281(13) 0.0284(6) Uani 1 1 d . . . C45 C 0.2968(2) -0.07347(19) 0.19280(17) 0.0414(7) Uani 1 1 d . . . H45A H 0.2659 -0.1142 0.1471 0.050 Uiso 1 1 calc R . . H45B H 0.2720 -0.1064 0.2296 0.050 Uiso 1 1 calc R . . C46 C 0.4144(2) -0.0546(2) 0.20071(18) 0.0456(8) Uani 1 1 d . . . C47 C 0.4554(3) -0.0134(2) 0.1401(2) 0.0636(10) Uani 1 1 d . . . H47A H 0.4381 0.0451 0.1399 0.095 Uiso 1 1 calc R . . H47B H 0.4235 -0.0557 0.0959 0.095 Uiso 1 1 calc R . . H47C H 0.5309 -0.0031 0.1456 0.095 Uiso 1 1 calc R . . C48 C 0.4661(3) 0.0096(2) 0.2692(2) 0.0617(10) Uani 1 1 d . . . H48A H 0.4387 -0.0162 0.3079 0.092 Uiso 1 1 calc R . . H48B H 0.4518 0.0693 0.2694 0.092 Uiso 1 1 calc R . . H48C H 0.5411 0.0172 0.2744 0.092 Uiso 1 1 calc R . . C49 C 0.4389(3) -0.1477(2) 0.1994(2) 0.0693(12) Uani 1 1 d . . . H49A H 0.4144 -0.1735 0.2388 0.104 Uiso 1 1 calc R . . H49B H 0.5140 -0.1392 0.2029 0.104 Uiso 1 1 calc R . . H49C H 0.4040 -0.1895 0.1556 0.104 Uiso 1 1 calc R . . B1 B 0.1123(2) 0.6647(2) 0.33878(15) 0.0274(6) Uani 1 1 d . . . C50 C 0.2377(2) 0.67925(18) 0.36016(13) 0.0304(6) Uani 1 1 d . . . C51 C 0.2850(2) 0.6078(2) 0.35128(14) 0.0377(7) Uani 1 1 d . . . H51A H 0.2419 0.5469 0.3371 0.045 Uiso 1 1 calc R . . C52 C 0.3922(2) 0.6208(3) 0.36205(15) 0.0480(8) Uani 1 1 d . . . H52A H 0.4204 0.5696 0.3549 0.058 Uiso 1 1 calc R . . C53 C 0.4569(3) 0.7078(3) 0.38296(17) 0.0572(10) Uani 1 1 d . . . H53A H 0.5300 0.7175 0.3901 0.069 Uiso 1 1 calc R . . C54 C 0.4137(3) 0.7806(3) 0.39339(19) 0.0589(10) Uani 1 1 d . . . H54A H 0.4575 0.8410 0.4083 0.071 Uiso 1 1 calc R . . C55 C 0.3061(2) 0.7666(2) 0.38236(16) 0.0444(8) Uani 1 1 d . . . H55A H 0.2785 0.8181 0.3902 0.053 Uiso 1 1 calc R . . C56 C 0.0769(2) 0.74170(17) 0.39246(13) 0.0280(6) Uani 1 1 d . . . C57 C 0.0538(2) 0.72997(18) 0.45845(13) 0.0305(6) Uani 1 1 d . . . H57A H 0.0561 0.6739 0.4724 0.037 Uiso 1 1 calc R . . C58 C 0.0275(2) 0.79597(19) 0.50469(15) 0.0370(7) Uani 1 1 d . . . H58A H 0.0133 0.7847 0.5492 0.044 Uiso 1 1 calc R . . C59 C 0.0220(2) 0.87738(19) 0.48640(16) 0.0431(8) Uani 1 1 d . . . H59A H 0.0030 0.9224 0.5175 0.052 Uiso 1 1 calc R . . C60 C 0.0449(3) 0.8927(2) 0.42165(17) 0.0511(9) Uani 1 1 d . . . H60A H 0.0421 0.9489 0.4082 0.061 Uiso 1 1 calc R . . C61 C 0.0717(2) 0.82624(18) 0.37651(15) 0.0406(7) Uani 1 1 d . . . H61A H 0.0873 0.8387 0.3325 0.049 Uiso 1 1 calc R . . C62 C 0.04618(19) 0.56147(16) 0.34554(13) 0.0252(5) Uani 1 1 d . . . C63 C 0.0718(2) 0.52285(17) 0.40275(14) 0.0302(6) Uani 1 1 d . . . H63A H 0.1305 0.5562 0.4364 0.036 Uiso 1 1 calc R . . C64 C 0.0157(2) 0.43825(18) 0.41276(15) 0.0343(6) Uani 1 1 d . . . H64A H 0.0357 0.4157 0.4529 0.041 Uiso 1 1 calc R . . C65 C -0.0687(2) 0.38710(18) 0.36442(15) 0.0342(7) Uani 1 1 d . . . H65A H -0.1068 0.3288 0.3705 0.041 Uiso 1 1 calc R . . C66 C -0.0971(2) 0.42232(17) 0.30680(15) 0.0320(6) Uani 1 1 d . . . H66A H -0.1555 0.3881 0.2732 0.038 Uiso 1 1 calc R . . C67 C -0.04056(19) 0.50726(17) 0.29793(14) 0.0278(6) Uani 1 1 d . . . H67A H -0.0616 0.5296 0.2579 0.033 Uiso 1 1 calc R . . C68 C 0.0889(2) 0.67644(16) 0.25748(13) 0.0270(6) Uani 1 1 d . . . C69 C -0.0063(2) 0.68784(18) 0.22863(14) 0.0338(6) Uani 1 1 d . . . H69A H -0.0563 0.6936 0.2584 0.041 Uiso 1 1 calc R . . C70 C -0.0307(2) 0.69104(19) 0.15906(15) 0.0418(7) Uani 1 1 d . . . H70A H -0.0966 0.6981 0.1419 0.050 Uiso 1 1 calc R . . C71 C 0.0405(3) 0.6839(2) 0.11457(16) 0.0466(8) Uani 1 1 d . . . H71A H 0.0242 0.6861 0.0667 0.056 Uiso 1 1 calc R . . C72 C 0.1354(3) 0.6736(2) 0.14039(15) 0.0443(8) Uani 1 1 d . . . H72A H 0.1852 0.6690 0.1103 0.053 Uiso 1 1 calc R . . C73 C 0.1585(2) 0.66984(18) 0.21026(14) 0.0354(6) Uani 1 1 d . . . H73A H 0.2245 0.6625 0.2267 0.042 Uiso 1 1 calc R . . C74 C 0.2636(7) 0.1064(6) 0.6502(5) 0.087(3) Uiso 0.50 1 d P A 1 H74A H 0.2772 0.0744 0.6882 0.131 Uiso 0.50 1 calc PR A 1 H74B H 0.1891 0.1010 0.6405 0.131 Uiso 0.50 1 calc PR A 1 H74C H 0.3017 0.1712 0.6640 0.131 Uiso 0.50 1 calc PR A 1 C75 C 0.2977(8) 0.0650(7) 0.5872(5) 0.097(3) Uiso 0.50 1 d P A 1 H75A H 0.3722 0.0687 0.5996 0.116 Uiso 0.50 1 calc PR A 1 H75B H 0.2602 -0.0009 0.5761 0.116 Uiso 0.50 1 calc PR A 1 C76 C 0.2875(7) 0.0961(6) 0.5313(4) 0.061(2) Uiso 0.50 1 d P A 1 H76A H 0.3283 0.1611 0.5423 0.074 Uiso 0.50 1 calc PR A 1 H76B H 0.2138 0.0962 0.5212 0.074 Uiso 0.50 1 calc PR A 1 C77 C 0.3172(9) 0.0510(8) 0.4600(6) 0.090(3) Uiso 0.50 1 d P A 1 H77A H 0.3938 0.0648 0.4658 0.108 Uiso 0.50 1 calc PR A 1 H77B H 0.2905 -0.0163 0.4542 0.108 Uiso 0.50 1 calc PR A 1 C78 C 0.2825(9) 0.0762(7) 0.3954(5) 0.060(3) Uiso 0.50 1 d P A 1 H78A H 0.3072 0.0429 0.3568 0.091 Uiso 0.50 1 calc PR A 1 H78B H 0.3104 0.1423 0.3988 0.091 Uiso 0.50 1 calc PR A 1 H78C H 0.2066 0.0605 0.3869 0.091 Uiso 0.50 1 calc PR A 1 O3 O 0.2198(8) 0.1090(7) 0.4360(6) 0.158(3) Uiso 0.50 1 d P B 2 C79 C 0.3137(14) 0.0928(13) 0.4066(10) 0.144(8) Uiso 0.50 1 d P B 2 H79A H 0.2915 0.0520 0.3601 0.173 Uiso 0.50 1 calc PR B 2 H79B H 0.3583 0.1518 0.4006 0.173 Uiso 0.50 1 calc PR B 2 C80 C 0.3709(10) 0.0527(9) 0.4508(6) 0.106(4) Uiso 0.50 1 d P B 2 H80A H 0.4430 0.0915 0.4651 0.128 Uiso 0.50 1 calc PR B 2 H80B H 0.3726 -0.0086 0.4267 0.128 Uiso 0.50 1 calc PR B 2 C81 C 0.3152(7) 0.0448(7) 0.5154(6) 0.082(3) Uiso 0.50 1 d P B 2 H81A H 0.2641 -0.0153 0.5103 0.099 Uiso 0.50 1 calc PR B 2 H81B H 0.3645 0.0574 0.5593 0.099 Uiso 0.50 1 calc PR B 2 C82 C 0.2646(10) 0.1209(9) 0.5096(7) 0.112(4) Uiso 0.50 1 d P B 2 H82A H 0.2096 0.1181 0.5393 0.135 Uiso 0.50 1 calc PR B 2 H82B H 0.3164 0.1810 0.5249 0.135 Uiso 0.50 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 0.02422(19) 0.02739(19) 0.02402(19) 0.00482(14) 0.00585(14) 0.00917(15) Co2 0.02550(19) 0.02133(18) 0.02749(19) 0.00100(14) 0.00465(15) 0.00745(14) O1 0.0316(10) 0.0354(11) 0.0261(10) 0.0069(8) 0.0044(8) 0.0102(9) O2 0.0333(10) 0.0279(10) 0.0339(11) 0.0011(8) 0.0094(8) 0.0101(8) N1 0.0229(11) 0.0313(12) 0.0264(12) 0.0020(9) 0.0029(9) 0.0081(9) N2 0.0288(12) 0.0299(12) 0.0307(12) 0.0039(10) 0.0067(10) 0.0067(10) N3 0.0224(11) 0.0289(11) 0.0259(12) 0.0050(9) 0.0035(9) 0.0077(9) N4 0.0233(11) 0.0287(11) 0.0241(11) 0.0028(9) 0.0053(9) 0.0081(9) N5 0.0545(17) 0.0274(13) 0.0380(14) 0.0080(11) -0.0030(12) 0.0063(12) N6 0.0349(13) 0.0335(13) 0.0277(12) 0.0058(10) 0.0101(10) 0.0151(11) N7 0.0259(12) 0.0228(11) 0.0347(13) 0.0010(9) 0.0042(10) 0.0077(9) N8 0.0369(13) 0.0259(12) 0.0331(13) 0.0027(10) 0.0035(10) 0.0119(10) N9 0.0265(12) 0.0238(11) 0.0301(12) 0.0024(9) 0.0023(9) 0.0065(9) N10 0.0215(11) 0.0277(11) 0.0263(11) 0.0009(9) 0.0040(9) 0.0071(9) N11 0.0601(18) 0.0444(15) 0.0290(14) 0.0062(11) 0.0085(12) 0.0251(14) N12 0.0333(13) 0.0196(12) 0.0496(15) 0.0059(11) 0.0121(11) 0.0069(10) C1 0.0234(14) 0.0403(16) 0.0293(15) 0.0001(12) 0.0011(11) 0.0084(12) C2 0.0241(14) 0.0361(15) 0.0314(15) 0.0002(12) 0.0076(12) 0.0093(12) C3 0.0268(15) 0.0399(17) 0.0387(17) -0.0032(13) 0.0071(13) 0.0034(12) C4 0.0326(16) 0.0367(17) 0.051(2) 0.0014(14) 0.0094(14) 0.0000(13) C5 0.0426(18) 0.0299(15) 0.0509(19) 0.0093(14) 0.0116(15) 0.0036(13) C6 0.0355(16) 0.0329(15) 0.0354(16) 0.0040(12) 0.0081(13) 0.0096(12) C7 0.060(2) 0.0335(16) 0.0429(18) 0.0115(14) 0.0067(16) 0.0111(15) C8 0.061(2) 0.0360(16) 0.0290(15) 0.0058(12) 0.0058(14) 0.0210(15) C9 0.082(3) 0.0406(18) 0.0310(17) 0.0093(13) 0.0059(16) 0.0258(17) C10 0.112(3) 0.045(2) 0.044(2) 0.0086(16) 0.000(2) 0.042(2) C11 0.058(2) 0.088(3) 0.043(2) 0.0094(19) 0.0075(17) 0.028(2) C12 0.0300(15) 0.0396(16) 0.0268(14) 0.0099(12) 0.0045(11) 0.0123(12) C13 0.0239(14) 0.0313(14) 0.0309(15) 0.0077(11) 0.0015(11) 0.0059(11) C14 0.0329(15) 0.0360(15) 0.0361(16) 0.0140(12) 0.0040(12) 0.0123(12) C15 0.0332(16) 0.0337(15) 0.0489(18) 0.0120(13) 0.0055(14) 0.0159(13) C16 0.0301(15) 0.0327(15) 0.0386(16) 0.0036(12) 0.0078(12) 0.0130(12) C17 0.0257(14) 0.0241(13) 0.0337(15) 0.0065(11) 0.0054(11) 0.0048(11) C18 0.0462(18) 0.0442(17) 0.0377(17) 0.0083(13) 0.0144(14) 0.0199(14) C19 0.067(2) 0.0480(19) 0.0350(17) 0.0106(14) 0.0182(16) 0.0215(17) C20 0.087(3) 0.052(2) 0.059(2) 0.0241(18) 0.033(2) 0.023(2) C21 0.072(3) 0.076(3) 0.0354(19) 0.0103(17) 0.0042(17) 0.029(2) C22 0.098(3) 0.081(3) 0.050(2) 0.024(2) 0.040(2) 0.041(2) C23 0.0282(14) 0.0379(15) 0.0233(14) -0.0012(11) 0.0047(11) 0.0119(12) C24 0.0304(14) 0.0272(13) 0.0257(14) 0.0022(11) 0.0075(11) 0.0089(11) C25 0.0308(15) 0.0323(15) 0.0270(14) -0.0007(11) 0.0109(12) 0.0091(12) C26 0.0262(14) 0.0258(13) 0.0302(14) 0.0019(11) 0.0081(11) 0.0088(11) C27 0.0284(14) 0.0321(15) 0.0352(15) 0.0039(12) 0.0100(12) 0.0099(12) C28 0.0303(15) 0.0247(14) 0.0432(17) 0.0017(12) 0.0079(13) 0.0117(11) C29 0.0315(15) 0.0251(14) 0.0418(17) 0.0009(12) 0.0012(13) 0.0064(12) C30 0.0488(19) 0.0352(16) 0.051(2) 0.0072(14) 0.0032(15) 0.0212(14) C31 0.060(2) 0.050(2) 0.050(2) 0.0133(16) -0.0041(17) 0.0255(17) C32 0.064(2) 0.0490(19) 0.0345(17) 0.0088(14) -0.0019(15) 0.0236(17) C33 0.0472(18) 0.0340(16) 0.0308(16) 0.0017(12) 0.0008(13) 0.0126(14) C34 0.060(2) 0.063(2) 0.0352(18) 0.0069(15) 0.0103(16) 0.0238(18) C35 0.074(3) 0.064(2) 0.042(2) -0.0021(17) 0.0002(18) 0.035(2) C36 0.075(3) 0.075(3) 0.063(3) 0.000(2) 0.004(2) 0.014(2) C37 0.100(3) 0.127(4) 0.042(2) -0.014(2) 0.007(2) 0.054(3) C38 0.139(4) 0.061(3) 0.079(3) -0.011(2) -0.015(3) 0.053(3) C39 0.0260(14) 0.0306(15) 0.0430(17) 0.0023(12) 0.0041(12) 0.0084(11) C40 0.0243(14) 0.0285(14) 0.0326(15) 0.0021(11) 0.0012(11) 0.0074(11) C41 0.0250(14) 0.0365(16) 0.0433(17) 0.0070(13) 0.0053(12) 0.0066(12) C42 0.0327(16) 0.0304(15) 0.0459(18) 0.0095(13) 0.0068(13) 0.0013(12) C43 0.0360(16) 0.0225(13) 0.0396(16) 0.0067(12) 0.0057(13) 0.0069(12) C44 0.0315(15) 0.0245(13) 0.0286(14) 0.0037(11) 0.0023(11) 0.0083(11) C45 0.0402(17) 0.0263(15) 0.058(2) 0.0011(13) 0.0095(15) 0.0119(13) C46 0.0428(18) 0.0352(16) 0.066(2) 0.0127(15) 0.0146(16) 0.0199(14) C47 0.069(2) 0.056(2) 0.084(3) 0.021(2) 0.043(2) 0.0327(19) C48 0.046(2) 0.060(2) 0.075(3) 0.0094(19) -0.0037(18) 0.0157(18) C49 0.058(2) 0.046(2) 0.120(4) 0.024(2) 0.028(2) 0.0321(18) B1 0.0306(16) 0.0246(15) 0.0248(15) 0.0026(12) 0.0054(13) 0.0040(12) C50 0.0326(15) 0.0357(15) 0.0214(13) 0.0073(11) 0.0055(11) 0.0042(12) C51 0.0312(16) 0.0446(17) 0.0333(16) 0.0023(13) 0.0035(13) 0.0065(13) C52 0.0388(18) 0.074(2) 0.0355(17) 0.0127(16) 0.0074(14) 0.0212(17) C53 0.0306(18) 0.093(3) 0.047(2) 0.027(2) 0.0046(15) 0.0077(19) C54 0.041(2) 0.059(2) 0.063(2) 0.0216(18) -0.0029(17) -0.0157(17) C55 0.0384(17) 0.0415(17) 0.0481(19) 0.0142(14) 0.0021(14) -0.0009(14) C56 0.0292(14) 0.0227(13) 0.0274(14) 0.0029(11) 0.0024(11) 0.0004(11) C57 0.0314(15) 0.0274(14) 0.0301(15) 0.0031(11) 0.0022(12) 0.0056(11) C58 0.0372(16) 0.0402(17) 0.0288(15) -0.0016(12) 0.0067(13) 0.0058(13) C59 0.054(2) 0.0314(16) 0.0415(18) -0.0081(13) 0.0115(15) 0.0156(14) C60 0.085(3) 0.0277(16) 0.0449(19) 0.0056(14) 0.0168(18) 0.0217(16) C61 0.060(2) 0.0283(15) 0.0339(16) 0.0042(12) 0.0139(14) 0.0107(14) C62 0.0287(14) 0.0220(13) 0.0268(14) 0.0032(10) 0.0078(11) 0.0096(11) C63 0.0337(15) 0.0277(14) 0.0295(14) 0.0049(11) 0.0046(12) 0.0093(12) C64 0.0438(17) 0.0347(15) 0.0357(16) 0.0159(12) 0.0190(13) 0.0201(13) C65 0.0348(16) 0.0230(14) 0.0497(18) 0.0097(12) 0.0215(14) 0.0086(12) C66 0.0269(14) 0.0243(14) 0.0423(17) 0.0017(12) 0.0084(12) 0.0038(11) C67 0.0289(14) 0.0249(13) 0.0309(14) 0.0036(11) 0.0054(11) 0.0107(11) C68 0.0333(15) 0.0174(12) 0.0266(14) 0.0033(10) 0.0031(11) 0.0010(11) C69 0.0426(17) 0.0262(14) 0.0321(15) 0.0073(11) 0.0063(13) 0.0069(12) C70 0.0494(19) 0.0353(16) 0.0387(17) 0.0115(13) -0.0043(15) 0.0095(14) C71 0.066(2) 0.0415(18) 0.0279(16) 0.0091(13) -0.0010(15) 0.0072(16) C72 0.057(2) 0.0453(18) 0.0300(16) 0.0079(13) 0.0140(15) 0.0085(15) C73 0.0418(17) 0.0333(15) 0.0293(15) 0.0072(12) 0.0061(13) 0.0059(13) _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 1.9379(17) . ? Co1 N4 2.034(2) . ? Co1 N3 2.102(2) . ? Co1 N2 2.107(2) . ? Co1 N1 2.192(2) . ? Co2 O2 1.9444(17) . ? Co2 N10 2.046(2) . ? Co2 N8 2.104(2) . ? Co2 N9 2.119(2) . ? Co2 N7 2.195(2) . ? N1 C12 1.470(3) . ? N1 C23 1.472(3) . ? N1 C1 1.473(3) . ? N2 C2 1.353(3) . ? N2 C6 1.364(3) . ? N3 C13 1.353(3) . ? N3 C17 1.360(3) . ? N4 C24 1.343(3) . ? N4 N10 1.375(3) . ? N5 C6 1.342(4) . ? N5 C7 1.451(4) . ? N6 C17 1.345(3) . ? N6 C18 1.449(3) . ? N7 C39 1.465(3) . ? N7 C28 1.472(3) . ? N7 C27 1.474(3) . ? N8 C33 1.360(3) . ? N8 C29 1.362(3) . ? N9 C40 1.355(3) . ? N9 C44 1.366(3) . ? N10 C26 1.341(3) . ? N11 C33 1.354(4) . ? N11 C34 1.448(4) . ? N12 C44 1.338(3) . ? N12 C45 1.447(3) . ? C1 C2 1.494(4) . ? C2 C3 1.373(4) . ? C3 C4 1.384(4) . ? C4 C5 1.353(4) . ? C5 C6 1.417(4) . ? C7 C8 1.523(4) . ? C8 C11 1.518(4) . ? C8 C10 1.529(4) . ? C8 C9 1.533(4) . ? C12 C13 1.507(4) . ? C13 C14 1.376(4) . ? C14 C15 1.388(4) . ? C15 C16 1.371(4) . ? C16 C17 1.411(4) . ? C18 C19 1.524(4) . ? C19 C20 1.521(4) . ? C19 C22 1.525(4) . ? C19 C21 1.550(5) . ? C23 C24 1.494(4) . ? C24 C25 1.384(3) . ? C25 C26 1.387(4) . ? C26 C27 1.493(4) . ? C28 C29 1.498(4) . ? C29 C30 1.379(4) . ? C30 C31 1.385(4) . ? C31 C32 1.370(4) . ? C32 C33 1.411(4) . ? C34 C35 1.519(5) . ? C35 C38 1.513(5) . ? C35 C36 1.523(5) . ? C35 C37 1.536(5) . ? C39 C40 1.513(4) . ? C40 C41 1.362(4) . ? C41 C42 1.397(4) . ? C42 C43 1.359(4) . ? C43 C44 1.413(4) . ? C45 C46 1.523(4) . ? C46 C48 1.516(5) . ? C46 C47 1.531(5) . ? C46 C49 1.538(4) . ? B1 C68 1.642(4) . ? B1 C50 1.645(4) . ? B1 C56 1.648(4) . ? B1 C62 1.652(4) . ? C50 C51 1.392(4) . ? C50 C55 1.398(4) . ? C51 C52 1.394(4) . ? C52 C53 1.374(5) . ? C53 C54 1.376(5) . ? C54 C55 1.397(4) . ? C56 C57 1.397(4) . ? C56 C61 1.398(4) . ? C57 C58 1.387(4) . ? C58 C59 1.370(4) . ? C59 C60 1.385(4) . ? C60 C61 1.384(4) . ? C62 C63 1.401(3) . ? C62 C67 1.402(3) . ? C63 C64 1.390(4) . ? C64 C65 1.377(4) . ? C65 C66 1.387(4) . ? C66 C67 1.389(4) . ? C68 C73 1.400(4) . ? C68 C69 1.405(4) . ? C69 C70 1.383(4) . ? C70 C71 1.378(4) . ? C71 C72 1.376(4) . ? C72 C73 1.388(4) . ? C74 C75 1.471(12) . ? C75 C76 1.275(12) . ? C76 C77 1.597(14) . ? C77 C78 1.448(16) . ? O3 C82 1.469(13) . ? O3 C79 1.503(19) . ? C79 C80 1.41(2) . ? C80 C81 1.551(15) . ? C81 C82 1.501(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N4 106.28(8) . . ? O1 Co1 N3 101.94(8) . . ? N4 Co1 N3 114.64(8) . . ? O1 Co1 N2 100.48(8) . . ? N4 Co1 N2 116.10(8) . . ? N3 Co1 N2 114.73(8) . . ? O1 Co1 N1 176.51(8) . . ? N4 Co1 N1 76.99(8) . . ? N3 Co1 N1 77.50(8) . . ? N2 Co1 N1 76.78(8) . . ? O2 Co2 N10 106.61(8) . . ? O2 Co2 N8 102.23(8) . . ? N10 Co2 N8 115.00(8) . . ? O2 Co2 N9 100.11(8) . . ? N10 Co2 N9 117.25(8) . . ? N8 Co2 N9 112.95(8) . . ? O2 Co2 N7 176.81(8) . . ? N10 Co2 N7 76.25(8) . . ? N8 Co2 N7 77.51(8) . . ? N9 Co2 N7 77.17(8) . . ? C12 N1 C23 111.8(2) . . ? C12 N1 C1 112.7(2) . . ? C23 N1 C1 111.2(2) . . ? C12 N1 Co1 106.19(15) . . ? C23 N1 Co1 107.15(15) . . ? C1 N1 Co1 107.34(15) . . ? C2 N2 C6 118.2(2) . . ? C2 N2 Co1 116.54(18) . . ? C6 N2 Co1 125.30(18) . . ? C13 N3 C17 118.9(2) . . ? C13 N3 Co1 115.68(16) . . ? C17 N3 Co1 125.35(17) . . ? C24 N4 N10 107.36(19) . . ? C24 N4 Co1 116.93(17) . . ? N10 N4 Co1 135.52(16) . . ? C6 N5 C7 123.6(2) . . ? C17 N6 C18 122.3(2) . . ? C39 N7 C28 113.0(2) . . ? C39 N7 C27 111.7(2) . . ? C28 N7 C27 111.9(2) . . ? C39 N7 Co2 106.81(15) . . ? C28 N7 Co2 105.13(15) . . ? C27 N7 Co2 107.83(15) . . ? C33 N8 C29 119.0(2) . . ? C33 N8 Co2 125.89(18) . . ? C29 N8 Co2 115.07(18) . . ? C40 N9 C44 118.0(2) . . ? C40 N9 Co2 116.12(16) . . ? C44 N9 Co2 125.40(17) . . ? C26 N10 N4 107.6(2) . . ? C26 N10 Co2 116.97(16) . . ? N4 N10 Co2 135.11(15) . . ? C33 N11 C34 126.0(3) . . ? C44 N12 C45 123.3(2) . . ? N1 C1 C2 110.7(2) . . ? N2 C2 C3 123.0(3) . . ? N2 C2 C1 115.4(2) . . ? C3 C2 C1 121.6(3) . . ? C2 C3 C4 118.8(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 119.8(3) . . ? N5 C6 N2 116.8(2) . . ? N5 C6 C5 122.9(3) . . ? N2 C6 C5 120.3(3) . . ? N5 C7 C8 112.2(2) . . ? C11 C8 C7 110.9(3) . . ? C11 C8 C10 110.6(3) . . ? C7 C8 C10 107.5(3) . . ? C11 C8 C9 109.1(3) . . ? C7 C8 C9 110.8(3) . . ? C10 C8 C9 107.9(2) . . ? N1 C12 C13 110.0(2) . . ? N3 C13 C14 123.1(2) . . ? N3 C13 C12 115.4(2) . . ? C14 C13 C12 121.5(2) . . ? C13 C14 C15 117.9(3) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 C17 119.2(2) . . ? N6 C17 N3 117.1(2) . . ? N6 C17 C16 122.5(2) . . ? N3 C17 C16 120.4(2) . . ? N6 C18 C19 113.1(2) . . ? C20 C19 C18 111.1(3) . . ? C20 C19 C22 110.1(3) . . ? C18 C19 C22 107.1(3) . . ? C20 C19 C21 109.7(3) . . ? C18 C19 C21 109.5(3) . . ? C22 C19 C21 109.2(3) . . ? N1 C23 C24 108.1(2) . . ? N4 C24 C25 110.6(2) . . ? N4 C24 C23 116.9(2) . . ? C25 C24 C23 132.4(2) . . ? C24 C25 C26 103.9(2) . . ? N10 C26 C25 110.4(2) . . ? N10 C26 C27 117.2(2) . . ? C25 C26 C27 132.3(2) . . ? N7 C27 C26 107.7(2) . . ? N7 C28 C29 109.8(2) . . ? N8 C29 C30 122.9(3) . . ? N8 C29 C28 115.2(2) . . ? C30 C29 C28 121.9(3) . . ? C29 C30 C31 118.1(3) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 119.9(3) . . ? N11 C33 N8 115.8(3) . . ? N11 C33 C32 124.2(3) . . ? N8 C33 C32 119.9(3) . . ? N11 C34 C35 114.5(3) . . ? C38 C35 C34 109.7(3) . . ? C38 C35 C36 110.3(4) . . ? C34 C35 C36 110.0(3) . . ? C38 C35 C37 109.2(3) . . ? C34 C35 C37 107.2(3) . . ? C36 C35 C37 110.4(3) . . ? N7 C39 C40 109.5(2) . . ? N9 C40 C41 123.9(2) . . ? N9 C40 C39 114.3(2) . . ? C41 C40 C39 121.7(2) . . ? C40 C41 C42 117.8(3) . . ? C43 C42 C41 120.3(3) . . ? C42 C43 C44 119.3(2) . . ? N12 C44 N9 117.3(2) . . ? N12 C44 C43 122.2(2) . . ? N9 C44 C43 120.5(2) . . ? N12 C45 C46 113.7(2) . . ? C48 C46 C45 111.1(3) . . ? C48 C46 C47 109.5(3) . . ? C45 C46 C47 110.8(3) . . ? C48 C46 C49 109.6(3) . . ? C45 C46 C49 106.5(3) . . ? C47 C46 C49 109.2(3) . . ? C68 B1 C50 108.6(2) . . ? C68 B1 C56 111.4(2) . . ? C50 B1 C56 108.2(2) . . ? C68 B1 C62 108.6(2) . . ? C50 B1 C62 111.2(2) . . ? C56 B1 C62 108.8(2) . . ? C51 C50 C55 114.9(3) . . ? C51 C50 B1 123.2(2) . . ? C55 C50 B1 121.6(2) . . ? C50 C51 C52 123.5(3) . . ? C53 C52 C51 119.9(3) . . ? C52 C53 C54 118.7(3) . . ? C53 C54 C55 120.8(3) . . ? C54 C55 C50 122.2(3) . . ? C57 C56 C61 114.3(2) . . ? C57 C56 B1 123.3(2) . . ? C61 C56 B1 122.4(2) . . ? C58 C57 C56 123.4(3) . . ? C59 C58 C57 120.2(3) . . ? C58 C59 C60 118.7(3) . . ? C61 C60 C59 120.1(3) . . ? C60 C61 C56 123.2(3) . . ? C63 C62 C67 114.6(2) . . ? C63 C62 B1 121.0(2) . . ? C67 C62 B1 124.3(2) . . ? C64 C63 C62 123.4(3) . . ? C65 C64 C63 120.0(3) . . ? C64 C65 C66 118.8(2) . . ? C65 C66 C67 120.4(3) . . ? C66 C67 C62 122.8(2) . . ? C73 C68 C69 114.6(2) . . ? C73 C68 B1 123.2(2) . . ? C69 C68 B1 122.1(2) . . ? C70 C69 C68 123.2(3) . . ? C71 C70 C69 120.0(3) . . ? C72 C71 C70 119.1(3) . . ? C71 C72 C73 120.3(3) . . ? C72 C73 C68 122.8(3) . . ? C76 C75 C74 120.2(10) . . ? C75 C76 C77 122.7(10) . . ? C78 C77 C76 119.5(9) . . ? C82 O3 C79 95.9(10) . . ? C80 C79 O3 111.1(15) . . ? C79 C80 C81 106.6(12) . . ? C82 C81 C80 96.4(9) . . ? O3 C82 C81 107.4(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.728 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.056 #==END data_asb182 _database_code_depnum_ccdc_archive 'CCDC 847962' #TrackingRef '- 09092011.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H125 B Mn2 N12 O3' _chemical_formula_weight 1495.67 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 23.8786(15) _cell_length_b 20.3401(12) _cell_length_c 17.4648(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8482.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.57 _exptl_crystal_description spear _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8410 _exptl_absorpt_correction_T_max 0.9230 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67332 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17304 _reflns_number_gt 13820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1658P)^2^+4.3881P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 17304 _refine_ls_number_parameters 837 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2426 _refine_ls_wR_factor_gt 0.2210 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.49705(3) 0.72288(3) 1.01609(13) 0.03822(17) Uani 1 1 d . . . Mn2 Mn 0.61142(3) 0.83942(3) 0.88252(13) 0.0478(2) Uani 1 1 d . . . O1 O 0.49427(12) 0.69729(16) 0.9054(2) 0.0385(7) Uani 1 1 d . . . H1 H 0.5249 0.7066 0.8844 0.058 Uiso 1 1 calc R . . O2 O 0.61909(14) 0.74357(18) 0.8577(3) 0.0573(10) Uani 1 1 d . . . H2 H 0.5889 0.7242 0.8675 0.086 Uiso 1 1 calc R . . N1 N 0.49347(19) 0.7439(2) 1.1471(3) 0.0507(10) Uani 1 1 d . . . N2 N 0.40623(18) 0.71807(19) 1.0462(3) 0.0406(8) Uani 1 1 d . . . N3 N 0.5483(2) 0.6432(2) 1.0651(3) 0.0546(11) Uani 1 1 d . . . N4 N 0.53441(16) 0.81706(19) 1.0305(3) 0.0440(9) Uani 1 1 d . . . N5 N 0.37636(17) 0.71082(19) 0.9214(2) 0.0388(8) Uani 1 1 d . . . H5 H 0.4109 0.6997 0.9094 0.047 Uiso 1 1 calc R . . N6 N 0.5555(2) 0.5870(2) 0.9507(3) 0.0566(11) Uani 1 1 d . . . H6 H 0.5357 0.6196 0.9317 0.068 Uiso 1 1 calc R . . N7 N 0.61283(16) 0.9508(2) 0.8997(3) 0.0512(11) Uani 1 1 d . . . N8 N 0.57348(19) 0.8787(2) 0.7767(3) 0.0527(10) Uani 1 1 d . . . N9 N 0.70187(19) 0.8659(2) 0.8907(4) 0.0758(17) Uani 1 1 d . . . N10 N 0.56339(16) 0.85718(19) 0.9837(3) 0.0430(9) Uani 1 1 d . . . N11 N 0.5865(3) 0.7829(3) 0.7089(4) 0.086(2) Uani 1 1 d . . . H11 H 0.5833 0.7637 0.7538 0.103 Uiso 1 1 calc R . . N12 N 0.7324(2) 0.7582(3) 0.9017(4) 0.0811(19) Uani 1 1 d . . . H12 H 0.6978 0.7463 0.8910 0.097 Uiso 1 1 calc R . . C1 C 0.4433(3) 0.7125(3) 1.1749(3) 0.0553(13) Uani 1 1 d . . . H1A H 0.4344 0.7293 1.2267 0.066 Uiso 1 1 calc R . . H1B H 0.4497 0.6645 1.1789 0.066 Uiso 1 1 calc R . . C2 C 0.3939(2) 0.7253(2) 1.1218(3) 0.0468(12) Uani 1 1 d . . . C3 C 0.3420(2) 0.7392(3) 1.1483(3) 0.0535(13) Uani 1 1 d . . . H3A H 0.3350 0.7429 1.2017 0.064 Uiso 1 1 calc R . . C4 C 0.2996(2) 0.7479(3) 1.0959(3) 0.0615(15) Uani 1 1 d . . . H4A H 0.2635 0.7615 1.1125 0.074 Uiso 1 1 calc R . . C5 C 0.30931(19) 0.7369(3) 1.0202(3) 0.0488(11) Uani 1 1 d . . . H5A H 0.2794 0.7394 0.9844 0.059 Uiso 1 1 calc R . . C6 C 0.3639(2) 0.7218(2) 0.9951(3) 0.0375(9) Uani 1 1 d . . . C7 C 0.3349(2) 0.7165(3) 0.8601(3) 0.0431(10) Uani 1 1 d . . . H7A H 0.2990 0.6984 0.8792 0.052 Uiso 1 1 calc R . . H7B H 0.3288 0.7638 0.8497 0.052 Uiso 1 1 calc R . . C8 C 0.3480(3) 0.6841(6) 0.7876(4) 0.101(3) Uani 1 1 d . . . C9 C 0.2995(3) 0.6970(5) 0.7324(3) 0.081(2) Uani 1 1 d . . . H9A H 0.3002 0.7431 0.7163 0.121 Uiso 1 1 calc R . . H9B H 0.2639 0.6876 0.7581 0.121 Uiso 1 1 calc R . . H9C H 0.3034 0.6685 0.6874 0.121 Uiso 1 1 calc R . . C10 C 0.3971(5) 0.6700(7) 0.7577(8) 0.128(4) Uiso 1 1 d . . . H10A H 0.4155 0.6361 0.7886 0.192 Uiso 1 1 calc R . . H10B H 0.4204 0.7096 0.7568 0.192 Uiso 1 1 calc R . . H10C H 0.3920 0.6538 0.7053 0.192 Uiso 1 1 calc R . . C11 C 0.3390(5) 0.6008(6) 0.8121(8) 0.129(4) Uiso 1 1 d . . . H11A H 0.3730 0.5844 0.8370 0.194 Uiso 1 1 calc R . . H11B H 0.3317 0.5752 0.7657 0.194 Uiso 1 1 calc R . . H11C H 0.3072 0.5965 0.8473 0.194 Uiso 1 1 calc R . . C12 C 0.5453(3) 0.7147(4) 1.1778(4) 0.0710(18) Uani 1 1 d . . . H12A H 0.5413 0.7086 1.2337 0.085 Uiso 1 1 calc R . . H12B H 0.5768 0.7453 1.1689 0.085 Uiso 1 1 calc R . . C13 C 0.5587(3) 0.6494(3) 1.1415(4) 0.0688(17) Uani 1 1 d . . . C14 C 0.5825(4) 0.5984(4) 1.1839(4) 0.087(2) Uani 1 1 d . . . H14A H 0.5874 0.6020 1.2377 0.104 Uiso 1 1 calc R . . C15 C 0.5987(5) 0.5428(5) 1.1452(5) 0.111(3) Uani 1 1 d . . . H15A H 0.6163 0.5082 1.1727 0.134 Uiso 1 1 calc R . . C16 C 0.5905(4) 0.5358(4) 1.0693(5) 0.090(3) Uani 1 1 d . . . H16A H 0.6009 0.4962 1.0441 0.108 Uiso 1 1 calc R . . C17 C 0.5657(3) 0.5890(3) 1.0271(4) 0.0643(15) Uani 1 1 d . . . C18 C 0.5735(2) 0.5371(3) 0.8970(4) 0.0558(13) Uani 1 1 d . . . H18A H 0.6059 0.5134 0.9191 0.067 Uiso 1 1 calc R . . H18B H 0.5864 0.5590 0.8496 0.067 Uiso 1 1 calc R . . C19 C 0.5289(2) 0.4874(3) 0.8763(4) 0.0595(13) Uani 1 1 d . . . C20 C 0.4766(3) 0.5220(3) 0.8461(4) 0.0677(16) Uani 1 1 d . . . H20A H 0.4650 0.5561 0.8824 0.102 Uiso 1 1 calc R . . H20B H 0.4463 0.4899 0.8400 0.102 Uiso 1 1 calc R . . H20C H 0.4849 0.5422 0.7964 0.102 Uiso 1 1 calc R . . C21 C 0.5146(3) 0.4453(3) 0.9459(4) 0.0733(18) Uani 1 1 d . . . H21A H 0.5111 0.4735 0.9912 0.110 Uiso 1 1 calc R . . H21B H 0.5444 0.4130 0.9543 0.110 Uiso 1 1 calc R . . H21C H 0.4790 0.4224 0.9369 0.110 Uiso 1 1 calc R . . C22 C 0.5513(3) 0.4420(3) 0.8134(4) 0.0635(15) Uani 1 1 d . . . H22A H 0.5837 0.4176 0.8328 0.095 Uiso 1 1 calc R . . H22B H 0.5626 0.4684 0.7690 0.095 Uiso 1 1 calc R . . H22C H 0.5219 0.4110 0.7981 0.095 Uiso 1 1 calc R . . C23 C 0.4932(2) 0.8162(3) 1.1588(3) 0.0504(12) Uani 1 1 d . . . H23A H 0.4542 0.8326 1.1578 0.060 Uiso 1 1 calc R . . H23B H 0.5095 0.8268 1.2094 0.060 Uiso 1 1 calc R . . C24 C 0.5260(2) 0.8485(2) 1.0979(3) 0.0465(11) Uani 1 1 d . . . C25 C 0.5517(2) 0.9099(3) 1.0939(4) 0.0543(13) Uani 1 1 d . . . H25A H 0.5532 0.9426 1.1327 0.065 Uiso 1 1 calc R . . C26 C 0.57448(19) 0.9130(2) 1.0216(3) 0.0466(10) Uani 1 1 d . . . C27 C 0.6086(2) 0.9651(2) 0.9823(4) 0.0520(12) Uani 1 1 d . . . H27A H 0.5909 1.0085 0.9899 0.062 Uiso 1 1 calc R . . H27B H 0.6466 0.9666 1.0050 0.062 Uiso 1 1 calc R . . C28 C 0.5637(2) 0.9743(3) 0.8566(3) 0.0504(12) Uani 1 1 d . . . H28A H 0.5666 1.0226 0.8503 0.060 Uiso 1 1 calc R . . H28B H 0.5295 0.9650 0.8867 0.060 Uiso 1 1 calc R . . C29 C 0.5582(2) 0.9435(3) 0.7801(3) 0.0539(12) Uani 1 1 d . . . C30 C 0.5385(3) 0.9761(3) 0.7162(4) 0.0623(14) Uani 1 1 d . . . H30A H 0.5278 1.0210 0.7196 0.075 Uiso 1 1 calc R . . C31 C 0.5345(3) 0.9432(4) 0.6479(5) 0.083(2) Uani 1 1 d . . . H31A H 0.5220 0.9657 0.6034 0.099 Uiso 1 1 calc R . . C32 C 0.5485(4) 0.8782(4) 0.6435(5) 0.091(2) Uani 1 1 d . . . H32A H 0.5440 0.8548 0.5968 0.109 Uiso 1 1 calc R . . C33 C 0.5694(3) 0.8463(3) 0.7084(4) 0.0731(19) Uani 1 1 d . . . C34 C 0.6099(4) 0.7389(5) 0.6469(6) 0.097(2) Uiso 1 1 d . . . H34A H 0.6133 0.7649 0.5992 0.116 Uiso 1 1 calc R . . H34B H 0.6481 0.7252 0.6621 0.116 Uiso 1 1 calc R . . C35 C 0.5786(3) 0.6827(3) 0.6313(4) 0.0684(16) Uani 1 1 d . . . C36 C 0.5142(4) 0.7093(7) 0.6076(8) 0.121(4) Uani 1 1 d . . . H36A H 0.4868 0.6744 0.6178 0.181 Uiso 1 1 calc R . . H36B H 0.5134 0.7207 0.5531 0.181 Uiso 1 1 calc R . . H36C H 0.5049 0.7481 0.6382 0.181 Uiso 1 1 calc R . . C37 C 0.5648(4) 0.6407(4) 0.6997(4) 0.081(2) Uani 1 1 d . . . H37A H 0.5994 0.6234 0.7220 0.122 Uiso 1 1 calc R . . H37B H 0.5408 0.6041 0.6838 0.122 Uiso 1 1 calc R . . H37C H 0.5451 0.6673 0.7380 0.122 Uiso 1 1 calc R . . C38 C 0.5902(5) 0.6470(4) 0.5613(5) 0.099(3) Uani 1 1 d . . . H38A H 0.6274 0.6267 0.5647 0.148 Uiso 1 1 calc R . . H38B H 0.5893 0.6774 0.5178 0.148 Uiso 1 1 calc R . . H38C H 0.5619 0.6127 0.5541 0.148 Uiso 1 1 calc R . . C39 C 0.6655(2) 0.9763(3) 0.8680(5) 0.0674(18) Uani 1 1 d . . . H39A H 0.6726 1.0212 0.8877 0.081 Uiso 1 1 calc R . . H39B H 0.6631 0.9785 0.8115 0.081 Uiso 1 1 calc R . . C40 C 0.7130(2) 0.9301(3) 0.8919(6) 0.081(2) Uani 1 1 d . . . C41 C 0.7656(3) 0.9551(4) 0.9157(7) 0.106(3) Uani 1 1 d . . . H41A H 0.7723 1.0011 0.9188 0.127 Uiso 1 1 calc R . . C42 C 0.8061(3) 0.9108(5) 0.9339(8) 0.125(4) Uani 1 1 d . . . H42A H 0.8417 0.9265 0.9497 0.150 Uiso 1 1 calc R . . C43 C 0.7975(3) 0.8461(4) 0.9303(7) 0.111(4) Uani 1 1 d . . . H43A H 0.8268 0.8163 0.9425 0.133 Uiso 1 1 calc R . . C44 C 0.7446(2) 0.8229(4) 0.9084(5) 0.079(2) Uani 1 1 d . . . C45 C 0.7750(3) 0.7075(4) 0.9119(6) 0.083(2) Uani 1 1 d . . . H45A H 0.7874 0.7076 0.9660 0.100 Uiso 1 1 calc R . . H45B H 0.8078 0.7185 0.8797 0.100 Uiso 1 1 calc R . . C46 C 0.7552(4) 0.6407(4) 0.8917(8) 0.109(4) Uani 1 1 d . . . C47 C 0.8074(4) 0.5957(4) 0.8939(9) 0.137(5) Uani 1 1 d . . . H47A H 0.8274 0.5987 0.8450 0.206 Uiso 1 1 calc R . . H47B H 0.7957 0.5501 0.9025 0.206 Uiso 1 1 calc R . . H47C H 0.8322 0.6097 0.9355 0.206 Uiso 1 1 calc R . . C48 C 0.7129(5) 0.6259(6) 0.9574(10) 0.152(6) Uani 1 1 d . . . H48A H 0.7317 0.6310 1.0070 0.228 Uiso 1 1 calc R . . H48B H 0.6990 0.5807 0.9523 0.228 Uiso 1 1 calc R . . H48C H 0.6814 0.6566 0.9543 0.228 Uiso 1 1 calc R . . C49 C 0.7220(6) 0.6276(6) 0.8276(10) 0.183(8) Uani 1 1 d . . . H49A H 0.6850 0.6477 0.8345 0.275 Uiso 1 1 calc R . . H49B H 0.7177 0.5799 0.8216 0.275 Uiso 1 1 calc R . . H49C H 0.7399 0.6458 0.7818 0.275 Uiso 1 1 calc R . . B1 B 0.6238(2) 1.2011(3) 0.9344(3) 0.0446(11) Uiso 1 1 d . . . C50 C 0.6366(2) 1.1550(2) 1.0113(4) 0.0562(13) Uani 1 1 d . . . C51 C 0.6018(3) 1.1539(4) 1.0728(5) 0.083(2) Uani 1 1 d . . . H51A H 0.5696 1.1814 1.0730 0.099 Uiso 1 1 calc R . . C52 C 0.6120(3) 1.1130(5) 1.1362(6) 0.103(3) Uani 1 1 d . . . H52A H 0.5864 1.1116 1.1777 0.124 Uiso 1 1 calc R . . C53 C 0.6596(4) 1.0754(3) 1.1370(6) 0.089(3) Uani 1 1 d . . . H53A H 0.6676 1.0482 1.1799 0.107 Uiso 1 1 calc R . . C54 C 0.6949(4) 1.0767(4) 1.0774(7) 0.091(3) Uani 1 1 d . . . H54A H 0.7279 1.0506 1.0783 0.109 Uiso 1 1 calc R . . C55 C 0.6840(2) 1.1145(3) 1.0166(5) 0.076(2) Uani 1 1 d . . . H55A H 0.7095 1.1140 0.9749 0.091 Uiso 1 1 calc R . . C56 C 0.65063(19) 1.2753(2) 0.9474(3) 0.0425(10) Uani 1 1 d . . . C57 C 0.6520(2) 1.3061(2) 1.0193(3) 0.0495(11) Uani 1 1 d . . . H57A H 0.6390 1.2826 1.0629 0.059 Uiso 1 1 calc R . . C58 C 0.6718(3) 1.3704(3) 1.0290(3) 0.0560(14) Uani 1 1 d . . . H58A H 0.6721 1.3894 1.0786 0.067 Uiso 1 1 calc R . . C59 C 0.6907(2) 1.4059(2) 0.9681(3) 0.0527(13) Uani 1 1 d . . . H59A H 0.7044 1.4494 0.9747 0.063 Uiso 1 1 calc R . . C60 C 0.6894(2) 1.3773(3) 0.8971(3) 0.0550(13) Uani 1 1 d . . . H60A H 0.7021 1.4014 0.8539 0.066 Uiso 1 1 calc R . . C61 C 0.6697(2) 1.3135(2) 0.8875(3) 0.0479(11) Uani 1 1 d . . . H61A H 0.6693 1.2954 0.8374 0.057 Uiso 1 1 calc R . . C62 C 0.6505(2) 1.1669(3) 0.8577(4) 0.0648(18) Uani 1 1 d . . . C63 C 0.7084(3) 1.1674(4) 0.8432(6) 0.087(3) Uani 1 1 d . . . H63A H 0.7317 1.1912 0.8775 0.105 Uiso 1 1 calc R . . C64 C 0.7335(3) 1.1360(5) 0.7833(6) 0.110(4) Uani 1 1 d . . . H64A H 0.7731 1.1356 0.7791 0.132 Uiso 1 1 calc R . . C65 C 0.7017(3) 1.1054(5) 0.7297(6) 0.103(3) Uani 1 1 d . . . H65A H 0.7188 1.0827 0.6883 0.124 Uiso 1 1 calc R . . C66 C 0.6430(3) 1.1078(3) 0.7367(4) 0.0691(17) Uani 1 1 d . . . H66A H 0.6196 1.0893 0.6983 0.083 Uiso 1 1 calc R . . C67 C 0.6200(2) 1.1380(3) 0.8007(4) 0.0524(12) Uani 1 1 d . . . H67A H 0.5804 1.1386 0.8053 0.063 Uiso 1 1 calc R . . C68 C 0.5558(2) 1.2072(2) 0.9229(3) 0.0416(10) Uani 1 1 d . . . C69 C 0.5208(2) 1.1532(2) 0.9301(4) 0.0503(12) Uani 1 1 d . . . H69A H 0.5363 1.1129 0.9475 0.060 Uiso 1 1 calc R . . C70 C 0.4645(3) 1.1557(3) 0.9130(4) 0.0660(16) Uani 1 1 d . . . H70A H 0.4422 1.1172 0.9180 0.079 Uiso 1 1 calc R . . C71 C 0.4400(3) 1.2142(3) 0.8886(4) 0.0625(14) Uiso 1 1 d . . . H71A H 0.4015 1.2160 0.8752 0.075 Uiso 1 1 calc R . . C72 C 0.4732(2) 1.2692(3) 0.8843(4) 0.0516(11) Uiso 1 1 d . . . H72A H 0.4571 1.3100 0.8695 0.062 Uiso 1 1 calc R . . C73 C 0.5304(2) 1.2661(2) 0.9014(3) 0.0437(10) Uiso 1 1 d . . . H73A H 0.5524 1.3049 0.8983 0.052 Uiso 1 1 calc R . . O3 O 0.4284(3) 0.9882(4) 0.9466(4) 0.116(2) Uiso 1 1 d . . . C74 C 0.4205(5) 0.8849(6) 0.8877(8) 0.132(4) Uiso 1 1 d . . . H74A H 0.4263 0.9087 0.8395 0.198 Uiso 1 1 calc R . . H74B H 0.3883 0.8554 0.8825 0.198 Uiso 1 1 calc R . . H74C H 0.4540 0.8591 0.8997 0.198 Uiso 1 1 calc R . . C75 C 0.4098(3) 0.9324(4) 0.9500(5) 0.0817(19) Uiso 1 1 d . . . C76 C 0.3812(5) 0.9091(6) 1.0206(7) 0.118(3) Uiso 1 1 d . . . H76A H 0.3826 0.9437 1.0596 0.177 Uiso 1 1 calc R . . H76B H 0.4000 0.8696 1.0398 0.177 Uiso 1 1 calc R . . H76C H 0.3420 0.8988 1.0088 0.177 Uiso 1 1 calc R . . C77 C 0.2343(6) 0.4968(10) 1.1884(9) 0.205(2) Uiso 1 1 d D . . H77A H 0.2195 0.5001 1.2406 0.308 Uiso 1 1 calc R . . H77B H 0.2365 0.4504 1.1734 0.308 Uiso 1 1 calc R . . H77C H 0.2095 0.5203 1.1531 0.308 Uiso 1 1 calc R . . C78 C 0.2932(6) 0.5276(11) 1.1854(6) 0.205(2) Uiso 1 1 d D . . H78A H 0.2915 0.5741 1.2019 0.246 Uiso 1 1 calc R . . H78B H 0.3187 0.5037 1.2204 0.246 Uiso 1 1 calc R . . C79 C 0.3151(5) 0.5232(10) 1.1027(5) 0.205(2) Uiso 1 1 d D . . H79A H 0.2916 0.5506 1.0685 0.246 Uiso 1 1 calc R . . H79B H 0.3133 0.4772 1.0845 0.246 Uiso 1 1 calc R . . C80 C 0.3760(5) 0.5478(10) 1.1011(7) 0.205(2) Uiso 1 1 d D . . H80A H 0.3785 0.5919 1.1249 0.246 Uiso 1 1 calc R . . H80B H 0.4003 0.5174 1.1304 0.246 Uiso 1 1 calc R . . C81 C 0.3956(6) 0.5511(10) 1.0172(8) 0.205(2) Uiso 1 1 d D . . H81A H 0.4338 0.5687 1.0151 0.308 Uiso 1 1 calc R . . H81B H 0.3704 0.5799 0.9882 0.308 Uiso 1 1 calc R . . H81C H 0.3949 0.5069 0.9949 0.308 Uiso 1 1 calc R . . C82 C 0.6979(9) 0.7629(8) 1.1939(10) 0.205(2) Uiso 1 1 d D . . H82A H 0.6835 0.7178 1.1906 0.308 Uiso 1 1 calc R . . H82B H 0.6738 0.7887 1.2280 0.308 Uiso 1 1 calc R . . H82C H 0.7361 0.7622 1.2143 0.308 Uiso 1 1 calc R . . C83 C 0.6981(7) 0.7941(7) 1.1136(8) 0.205(2) Uiso 1 1 d D . . H83A H 0.6602 0.7915 1.0907 0.246 Uiso 1 1 calc R . . H83B H 0.7245 0.7703 1.0799 0.246 Uiso 1 1 calc R . . C84 C 0.7162(5) 0.8666(6) 1.1212(10) 0.205(2) Uiso 1 1 d D . . H84A H 0.7168 0.8877 1.0701 0.246 Uiso 1 1 calc R . . H84B H 0.6892 0.8907 1.1539 0.246 Uiso 1 1 calc R . . C85 C 0.7750(6) 0.8688(6) 1.1572(11) 0.205(2) Uiso 1 1 d D . . H85A H 0.7998 0.8367 1.1315 0.246 Uiso 1 1 calc R . . H85B H 0.7728 0.8572 1.2122 0.246 Uiso 1 1 calc R . . C86 C 0.7986(7) 0.9387(8) 1.1479(12) 0.205(2) Uiso 1 1 d D . . H86A H 0.8358 0.9411 1.1714 0.308 Uiso 1 1 calc R . . H86B H 0.7736 0.9702 1.1730 0.308 Uiso 1 1 calc R . . H86C H 0.8015 0.9494 1.0933 0.308 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0449(3) 0.0328(3) 0.0370(3) -0.0039(3) -0.0147(3) 0.0021(3) Mn2 0.0338(3) 0.0392(4) 0.0704(5) -0.0164(4) 0.0022(3) -0.0029(3) O1 0.0420(16) 0.0361(16) 0.0374(16) -0.0050(13) -0.0080(12) 0.0030(12) O2 0.0406(17) 0.0457(19) 0.085(3) -0.0208(19) 0.0070(16) 0.0012(15) N1 0.062(3) 0.048(2) 0.042(2) -0.0062(19) -0.0213(19) 0.0049(19) N2 0.053(2) 0.0380(19) 0.0303(17) 0.0022(15) -0.0025(16) -0.0071(16) N3 0.066(3) 0.047(2) 0.051(2) 0.0006(19) -0.024(2) 0.012(2) N4 0.0435(19) 0.041(2) 0.047(2) -0.0107(17) -0.0108(17) -0.0038(16) N5 0.043(2) 0.047(2) 0.0258(17) -0.0038(15) -0.0047(14) 0.0084(16) N6 0.071(3) 0.043(2) 0.056(3) 0.0041(19) -0.016(2) 0.018(2) N7 0.0404(19) 0.037(2) 0.076(3) -0.018(2) 0.0049(19) -0.0024(15) N8 0.049(2) 0.051(3) 0.058(3) -0.012(2) 0.0083(19) -0.0096(19) N9 0.041(2) 0.057(3) 0.129(5) -0.036(3) 0.012(3) -0.003(2) N10 0.0396(19) 0.0321(19) 0.057(2) -0.0116(17) -0.0095(17) 0.0009(15) N11 0.133(6) 0.057(3) 0.067(3) -0.025(3) 0.032(4) -0.028(3) N12 0.042(2) 0.057(3) 0.145(6) -0.028(3) -0.004(3) 0.007(2) C1 0.079(4) 0.053(3) 0.034(2) 0.006(2) -0.015(2) -0.004(3) C2 0.071(3) 0.045(3) 0.024(2) 0.0051(18) -0.011(2) -0.018(2) C3 0.065(3) 0.073(4) 0.022(2) -0.005(2) 0.009(2) -0.025(3) C4 0.051(3) 0.097(5) 0.037(3) -0.004(3) 0.012(2) -0.027(3) C5 0.044(2) 0.078(3) 0.0244(19) -0.003(2) 0.0011(19) -0.020(2) C6 0.045(2) 0.035(2) 0.033(2) 0.0039(16) -0.0034(16) -0.0055(17) C7 0.040(2) 0.055(3) 0.034(2) -0.0112(19) -0.0110(17) 0.0059(19) C8 0.065(4) 0.198(9) 0.040(3) -0.044(4) -0.019(3) 0.080(5) C9 0.060(3) 0.146(7) 0.036(3) -0.035(3) -0.016(2) 0.041(4) C12 0.077(4) 0.087(5) 0.049(3) -0.006(3) -0.035(3) 0.011(3) C13 0.080(4) 0.061(4) 0.066(4) 0.008(3) -0.029(3) 0.014(3) C14 0.110(6) 0.091(5) 0.060(4) 0.013(4) -0.021(4) 0.037(5) C15 0.168(9) 0.082(6) 0.085(6) 0.013(4) -0.042(6) 0.059(6) C16 0.121(6) 0.072(5) 0.076(5) 0.002(4) -0.029(4) 0.049(4) C17 0.075(4) 0.049(3) 0.069(4) 0.004(3) -0.026(3) 0.020(3) C18 0.058(3) 0.050(3) 0.060(3) 0.005(2) -0.004(2) 0.018(2) C19 0.067(3) 0.044(3) 0.068(3) 0.000(3) 0.012(3) 0.013(2) C20 0.065(4) 0.054(3) 0.084(4) -0.016(3) -0.015(3) 0.008(3) C21 0.094(4) 0.047(3) 0.079(4) -0.006(3) 0.021(4) 0.000(3) C22 0.082(4) 0.043(3) 0.066(3) -0.006(3) 0.014(3) 0.010(3) C23 0.058(3) 0.054(3) 0.038(2) -0.011(2) -0.017(2) -0.004(2) C24 0.044(2) 0.048(3) 0.048(3) -0.017(2) -0.016(2) 0.000(2) C25 0.052(3) 0.048(3) 0.062(3) -0.022(2) -0.016(2) 0.000(2) C26 0.042(2) 0.036(2) 0.062(3) -0.014(2) -0.009(2) 0.0005(18) C27 0.045(2) 0.036(2) 0.075(3) -0.013(2) -0.005(2) -0.008(2) C28 0.046(3) 0.040(2) 0.065(3) -0.007(2) 0.009(2) -0.003(2) C29 0.052(3) 0.050(3) 0.059(3) -0.006(2) 0.007(2) -0.014(2) C30 0.059(3) 0.059(3) 0.069(4) 0.002(3) -0.005(3) -0.005(3) C31 0.082(5) 0.088(5) 0.077(5) -0.004(4) -0.011(4) -0.014(4) C32 0.111(6) 0.093(6) 0.069(4) -0.021(4) 0.001(4) -0.036(5) C33 0.089(5) 0.062(4) 0.069(4) -0.010(3) 0.020(4) -0.025(3) C35 0.092(4) 0.057(3) 0.056(3) -0.016(3) 0.013(3) 0.009(3) C36 0.083(5) 0.170(11) 0.110(8) -0.017(7) -0.006(5) 0.005(6) C37 0.113(6) 0.059(4) 0.072(4) -0.019(3) 0.012(4) -0.017(4) C38 0.164(9) 0.069(5) 0.063(4) -0.021(3) 0.007(5) 0.000(5) C39 0.043(3) 0.049(3) 0.110(5) -0.026(3) 0.013(3) -0.014(2) C40 0.045(3) 0.055(3) 0.144(7) -0.036(4) 0.014(4) -0.012(2) C41 0.044(3) 0.086(5) 0.188(10) -0.060(6) 0.021(4) -0.013(3) C42 0.046(3) 0.094(6) 0.235(12) -0.076(7) -0.003(5) -0.010(4) C43 0.039(3) 0.091(6) 0.203(11) -0.054(6) 0.001(4) -0.002(3) C44 0.043(3) 0.080(4) 0.113(6) -0.035(4) 0.008(3) 0.002(3) C45 0.051(3) 0.082(5) 0.116(6) -0.025(4) -0.013(4) 0.013(3) C46 0.074(4) 0.065(4) 0.188(10) -0.018(6) -0.055(6) 0.012(4) C47 0.100(6) 0.075(5) 0.237(14) -0.029(7) -0.080(8) 0.033(5) C48 0.111(8) 0.103(8) 0.242(17) 0.047(10) -0.028(10) -0.003(6) C49 0.154(10) 0.141(10) 0.255(17) -0.120(11) -0.107(11) 0.099(9) C50 0.038(2) 0.038(2) 0.092(4) 0.010(3) -0.008(3) -0.0082(18) C51 0.067(4) 0.091(5) 0.090(5) 0.052(4) 0.005(4) 0.005(3) C52 0.077(5) 0.117(7) 0.116(7) 0.063(6) -0.015(4) -0.028(5) C53 0.089(5) 0.044(3) 0.135(7) 0.031(4) -0.077(6) -0.021(3) C54 0.082(5) 0.052(4) 0.139(8) -0.016(4) -0.064(5) -0.002(4) C55 0.054(3) 0.043(3) 0.132(6) -0.024(4) -0.042(4) 0.003(2) C56 0.041(2) 0.037(2) 0.050(3) 0.0018(19) 0.0071(19) 0.0002(18) C57 0.065(3) 0.045(2) 0.039(2) 0.008(2) 0.002(2) 0.012(2) C58 0.085(4) 0.043(3) 0.041(3) -0.001(2) -0.025(3) 0.015(2) C59 0.063(3) 0.030(2) 0.066(3) -0.001(2) -0.026(3) 0.003(2) C60 0.066(3) 0.054(3) 0.045(3) 0.012(2) 0.002(2) -0.021(2) C61 0.059(3) 0.051(3) 0.034(2) -0.007(2) 0.011(2) -0.018(2) C62 0.056(3) 0.038(3) 0.100(5) -0.009(3) 0.040(3) -0.008(2) C63 0.049(3) 0.073(4) 0.139(7) -0.049(4) 0.035(4) -0.020(3) C64 0.048(3) 0.115(6) 0.167(8) -0.068(6) 0.060(5) -0.025(4) C65 0.082(5) 0.103(6) 0.124(7) -0.048(5) 0.061(5) -0.024(4) C66 0.075(4) 0.060(4) 0.073(4) -0.009(3) 0.035(3) -0.001(3) C67 0.052(3) 0.039(3) 0.067(3) -0.001(2) 0.021(2) -0.006(2) C68 0.045(2) 0.037(2) 0.043(2) -0.0005(18) 0.0135(19) -0.0015(18) C69 0.045(3) 0.039(3) 0.067(3) 0.000(2) 0.010(2) 0.000(2) C70 0.053(3) 0.052(3) 0.093(4) -0.009(3) 0.019(3) -0.015(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 Mn1 O1 2.003(3) . ? Mn1 N4 2.128(4) . ? Mn1 N3 2.204(4) . ? Mn1 N2 2.234(4) . ? Mn1 N1 2.330(4) . ? Mn2 O2 2.006(4) . ? Mn2 N10 2.137(4) . ? Mn2 N8 2.207(5) . ? Mn2 N9 2.230(5) . ? Mn2 N7 2.285(4) . ? N1 C1 1.442(8) . ? N1 C12 1.473(7) . ? N1 C23 1.483(8) . ? N2 C6 1.351(6) . ? N2 C2 1.360(6) . ? N3 C17 1.352(8) . ? N3 C13 1.362(8) . ? N4 N10 1.346(6) . ? N4 C24 1.356(6) . ? N5 C6 1.340(6) . ? N5 C7 1.463(5) . ? N6 C17 1.357(8) . ? N6 C18 1.447(7) . ? N7 C39 1.468(7) . ? N7 C28 1.473(7) . ? N7 C27 1.476(8) . ? N8 C33 1.366(8) . ? N8 C29 1.369(7) . ? N9 C40 1.335(8) . ? N9 C44 1.377(9) . ? N10 C26 1.340(6) . ? N11 C33 1.352(10) . ? N11 C34 1.512(11) . ? N12 C44 1.353(9) . ? N12 C45 1.460(8) . ? C1 C2 1.523(7) . ? C2 C3 1.352(8) . ? C3 C4 1.378(8) . ? C4 C5 1.361(7) . ? C5 C6 1.408(7) . ? C7 C8 1.461(7) . ? C8 C10 1.315(14) . ? C8 C9 1.530(7) . ? C8 C11 1.759(16) . ? C12 C13 1.506(10) . ? C13 C14 1.396(9) . ? C14 C15 1.373(12) . ? C15 C16 1.347(12) . ? C16 C17 1.437(8) . ? C18 C19 1.513(9) . ? C19 C20 1.526(8) . ? C19 C21 1.526(9) . ? C19 C22 1.532(8) . ? C23 C24 1.475(8) . ? C24 C25 1.395(8) . ? C25 C26 1.377(9) . ? C26 C27 1.503(8) . ? C28 C29 1.483(8) . ? C29 C30 1.380(9) . ? C30 C31 1.372(10) . ? C31 C32 1.366(12) . ? C32 C33 1.398(12) . ? C34 C35 1.393(12) . ? C35 C38 1.448(9) . ? C35 C37 1.506(10) . ? C35 C36 1.682(13) . ? C39 C40 1.531(9) . ? C40 C41 1.416(9) . ? C41 C42 1.359(13) . ? C42 C43 1.333(12) . ? C43 C44 1.404(9) . ? C45 C46 1.481(11) . ? C46 C49 1.398(15) . ? C46 C47 1.547(11) . ? C46 C48 1.559(18) . ? B1 C62 1.640(8) . ? B1 C68 1.641(7) . ? B1 C56 1.655(7) . ? B1 C50 1.665(8) . ? C50 C51 1.359(10) . ? C50 C55 1.403(7) . ? C51 C52 1.405(10) . ? C52 C53 1.370(13) . ? C53 C54 1.340(13) . ? C54 C55 1.337(12) . ? C56 C61 1.380(7) . ? C56 C57 1.405(8) . ? C57 C58 1.401(8) . ? C58 C59 1.363(8) . ? C59 C60 1.369(8) . ? C60 C61 1.391(7) . ? C62 C67 1.365(9) . ? C62 C63 1.405(8) . ? C63 C64 1.364(10) . ? C64 C65 1.356(13) . ? C65 C66 1.408(11) . ? C66 C67 1.390(8) . ? C68 C69 1.385(7) . ? C68 C73 1.394(7) . ? C69 C70 1.378(9) . ? C70 C71 1.393(9) . ? C71 C72 1.374(8) . ? C72 C73 1.399(8) . ? O3 C75 1.220(10) . ? C74 C75 1.477(15) . ? C75 C76 1.487(14) . ? C77 C78 1.541(2) . ? C78 C79 1.539(2) . ? C79 C80 1.540(2) . ? C80 C81 1.539(2) . ? C82 C83 1.540(2) . ? C83 C84 1.541(2) . ? C84 C85 1.539(2) . ? C85 C86 1.540(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 N4 111.20(15) . . ? O1 Mn1 N3 101.67(15) . . ? N4 Mn1 N3 112.52(17) . . ? O1 Mn1 N2 100.60(13) . . ? N4 Mn1 N2 114.75(15) . . ? N3 Mn1 N2 114.56(18) . . ? O1 Mn1 N1 174.00(16) . . ? N4 Mn1 N1 74.57(17) . . ? N3 Mn1 N1 76.94(17) . . ? N2 Mn1 N1 74.98(15) . . ? O2 Mn2 N10 113.07(16) . . ? O2 Mn2 N8 102.03(17) . . ? N10 Mn2 N8 114.23(15) . . ? O2 Mn2 N9 99.19(16) . . ? N10 Mn2 N9 115.2(2) . . ? N8 Mn2 N9 111.3(2) . . ? O2 Mn2 N7 172.13(16) . . ? N10 Mn2 N7 74.46(16) . . ? N8 Mn2 N7 75.94(17) . . ? N9 Mn2 N7 74.84(16) . . ? C1 N1 C12 113.3(5) . . ? C1 N1 C23 112.9(5) . . ? C12 N1 C23 110.8(4) . . ? C1 N1 Mn1 106.2(3) . . ? C12 N1 Mn1 104.6(4) . . ? C23 N1 Mn1 108.5(3) . . ? C6 N2 C2 118.2(4) . . ? C6 N2 Mn1 124.6(3) . . ? C2 N2 Mn1 115.7(3) . . ? C17 N3 C13 120.0(5) . . ? C17 N3 Mn1 125.4(3) . . ? C13 N3 Mn1 114.4(4) . . ? N10 N4 C24 108.6(4) . . ? N10 N4 Mn1 133.6(3) . . ? C24 N4 Mn1 117.7(3) . . ? C6 N5 C7 122.6(4) . . ? C17 N6 C18 127.3(4) . . ? C39 N7 C28 112.0(5) . . ? C39 N7 C27 110.9(4) . . ? C28 N7 C27 112.4(4) . . ? C39 N7 Mn2 108.3(3) . . ? C28 N7 Mn2 104.1(3) . . ? C27 N7 Mn2 108.8(3) . . ? C33 N8 C29 118.8(6) . . ? C33 N8 Mn2 125.9(5) . . ? C29 N8 Mn2 115.0(4) . . ? C40 N9 C44 118.0(5) . . ? C40 N9 Mn2 115.5(4) . . ? C44 N9 Mn2 125.3(4) . . ? C26 N10 N4 108.3(4) . . ? C26 N10 Mn2 116.5(3) . . ? N4 N10 Mn2 132.5(3) . . ? C33 N11 C34 132.2(7) . . ? C44 N12 C45 121.8(5) . . ? N1 C1 C2 111.2(4) . . ? C3 C2 N2 123.6(5) . . ? C3 C2 C1 122.5(5) . . ? N2 C2 C1 113.9(5) . . ? C2 C3 C4 118.3(4) . . ? C5 C4 C3 119.9(5) . . ? C4 C5 C6 119.7(5) . . ? N5 C6 N2 117.3(4) . . ? N5 C6 C5 122.7(4) . . ? N2 C6 C5 120.0(4) . . ? C8 C7 N5 116.9(4) . . ? C10 C8 C7 129.4(8) . . ? C10 C8 C9 117.4(8) . . ? C7 C8 C9 107.8(4) . . ? C10 C8 C11 89.8(9) . . ? C7 C8 C11 101.4(7) . . ? C9 C8 C11 103.0(8) . . ? N1 C12 C13 112.5(5) . . ? N3 C13 C14 121.7(7) . . ? N3 C13 C12 117.0(5) . . ? C14 C13 C12 121.3(6) . . ? C15 C14 C13 117.7(7) . . ? C16 C15 C14 122.1(6) . . ? C15 C16 C17 119.0(7) . . ? N3 C17 N6 116.9(4) . . ? N3 C17 C16 119.3(6) . . ? N6 C17 C16 123.7(6) . . ? N6 C18 C19 114.4(5) . . ? C18 C19 C20 110.6(4) . . ? C18 C19 C21 110.0(6) . . ? C20 C19 C21 110.6(6) . . ? C18 C19 C22 109.1(5) . . ? C20 C19 C22 108.4(6) . . ? C21 C19 C22 108.1(5) . . ? C24 C23 N1 109.9(4) . . ? N4 C24 C25 108.3(5) . . ? N4 C24 C23 119.7(4) . . ? C25 C24 C23 132.0(5) . . ? C26 C25 C24 105.1(4) . . ? N10 C26 C25 109.7(5) . . ? N10 C26 C27 118.6(5) . . ? C25 C26 C27 131.6(5) . . ? N7 C27 C26 110.1(4) . . ? N7 C28 C29 113.2(4) . . ? N8 C29 C30 121.3(5) . . ? N8 C29 C28 114.9(5) . . ? C30 C29 C28 123.8(5) . . ? C31 C30 C29 119.5(6) . . ? C32 C31 C30 120.3(8) . . ? C31 C32 C33 119.4(7) . . ? N11 C33 N8 115.6(7) . . ? N11 C33 C32 123.7(7) . . ? N8 C33 C32 120.7(7) . . ? C35 C34 N11 115.3(7) . . ? C34 C35 C38 118.4(8) . . ? C34 C35 C37 115.3(7) . . ? C38 C35 C37 115.3(6) . . ? C34 C35 C36 106.0(7) . . ? C38 C35 C36 97.4(7) . . ? C37 C35 C36 100.1(7) . . ? N7 C39 C40 108.4(5) . . ? N9 C40 C41 122.3(7) . . ? N9 C40 C39 116.6(5) . . ? C41 C40 C39 121.1(6) . . ? C42 C41 C40 117.4(7) . . ? C43 C42 C41 122.4(7) . . ? C42 C43 C44 118.9(8) . . ? N12 C44 N9 116.0(5) . . ? N12 C44 C43 123.0(7) . . ? N9 C44 C43 121.0(7) . . ? N12 C45 C46 113.4(6) . . ? C49 C46 C45 123.1(10) . . ? C49 C46 C47 111.4(9) . . ? C45 C46 C47 106.3(6) . . ? C49 C46 C48 100.6(11) . . ? C45 C46 C48 102.0(9) . . ? C47 C46 C48 113.0(10) . . ? C62 B1 C68 108.5(4) . . ? C62 B1 C56 110.3(4) . . ? C68 B1 C56 109.3(4) . . ? C62 B1 C50 110.4(4) . . ? C68 B1 C50 108.8(4) . . ? C56 B1 C50 109.4(4) . . ? C51 C50 C55 115.6(7) . . ? C51 C50 B1 122.3(5) . . ? C55 C50 B1 122.1(6) . . ? C50 C51 C52 121.7(7) . . ? C53 C52 C51 118.9(9) . . ? C54 C53 C52 120.2(7) . . ? C55 C54 C53 120.3(7) . . ? C54 C55 C50 123.2(9) . . ? C61 C56 C57 114.7(4) . . ? C61 C56 B1 122.6(4) . . ? C57 C56 B1 122.5(4) . . ? C58 C57 C56 122.2(5) . . ? C59 C58 C57 120.9(5) . . ? C58 C59 C60 118.3(5) . . ? C59 C60 C61 120.9(5) . . ? C56 C61 C60 123.1(5) . . ? C67 C62 C63 113.4(6) . . ? C67 C62 B1 124.8(5) . . ? C63 C62 B1 121.8(6) . . ? C64 C63 C62 124.5(7) . . ? C65 C64 C63 120.0(6) . . ? C64 C65 C66 118.8(6) . . ? C67 C66 C65 118.6(7) . . ? C62 C67 C66 124.5(6) . . ? C69 C68 C73 116.3(5) . . ? C69 C68 B1 121.7(4) . . ? C73 C68 B1 121.9(4) . . ? C70 C69 C68 122.7(5) . . ? C69 C70 C71 120.5(5) . . ? C72 C71 C70 118.1(6) . . ? C71 C72 C73 120.9(5) . . ? C68 C73 C72 121.5(5) . . ? O3 C75 C74 120.7(9) . . ? O3 C75 C76 120.2(8) . . ? C74 C75 C76 118.8(9) . . ? C79 C78 C77 108.5(2) . . ? C78 C79 C80 108.6(2) . . ? C81 C80 C79 108.5(2) . . ? C82 C83 C84 108.5(2) . . ? C85 C84 C83 108.6(2) . . ? C84 C85 C86 108.6(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.189 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.085 #==END