# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Stefan Kaskel' _publ_contact_author_address ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; _publ_contact_author_email Stefan.Kaskel@chemie.tu-dresden.de _publ_contact_author_phone '00490351/46334885 ' _publ_contact_author_fax (+49)035146337287 loop_ _publ_author_name _publ_author_address P.Wollmann ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; I.Senkovska ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; S.Kaskel ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; U.Stoeck ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; R.Gruenker ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; K.Gedrich ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; ; N.Klein ; ;Department of Inorganic Chemistry University of Technology Dresden Mommsenstrasse 6 D-01069 Dresden Germany ; M.Leistner ;Department CVD / Process Monitoring Fraunhofer IWS Winterbergstr. 28, 01277 Dresden Germany ; O.Throl ;Department CVD / Process Monitoring Fraunhofer IWS Winterbergstr. 28, 01277 Dresden Germany ; W.Grahlert ;Department CVD / Process Monitoring Fraunhofer IWS Winterbergstr. 28, 01277 Dresden Germany ; _publ_section_title ; High-throughput discovery of porous materials ; data_Co2(BTB)(NO3) _database_code_depnum_ccdc_archive 'CCDC 801199' #TrackingRef '- DUT-27-CCDC-80199.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Co2(btb)(NO3)(DEF)3; (DUT-27)' _chemical_melting_point ? _chemical_formula_moiety 'C42 H48 Co3 N3 O12' _chemical_formula_sum 'C42 H48 Co3 N3 O12' _chemical_formula_weight 963.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting C2/c _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.853(6) _cell_length_b 16.823(3) _cell_length_c 20.998(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.28(3) _cell_angle_gamma 90.00 _cell_volume 8822(3) _cell_formula_units_Z 8 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used 5540 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3983 _exptl_absorpt_coefficient_mu 1.178 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Absorption cooefficient is given for the solvent free framework. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'beamline BL14.2 BESSY-II' _diffrn_radiation_monochromator Si-111 _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5540 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.13 _reflns_number_total 5540 _reflns_number_gt 5227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement 'HKL 2000' _computing_data_reduction 'HKL 2000' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.0945P)^2^+43.7632P] 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_number_reflns 5540 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _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 0.27452(3) 0.03308(4) 0.78567(4) 0.0422(3) Uani 1 1 d . . . Co2 Co 0.34184(3) 0.00497(4) 0.96009(4) 0.0430(3) Uani 1 1 d . A . C1 C 0.3403(2) 0.1596(3) 0.8793(3) 0.0447(12) Uani 1 1 d . . . C2 C 0.36474(19) 0.2406(3) 0.8852(3) 0.0444(12) Uani 1 1 d . . . C3 C 0.3388(2) 0.2991(3) 0.8354(3) 0.0577(15) Uani 1 1 d . . . H3 H 0.3047 0.2891 0.7993 0.069 Uiso 1 1 calc R . . C4 C 0.3622(2) 0.3714(3) 0.8380(3) 0.0571(15) Uani 1 1 d . . . H4 H 0.3434 0.4101 0.8046 0.068 Uiso 1 1 calc R . . C5 C 0.41352(18) 0.3879(3) 0.8899(3) 0.0404(11) Uani 1 1 d . . . C6 C 0.4392(2) 0.3305(3) 0.9407(3) 0.0530(13) Uani 1 1 d . . . H6 H 0.4734 0.3403 0.9762 0.064 Uiso 1 1 calc R . . C7 C 0.4149(2) 0.2589(3) 0.9395(3) 0.0530(14) Uani 1 1 d . . . H7 H 0.4323 0.2222 0.9755 0.064 Uiso 1 1 calc R . . C8 C 0.44024(19) 0.4644(3) 0.8891(3) 0.0390(11) Uani 1 1 d . . . C9 C 0.41280(18) 0.5361(2) 0.8798(2) 0.0369(11) Uani 1 1 d . . . H9 H 0.3784 0.5361 0.8764 0.044 Uiso 1 1 calc R . . C10 C 0.43624(17) 0.6076(2) 0.8754(2) 0.0351(10) Uani 1 1 d . . . C11 C 0.48744(18) 0.6067(3) 0.8797(3) 0.0397(11) Uani 1 1 d . . . H11 H 0.5031 0.6542 0.8762 0.048 Uiso 1 1 calc R . . C12 C 0.51583(19) 0.5361(3) 0.8891(3) 0.0428(12) Uani 1 1 d . . . C13 C 0.49173(19) 0.4656(3) 0.8953(3) 0.0455(12) Uani 1 1 d . . . H13 H 0.5108 0.4182 0.9038 0.055 Uiso 1 1 calc R . . C14 C 0.56848(19) 0.5349(3) 0.8868(3) 0.0447(12) Uani 1 1 d . . . C15 C 0.5717(3) 0.5405(9) 0.8254(4) 0.149(6) Uani 1 1 d . . . H15 H 0.5402 0.5474 0.7839 0.179 Uiso 1 1 calc R . . C16 C 0.1661(2) 0.0297(3) 0.8781(3) 0.0490(13) Uani 1 1 d . . . C17 C 0.2174(2) 0.0271(3) 0.8714(3) 0.0514(13) Uani 1 1 d . A . C18 C 0.1644(3) 0.0196(6) 0.9419(4) 0.104(3) Uani 1 1 d . . . H18 H 0.1960 0.0097 0.9826 0.125 Uiso 1 1 calc R . . C19 C 0.6163(3) 0.5241(7) 0.9465(4) 0.112(3) Uani 1 1 d . . . H19 H 0.6164 0.5198 0.9906 0.134 Uiso 1 1 calc R . . C20 C 0.1190(3) 0.0366(8) 0.8206(4) 0.130(4) Uani 1 1 d . . . H20 H 0.1185 0.0389 0.7760 0.156 Uiso 1 1 calc R . . C21 C 0.40558(18) 0.6826(2) 0.8647(2) 0.0367(10) Uani 1 1 d . . . C22 C 0.4292(2) 0.7521(3) 0.9004(3) 0.0491(13) Uani 1 1 d . . . H22 H 0.4656 0.7524 0.9313 0.059 Uiso 1 1 calc R . . C23 C 0.3995(2) 0.8210(3) 0.8909(3) 0.0491(13) Uani 1 1 d . . . H23 H 0.4158 0.8664 0.9168 0.059 Uiso 1 1 calc R . . C24 C 0.34569(18) 0.8227(3) 0.8429(2) 0.0383(11) Uani 1 1 d . . . C25 C 0.32192(19) 0.7534(3) 0.8067(3) 0.0438(12) Uani 1 1 d . . . H25 H 0.2858 0.7536 0.7748 0.053 Uiso 1 1 calc R . . C26 C 0.35100(19) 0.6851(3) 0.8176(3) 0.0424(11) Uani 1 1 d . . . H26 H 0.3342 0.6392 0.7931 0.051 Uiso 1 1 calc R . . C27 C 0.31461(19) 0.8978(3) 0.8250(3) 0.0413(11) Uani 1 1 d . . . O1 O 0.33546(13) -0.03891(17) 0.86165(19) 0.0447(8) Uani 1 1 d . . . O2 O 0.27128(15) 0.9022(2) 0.7720(2) 0.0619(11) Uani 1 1 d . . . O3 O 0.30311(15) 0.1417(2) 0.8200(2) 0.0618(11) Uani 1 1 d . . . O4 O 0.35960(15) 0.11564(19) 0.9332(2) 0.0549(9) Uani 1 1 d . . . O5 O 0.21286(15) 0.0307(2) 0.8090(2) 0.0583(10) Uani 1 1 d . . . O6 O 0.35392(19) 0.0545(3) 1.0582(2) 0.0679(11) Uani 1 1 d . . . O7 O 0.4248(2) -0.0219(3) 1.0099(3) 0.0841(15) Uani 1 1 d . . . O8 O 0.3343(2) -0.1116(3) 0.9895(3) 0.0960(16) Uani 1 1 d . . . O9 O 0.26067(16) 0.0203(3) 0.9272(2) 0.0749(13) Uani 1 1 d . . . N1 N 0.5069(3) -0.0201(7) 1.1052(4) 0.120(3) Uani 1 1 d . . . C111 C 0.3368(4) -0.1339(5) 1.0462(5) 0.096(2) Uani 1 1 d . A . C112 C 0.3479(9) -0.2368(9) 1.1407(10) 0.240(10) Uani 1 1 d . A . H11A H 0.3822 -0.2633 1.1652 0.288 Uiso 1 1 calc R . . H11B H 0.3473 -0.1909 1.1683 0.288 Uiso 1 1 calc R . . C113 C 0.3046(11) -0.2905(15) 1.1302(16) 0.352(18) Uani 1 1 d . . . H11C H 0.3066 -0.3054 1.1755 0.529 Uiso 1 1 calc R . . H11D H 0.3073 -0.3372 1.1058 0.529 Uiso 1 1 calc R . . H11E H 0.2710 -0.2647 1.1025 0.529 Uiso 1 1 calc R . . C114 C 0.3353(10) -0.2744(7) 1.0138(9) 0.233(10) Uani 1 1 d . A . H11F H 0.3046 -0.3058 1.0086 0.279 Uiso 1 1 calc R . . H11G H 0.3243 -0.2469 0.9690 0.279 Uiso 1 1 calc R . . C115 C 0.3657(11) -0.3209(12) 1.0138(14) 0.310(16) Uani 1 1 d . . . H11H H 0.3497 -0.3518 0.9710 0.466 Uiso 1 1 calc R . . H11I H 0.3756 -0.3553 1.0542 0.466 Uiso 1 1 calc R . . H11J H 0.3969 -0.2944 1.0162 0.466 Uiso 1 1 calc R . . N2 N 0.3383(4) -0.2110(4) 1.0640(4) 0.119(3) Uani 1 1 d . . . C211 C 0.4589(4) 0.0128(6) 1.0620(6) 0.108(3) Uani 1 1 d . A . C212 C 0.5460(6) 0.0182(13) 1.1660(9) 0.238(11) Uani 1 1 d . A . H21A H 0.5329 0.0700 1.1711 0.286 Uiso 1 1 calc R . . H21B H 0.5783 0.0260 1.1599 0.286 Uiso 1 1 calc R . . C213 C 0.5598(13) -0.032(3) 1.2348(13) 0.53(4) Uani 1 1 d . . . H21C H 0.5846 -0.0028 1.2754 0.792 Uiso 1 1 calc R A . H21D H 0.5756 -0.0814 1.2315 0.792 Uiso 1 1 calc R . . H21E H 0.5277 -0.0418 1.2396 0.792 Uiso 1 1 calc R . . C214 C 0.5196(4) -0.0968(8) 1.0932(7) 0.137(4) Uani 1 1 d . A . H21F H 0.5581 -0.1035 1.1159 0.164 Uiso 1 1 calc R . . H21G H 0.5069 -0.1051 1.0426 0.164 Uiso 1 1 calc R . . C215 C 0.4955(10) -0.1546(14) 1.1206(12) 0.309(14) Uani 1 1 d . . . H21H H 0.5093 -0.2064 1.1188 0.463 Uiso 1 1 calc R A . H21I H 0.4574 -0.1542 1.0925 0.463 Uiso 1 1 calc R . . H21J H 0.5039 -0.1417 1.1690 0.463 Uiso 1 1 calc R . . N3 N 0.3308(5) 0.1498(7) 1.1131(4) 0.169(5) Uani 1 1 d . . . C31A C 0.3212(4) 0.0885(5) 1.0685(5) 0.074(4) Uani 0.75(2) 1 d P A 1 C31B C 0.3571(13) 0.1306(16) 1.0636(11) 0.071(12) Uani 0.25(2) 1 d P A 2 C312 C 0.2782(5) 0.1763(8) 1.1188(6) 0.154(5) Uani 1 1 d . A . H31A H 0.2473 0.1474 1.0849 0.185 Uiso 1 1 calc R . . H31B H 0.2817 0.1666 1.1663 0.185 Uiso 1 1 calc R . . C313 C 0.2731(9) 0.2580(11) 1.1035(13) 0.311(15) Uani 1 1 d . . . H31C H 0.2403 0.2772 1.1024 0.467 Uiso 1 1 calc R A . H31D H 0.2727 0.2667 1.0581 0.467 Uiso 1 1 calc R . . H31E H 0.3028 0.2859 1.1394 0.467 Uiso 1 1 calc R . . C314 C 0.3699(15) 0.1468(18) 1.171(2) 0.378(13) Uani 1 1 d . A . H31F H 0.3883 0.0962 1.1786 0.454 Uiso 1 1 calc R . . H31G H 0.3607 0.1573 1.2096 0.454 Uiso 1 1 calc R . . C315 C 0.4053(13) 0.2215(15) 1.1591(18) 0.378(13) Uani 1 1 d . . . H31H H 0.4426 0.2144 1.1905 0.567 Uiso 1 1 calc R A . H31I H 0.3934 0.2713 1.1693 0.567 Uiso 1 1 calc R . . H31J H 0.4003 0.2214 1.1108 0.567 Uiso 1 1 calc R . . N4 N 0.2658(3) 0.0504(4) 0.6600(4) 0.0903(18) Uani 1 1 d . . . O10 O 0.2572(4) -0.0570(6) 1.0970(4) 0.163(3) Uani 1 1 d . . . O11 O 0.3120(3) 0.0400(4) 0.7071(4) 0.1092(19) Uani 1 1 d . . . O12 O 0.2288(2) 0.0506(3) 0.6773(3) 0.0847(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0376(4) 0.0280(4) 0.0644(5) 0.0040(3) 0.0257(3) 0.0058(3) Co2 0.0450(4) 0.0310(4) 0.0587(5) -0.0009(3) 0.0281(3) -0.0020(3) C1 0.039(3) 0.024(2) 0.076(4) 0.000(2) 0.029(3) 0.002(2) C2 0.039(3) 0.024(2) 0.073(3) 0.006(2) 0.028(3) 0.002(2) C3 0.033(3) 0.039(3) 0.087(4) 0.013(3) 0.013(3) -0.002(2) C4 0.036(3) 0.035(3) 0.089(4) 0.022(3) 0.019(3) 0.005(2) C5 0.034(3) 0.023(2) 0.066(3) 0.005(2) 0.024(2) 0.0039(19) C6 0.046(3) 0.032(3) 0.065(3) 0.006(2) 0.010(3) -0.004(2) C7 0.057(3) 0.028(3) 0.062(3) 0.009(2) 0.015(3) 0.000(2) C8 0.037(3) 0.026(2) 0.056(3) 0.005(2) 0.021(2) 0.0012(18) C9 0.030(2) 0.029(2) 0.051(3) 0.0034(19) 0.018(2) 0.0041(18) C10 0.033(3) 0.025(2) 0.048(3) -0.0019(19) 0.018(2) 0.0012(18) C11 0.033(3) 0.027(2) 0.059(3) -0.002(2) 0.021(2) -0.0040(19) C12 0.032(3) 0.036(3) 0.062(3) -0.003(2) 0.023(2) -0.001(2) C13 0.037(3) 0.027(2) 0.075(3) 0.005(2) 0.027(3) 0.0080(19) C14 0.033(3) 0.034(3) 0.070(3) -0.002(2) 0.025(3) 0.0004(19) C15 0.025(4) 0.354(18) 0.063(5) 0.030(7) 0.015(3) 0.034(6) C16 0.037(3) 0.046(3) 0.070(4) -0.007(2) 0.029(3) -0.003(2) C17 0.038(3) 0.043(3) 0.079(4) -0.003(3) 0.031(3) 0.003(2) C18 0.041(4) 0.192(10) 0.075(5) 0.018(5) 0.023(4) 0.005(4) C19 0.044(4) 0.227(11) 0.070(5) 0.012(5) 0.031(4) 0.001(5) C20 0.049(5) 0.284(15) 0.066(5) 0.031(6) 0.035(4) 0.033(6) C21 0.035(3) 0.023(2) 0.053(3) 0.0007(19) 0.021(2) 0.0007(19) C22 0.033(3) 0.033(3) 0.064(3) -0.003(2) 0.006(2) 0.003(2) C23 0.048(3) 0.026(2) 0.065(3) -0.009(2) 0.017(3) 0.001(2) C24 0.038(3) 0.028(2) 0.050(3) 0.001(2) 0.020(2) 0.0044(19) C25 0.030(3) 0.030(2) 0.065(3) -0.002(2) 0.015(2) 0.0020(19) C26 0.038(3) 0.024(2) 0.061(3) -0.007(2) 0.018(2) -0.0025(19) C27 0.042(3) 0.027(2) 0.058(3) -0.003(2) 0.024(3) 0.003(2) O1 0.045(2) 0.0259(17) 0.064(2) -0.0029(15) 0.0250(17) 0.0042(14) O2 0.050(2) 0.037(2) 0.077(3) -0.0076(17) 0.008(2) 0.0147(16) O3 0.053(2) 0.0297(18) 0.086(3) 0.0062(18) 0.016(2) -0.0066(16) O4 0.064(2) 0.0289(18) 0.072(2) 0.0021(18) 0.030(2) -0.0047(16) O5 0.044(2) 0.058(2) 0.082(3) 0.0087(19) 0.036(2) 0.0081(17) O6 0.085(3) 0.060(3) 0.072(3) -0.009(2) 0.047(2) 0.002(2) O7 0.071(3) 0.084(3) 0.076(3) -0.017(3) 0.013(3) 0.024(3) O8 0.155(5) 0.052(3) 0.094(3) 0.011(2) 0.067(4) -0.012(3) O9 0.039(2) 0.112(4) 0.079(3) -0.010(3) 0.031(2) -0.002(2) N1 0.052(4) 0.202(10) 0.097(5) 0.009(5) 0.024(4) 0.007(5) C111 0.121(7) 0.064(5) 0.128(7) 0.025(5) 0.076(6) 0.008(4) C112 0.43(3) 0.135(11) 0.29(2) 0.008(12) 0.29(2) -0.050(15) C113 0.42(4) 0.26(3) 0.53(5) 0.10(3) 0.36(4) -0.01(3) C114 0.47(4) 0.069(7) 0.239(17) 0.042(9) 0.23(2) 0.024(12) C115 0.54(4) 0.155(17) 0.45(4) 0.04(2) 0.42(4) 0.09(2) N2 0.179(8) 0.070(5) 0.137(6) 0.034(4) 0.098(6) 0.018(5) C211 0.078(6) 0.133(8) 0.118(7) 0.005(6) 0.050(6) -0.003(5) C212 0.115(10) 0.40(3) 0.151(12) 0.035(15) 0.018(9) -0.127(14) C213 0.33(4) 0.96(9) 0.153(19) 0.12(4) -0.02(2) -0.28(5) C214 0.101(7) 0.165(11) 0.149(9) 0.020(8) 0.059(7) 0.056(8) C215 0.44(4) 0.27(3) 0.33(3) -0.02(2) 0.27(3) -0.13(3) N3 0.197(10) 0.166(9) 0.090(5) -0.033(5) 0.016(6) 0.122(8) C31A 0.084(7) 0.052(6) 0.103(7) -0.011(5) 0.057(6) 0.001(5) C31B 0.13(3) 0.061(19) 0.039(13) -0.013(11) 0.053(15) -0.003(16) C312 0.206(13) 0.171(12) 0.140(9) 0.012(8) 0.127(9) 0.074(10) C313 0.44(3) 0.190(16) 0.50(4) 0.15(2) 0.38(3) 0.20(2) C314 0.53(4) 0.21(2) 0.55(4) -0.05(3) 0.39(3) -0.02(2) C315 0.53(4) 0.21(2) 0.55(4) -0.05(3) 0.39(3) -0.02(2) N4 0.083(5) 0.101(5) 0.094(5) 0.015(4) 0.045(4) 0.007(4) O10 0.206(9) 0.219(9) 0.097(5) -0.010(5) 0.096(5) -0.006(7) O11 0.090(4) 0.142(6) 0.128(5) -0.002(4) 0.077(4) 0.014(4) O12 0.082(3) 0.094(4) 0.083(3) -0.005(3) 0.041(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 1.984(4) . ? Co1 O3 1.996(4) . ? Co1 O12 2.079(5) . ? Co1 O1 2.120(3) . ? Co1 O2 2.217(4) 1_545 ? Co1 O11 2.313(5) . ? Co1 C27 2.509(5) 1_545 ? Co2 O9 2.067(4) . ? Co2 O4 2.068(3) . ? Co2 O8 2.094(5) . ? Co2 O6 2.106(4) . ? Co2 O7 2.121(5) . ? Co2 O1 2.127(4) . ? C1 O3 1.254(6) . ? C1 O4 1.255(6) . ? C1 C2 1.504(7) . ? C2 C3 1.383(7) . ? C2 C7 1.391(7) . ? C3 C4 1.369(7) . ? C3 H3 0.9300 . ? C4 C5 1.389(7) . ? C4 H4 0.9300 . ? C5 C6 1.380(7) . ? C5 C8 1.491(6) . ? C6 C7 1.375(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.382(7) . ? C8 C9 1.394(6) . ? C9 C10 1.391(6) . ? C9 H9 0.9300 . ? C10 C11 1.388(7) . ? C10 C21 1.484(6) . ? C11 C12 1.391(7) . ? C11 H11 0.9300 . ? C12 C13 1.398(7) . ? C12 C14 1.488(7) . ? C13 H13 0.9300 . ? C14 C15 1.335(10) . ? C14 C19 1.378(9) . ? C15 C20 1.368(11) 3 ? C15 H15 0.9300 . ? C16 C20 1.337(10) . ? C16 C18 1.371(10) . ? C16 C17 1.499(8) . ? C17 O9 1.259(7) . ? C17 O5 1.261(7) . ? C18 C19 1.387(11) 3_445 ? C18 H18 0.9300 . ? C19 C18 1.387(11) 3 ? C19 H19 0.9300 . ? C20 C15 1.368(11) 3_445 ? C20 H20 0.9300 . ? C21 C22 1.387(7) . ? C21 C26 1.400(7) . ? C22 C23 1.386(7) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 H23 0.9300 . ? C24 C25 1.388(7) . ? C24 C27 1.482(6) . ? C25 C26 1.367(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O2 1.228(6) . ? C27 O1 1.292(6) 1_565 ? C27 Co1 2.509(5) 1_565 ? O1 C27 1.292(6) 1_545 ? O2 Co1 2.217(4) 1_565 ? O6 C31A 1.175(10) . ? O6 C31B 1.29(3) . ? O7 C211 1.234(11) . ? O8 C111 1.222(9) . ? N1 C211 1.357(12) . ? N1 C214 1.389(14) . ? N1 C212 1.415(17) . ? C111 N2 1.346(10) . ? C112 C113 1.45(3) . ? C112 N2 1.571(17) . ? C112 H11A 0.9700 . ? C112 H11B 0.9700 . ? C113 H11C 0.9600 . ? C113 H11D 0.9600 . ? C113 H11E 0.9600 . ? C114 C115 1.15(2) . ? C114 N2 1.476(16) . ? C114 H11F 0.9700 . ? C114 H11G 0.9700 . ? C115 H11H 0.9600 . ? C115 H11I 0.9600 . ? C115 H11J 0.9600 . ? C212 C213 1.56(3) . ? C212 H21A 0.9700 . ? C212 H21B 0.9700 . ? C213 H21C 0.9600 . ? C213 H21D 0.9600 . ? C213 H21E 0.9600 . ? C214 C215 1.438(19) . ? C214 H21F 0.9700 . ? C214 H21G 0.9700 . ? C215 H21H 0.9600 . ? C215 H21I 0.9600 . ? C215 H21J 0.9600 . ? N3 C314 1.22(4) . ? N3 C31A 1.338(12) . ? N3 C31B 1.55(3) . ? N3 C312 1.585(15) . ? C312 C313 1.40(2) . ? C312 H31A 0.9700 . ? C312 H31B 0.9700 . ? C313 H31C 0.9600 . ? C313 H31D 0.9600 . ? C313 H31E 0.9600 . ? C314 C315 1.68(3) . ? C314 H31F 0.9700 . ? C314 H31G 0.9700 . ? C315 H31H 0.9600 . ? C315 H31I 0.9600 . ? C315 H31J 0.9600 . ? N4 O12 1.237(8) . ? N4 O11 1.238(8) . ? N4 O10 1.241(9) 6 ? O10 N4 1.241(9) 6_556 ? 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 O3 100.33(17) . . ? O5 Co1 O12 95.5(2) . . ? O3 Co1 O12 102.63(19) . . ? O5 Co1 O1 107.13(15) . . ? O3 Co1 O1 101.11(14) . . ? O12 Co1 O1 143.46(17) . . ? O5 Co1 O2 91.24(16) . 1_545 ? O3 Co1 O2 160.51(15) . 1_545 ? O12 Co1 O2 91.70(18) . 1_545 ? O1 Co1 O2 60.20(13) . 1_545 ? O5 Co1 O11 152.9(2) . . ? O3 Co1 O11 88.8(2) . . ? O12 Co1 O11 57.5(2) . . ? O1 Co1 O11 95.9(2) . . ? O2 Co1 O11 87.9(2) 1_545 . ? O5 Co1 C27 102.03(16) . 1_545 ? O3 Co1 C27 131.57(16) . 1_545 ? O12 Co1 C27 117.18(18) . 1_545 ? O1 Co1 C27 30.99(14) . 1_545 ? O2 Co1 C27 29.31(14) 1_545 1_545 ? O11 Co1 C27 90.3(2) . 1_545 ? O9 Co2 O4 98.94(18) . . ? O9 Co2 O8 88.7(2) . . ? O4 Co2 O8 172.2(2) . . ? O9 Co2 O6 87.40(19) . . ? O4 Co2 O6 87.56(16) . . ? O8 Co2 O6 94.33(19) . . ? O9 Co2 O7 169.4(2) . . ? O4 Co2 O7 89.24(19) . . ? O8 Co2 O7 83.4(2) . . ? O6 Co2 O7 86.27(19) . . ? O9 Co2 O1 96.34(16) . . ? O4 Co2 O1 88.51(14) . . ? O8 Co2 O1 89.16(17) . . ? O6 Co2 O1 174.95(16) . . ? O7 Co2 O1 90.52(16) . . ? O3 C1 O4 126.1(4) . . ? O3 C1 C2 116.4(5) . . ? O4 C1 C2 117.6(5) . . ? C3 C2 C7 117.5(4) . . ? C3 C2 C1 121.1(5) . . ? C7 C2 C1 121.4(4) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C8 121.5(4) . . ? C4 C5 C8 120.6(4) . . ? C7 C6 C5 121.1(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 121.1(5) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C13 C8 C9 118.8(4) . . ? C13 C8 C5 120.9(4) . . ? C9 C8 C5 120.2(4) . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 118.9(4) . . ? C11 C10 C21 121.7(4) . . ? C9 C10 C21 119.3(4) . . ? C10 C11 C12 121.5(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 118.1(4) . . ? C11 C12 C14 120.9(4) . . ? C13 C12 C14 120.8(4) . . ? C8 C13 C12 121.6(4) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C19 115.8(6) . . ? C15 C14 C12 121.2(5) . . ? C19 C14 C12 122.9(5) . . ? C14 C15 C20 123.2(7) . 3 ? C14 C15 H15 118.4 . . ? C20 C15 H15 118.4 3 . ? C20 C16 C18 116.8(6) . . ? C20 C16 C17 120.8(6) . . ? C18 C16 C17 122.3(6) . . ? O9 C17 O5 125.9(5) . . ? O9 C17 C16 118.3(6) . . ? O5 C17 C16 115.8(5) . . ? C16 C18 C19 120.7(7) . 3_445 ? C16 C18 H18 119.6 . . ? C19 C18 H18 119.6 3_445 . ? C14 C19 C18 121.3(7) . 3 ? C14 C19 H19 119.3 . . ? C18 C19 H19 119.3 3 . ? C16 C20 C15 121.8(7) . 3_445 ? C16 C20 H20 119.1 . . ? C15 C20 H20 119.1 3_445 . ? C22 C21 C26 117.7(4) . . ? C22 C21 C10 122.1(4) . . ? C26 C21 C10 120.2(4) . . ? C23 C22 C21 121.1(4) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 118.7(4) . . ? C23 C24 C27 121.6(4) . . ? C25 C24 C27 119.5(4) . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 121.3(4) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.3 . . ? O2 C27 O1 119.5(4) . 1_565 ? O2 C27 C24 120.7(4) . . ? O1 C27 C24 119.5(4) 1_565 . ? O2 C27 Co1 62.1(3) . 1_565 ? O1 C27 Co1 57.7(2) 1_565 1_565 ? C24 C27 Co1 168.9(4) . 1_565 ? C27 O1 Co1 91.3(3) 1_545 . ? C27 O1 Co2 133.5(3) 1_545 . ? Co1 O1 Co2 103.16(13) . . ? C27 O2 Co1 88.6(3) . 1_565 ? C1 O3 Co1 126.9(3) . . ? C1 O4 Co2 135.9(3) . . ? C17 O5 Co1 123.9(4) . . ? C31A O6 C31B 61.7(14) . . ? C31A O6 Co2 124.9(6) . . ? C31B O6 Co2 117.1(9) . . ? C211 O7 Co2 125.4(6) . . ? C111 O8 Co2 127.3(5) . . ? C17 O9 Co2 140.9(4) . . ? C211 N1 C214 120.8(10) . . ? C211 N1 C212 123.6(14) . . ? C214 N1 C212 115.5(12) . . ? O8 C111 N2 123.2(8) . . ? C113 C112 N2 105.3(19) . . ? C113 C112 H11A 110.7 . . ? N2 C112 H11A 110.7 . . ? C113 C112 H11B 110.7 . . ? N2 C112 H11B 110.7 . . ? H11A C112 H11B 108.8 . . ? C112 C113 H11C 109.5 . . ? C112 C113 H11D 109.5 . . ? H11C C113 H11D 109.5 . . ? C112 C113 H11E 109.5 . . ? H11C C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C115 C114 N2 133(3) . . ? C115 C114 H11F 104.0 . . ? N2 C114 H11F 104.0 . . ? C115 C114 H11G 104.0 . . ? N2 C114 H11G 104.0 . . ? H11F C114 H11G 105.4 . . ? C114 C115 H11H 109.5 . . ? C114 C115 H11I 109.5 . . ? H11H C115 H11I 109.5 . . ? C114 C115 H11J 109.5 . . ? H11H C115 H11J 109.5 . . ? H11I C115 H11J 109.5 . . ? C111 N2 C114 120.9(8) . . ? C111 N2 C112 121.4(9) . . ? C114 N2 C112 117.5(9) . . ? O7 C211 N1 122.8(10) . . ? N1 C212 C213 111.4(16) . . ? N1 C212 H21A 109.3 . . ? C213 C212 H21A 109.3 . . ? N1 C212 H21B 109.3 . . ? C213 C212 H21B 109.3 . . ? H21A C212 H21B 108.0 . . ? C212 C213 H21C 109.5 . . ? C212 C213 H21D 109.5 . . ? H21C C213 H21D 109.5 . . ? C212 C213 H21E 109.5 . . ? H21C C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? N1 C214 C215 110.8(14) . . ? N1 C214 H21F 109.5 . . ? C215 C214 H21F 109.5 . . ? N1 C214 H21G 109.5 . . ? C215 C214 H21G 109.5 . . ? H21F C214 H21G 108.1 . . ? C214 C215 H21H 109.5 . . ? C214 C215 H21I 109.5 . . ? H21H C215 H21I 109.5 . . ? C214 C215 H21J 109.5 . . ? H21H C215 H21J 109.5 . . ? H21I C215 H21J 109.5 . . ? C314 N3 C31A 118.5(17) . . ? C314 N3 C31B 100(2) . . ? C31A N3 C31B 51.4(11) . . ? C314 N3 C312 112.5(18) . . ? C31A N3 C312 111.4(11) . . ? C31B N3 C312 146.8(13) . . ? O6 C31A N3 125.0(10) . . ? O6 C31B N3 103.5(19) . . ? C313 C312 N3 105.1(12) . . ? C313 C312 H31A 110.7 . . ? N3 C312 H31A 110.7 . . ? C313 C312 H31B 110.7 . . ? N3 C312 H31B 110.7 . . ? H31A C312 H31B 108.8 . . ? C312 C313 H31C 109.5 . . ? C312 C313 H31D 109.5 . . ? H31C C313 H31D 109.5 . . ? C312 C313 H31E 109.5 . . ? H31C C313 H31E 109.5 . . ? H31D C313 H31E 109.5 . . ? N3 C314 C315 98(3) . . ? N3 C314 H31F 112.1 . . ? C315 C314 H31F 112.1 . . ? N3 C314 H31G 112.1 . . ? C315 C314 H31G 112.1 . . ? H31F C314 H31G 109.7 . . ? C314 C315 H31H 109.5 . . ? C314 C315 H31I 109.5 . . ? H31H C315 H31I 109.5 . . ? C314 C315 H31J 109.5 . . ? H31H C315 H31J 109.5 . . ? H31I C315 H31J 109.5 . . ? O12 N4 O11 118.2(7) . . ? O12 N4 O10 121.4(8) . 6 ? O11 N4 O10 120.4(8) . 6 ? N4 O11 Co1 86.6(4) . . ? N4 O12 Co1 97.7(4) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.723 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.075 # Attachment '- DUT-28-RT-CCDC-80200.cif' data_Co22(BTB)12_data_us-67-ds4 _database_code_depnum_ccdc_archive 'CCDC 801200' #TrackingRef '- DUT-28-RT-CCDC-80200.cif' _audit_creation_method SHELXL-97 _chemical_name_common 'Co22(btb)12 (DUT-28(RT))' _chemical_formula_moiety 'C324 H180 Co22 O120' _chemical_formula_sum 'C162 H90 Co11 O60' _chemical_properties_physical moisture-sensitive _exptl_crystal_recrystallization_method DEF _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour purple _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100 _chemical_formula_weight 3644.58 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_int_tables_number 12 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 32.989(7) _cell_length_b 39.080(8) _cell_length_c 27.682(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.04(3) _cell_angle_gamma 90.00 _cell_volume 29572(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 769 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 36.82 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3653 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95142 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 31.00 _reflns_number_total 22341 _reflns_number_gt 13193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement XDS _computing_data_reduction XDSCONV _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.1759P)^2^] 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_number_reflns 22341 _refine_ls_number_parameters 615 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2567 _refine_ls_wR_factor_gt 0.2367 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.011 _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 0.5000 0.0000 0.5000 0.0887(2) Uani 1 4 d S . . Co2 Co 0.384779(18) 0.0000 0.47762(2) 0.0966(2) Uani 1 2 d S . . Co3 Co 0.136359(16) -0.270575(11) 0.033482(19) 0.1132(2) Uani 1 1 d . . . Co4 Co 0.22186(2) -0.309868(19) 0.15597(3) 0.1685(3) Uani 1 1 d . . . O1 O 0.3351(5) 0.0452(3) 0.4337(4) 0.404(11) Uani 0.50 1 d P A . O2 O 0.29022(14) -0.31570(12) 0.1612(2) 0.258(2) Uani 1 1 d . . . O3 O 0.08299(17) -0.24629(8) -0.04390(13) 0.2179(18) Uani 1 1 d . . . O4 O 0.42247(10) 0.0000 0.43543(11) 0.1212(10) Uani 1 2 d S . . O6 O 0.35309(13) 0.02059(12) 0.39188(16) 0.1182(13) Uani 0.50 1 d P . . O7 O 0.09426(19) -0.28514(10) 0.0591(2) 0.201(2) Uani 1 1 d . . . O8 O 0.13654(9) -0.31543(6) -0.00049(11) 0.1197(6) Uani 1 1 d . . . O9 O 0.19056(10) -0.34176(6) 0.08295(12) 0.1404(8) Uani 1 1 d . . . O10 O 0.2451(2) -0.35507(11) 0.20683(16) 0.273(2) Uani 1 1 d . . . O11 O 0.15699(16) -0.30044(9) 0.1466(2) 0.1974(15) Uani 1 1 d . . . O12 O 0.26109(18) -0.28021(12) 0.23595(18) 0.246(2) Uani 1 1 d . . . O13 O 0.1226(2) -0.21781(9) 0.0489(4) 0.400(5) Uani 1 1 d . . . O14 O 0.32574(18) 0.0000 0.4847(3) 0.228(3) Uani 1 2 d S A . C1 C 0.48745(10) -0.17535(7) 0.18877(13) 0.0965(7) Uani 1 1 d . . . O15 O 0.19323(14) -0.24708(9) 0.02401(19) 0.1822(13) Uani 1 1 d . . . O16 O 0.21325(13) -0.26381(7) 0.11054(16) 0.1696(12) Uani 1 1 d . . . C2 C 0.22184(18) -0.25327(14) 0.0774(2) 0.1582(17) Uani 1 1 d D . . C3 C 0.27616(16) -0.23677(11) 0.1116(2) 0.1629(19) Uani 1 1 d D . . C4 C 0.29129(15) -0.22668(10) 0.0777(2) 0.1496(15) Uani 1 1 d . . . H4 H 0.2713 -0.2298 0.0375 0.179 Uiso 1 1 calc R . . C5 C 0.33747(12) -0.21146(9) 0.10339(18) 0.1307(12) Uani 1 1 d . . . H5 H 0.3482 -0.2054 0.0798 0.157 Uiso 1 1 calc R . . C6 C 0.36720(12) -0.20515(8) 0.16198(16) 0.1177(10) Uani 1 1 d . . . C7 C 0.35135(17) -0.21571(10) 0.1975(2) 0.1576(17) Uani 1 1 d . . . H7 H 0.3709 -0.2123 0.2376 0.189 Uiso 1 1 calc R . . C8 C 0.30579(17) -0.23141(11) 0.1714(2) 0.175(2) Uani 1 1 d . . . H8 H 0.2950 -0.2384 0.1944 0.210 Uiso 1 1 calc R . . C9 C 0.41418(10) -0.18709(7) 0.18665(13) 0.1001(8) Uani 1 1 d . . . C10 C 0.42907(11) -0.16291(7) 0.23078(13) 0.1057(9) Uani 1 1 d . . . H10 H 0.4093 -0.1588 0.2443 0.127 Uiso 1 1 calc R . . C11 C 0.50121(10) -0.15122(7) 0.23295(13) 0.1037(8) Uani 1 1 d . . . H11 H 0.5301 -0.1390 0.2481 0.124 Uiso 1 1 calc R . . C12 C 0.47243(10) -0.14499(7) 0.25495(13) 0.1040(8) Uani 1 1 d . A . C13 C 0.44350(10) -0.19297(7) 0.16624(13) 0.0993(8) Uani 1 1 d . . . H13 H 0.4337 -0.2090 0.1369 0.119 Uiso 1 1 calc R . . C14 C 0.48894(11) -0.11948(8) 0.30236(15) 0.1085(9) Uani 1 1 d . . . C15 C 0.36086(15) -0.03077(8) 0.08970(13) 0.1304(11) Uani 1 1 d . . . C16 C 0.36794(14) -0.03055(9) 0.14439(13) 0.1270(11) Uani 1 1 d . A . H16 H 0.3700 -0.0511 0.1625 0.152 Uiso 1 1 calc R . . C17 C 0.51816(11) -0.18231(8) 0.16664(16) 0.1075(9) Uani 1 1 d . . . C18 C 0.3574(2) 0.0000 0.06295(19) 0.1423(19) Uani 1 2 d S . . H18 H 0.3527 0.0000 0.0265 0.171 Uiso 1 2 calc SR . . C19 C 0.51975(11) -0.07289(8) 0.39374(14) 0.1086(9) Uani 1 1 d . . . C20 C 0.53585(14) -0.04720(8) 0.44210(15) 0.1070(9) Uani 1 1 d . . . C21 C 0.49882(12) -0.19025(8) 0.11024(16) 0.1172(10) Uani 1 1 d . . . H21 H 0.4650 -0.1911 0.0839 0.141 Uiso 1 1 calc R . . C22 C 0.12257(14) -0.37694(8) -0.06286(15) 0.1234(10) Uani 1 1 d . . . H22 H 0.1038 -0.3582 -0.0848 0.148 Uiso 1 1 calc R . . C23 C 0.38165(15) -0.09341(9) 0.08910(14) 0.1364(12) Uani 1 1 d . . . H23 H 0.4034 -0.0922 0.1294 0.164 Uiso 1 1 calc R . . C24 C 0.35545(15) -0.06425(8) 0.05981(13) 0.1274(11) Uani 1 1 d . . . C25 C 0.31703(16) -0.09768(10) -0.02830(16) 0.1474(14) Uani 1 1 d . . . H25 H 0.2941 -0.0994 -0.0683 0.177 Uiso 1 1 calc R . . O17A O 0.5034(3) -0.03310(18) 0.4461(3) 0.0963(16) Uani 0.633(10) 1 d P A 1 O18A O 0.4183(3) 0.0425(2) 0.5240(4) 0.127(2) Uani 0.633(10) 1 d P . 1 C26A C 0.4545(2) -0.0994(2) 0.3048(4) 0.123(3) Uani 0.633(10) 1 d P A 1 H26A H 0.4214 -0.1009 0.2750 0.148 Uiso 0.633(10) 1 calc PR A 1 C27A C 0.4694(2) -0.0773(2) 0.3515(4) 0.123(2) Uani 0.633(10) 1 d P A 1 H27A H 0.4464 -0.0656 0.3546 0.147 Uiso 0.633(10) 1 calc PR A 1 C28A C 0.5380(2) -0.11525(18) 0.3491(3) 0.118(2) Uani 0.633(10) 1 d P A 1 H28A H 0.5614 -0.1293 0.3505 0.141 Uiso 0.633(10) 1 calc PR A 1 C29A C 0.5534(2) -0.09133(19) 0.3930(3) 0.124(2) Uani 0.633(10) 1 d P A 1 H29A H 0.5866 -0.0882 0.4214 0.149 Uiso 0.633(10) 1 calc PR A 1 O17B O 0.5125(4) -0.0442(3) 0.4619(4) 0.0718(19) Uani 0.367(10) 1 d P A 2 O18B O 0.4249(5) 0.0309(4) 0.5461(6) 0.111(4) Uani 0.367(10) 1 d P . 2 C26B C 0.4716(5) -0.1189(3) 0.3364(5) 0.112(4) Uani 0.367(10) 1 d P A 2 H26B H 0.4487 -0.1353 0.3302 0.134 Uiso 0.367(10) 1 calc PR A 2 C27B C 0.4861(4) -0.0956(3) 0.3791(5) 0.094(3) Uani 0.367(10) 1 d P A 2 H27B H 0.4710 -0.0958 0.3991 0.113 Uiso 0.367(10) 1 calc PR A 2 C28B C 0.5204(4) -0.0943(4) 0.3087(7) 0.130(5) Uani 0.367(10) 1 d P A 2 H28B H 0.5295 -0.0922 0.2825 0.157 Uiso 0.367(10) 1 calc PR A 2 C29B C 0.5388(5) -0.0714(5) 0.3569(7) 0.149(7) Uani 0.367(10) 1 d P A 2 H29B H 0.5629 -0.0556 0.3649 0.179 Uiso 0.367(10) 1 calc PR A 2 C30 C 0.37722(17) 0.00635(12) 0.22992(13) 0.113(2) Uani 0.50 1 d PG . . C31 C 0.34708(15) 0.02783(11) 0.23658(13) 0.1181(19) Uani 0.50 1 d PG . . H31 H 0.3246 0.0418 0.2060 0.142 Uiso 0.50 1 calc PR . . C32 C 0.35057(14) 0.02835(10) 0.28899(15) 0.1062(16) Uani 0.50 1 d PG A . H32 H 0.3304 0.0427 0.2934 0.127 Uiso 0.50 1 calc PR . . C33 C 0.38419(15) 0.00740(11) 0.33475(11) 0.096(2) Uani 0.50 1 d PG . . C34 C 0.41433(14) -0.01407(9) 0.32809(13) 0.1103(19) Uani 0.50 1 d PG A . H34 H 0.4368 -0.0281 0.3587 0.132 Uiso 0.50 1 calc PR . . C35 C 0.41085(15) -0.01460(10) 0.27568(17) 0.1074(18) Uani 0.50 1 d PG . . H35 H 0.4310 -0.0290 0.2712 0.129 Uiso 0.50 1 calc PR A . C36 C 0.15522(13) -0.37387(9) -0.00234(15) 0.1171(9) Uani 1 1 d . . . C37 C 0.38835(19) 0.0000 0.3905(2) 0.143(2) Uani 1 2 d S . . C38 C 0.58010(16) -0.19598(9) 0.1301(2) 0.1251(11) Uani 1 1 d . . . C39 C 0.37186(19) 0.0000 0.17167(18) 0.1235(14) Uani 1 2 d S . . C40 C 0.16108(14) -0.34122(10) 0.02941(17) 0.1155(9) Uani 1 1 d . . . C41 C 0.52877(17) -0.19703(10) 0.0916(2) 0.1402(13) Uani 1 1 d . . . H41 H 0.5149 -0.2025 0.0526 0.168 Uiso 1 1 calc R . . C42 C 0.56941(13) -0.18106(11) 0.20628(18) 0.1422(13) Uani 1 1 d . . . H42 H 0.5836 -0.1764 0.2455 0.171 Uiso 1 1 calc R . . C43 C 0.32270(17) -0.06697(10) -0.00097(15) 0.1554(15) Uani 1 1 d . . . H43 H 0.3048 -0.0480 -0.0227 0.186 Uiso 1 1 calc R . . C44 C 0.59872(14) -0.18721(11) 0.1843(2) 0.1416(13) Uani 1 1 d . . . H44 H 0.6325 -0.1849 0.2094 0.170 Uiso 1 1 calc R . . C45 C 0.1079(3) -0.29485(13) 0.1018(4) 0.181(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0891(4) 0.1214(5) 0.0594(4) 0.000 0.0439(3) 0.000 Co2 0.0857(3) 0.1227(4) 0.0761(3) 0.000 0.0419(3) 0.000 Co3 0.1250(3) 0.1362(4) 0.1148(4) -0.0179(2) 0.0895(3) -0.0303(2) Co4 0.1627(5) 0.2083(7) 0.1163(4) -0.0262(4) 0.0669(4) 0.0234(4) O1 0.448(17) 0.311(12) 0.181(7) -0.016(7) 0.009(9) 0.264(13) O2 0.163(3) 0.260(4) 0.288(5) 0.019(4) 0.086(3) -0.043(3) O3 0.330(5) 0.132(2) 0.140(2) 0.0082(17) 0.100(3) -0.009(2) O4 0.0845(17) 0.220(3) 0.0563(15) 0.000 0.0377(14) 0.000 O6 0.084(2) 0.182(4) 0.073(2) -0.007(2) 0.0341(18) 0.009(2) O7 0.306(5) 0.150(2) 0.328(6) 0.017(3) 0.288(5) -0.012(2) O8 0.1329(17) 0.1224(16) 0.1338(18) -0.0132(14) 0.0931(15) -0.0126(13) O9 0.168(2) 0.1414(18) 0.1234(19) -0.0228(14) 0.0892(18) -0.0040(15) O10 0.357(6) 0.205(3) 0.156(3) 0.053(3) 0.082(3) 0.039(4) O11 0.207(3) 0.191(3) 0.284(5) -0.048(3) 0.193(4) -0.055(3) O12 0.260(4) 0.272(4) 0.193(3) -0.056(3) 0.119(3) -0.117(4) O13 0.352(7) 0.114(2) 0.925(16) -0.021(5) 0.476(10) -0.021(3) O14 0.157(4) 0.344(8) 0.240(6) 0.000 0.146(4) 0.000 C1 0.1028(18) 0.1077(18) 0.106(2) -0.0152(15) 0.0748(16) -0.0107(15) O15 0.186(3) 0.207(3) 0.197(3) -0.053(3) 0.134(3) -0.075(2) O16 0.238(3) 0.1360(19) 0.212(3) -0.0683(19) 0.173(3) -0.074(2) C2 0.180(4) 0.232(5) 0.130(4) -0.009(3) 0.129(4) 0.014(3) C3 0.172(3) 0.178(3) 0.216(5) -0.117(3) 0.156(4) -0.097(3) C4 0.145(3) 0.169(3) 0.188(4) -0.092(3) 0.126(3) -0.058(2) C5 0.132(2) 0.140(3) 0.162(3) -0.073(2) 0.108(2) -0.059(2) C6 0.137(2) 0.129(2) 0.132(3) -0.056(2) 0.103(2) -0.0483(19) C7 0.220(4) 0.165(3) 0.176(4) -0.079(3) 0.165(4) -0.097(3) C8 0.209(4) 0.200(4) 0.222(5) -0.113(4) 0.186(4) -0.119(3) C9 0.115(2) 0.1038(18) 0.110(2) -0.0219(15) 0.0806(17) -0.0263(15) C10 0.116(2) 0.121(2) 0.115(2) -0.0392(17) 0.0863(18) -0.0293(16) C11 0.0985(18) 0.115(2) 0.121(2) -0.0254(16) 0.0759(17) -0.0189(15) C12 0.1078(19) 0.116(2) 0.116(2) -0.0320(16) 0.0798(17) -0.0232(16) C13 0.114(2) 0.0985(18) 0.109(2) -0.0213(14) 0.0770(17) -0.0069(15) C14 0.106(2) 0.120(2) 0.124(2) -0.0376(17) 0.079(2) -0.0260(17) C15 0.185(3) 0.120(2) 0.0762(18) 0.0016(16) 0.067(2) 0.004(2) C16 0.180(3) 0.119(2) 0.087(2) 0.0093(16) 0.077(2) 0.008(2) C17 0.112(2) 0.115(2) 0.132(3) -0.0088(17) 0.090(2) -0.0006(16) C18 0.225(6) 0.109(3) 0.077(2) 0.000 0.075(3) 0.000 C19 0.104(2) 0.116(2) 0.113(2) -0.0249(17) 0.0656(18) -0.0123(18) C20 0.116(2) 0.105(2) 0.095(2) -0.0157(16) 0.056(2) 0.0003(19) C21 0.123(2) 0.152(3) 0.122(3) -0.037(2) 0.096(2) -0.0260(19) C22 0.158(3) 0.107(2) 0.107(2) 0.0019(18) 0.075(2) 0.0091(19) C23 0.187(3) 0.124(3) 0.0822(18) 0.0065(19) 0.066(2) 0.008(2) C24 0.200(3) 0.105(2) 0.0825(18) -0.0036(16) 0.082(2) -0.010(2) C25 0.187(4) 0.130(3) 0.097(2) -0.003(2) 0.063(2) 0.004(3) O17A 0.105(3) 0.102(4) 0.076(4) -0.002(2) 0.048(3) 0.000(3) O18A 0.109(3) 0.134(5) 0.108(5) -0.025(3) 0.043(3) 0.004(3) C26A 0.089(3) 0.169(6) 0.114(5) -0.062(5) 0.059(3) -0.016(4) C27A 0.099(4) 0.147(6) 0.123(5) -0.036(5) 0.063(4) -0.005(4) C28A 0.101(4) 0.139(5) 0.114(5) -0.032(4) 0.060(3) -0.007(3) C29A 0.102(3) 0.150(5) 0.110(5) -0.022(4) 0.053(3) 0.019(3) O17B 0.092(4) 0.086(5) 0.054(4) 0.020(3) 0.051(3) 0.017(3) O18B 0.100(7) 0.138(9) 0.120(9) -0.053(6) 0.077(7) -0.041(6) C26B 0.122(8) 0.138(9) 0.102(7) -0.041(6) 0.079(7) -0.050(7) C27B 0.120(7) 0.106(7) 0.088(6) -0.004(5) 0.078(6) -0.009(6) C28B 0.131(8) 0.181(11) 0.133(10) -0.071(9) 0.107(8) -0.056(8) C29B 0.143(10) 0.214(15) 0.157(12) -0.108(11) 0.124(10) -0.106(10) C30 0.146(4) 0.105(6) 0.065(3) 0.007(3) 0.045(3) -0.011(4) C31 0.132(5) 0.124(5) 0.091(4) 0.018(3) 0.058(4) 0.030(4) C32 0.120(4) 0.115(4) 0.071(3) 0.003(3) 0.046(3) 0.005(3) C33 0.096(3) 0.124(7) 0.058(2) 0.000(3) 0.037(2) -0.005(3) C34 0.114(4) 0.115(4) 0.078(4) -0.006(2) 0.039(3) -0.002(3) C35 0.128(4) 0.128(5) 0.071(3) 0.008(2) 0.059(3) 0.021(3) C36 0.144(3) 0.117(2) 0.113(2) -0.0067(19) 0.086(2) -0.017(2) C37 0.099(3) 0.247(7) 0.075(3) 0.000 0.043(3) 0.000 C38 0.148(3) 0.127(2) 0.167(4) -0.003(2) 0.129(3) 0.012(2) C39 0.146(4) 0.141(4) 0.079(3) 0.000 0.061(3) 0.000 C40 0.134(3) 0.133(3) 0.105(2) -0.017(2) 0.082(2) -0.011(2) C41 0.181(4) 0.154(3) 0.151(3) -0.043(2) 0.133(3) -0.025(3) C42 0.110(2) 0.192(4) 0.146(3) 0.001(3) 0.086(2) 0.011(2) C43 0.225(4) 0.130(3) 0.090(2) -0.0041(19) 0.076(3) 0.012(3) C44 0.121(2) 0.200(4) 0.150(3) 0.035(3) 0.104(3) 0.035(2) C45 0.192(5) 0.130(4) 0.346(9) -0.065(4) 0.228(6) -0.055(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 O17A 2.024(8) 5_656 ? Co1 O17A 2.024(8) 2_656 ? Co1 O17A 2.024(8) . ? Co1 O17A 2.024(8) 6 ? Co1 O4 2.149(3) 5_656 ? Co1 O4 2.149(3) . ? Co1 O17B 2.180(11) 5_656 ? Co1 O17B 2.180(11) . ? Co1 O17B 2.180(11) 2_656 ? Co1 O17B 2.180(11) 6 ? Co2 O18B 1.998(14) 6 ? Co2 O18B 1.998(14) . ? Co2 O18A 2.011(10) . ? Co2 O18A 2.011(10) 6 ? Co2 O14 2.063(4) . ? Co2 O4 2.130(3) . ? Co2 O6 2.144(4) 6 ? Co2 O6 2.144(4) . ? Co2 O1 2.248(7) 6 ? Co2 O1 2.248(7) . ? Co2 C37 2.479(5) . ? Co3 O7 1.965(3) . ? Co3 O8 1.991(2) . ? Co3 O3 2.090(3) . ? Co3 O13 2.204(4) . ? Co3 O16 2.235(4) . ? Co3 O15 2.232(3) . ? Co3 C2 2.460(5) . ? Co4 O11 2.040(4) . ? Co4 O9 2.090(3) . ? Co4 O10 2.117(4) . ? Co4 O16 2.122(3) . ? Co4 O12 2.171(4) . ? Co4 O2 2.189(5) . ? O4 C37 1.116(5) . ? O6 C37 1.433(6) . ? O6 O6 1.610(9) 6 ? O7 C45 1.071(9) . ? O8 C40 1.267(4) . ? O9 C40 1.237(4) . ? O11 C45 1.401(8) . ? C1 C13 1.398(4) . ? C1 C11 1.403(4) . ? C1 C17 1.473(4) . ? O15 C2 1.253(5) . ? O16 C2 1.176(5) . ? C2 C3 1.620(5) . ? C3 C4 1.346(5) . ? C3 C8 1.388(6) . ? C4 C5 1.403(4) . ? C4 H4 0.9300 . ? C5 C6 1.368(5) . ? C5 H5 0.9300 . ? C6 C7 1.409(4) . ? C6 C9 1.477(4) . ? C7 C8 1.393(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C13 1.385(4) . ? C9 C10 1.398(4) . ? C10 C12 1.383(4) . ? C10 H10 0.9300 . ? C11 C12 1.407(4) . ? C11 H11 0.9300 . ? C12 C14 1.487(4) . ? C13 H13 0.9300 . ? C14 C26B 1.347(10) . ? C14 C28B 1.368(11) . ? C14 C28A 1.405(6) . ? C14 C26A 1.415(7) . ? C15 C18 1.383(4) . ? C15 C16 1.397(4) . ? C15 C24 1.504(4) . ? C16 C39 1.380(4) . ? C16 H16 0.9300 . ? C17 C21 1.351(4) . ? C17 C42 1.410(5) . ? C18 C15 1.383(4) 6 ? C18 H18 0.9300 . ? C19 C27B 1.296(9) . ? C19 C29A 1.334(7) . ? C19 C27A 1.408(7) . ? C19 C29B 1.469(11) . ? C19 C20 1.512(4) . ? C20 O17B 1.176(11) . ? C20 O17A 1.264(7) . ? C20 O18A 1.271(9) 5_656 ? C20 O18B 1.311(13) 5_656 ? C21 C41 1.373(4) . ? C21 H21 0.9300 . ? C22 C23 1.333(4) 7_545 ? C22 C36 1.400(4) . ? C22 H22 0.9300 . ? C23 C22 1.333(4) 7_545 ? C23 C24 1.385(5) . ? C23 H23 0.9300 . ? C24 C43 1.405(5) . ? C25 C43 1.374(5) . ? C25 C36 1.387(5) 7_545 ? C25 H25 0.9300 . ? O18A C20 1.271(9) 5_656 ? C26A C27A 1.394(8) . ? C26A H26A 0.9300 . ? C27A H27A 0.9300 . ? C28A C29A 1.386(8) . ? C28A H28A 0.9300 . ? C29A H29A 0.9300 . ? O18B C20 1.311(13) 5_656 ? C26B C27B 1.352(13) . ? C26B H26B 0.9300 . ? C27B H27B 0.9300 . ? C28B C29B 1.429(13) . ? C28B H28B 0.9300 . ? C29B H29B 0.9300 . ? C30 C30 0.497(10) 6 ? C30 C35 1.169(2) 6 ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C30 C39 1.541(5) . ? C30 C31 1.736(7) 6 ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C33 0.579(9) 6 ? C33 C34 1.1383(17) 6 ? C33 C34 1.3900 . ? C33 C37 1.499(6) . ? C33 C32 1.793(6) 6 ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C25 1.387(5) 7_545 ? C36 C40 1.500(5) . ? C37 O6 1.433(6) 6 ? C37 C33 1.499(6) 6 ? C38 C44 1.309(5) . ? C38 C41 1.409(5) . ? C38 C45 1.544(6) 8_545 ? C39 C16 1.380(4) 6 ? C39 C30 1.541(5) 6 ? C41 H41 0.9300 . ? C42 C44 1.422(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C38 1.544(6) 8_445 ? 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 O17A Co1 O17A 79.4(4) 5_656 2_656 ? O17A Co1 O17A 180.0(3) 5_656 . ? O17A Co1 O17A 100.6(4) 2_656 . ? O17A Co1 O17A 100.6(4) 5_656 6 ? O17A Co1 O17A 180.000(1) 2_656 6 ? O17A Co1 O17A 79.4(4) . 6 ? O17A Co1 O4 85.3(2) 5_656 5_656 ? O17A Co1 O4 85.3(2) 2_656 5_656 ? O17A Co1 O4 94.7(2) . 5_656 ? O17A Co1 O4 94.7(2) 6 5_656 ? O17A Co1 O4 94.7(2) 5_656 . ? O17A Co1 O4 94.7(2) 2_656 . ? O17A Co1 O4 85.3(2) . . ? O17A Co1 O4 85.3(2) 6 . ? O4 Co1 O4 180.00(12) 5_656 . ? O17A Co1 O17B 14.94(19) 5_656 5_656 ? O17A Co1 O17B 92.7(3) 2_656 5_656 ? O17A Co1 O17B 165.06(19) . 5_656 ? O17A Co1 O17B 87.3(3) 6 5_656 ? O4 Co1 O17B 93.3(3) 5_656 5_656 ? O4 Co1 O17B 86.7(3) . 5_656 ? O17A Co1 O17B 165.06(19) 5_656 . ? O17A Co1 O17B 87.3(3) 2_656 . ? O17A Co1 O17B 14.94(19) . . ? O17A Co1 O17B 92.7(3) 6 . ? O4 Co1 O17B 86.7(3) 5_656 . ? O4 Co1 O17B 93.3(3) . . ? O17B Co1 O17B 180.0(3) 5_656 . ? O17A Co1 O17B 92.7(3) 5_656 2_656 ? O17A Co1 O17B 14.94(19) 2_656 2_656 ? O17A Co1 O17B 87.3(3) . 2_656 ? O17A Co1 O17B 165.06(19) 6 2_656 ? O4 Co1 O17B 93.3(3) 5_656 2_656 ? O4 Co1 O17B 86.7(3) . 2_656 ? O17B Co1 O17B 104.8(4) 5_656 2_656 ? O17B Co1 O17B 75.2(4) . 2_656 ? O17A Co1 O17B 87.3(3) 5_656 6 ? O17A Co1 O17B 165.06(19) 2_656 6 ? O17A Co1 O17B 92.7(3) . 6 ? O17A Co1 O17B 14.94(19) 6 6 ? O4 Co1 O17B 86.7(3) 5_656 6 ? O4 Co1 O17B 93.3(3) . 6 ? O17B Co1 O17B 75.2(4) 5_656 6 ? O17B Co1 O17B 104.8(4) . 6 ? O17B Co1 O17B 180.0(7) 2_656 6 ? O18B Co2 O18B 74.4(8) 6 . ? O18B Co2 O18A 93.3(5) 6 . ? O18B Co2 O18A 19.9(4) . . ? O18B Co2 O18A 19.9(4) 6 6 ? O18B Co2 O18A 93.3(5) . 6 ? O18A Co2 O18A 111.5(4) . 6 ? O18B Co2 O14 93.9(4) 6 . ? O18B Co2 O14 93.9(4) . . ? O18A Co2 O14 98.6(3) . . ? O18A Co2 O14 98.6(3) 6 . ? O18B Co2 O4 103.9(3) 6 . ? O18B Co2 O4 103.9(3) . . ? O18A Co2 O4 94.0(3) . . ? O18A Co2 O4 94.0(3) 6 . ? O14 Co2 O4 157.47(19) . . ? O18B Co2 O6 118.5(4) 6 6 ? O18B Co2 O6 158.5(4) . 6 ? O18A Co2 O6 140.4(3) . 6 ? O18A Co2 O6 98.6(2) 6 6 ? O14 Co2 O6 101.7(2) . 6 ? O4 Co2 O6 57.69(12) . 6 ? O18B Co2 O6 158.5(4) 6 . ? O18B Co2 O6 118.5(4) . . ? O18A Co2 O6 98.6(2) . . ? O18A Co2 O6 140.4(3) 6 . ? O14 Co2 O6 101.7(2) . . ? O4 Co2 O6 57.69(12) . . ? O6 Co2 O6 44.1(2) 6 . ? O18B Co2 O1 86.1(5) 6 6 ? O18B Co2 O1 151.9(5) . 6 ? O18A Co2 O1 165.5(6) . 6 ? O18A Co2 O1 70.7(4) 6 6 ? O14 Co2 O1 67.0(5) . 6 ? O4 Co2 O1 100.2(5) . 6 ? O6 Co2 O1 49.5(3) 6 6 ? O6 Co2 O1 86.6(3) . 6 ? O18B Co2 O1 151.9(5) 6 . ? O18B Co2 O1 86.1(5) . . ? O18A Co2 O1 70.7(4) . . ? O18A Co2 O1 165.5(6) 6 . ? O14 Co2 O1 67.0(5) . . ? O4 Co2 O1 100.2(5) . . ? O6 Co2 O1 86.6(3) 6 . ? O6 Co2 O1 49.5(3) . . ? O1 Co2 O1 103.6(8) 6 . ? O18B Co2 C37 123.8(3) 6 . ? O18B Co2 C37 123.8(3) . . ? O18A Co2 C37 108.3(3) . . ? O18A Co2 C37 108.3(3) 6 . ? O14 Co2 C37 130.8(2) . . ? O4 Co2 C37 26.68(12) . . ? O6 Co2 C37 35.16(13) 6 . ? O6 Co2 C37 35.16(13) . . ? O1 Co2 C37 83.8(4) 6 . ? O1 Co2 C37 83.8(4) . . ? O7 Co3 O8 96.05(14) . . ? O7 Co3 O3 98.1(2) . . ? O8 Co3 O3 98.00(12) . . ? O7 Co3 O13 86.37(18) . . ? O8 Co3 O13 166.1(3) . . ? O3 Co3 O13 68.1(3) . . ? O7 Co3 O16 110.09(19) . . ? O8 Co3 O16 104.65(10) . . ? O3 Co3 O16 141.20(13) . . ? O13 Co3 O16 87.2(2) . . ? O7 Co3 O15 166.45(19) . . ? O8 Co3 O15 94.68(11) . . ? O3 Co3 O15 88.51(18) . . ? O13 Co3 O15 85.19(15) . . ? O16 Co3 O15 58.94(13) . . ? O7 Co3 C2 138.4(2) . . ? O8 Co3 C2 99.77(13) . . ? O3 Co3 C2 117.17(19) . . ? O13 Co3 C2 87.18(18) . . ? O16 Co3 C2 28.51(12) . . ? O15 Co3 C2 30.50(13) . . ? O11 Co4 O9 94.01(14) . . ? O11 Co4 O10 101.5(2) . . ? O9 Co4 O10 86.82(15) . . ? O11 Co4 O16 89.37(15) . . ? O9 Co4 O16 95.90(11) . . ? O10 Co4 O16 168.65(19) . . ? O11 Co4 O12 90.97(19) . . ? O9 Co4 O12 173.96(18) . . ? O10 Co4 O12 88.86(18) . . ? O16 Co4 O12 87.55(15) . . ? O11 Co4 O2 174.70(17) . . ? O9 Co4 O2 86.26(16) . . ? O10 Co4 O2 83.8(2) . . ? O16 Co4 O2 85.34(16) . . ? O12 Co4 O2 89.1(2) . . ? C37 O4 Co2 94.4(3) . . ? C37 O4 Co1 156.2(4) . . ? Co2 O4 Co1 109.41(12) . . ? C37 O6 O6 55.8(2) . 6 ? C37 O6 Co2 85.3(3) . . ? O6 O6 Co2 67.95(12) 6 . ? C45 O7 Co3 123.8(5) . . ? C40 O8 Co3 124.1(2) . . ? C40 O9 Co4 141.3(3) . . ? C45 O11 Co4 138.7(4) . . ? C13 C1 C11 117.9(2) . . ? C13 C1 C17 120.4(2) . . ? C11 C1 C17 121.6(2) . . ? C2 O15 Co3 84.8(3) . . ? C2 O16 Co4 138.5(3) . . ? C2 O16 Co3 86.4(3) . . ? Co4 O16 Co3 99.74(10) . . ? O16 C2 O15 129.5(5) . . ? O16 C2 C3 110.7(4) . . ? O15 C2 C3 118.0(5) . . ? O16 C2 Co3 65.1(3) . . ? O15 C2 Co3 64.7(3) . . ? C3 C2 Co3 170.2(3) . . ? C4 C3 C8 119.9(3) . . ? C4 C3 C2 115.4(4) . . ? C8 C3 C2 124.6(4) . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 118.3(3) . . ? C5 C6 C9 120.3(3) . . ? C7 C6 C9 121.4(3) . . ? C8 C7 C6 118.7(4) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C3 C8 C7 121.4(4) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C13 C9 C10 119.0(2) . . ? C13 C9 C6 121.6(2) . . ? C10 C9 C6 119.4(2) . . ? C12 C10 C9 121.8(2) . . ? C12 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C1 C11 C12 121.8(2) . . ? C1 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C10 C12 C11 118.0(2) . . ? C10 C12 C14 122.3(2) . . ? C11 C12 C14 119.7(2) . . ? C9 C13 C1 121.5(2) . . ? C9 C13 H13 119.2 . . ? C1 C13 H13 119.2 . . ? C26B C14 C28B 119.1(6) . . ? C26B C14 C28A 94.3(6) . . ? C28B C14 C28A 52.9(6) . . ? C28B C14 C26A 99.6(6) . . ? C28A C14 C26A 115.6(4) . . ? C26B C14 C12 122.5(5) . . ? C28B C14 C12 118.2(5) . . ? C28A C14 C12 123.7(3) . . ? C26A C14 C12 120.5(3) . . ? C18 C15 C16 119.2(3) . . ? C18 C15 C24 120.9(3) . . ? C16 C15 C24 119.9(3) . . ? C39 C16 C15 120.4(3) . . ? C39 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C21 C17 C42 119.5(3) . . ? C21 C17 C1 122.2(3) . . ? C42 C17 C1 118.3(3) . . ? C15 C18 C15 120.8(4) 6 . ? C15 C18 H18 119.6 6 . ? C15 C18 H18 119.6 . . ? C27B C19 C29A 101.5(6) . . ? C29A C19 C27A 121.8(4) . . ? C27B C19 C29B 115.7(6) . . ? C29A C19 C29B 47.7(7) . . ? C27A C19 C29B 101.1(6) . . ? C27B C19 C20 123.1(5) . . ? C29A C19 C20 119.3(4) . . ? C27A C19 C20 118.9(4) . . ? C29B C19 C20 120.9(5) . . ? O17B C20 O18A 117.6(7) . 5_656 ? O17A C20 O18A 126.2(6) . 5_656 ? O17A C20 O18B 122.3(7) . 5_656 ? O17B C20 C19 118.8(6) . . ? O17A C20 C19 118.2(4) . . ? O18A C20 C19 115.6(6) 5_656 . ? O18B C20 C19 110.6(7) 5_656 . ? C17 C21 C41 120.3(3) . . ? C17 C21 H21 119.8 . . ? C41 C21 H21 119.8 . . ? C23 C22 C36 120.1(3) 7_545 . ? C23 C22 H22 119.9 7_545 . ? C36 C22 H22 119.9 . . ? C22 C23 C24 123.7(3) 7_545 . ? C22 C23 H23 118.1 7_545 . ? C24 C23 H23 118.1 . . ? C23 C24 C43 116.6(3) . . ? C23 C24 C15 123.4(3) . . ? C43 C24 C15 120.0(3) . . ? C43 C25 C36 121.6(3) . 7_545 ? C43 C25 H25 119.2 . . ? C36 C25 H25 119.2 7_545 . ? C20 O17A Co1 137.9(5) . . ? C20 O18A Co2 126.3(7) 5_656 . ? C27A C26A C14 120.8(5) . . ? C27A C26A H26A 119.6 . . ? C14 C26A H26A 119.6 . . ? C26A C27A C19 119.1(5) . . ? C26A C27A H27A 120.4 . . ? C19 C27A H27A 120.4 . . ? C29A C28A C14 123.8(5) . . ? C29A C28A H28A 118.1 . . ? C14 C28A H28A 118.1 . . ? C19 C29A C28A 118.5(5) . . ? C19 C29A H29A 120.8 . . ? C28A C29A H29A 120.8 . . ? C20 O17B Co1 131.0(7) . . ? C20 O18B Co2 124.6(9) 5_656 . ? C14 C26B C27B 122.8(8) . . ? C14 C26B H26B 118.6 . . ? C27B C26B H26B 118.6 . . ? C19 C27B C26B 123.9(8) . . ? C19 C27B H27B 118.1 . . ? C26B C27B H27B 118.1 . . ? C14 C28B C29B 117.8(9) . . ? C14 C28B H28B 121.1 . . ? C29B C28B H28B 121.1 . . ? C28B C29B C19 120.0(7) . . ? C28B C29B H29B 120.0 . . ? C19 C29B H29B 120.0 . . ? C30 C30 C35 106.0(4) 6 6 ? C35 C30 C31 90.3(2) 6 . ? C30 C30 C35 53.91(15) 6 . ? C35 C30 C35 52.1(4) 6 . ? C31 C30 C35 120.0 . . ? C30 C30 C39 80.72(18) 6 . ? C35 C30 C39 131.5(4) 6 . ? C31 C30 C39 124.4(3) . . ? C35 C30 C39 115.1(3) . . ? C35 C30 C31 110.5(3) 6 6 ? C31 C30 C31 87.47(18) . 6 ? C35 C30 C31 70.26(10) . 6 ? C39 C30 C31 104.5(4) . 6 ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C33 C34 103.2(4) 6 6 ? C33 C33 C34 52.9 6 . ? C34 C33 C34 50.4(4) 6 . ? C34 C33 C32 92.4(2) 6 . ? C34 C33 C32 120.0 . . ? C33 C33 C37 78.9(3) 6 . ? C34 C33 C37 128.8(3) 6 . ? C34 C33 C37 111.1(3) . . ? C32 C33 C37 128.2(3) . . ? C34 C33 C32 108.4(3) 6 6 ? C34 C33 C32 68.98(9) . 6 ? C32 C33 C32 87.30(17) . 6 ? C37 C33 C32 103.9(4) . 6 ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C25 C36 C22 117.7(3) 7_545 . ? C25 C36 C40 120.0(3) 7_545 . ? C22 C36 C40 122.3(3) . . ? O4 C37 O6 107.3(4) . 6 ? O4 C37 O6 107.3(4) . . ? O6 C37 O6 68.4(5) 6 . ? O4 C37 C33 126.9(5) . 6 ? O6 C37 C33 108.1(4) 6 6 ? O6 C37 C33 121.9(4) . 6 ? O4 C37 C33 126.9(5) . . ? O6 C37 C33 121.9(4) 6 . ? O6 C37 C33 108.1(3) . . ? O4 C37 Co2 58.9(3) . . ? O6 C37 Co2 59.5(3) 6 . ? O6 C37 Co2 59.5(3) . . ? C33 C37 Co2 167.0(2) 6 . ? C33 C37 Co2 167.0(2) . . ? C44 C38 C41 118.0(3) . . ? C44 C38 C45 127.6(5) . 8_545 ? C41 C38 C45 114.4(5) . 8_545 ? C16 C39 C16 119.9(4) . 6 ? C16 C39 C30 129.3(3) . . ? C16 C39 C30 110.7(3) 6 . ? C16 C39 C30 110.7(3) . 6 ? C16 C39 C30 129.3(3) 6 6 ? O9 C40 O8 125.6(3) . . ? O9 C40 C36 116.4(4) . . ? O8 C40 C36 117.9(3) . . ? C21 C41 C38 121.6(3) . . ? C21 C41 H41 119.2 . . ? C38 C41 H41 119.2 . . ? C17 C42 C44 117.9(4) . . ? C17 C42 H42 121.1 . . ? C44 C42 H42 121.1 . . ? C25 C43 C24 120.1(4) . . ? C25 C43 H43 119.9 . . ? C24 C43 H43 119.9 . . ? C38 C44 C42 122.6(4) . . ? C38 C44 H44 118.7 . . ? C42 C44 H44 118.7 . . ? O7 C45 O11 126.5(4) . . ? O7 C45 C38 129.8(7) . 8_445 ? O11 C45 C38 103.6(7) . 8_445 ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 1.013 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.102 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.012 -0.003 -0.013 23117.8 5115.7 _platon_squeeze_details ; ; # Attachment '- DUT-28-LT-CCDC-80201.cif' data_usd-35-ds3-sq _database_code_depnum_ccdc_archive 'CCDC 801201' #TrackingRef '- DUT-28-LT-CCDC-80201.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'Co22(btb)12 (DUT-28(LT))' _chemical_formula_moiety 'C324 H180 Co22 O120' _chemical_formula_sum 'C162 H90 Co11 O60' _chemical_properties_physical moisture-sensitive _exptl_crystal_recrystallization_method DEF _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour purple _diffrn_ambient_temperature 100K _diffrn_ambient_pressure 100 _chemical_formula_weight 3644.58 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 45.386(9) _cell_length_b 35.904(7) _cell_length_c 33.184(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.91(3) _cell_angle_gamma 90.00 _cell_volume 53876(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4714 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 25.5 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7460 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Absorption cooefficient is given for the solvent free framework. ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99640 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.50 _reflns_number_total 25433 _reflns_number_gt 18857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement XDS _computing_data_reduction XDSCONV _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.1461P)^2^] 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 25433 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2252 _refine_ls_wR_factor_gt 0.2133 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.003 _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 C1 C 0.97644(9) 0.21533(13) 0.18217(16) 0.0488(12) Uani 1 1 d . . . C2 C 1.29102(9) 0.00794(13) 0.51449(14) 0.0547(10) Uani 1 1 d . . . C3 C 0.95676(9) 0.16523(13) 0.13427(12) 0.0528(13) Uani 1 1 d . . . H3 H 0.9705 0.1726 0.1165 0.063 Uiso 1 1 calc R . . C4 C 1.28211(13) -0.00882(14) 0.47175(16) 0.0657(16) Uani 1 1 d . . . C5 C 0.95528(8) 0.18363(12) 0.17153(13) 0.0460(12) Uani 1 1 d . . . C6 C 0.93435(9) 0.17377(12) 0.19786(13) 0.0497(12) Uani 1 1 d . . . H6 H 0.9332 0.1865 0.2221 0.060 Uiso 1 1 calc R . . C7 C 0.91490(8) 0.14390(12) 0.18682(13) 0.0488(12) Uani 1 1 d . . . H7 H 0.9009 0.1368 0.2042 0.059 Uiso 1 1 calc R . . C8 C 0.93771(9) 0.13625(14) 0.12444(14) 0.0594(14) Uani 1 1 d . . . H8 H 0.9387 0.1236 0.1001 0.071 Uiso 1 1 calc R . . C9 C 0.91628(8) 0.12539(12) 0.15139(13) 0.0472(12) Uani 1 1 d . . . C10 C 0.89671(8) 0.09296(13) 0.14067(13) 0.0492(12) Uani 1 1 d . . . C11 C 0.88587(8) 0.08703(12) 0.09969(12) 0.0464(12) Uani 1 1 d . . . H11 H 0.8914 0.1027 0.0794 0.056 Uiso 1 1 calc R . . C12 C 0.86638(8) 0.05661(12) 0.09031(13) 0.0457(12) Uani 1 1 d . . . C13 C 0.85917(8) 0.03375(13) 0.12100(13) 0.0504(13) Uani 1 1 d . . . H13 H 0.8465 0.0138 0.1149 0.060 Uiso 1 1 calc R . . C14 C 0.87025(8) 0.03952(12) 0.16166(13) 0.0460(12) Uani 1 1 d . . . C15 C 0.88875(8) 0.06896(12) 0.17062(12) 0.0459(12) Uani 1 1 d . . . H15 H 0.8961 0.0730 0.1973 0.055 Uiso 1 1 calc R . . C16 C 0.86084(8) 0.01447(12) 0.19408(13) 0.0493(13) Uani 1 1 d . . . C17 C 0.83309(9) 0.00195(14) 0.19387(14) 0.0584(14) Uani 1 1 d . . . H17 H 0.8197 0.0072 0.1718 0.070 Uiso 1 1 calc R . . C18 C 0.88149(9) 0.00432(14) 0.22622(14) 0.0631(15) Uani 1 1 d . . . H18 H 0.9012 0.0112 0.2257 0.076 Uiso 1 1 calc R . . C19 C 0.82379(9) -0.01849(15) 0.22557(14) 0.0633(14) Uani 1 1 d . . . H19 H 0.8042 -0.0263 0.2250 0.076 Uiso 1 1 calc R . . C20 C 0.87270(9) -0.01570(14) 0.25849(14) 0.0638(15) Uani 1 1 d . . . H20 H 0.8864 -0.0213 0.2801 0.077 Uiso 1 1 calc R . . C21 C 0.84410(9) -0.02753(14) 0.25907(13) 0.0600(14) Uani 1 1 d . . . C22 C 0.83347(12) -0.04660(16) 0.29453(15) 0.0756(17) Uani 1 1 d . . . C23 C 0.85359(9) 0.05129(13) 0.04883(14) 0.0513(13) Uani 1 1 d . . . C24 C 0.86995(10) 0.05937(14) 0.01661(16) 0.0652(15) Uani 1 1 d . . . H24 H 0.8892 0.0680 0.0222 0.078 Uiso 1 1 calc R . . C25 C 0.85905(9) 0.05529(14) -0.02407(13) 0.0656(15) Uani 1 1 d . . . H25 H 0.8705 0.0608 -0.0452 0.079 Uiso 1 1 calc R . . C26 C 0.82569(9) 0.03827(12) 0.04078(14) 0.0572(14) Uani 1 1 d . . . H26 H 0.8143 0.0325 0.0619 0.069 Uiso 1 1 calc R . . C27 C 0.82932(9) 0.04211(13) -0.03113(15) 0.0566(14) Uani 1 1 d . . . C28 C 0.81372(10) 0.03336(13) -0.00001(15) 0.0613(15) Uani 1 1 d . . . H28 H 0.7947 0.0239 -0.0051 0.074 Uiso 1 1 calc R . . C29 C 0.81648(11) 0.03927(14) -0.07439(16) 0.0567(14) Uani 1 1 d . . . C30 C 1.05549(10) 0.25339(14) 0.19730(14) 0.0497(13) Uani 1 1 d . . . C31 C 1.08159(8) 0.24415(13) 0.22646(14) 0.0513(13) Uani 1 1 d . . . C32 C 1.10175(8) 0.21707(13) 0.21711(14) 0.0562(13) Uani 1 1 d . . . H32 H 1.0985 0.2032 0.1935 0.067 Uiso 1 1 calc R . . C33 C 1.12715(9) 0.21087(13) 0.24362(15) 0.0590(13) Uani 1 1 d . . . H33 H 1.1401 0.1916 0.2388 0.071 Uiso 1 1 calc R . . C34 C 1.08641(8) 0.26555(13) 0.25998(13) 0.0508(12) Uani 1 1 d . . . H34 H 1.0725 0.2832 0.2662 0.061 Uiso 1 1 calc R . . C35 C 1.11300(9) 0.26064(13) 0.28557(14) 0.0569(14) Uani 1 1 d . . . H35 H 1.1169 0.2758 0.3081 0.068 Uiso 1 1 calc R . . C36 C 1.13277(8) 0.23384(13) 0.27714(14) 0.0545(13) Uani 1 1 d . . . C37 C 1.16182(8) 0.22916(13) 0.30268(13) 0.0521(13) Uani 1 1 d . . . C38 C 1.17836(9) 0.26099(13) 0.31317(16) 0.0688(16) Uani 1 1 d . . . H38 H 1.1709 0.2844 0.3059 0.083 Uiso 1 1 calc R . . C39 C 1.20644(8) 0.25754(14) 0.33486(16) 0.0666(15) Uani 1 1 d . . . C40 C 1.17199(8) 0.19447(13) 0.31447(14) 0.0553(13) Uani 1 1 d . . . H40 H 1.1605 0.1735 0.3079 0.066 Uiso 1 1 calc R . . C41 C 1.21479(9) 0.32540(14) 0.34990(14) 0.0599(14) Uani 1 1 d . . . H41 H 1.1946 0.3281 0.3520 0.072 Uiso 1 1 calc R . . C42 C 1.25600(9) 0.28773(13) 0.33858(17) 0.0779(18) Uani 1 1 d . . . H42 H 1.2638 0.2645 0.3331 0.093 Uiso 1 1 calc R . . C43 C 1.22554(9) 0.29166(14) 0.34205(15) 0.0649(15) Uani 1 1 d . . . C44 C 1.23296(9) 0.35634(13) 0.35492(14) 0.0612(14) Uani 1 1 d . . . H44 H 1.2249 0.3794 0.3605 0.073 Uiso 1 1 calc R . . C45 C 1.27425(10) 0.31842(14) 0.34339(16) 0.0750(17) Uani 1 1 d . . . H45 H 1.2944 0.3159 0.3411 0.090 Uiso 1 1 calc R . . C46 C 1.19994(9) 0.19061(13) 0.33671(15) 0.0647(15) Uani 1 1 d . . . C47 C 1.21612(9) 0.22291(12) 0.34678(15) 0.0621(15) Uani 1 1 d . . . H47 H 1.2342 0.2207 0.3622 0.075 Uiso 1 1 calc R . . C48 C 1.21112(9) 0.15381(13) 0.34939(16) 0.0659(16) Uani 1 1 d . . . C49 C 1.24211(9) 0.14720(14) 0.35363(16) 0.0717(17) Uani 1 1 d . . . H49 H 1.2551 0.1662 0.3483 0.086 Uiso 1 1 calc R . . C50 C 1.19301(9) 0.12383(14) 0.35702(15) 0.0672(16) Uani 1 1 d . . . H50 H 1.1726 0.1271 0.3543 0.081 Uiso 1 1 calc R . . C51 C 1.20423(9) 0.08985(13) 0.36840(15) 0.0622(15) Uani 1 1 d . . . H51 H 1.1913 0.0704 0.3727 0.075 Uiso 1 1 calc R . . C52 C 1.23455(9) 0.08369(13) 0.37378(15) 0.0587(14) Uani 1 1 d . . . C53 C 1.25307(9) 0.11253(13) 0.36568(17) 0.0722(17) Uani 1 1 d . . . H53 H 1.2734 0.1087 0.3683 0.087 Uiso 1 1 calc R . . C54 C 1.24706(9) 0.04635(13) 0.38632(13) 0.0514(13) Uani 1 1 d . . . C55 C 0.93924(8) 0.33715(13) 0.17404(15) 0.0553(14) Uani 1 1 d . . . C56 C 0.96758(9) 0.31506(14) 0.17910(16) 0.0537(14) Uani 1 1 d . . . C57 C 0.92122(9) 0.33586(15) 0.13769(14) 0.0678(15) Uani 1 1 d . . . H57 H 0.9267 0.3217 0.1161 0.081 Uiso 1 1 calc R . . C58 C 0.89497(9) 0.35606(15) 0.13415(15) 0.0668(16) Uani 1 1 d . . . H58 H 0.8837 0.3562 0.1094 0.080 Uiso 1 1 calc R . . C59 C 0.90331(9) 0.37709(14) 0.20332(14) 0.0595(14) Uani 1 1 d . . . H59 H 0.8977 0.3915 0.2247 0.071 Uiso 1 1 calc R . . C60 C 0.88509(8) 0.37568(13) 0.16566(13) 0.0490(12) Uani 1 1 d . . . C61 C 0.85750(9) 0.39808(13) 0.16284(14) 0.0530(13) Uani 1 1 d . . . C62 C 0.84713(9) 0.41593(14) 0.12652(14) 0.0633(15) Uani 1 1 d . . . H62 H 0.8572 0.4130 0.1035 0.076 Uiso 1 1 calc R . . C63 C 0.82199(10) 0.43769(13) 0.12509(14) 0.0545(13) Uani 1 1 d . . . C64 C 0.81116(10) 0.45750(13) 0.08646(14) 0.0545(13) Uani 1 1 d . . . C65 C 0.83014(11) 0.46646(15) 0.05826(16) 0.0727(17) Uani 1 1 d . . . H65 H 0.8501 0.4613 0.0643 0.087 Uiso 1 1 calc R . . C66 C 0.78139(9) 0.46613(12) 0.07825(13) 0.0524(13) Uani 1 1 d . . . H66 H 0.7678 0.4603 0.0967 0.063 Uiso 1 1 calc R . . C67 C 0.77228(9) 0.48386(13) 0.04167(13) 0.0536(13) Uani 1 1 d . . . H67 H 0.7524 0.4901 0.0363 0.064 Uiso 1 1 calc R . . C68 C 0.82158(9) 0.48288(14) 0.02072(14) 0.0661(15) Uani 1 1 d . . . H68 H 0.8348 0.4874 0.0014 0.079 Uiso 1 1 calc R . . C69 C 0.84184(9) 0.40205(13) 0.19582(14) 0.0560(14) Uani 1 1 d . . . H69 H 0.8481 0.3893 0.2194 0.067 Uiso 1 1 calc R . . C70 C 0.80719(10) 0.44227(13) 0.15885(15) 0.0599(15) Uani 1 1 d . . . H70 H 0.7905 0.4574 0.1574 0.072 Uiso 1 1 calc R . . C71 C 0.81639(9) 0.42488(12) 0.19558(12) 0.0487(12) Uani 1 1 d . . . C72 C 0.80138(9) 0.42956(13) 0.23231(13) 0.0572(14) Uani 1 1 d . . . C73 C 0.77070(9) 0.43224(13) 0.23207(14) 0.0561(14) Uani 1 1 d . . . H73 H 0.7590 0.4297 0.2078 0.067 Uiso 1 1 calc R . . C74 C 0.75767(9) 0.43854(13) 0.26702(14) 0.0586(14) Uani 1 1 d . . . H74 H 0.7372 0.4397 0.2663 0.070 Uiso 1 1 calc R . . C75 C 0.77433(9) 0.44330(13) 0.30342(13) 0.0547(10) Uani 1 1 d . . . C76 C 0.80416(9) 0.44060(13) 0.30387(13) 0.0579(14) Uani 1 1 d . . . H76 H 0.8155 0.4433 0.3284 0.070 Uiso 1 1 calc R . . C77 C 0.81813(10) 0.43407(14) 0.26992(15) 0.0670(15) Uani 1 1 d . . . H77 H 0.8386 0.4326 0.2714 0.080 Uiso 1 1 calc R . . C78 C 0.92927(9) 0.35670(13) 0.20726(15) 0.0556(14) Uani 1 1 d . . . H78 H 0.9403 0.3558 0.2322 0.067 Uiso 1 1 calc R . . C79 C 0.78278(10) 0.11322(16) -0.14459(14) 0.0605(14) Uani 1 1 d . . . C80 C 1.26244(9) 0.35328(13) 0.35169(14) 0.0596(15) Uani 1 1 d . . . C81 C 1.26005(11) -0.04739(14) 0.34013(14) 0.0619(14) Uani 1 1 d . . . O1 O 0.99165(7) 0.22536(9) 0.15449(10) 0.0627(9) Uani 1 1 d . . . O2 O 0.97664(5) 0.22923(8) 0.21705(9) 0.0506(8) Uani 1 1 d . . . O3 O 0.97750(6) 0.30366(10) 0.14817(10) 0.0638(9) Uani 1 1 d . . . O4 O 0.97840(5) 0.31110(8) 0.21569(8) 0.0550(8) Uani 1 1 d . . . O5 O 1.03377(5) 0.27192(8) 0.20863(8) 0.0431(7) Uani 1 1 d . . . O6 O 1.05604(5) 0.24376(9) 0.16070(10) 0.0596(9) Uani 1 1 d . . . O7 O 1.27408(6) 0.04394(8) 0.39409(10) 0.0654(10) Uani 1 1 d . . . O8 O 1.22906(6) 0.01991(8) 0.38881(8) 0.0512(8) Uani 1 1 d . . . O9 O 0.79161(7) 0.02330(9) -0.08076(8) 0.0636(9) Uani 1 1 d . . . O10 O 0.82968(7) 0.05015(10) -0.10323(10) 0.0615(10) Uani 1 1 d . . . O11 O 0.85321(6) -0.06239(9) 0.31925(9) 0.0695(10) Uani 1 1 d . . . O12 O 0.80640(6) -0.04585(11) 0.30006(9) 0.0787(11) Uani 1 1 d . . . O13 O 0.77108(6) 0.08198(9) -0.13994(8) 0.0544(9) Uani 1 1 d . . . O14 O 0.80963(7) 0.11972(9) -0.14595(9) 0.0643(9) Uani 1 1 d . . . O15 O 1.23266(6) -0.05135(8) 0.34276(8) 0.0573(9) Uani 1 1 d . . . O16 O 1.30159(8) -0.01588(11) 0.44885(10) 0.0733(11) Uani 1 1 d . . . O17 O 0.75595(7) 0.00353(9) -0.16794(12) 0.0932(13) Uani 1 1 d . . . O18 O 1.34186(7) -0.03425(11) 0.39152(11) 0.0914(13) Uani 1 1 d . . . O19 O 1.25437(6) -0.01446(9) 0.46435(9) 0.0665(10) Uani 1 1 d . . . O20 O 0.89276(7) 0.07335(11) -0.11119(10) 0.0966(13) Uani 1 1 d . . . O21 O 1.19717(6) -0.04297(9) 0.42278(11) 0.0795(11) Uani 1 1 d . . . O22 O 0.85210(8) 0.12874(12) -0.07854(11) 0.1088(15) Uani 1 1 d . . . O23 O 1.33671(7) 0.04695(15) 0.42029(14) 0.1328(19) Uani 1 1 d . . . O24 O 1.27646(6) -0.03586(8) 0.37227(8) 0.0574(9) Uani 1 1 d . . . O25 O 1.24853(8) -0.08846(9) 0.42422(10) 0.0853(12) Uani 1 1 d . . . O26 O 1.00954(7) 0.26602(12) 0.08397(10) 0.0897(12) Uani 1 1 d . . . O28 O 1.04003(8) 0.32143(12) 0.13603(12) 0.1022(13) Uani 1 1 d . . . O29 O 0.87067(7) 0.13831(11) -0.16204(12) 0.0969(13) Uani 1 1 d . . . O30 O 1.31471(8) 0.02311(12) 0.33606(12) 0.0994(13) Uani 1 1 d . . . O31 O 0.81408(18) -0.01789(16) -0.15133(15) 0.206(4) Uani 1 1 d . . . Co1 Co 1.0000 0.26941(2) 0.2500 0.0414(3) Uani 1 2 d S . . Co2 Co 0.792816(13) 0.033222(17) -0.144361(18) 0.0597(3) Uani 1 1 d . . . Co3 Co 1.238967(12) -0.032935(16) 0.407452(17) 0.0518(2) Uani 1 1 d . . . Co4 Co 0.850420(12) 0.095376(19) -0.130918(18) 0.0640(3) Uani 1 1 d . . . Co5 Co 1.015023(11) 0.273346(18) 0.146606(17) 0.0536(2) Uani 1 1 d . . . Co6 Co 1.307235(12) 0.003971(18) 0.393168(19) 0.0636(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(2) 0.066(3) 0.043(3) 0.004(3) -0.016(2) -0.003(2) C2 0.0475(19) 0.070(2) 0.040(2) -0.0098(18) -0.0355(18) 0.0081(17) C3 0.044(2) 0.079(4) 0.033(3) -0.007(2) -0.010(2) -0.007(2) C4 0.082(4) 0.061(3) 0.046(3) -0.008(3) -0.047(3) 0.011(3) C5 0.034(2) 0.061(3) 0.040(3) 0.001(2) -0.018(2) -0.001(2) C6 0.045(2) 0.059(3) 0.042(3) -0.003(2) -0.014(2) -0.013(2) C7 0.044(2) 0.065(3) 0.034(3) 0.005(2) -0.014(2) -0.013(2) C8 0.046(2) 0.079(4) 0.049(3) -0.012(3) -0.023(3) -0.007(3) C9 0.037(2) 0.064(3) 0.036(3) 0.000(3) -0.022(2) -0.014(2) C10 0.031(2) 0.066(3) 0.048(3) 0.001(3) -0.014(2) -0.005(2) C11 0.049(2) 0.057(3) 0.029(2) 0.008(2) -0.027(2) -0.010(2) C12 0.048(2) 0.053(3) 0.031(3) 0.003(2) -0.023(2) 0.000(2) C13 0.041(2) 0.066(3) 0.038(3) -0.006(3) -0.033(2) -0.004(2) C14 0.035(2) 0.057(3) 0.042(3) 0.013(2) -0.018(2) 0.005(2) C15 0.043(2) 0.056(3) 0.034(3) 0.000(2) -0.023(2) -0.019(2) C16 0.034(2) 0.063(3) 0.045(3) 0.001(3) -0.032(2) -0.010(2) C17 0.045(3) 0.083(4) 0.041(3) 0.009(3) -0.032(2) -0.006(2) C18 0.049(3) 0.079(4) 0.055(3) 0.033(3) -0.028(2) -0.020(2) C19 0.050(3) 0.095(4) 0.039(3) 0.012(3) -0.026(2) -0.015(3) C20 0.037(3) 0.092(4) 0.056(3) 0.021(3) -0.035(2) -0.016(2) C21 0.055(3) 0.088(4) 0.033(3) 0.023(3) -0.023(2) -0.009(3) C22 0.064(3) 0.104(4) 0.052(3) 0.007(3) -0.041(3) -0.012(3) C23 0.044(3) 0.060(3) 0.045(3) 0.007(3) -0.022(3) 0.001(2) C24 0.047(3) 0.076(4) 0.065(4) 0.004(3) -0.038(3) -0.007(2) C25 0.045(3) 0.108(4) 0.038(3) -0.005(3) -0.032(2) -0.003(3) C26 0.053(3) 0.070(3) 0.043(3) -0.011(2) -0.027(2) -0.007(2) C27 0.046(3) 0.069(3) 0.048(3) 0.005(3) -0.036(3) -0.001(2) C28 0.055(3) 0.078(4) 0.044(3) 0.011(3) -0.035(3) -0.019(3) C29 0.057(3) 0.067(3) 0.040(3) 0.002(3) -0.033(3) 0.009(3) C30 0.040(3) 0.068(3) 0.037(3) 0.006(3) -0.017(2) -0.027(3) C31 0.027(2) 0.067(3) 0.056(3) 0.001(3) -0.022(2) -0.006(2) C32 0.031(2) 0.069(3) 0.064(3) -0.003(3) -0.022(2) 0.005(2) C33 0.040(2) 0.056(3) 0.079(3) 0.000(3) -0.010(2) 0.002(2) C34 0.023(2) 0.068(3) 0.060(3) -0.006(3) -0.012(2) 0.007(2) C35 0.039(2) 0.055(3) 0.072(3) 0.000(3) -0.024(2) -0.004(2) C36 0.023(2) 0.065(3) 0.071(3) -0.010(3) -0.020(2) 0.003(2) C37 0.027(2) 0.059(3) 0.066(3) -0.001(3) -0.023(2) 0.009(2) C38 0.035(2) 0.053(3) 0.111(4) 0.014(3) -0.034(3) -0.006(2) C39 0.031(2) 0.067(4) 0.096(4) 0.001(3) -0.032(3) -0.005(2) C40 0.025(2) 0.054(3) 0.083(3) -0.006(3) -0.018(2) 0.000(2) C41 0.030(2) 0.061(4) 0.083(3) 0.006(3) -0.031(2) -0.005(3) C42 0.032(2) 0.049(3) 0.144(5) 0.011(3) -0.039(3) -0.005(2) C43 0.036(3) 0.049(3) 0.103(4) 0.003(3) -0.034(3) 0.002(2) C44 0.041(3) 0.057(3) 0.080(3) 0.006(3) -0.024(2) -0.005(2) C45 0.044(2) 0.059(4) 0.115(4) 0.001(3) -0.037(3) -0.002(3) C46 0.039(2) 0.055(3) 0.092(4) -0.003(3) -0.037(3) 0.004(2) C47 0.035(2) 0.045(3) 0.099(4) 0.005(3) -0.039(3) 0.000(2) C48 0.039(2) 0.043(3) 0.109(4) -0.012(3) -0.036(3) 0.008(2) C49 0.033(2) 0.059(3) 0.117(4) -0.008(3) -0.034(3) -0.008(2) C50 0.031(2) 0.062(4) 0.103(4) 0.006(3) -0.028(2) -0.004(3) C51 0.038(2) 0.048(3) 0.095(4) 0.007(3) -0.027(3) -0.002(2) C52 0.036(2) 0.051(3) 0.083(3) -0.006(3) -0.032(2) 0.008(3) C53 0.033(2) 0.051(3) 0.126(5) -0.015(3) -0.035(3) 0.007(3) C54 0.037(3) 0.056(3) 0.056(3) -0.011(3) -0.026(2) 0.001(3) C55 0.035(2) 0.067(3) 0.058(3) 0.013(3) -0.030(3) 0.005(2) C56 0.038(3) 0.076(4) 0.041(3) 0.020(3) -0.032(3) -0.007(2) C57 0.055(3) 0.103(4) 0.042(3) -0.003(3) -0.020(2) 0.016(3) C58 0.052(3) 0.096(4) 0.046(3) 0.018(3) -0.035(3) 0.021(3) C59 0.052(3) 0.075(3) 0.047(3) -0.002(3) -0.019(2) 0.018(3) C60 0.038(2) 0.075(3) 0.029(3) -0.001(3) -0.025(2) 0.016(2) C61 0.046(3) 0.071(3) 0.037(3) 0.008(3) -0.024(3) 0.006(2) C62 0.045(2) 0.093(4) 0.046(3) 0.005(3) -0.027(2) 0.012(3) C63 0.058(3) 0.064(3) 0.036(3) 0.012(3) -0.033(3) 0.016(3) C64 0.051(3) 0.068(3) 0.041(3) 0.007(3) -0.019(3) 0.007(2) C65 0.055(3) 0.102(4) 0.054(3) 0.022(3) -0.034(3) 0.006(3) C66 0.050(3) 0.066(3) 0.036(3) 0.004(2) -0.022(2) 0.010(2) C67 0.043(2) 0.074(3) 0.040(3) 0.008(3) -0.021(2) 0.005(2) C68 0.055(3) 0.085(4) 0.053(3) 0.030(3) -0.022(2) -0.004(3) C69 0.050(3) 0.070(3) 0.041(3) 0.014(3) -0.033(3) 0.006(2) C70 0.056(3) 0.062(3) 0.054(3) -0.016(3) -0.039(3) 0.011(2) C71 0.052(3) 0.062(3) 0.027(3) 0.005(2) -0.030(2) 0.003(2) C72 0.063(3) 0.076(3) 0.027(3) -0.004(2) -0.035(2) 0.014(2) C73 0.039(2) 0.082(4) 0.041(3) -0.017(3) -0.036(2) 0.011(2) C74 0.047(2) 0.073(3) 0.050(3) -0.012(3) -0.031(3) 0.019(2) C75 0.0475(19) 0.070(2) 0.040(2) -0.0098(18) -0.0355(18) 0.0081(17) C76 0.059(3) 0.083(4) 0.025(3) -0.016(2) -0.036(2) 0.028(2) C77 0.053(3) 0.095(4) 0.046(3) -0.001(3) -0.035(3) 0.016(3) C78 0.042(2) 0.062(3) 0.056(3) 0.009(3) -0.034(2) 0.000(2) C79 0.042(3) 0.071(4) 0.062(3) -0.014(3) -0.030(2) 0.002(3) C80 0.046(3) 0.055(3) 0.071(3) 0.017(3) -0.035(2) -0.015(3) C81 0.060(3) 0.083(4) 0.038(3) 0.010(3) -0.028(3) 0.014(3) O1 0.0511(17) 0.079(2) 0.053(2) 0.0013(18) -0.0254(18) -0.0155(17) O2 0.0338(14) 0.069(2) 0.045(2) -0.0009(17) -0.0203(14) -0.0026(13) O3 0.0511(18) 0.096(3) 0.040(2) 0.0042(19) -0.0172(16) 0.0245(17) O4 0.0370(14) 0.070(2) 0.0526(19) -0.0011(16) -0.0243(15) 0.0027(14) O5 0.0193(13) 0.0603(19) 0.0470(17) -0.0017(15) -0.0131(13) 0.0051(13) O6 0.0327(15) 0.082(2) 0.062(2) 0.0023(19) -0.0094(15) 0.0039(15) O7 0.0451(18) 0.058(2) 0.087(2) -0.0097(18) -0.0286(17) 0.0105(15) O8 0.0445(16) 0.0512(19) 0.0542(19) -0.0015(16) -0.0178(14) 0.0047(16) O9 0.0640(19) 0.081(2) 0.0389(18) -0.0002(16) -0.0343(16) 0.0021(18) O10 0.0551(18) 0.087(3) 0.0358(19) -0.0069(19) -0.0340(17) 0.0225(17) O11 0.0649(18) 0.092(3) 0.0445(18) 0.0185(18) -0.0355(17) -0.0193(17) O12 0.0422(19) 0.134(3) 0.054(2) 0.039(2) -0.0294(16) -0.0212(18) O13 0.0484(16) 0.061(2) 0.0476(18) 0.0017(16) -0.0307(14) 0.0073(17) O14 0.059(2) 0.063(2) 0.067(2) -0.0008(17) -0.0189(16) 0.0072(16) O15 0.0484(18) 0.071(2) 0.0469(18) -0.0147(16) -0.0263(15) 0.0115(15) O16 0.064(2) 0.103(3) 0.047(2) -0.027(2) -0.0303(19) 0.028(2) O17 0.070(2) 0.078(2) 0.121(3) -0.018(2) -0.055(2) 0.0210(18) O18 0.0627(19) 0.125(3) 0.079(2) -0.019(2) -0.0395(19) 0.018(2) O19 0.0586(19) 0.075(2) 0.059(2) -0.0184(17) -0.0378(17) 0.0071(16) O20 0.078(2) 0.139(3) 0.061(2) -0.008(2) -0.0594(19) -0.013(2) O21 0.0622(18) 0.068(2) 0.104(3) -0.012(2) -0.0197(19) -0.0020(17) O22 0.109(3) 0.135(4) 0.072(2) -0.041(2) -0.053(2) 0.005(3) O23 0.0406(18) 0.203(5) 0.146(4) 0.044(3) -0.048(2) -0.034(2) O24 0.0558(17) 0.068(2) 0.0424(18) -0.0191(15) -0.0337(16) 0.0183(15) O25 0.113(3) 0.062(2) 0.075(2) 0.0018(19) -0.022(2) 0.011(2) O26 0.084(2) 0.133(3) 0.050(2) 0.010(2) -0.0081(18) 0.002(2) O28 0.088(2) 0.110(3) 0.106(3) 0.039(3) -0.009(2) -0.020(2) O29 0.072(2) 0.095(3) 0.120(3) -0.020(2) -0.012(2) -0.017(2) O30 0.106(3) 0.107(3) 0.083(3) -0.009(2) -0.009(2) 0.019(2) O31 0.367(9) 0.138(5) 0.097(4) -0.059(3) -0.083(5) 0.146(6) Co1 0.0234(4) 0.0553(6) 0.0412(5) 0.000 -0.0225(3) 0.000 Co2 0.0601(4) 0.0653(5) 0.0460(4) -0.0143(3) -0.0398(3) 0.0199(3) Co3 0.0514(4) 0.0536(4) 0.0445(4) -0.0094(3) -0.0300(3) 0.0067(3) Co4 0.0512(4) 0.0799(5) 0.0544(4) -0.0186(4) -0.0335(3) 0.0120(3) Co5 0.0326(3) 0.0751(5) 0.0497(4) 0.0104(3) -0.0162(3) -0.0017(3) Co6 0.0450(4) 0.0708(5) 0.0689(5) -0.0094(4) -0.0309(3) 0.0113(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 C1 O1 1.249(5) . ? C1 O2 1.260(5) . ? C1 C5 1.511(6) . ? C2 C67 1.325(6) 8_556 ? C2 C68 1.423(6) 8_556 ? C2 C4 1.562(7) . ? C3 C8 1.374(6) . ? C3 C5 1.408(6) . ? C4 O16 1.240(6) . ? C4 O19 1.278(6) . ? C5 C6 1.390(6) . ? C6 C7 1.418(6) . ? C7 C9 1.357(6) . ? C8 C9 1.430(6) . ? C9 C10 1.489(6) . ? C10 C15 1.387(6) . ? C10 C11 1.422(6) . ? C11 C12 1.423(6) . ? C12 C13 1.369(6) . ? C12 C23 1.460(6) . ? C13 C14 1.414(6) . ? C14 C15 1.367(6) . ? C14 C16 1.493(6) . ? C16 C17 1.337(6) . ? C16 C18 1.406(5) . ? C17 C19 1.378(6) . ? C18 C20 1.377(6) . ? C19 C21 1.420(5) . ? C20 C21 1.367(6) . ? C21 C22 1.478(7) . ? C22 O12 1.258(6) . ? C22 O11 1.293(5) . ? C23 C26 1.355(6) . ? C23 C24 1.383(7) . ? C24 C25 1.405(6) . ? C25 C27 1.430(6) . ? C26 C28 1.426(6) . ? C27 C28 1.338(7) . ? C27 C29 1.506(7) . ? C29 O10 1.235(6) . ? C29 O9 1.268(6) . ? C29 Co2 2.483(4) . ? C30 O6 1.265(5) . ? C30 O5 1.273(6) . ? C30 C31 1.501(5) . ? C30 Co5 2.487(4) . ? C31 C34 1.354(6) . ? C31 C32 1.388(6) . ? C32 C33 1.406(5) . ? C33 C36 1.390(6) . ? C34 C35 1.426(5) . ? C35 C36 1.361(6) . ? C36 C37 1.515(5) . ? C37 C40 1.373(6) . ? C37 C38 1.395(6) . ? C38 C39 1.414(5) . ? C39 C47 1.366(6) . ? C39 C43 1.508(6) . ? C40 C46 1.419(5) . ? C41 C43 1.340(6) . ? C41 C44 1.385(6) . ? C42 C45 1.380(6) . ? C42 C43 1.404(6) . ? C44 C80 1.356(6) . ? C45 C80 1.398(7) . ? C46 C47 1.398(6) . ? C46 C48 1.464(6) . ? C48 C50 1.391(7) . ? C48 C49 1.422(6) . ? C49 C53 1.387(6) . ? C50 C51 1.363(6) . ? C51 C52 1.390(6) . ? C52 C53 1.375(7) . ? C52 C54 1.501(6) . ? C54 O7 1.234(5) . ? C54 O8 1.260(5) . ? C55 C57 1.399(6) . ? C55 C78 1.414(6) . ? C55 C56 1.508(6) . ? C56 O3 1.226(5) . ? C56 O4 1.278(5) . ? C57 C58 1.391(6) . ? C58 C60 1.368(6) . ? C59 C78 1.384(6) . ? C59 C60 1.439(5) . ? C60 C61 1.485(6) . ? C61 C69 1.362(6) . ? C61 C62 1.410(6) . ? C62 C63 1.380(6) . ? C63 C70 1.365(7) . ? C63 C64 1.511(6) . ? C64 C65 1.363(7) . ? C64 C66 1.390(6) . ? C65 C68 1.403(7) . ? C66 C67 1.401(6) . ? C67 C2 1.325(6) 8_455 ? C68 C2 1.423(6) 8_455 ? C69 C71 1.416(6) . ? C70 C71 1.401(6) . ? C71 C72 1.456(6) . ? C72 C73 1.395(6) . ? C72 C77 1.414(6) . ? C73 C74 1.365(6) . ? C74 C75 1.380(5) . ? C75 C76 1.356(6) . ? C75 C81 1.467(7) 3_455 ? C76 C77 1.360(6) . ? C79 O14 1.246(5) . ? C79 O13 1.256(6) . ? C79 C80 1.515(6) 8_455 ? C80 C79 1.515(6) 8_556 ? C81 O15 1.262(6) . ? C81 O24 1.314(5) . ? C81 C75 1.467(7) 3_545 ? O1 Co5 2.052(4) . ? O2 Co1 2.050(3) . ? O3 Co5 2.026(3) . ? O4 Co1 2.075(3) . ? O5 Co1 2.145(3) . ? O5 Co5 2.159(2) . ? O6 Co5 2.159(3) . ? O7 Co6 2.082(3) . ? O8 Co3 2.034(3) . ? O9 Co2 2.146(3) . ? O10 Co4 2.125(4) . ? O10 Co2 2.154(2) . ? O11 Co4 2.047(3) 6_556 ? O12 Co2 2.045(4) 6_556 ? O13 Co2 2.021(3) . ? O14 Co4 2.069(3) . ? O15 Co3 2.241(3) . ? O16 Co6 2.017(4) . ? O17 Co2 2.080(3) . ? O18 Co6 2.091(3) . ? O19 Co3 2.066(3) . ? O20 Co4 2.129(3) . ? O21 Co3 2.038(4) . ? O22 Co4 2.107(3) . ? O23 Co6 2.185(4) . ? O24 Co6 2.076(3) . ? O24 Co3 2.147(3) . ? O25 Co3 2.105(3) . ? O26 Co5 2.089(3) . ? O28 Co5 2.112(4) . ? O29 Co4 2.110(4) . ? O30 Co6 2.071(4) . ? O31 Co2 2.095(5) . ? Co1 O2 2.050(3) 2_755 ? Co1 O4 2.075(3) 2_755 ? Co1 O5 2.145(3) 2_755 ? Co2 O12 2.045(4) 6 ? Co4 O11 2.047(3) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 126.9(4) . . ? O1 C1 C5 115.2(4) . . ? O2 C1 C5 117.9(5) . . ? C67 C2 C68 121.6(4) 8_556 8_556 ? C67 C2 C4 124.9(4) 8_556 . ? C68 C2 C4 113.2(5) 8_556 . ? C8 C3 C5 119.1(4) . . ? O16 C4 O19 126.3(4) . . ? O16 C4 C2 119.5(4) . . ? O19 C4 C2 114.2(6) . . ? C6 C5 C3 121.3(4) . . ? C6 C5 C1 120.0(4) . . ? C3 C5 C1 118.8(4) . . ? C5 C6 C7 118.3(4) . . ? C9 C7 C6 121.4(4) . . ? C3 C8 C9 120.4(4) . . ? C7 C9 C8 119.5(4) . . ? C7 C9 C10 121.3(4) . . ? C8 C9 C10 119.2(4) . . ? C15 C10 C11 120.1(4) . . ? C15 C10 C9 120.1(3) . . ? C11 C10 C9 119.8(4) . . ? C10 C11 C12 118.8(4) . . ? C13 C12 C11 118.8(3) . . ? C13 C12 C23 121.5(4) . . ? C11 C12 C23 119.7(4) . . ? C12 C13 C14 122.3(4) . . ? C15 C14 C13 118.9(4) . . ? C15 C14 C16 121.2(3) . . ? C13 C14 C16 119.9(4) . . ? C14 C15 C10 121.2(4) . . ? C17 C16 C18 118.9(5) . . ? C17 C16 C14 121.8(3) . . ? C18 C16 C14 119.3(4) . . ? C16 C17 C19 121.7(4) . . ? C20 C18 C16 120.4(4) . . ? C17 C19 C21 119.9(4) . . ? C21 C20 C18 120.8(3) . . ? C20 C21 C19 118.1(5) . . ? C20 C21 C22 122.0(4) . . ? C19 C21 C22 119.7(4) . . ? O12 C22 O11 123.3(5) . . ? O12 C22 C21 119.7(4) . . ? O11 C22 C21 116.9(5) . . ? C26 C23 C24 118.3(4) . . ? C26 C23 C12 121.4(5) . . ? C24 C23 C12 120.3(4) . . ? C23 C24 C25 123.5(4) . . ? C24 C25 C27 116.2(5) . . ? C23 C26 C28 120.2(5) . . ? C28 C27 C25 120.3(4) . . ? C28 C27 C29 122.2(4) . . ? C25 C27 C29 117.5(5) . . ? C27 C28 C26 121.3(4) . . ? O10 C29 O9 119.9(4) . . ? O10 C29 C27 122.9(5) . . ? O9 C29 C27 117.1(6) . . ? O10 C29 Co2 60.2(2) . . ? O9 C29 Co2 59.8(2) . . ? C27 C29 Co2 176.9(5) . . ? O6 C30 O5 120.4(3) . . ? O6 C30 C31 118.6(5) . . ? O5 C30 C31 120.9(4) . . ? O6 C30 Co5 60.24(19) . . ? O5 C30 Co5 60.23(19) . . ? C31 C30 Co5 174.8(3) . . ? C34 C31 C32 121.2(3) . . ? C34 C31 C30 117.8(5) . . ? C32 C31 C30 120.6(4) . . ? C31 C32 C33 119.4(4) . . ? C36 C33 C32 119.4(4) . . ? C31 C34 C35 119.2(4) . . ? C36 C35 C34 120.3(4) . . ? C35 C36 C33 120.3(3) . . ? C35 C36 C37 121.4(4) . . ? C33 C36 C37 118.2(4) . . ? C40 C37 C38 120.8(3) . . ? C40 C37 C36 121.0(4) . . ? C38 C37 C36 118.2(4) . . ? C37 C38 C39 119.8(4) . . ? C47 C39 C38 118.7(4) . . ? C47 C39 C43 121.8(3) . . ? C38 C39 C43 119.4(4) . . ? C37 C40 C46 120.0(4) . . ? C43 C41 C44 121.7(4) . . ? C45 C42 C43 119.7(5) . . ? C41 C43 C42 119.0(4) . . ? C41 C43 C39 123.4(4) . . ? C42 C43 C39 117.5(4) . . ? C80 C44 C41 120.5(5) . . ? C42 C45 C80 120.1(4) . . ? C47 C46 C40 118.1(4) . . ? C47 C46 C48 121.2(3) . . ? C40 C46 C48 120.7(4) . . ? C39 C47 C46 122.5(3) . . ? C50 C48 C49 116.6(4) . . ? C50 C48 C46 123.7(4) . . ? C49 C48 C46 119.6(4) . . ? C53 C49 C48 120.4(4) . . ? C51 C50 C48 122.0(4) . . ? C50 C51 C52 121.4(4) . . ? C53 C52 C51 118.0(4) . . ? C53 C52 C54 120.3(4) . . ? C51 C52 C54 121.6(4) . . ? C52 C53 C49 121.5(4) . . ? O7 C54 O8 124.9(4) . . ? O7 C54 C52 117.8(4) . . ? O8 C54 C52 117.3(3) . . ? C57 C55 C78 119.1(4) . . ? C57 C55 C56 120.6(5) . . ? C78 C55 C56 120.1(4) . . ? O3 C56 O4 128.3(4) . . ? O3 C56 C55 116.9(4) . . ? O4 C56 C55 114.8(5) . . ? C58 C57 C55 119.3(5) . . ? C60 C58 C57 122.6(4) . . ? C78 C59 C60 119.0(5) . . ? C58 C60 C59 118.7(4) . . ? C58 C60 C61 124.1(3) . . ? C59 C60 C61 117.0(4) . . ? C69 C61 C62 118.7(4) . . ? C69 C61 C60 120.1(4) . . ? C62 C61 C60 121.2(5) . . ? C63 C62 C61 120.1(5) . . ? C70 C63 C62 120.2(4) . . ? C70 C63 C64 119.5(4) . . ? C62 C63 C64 120.2(5) . . ? C65 C64 C66 118.3(4) . . ? C65 C64 C63 121.0(4) . . ? C66 C64 C63 120.7(5) . . ? C64 C65 C68 124.4(4) . . ? C64 C66 C67 118.7(5) . . ? C2 C67 C66 122.1(4) 8_455 . ? C65 C68 C2 114.7(5) . 8_455 ? C61 C69 C71 122.5(4) . . ? C63 C70 C71 122.0(4) . . ? C70 C71 C69 116.4(5) . . ? C70 C71 C72 123.4(4) . . ? C69 C71 C72 120.1(4) . . ? C73 C72 C77 117.3(5) . . ? C73 C72 C71 122.8(3) . . ? C77 C72 C71 119.8(4) . . ? C74 C73 C72 120.7(3) . . ? C73 C74 C75 121.3(4) . . ? C76 C75 C74 118.2(5) . . ? C76 C75 C81 121.3(3) . 3_455 ? C74 C75 C81 120.5(4) . 3_455 ? C75 C76 C77 122.6(3) . . ? C76 C77 C72 119.8(4) . . ? C59 C78 C55 121.1(4) . . ? O14 C79 O13 126.7(4) . . ? O14 C79 C80 116.1(5) . 8_455 ? O13 C79 C80 117.3(4) . 8_455 ? C44 C80 C45 119.1(4) . . ? C44 C80 C79 121.8(5) . 8_556 ? C45 C80 C79 119.1(4) . 8_556 ? O15 C81 O24 118.2(5) . . ? O15 C81 C75 122.7(4) . 3_545 ? O24 C81 C75 119.1(4) . 3_545 ? C1 O1 Co5 131.3(3) . . ? C1 O2 Co1 137.0(3) . . ? C56 O3 Co5 124.8(3) . . ? C56 O4 Co1 136.6(3) . . ? C30 O5 Co1 141.4(3) . . ? C30 O5 Co5 89.0(2) . . ? Co1 O5 Co5 111.49(10) . . ? C30 O6 Co5 89.2(3) . . ? C54 O7 Co6 138.7(3) . . ? C54 O8 Co3 126.5(2) . . ? C29 O9 Co2 89.5(3) . . ? C29 O10 Co4 147.0(3) . . ? C29 O10 Co2 90.0(3) . . ? Co4 O10 Co2 106.88(14) . . ? C22 O11 Co4 132.8(3) . 6_556 ? C22 O12 Co2 120.7(3) . 6_556 ? C79 O13 Co2 123.4(3) . . ? C79 O14 Co4 140.4(3) . . ? C81 O15 Co3 89.3(2) . . ? C4 O16 Co6 130.0(3) . . ? C4 O19 Co3 118.5(3) . . ? C81 O24 Co6 143.7(3) . . ? C81 O24 Co3 92.1(3) . . ? Co6 O24 Co3 109.06(12) . . ? O2 Co1 O2 90.53(14) . 2_755 ? O2 Co1 O4 177.05(11) . 2_755 ? O2 Co1 O4 90.95(10) 2_755 2_755 ? O2 Co1 O4 90.95(10) . . ? O2 Co1 O4 177.05(11) 2_755 . ? O4 Co1 O4 87.69(15) 2_755 . ? O2 Co1 O5 93.06(11) . . ? O2 Co1 O5 90.33(11) 2_755 . ? O4 Co1 O5 89.49(11) 2_755 . ? O4 Co1 O5 87.04(11) . . ? O2 Co1 O5 90.33(11) . 2_755 ? O2 Co1 O5 93.06(11) 2_755 2_755 ? O4 Co1 O5 87.04(11) 2_755 2_755 ? O4 Co1 O5 89.49(11) . 2_755 ? O5 Co1 O5 175.18(15) . 2_755 ? O13 Co2 O12 93.44(14) . 6 ? O13 Co2 O17 95.13(12) . . ? O12 Co2 O17 93.98(15) 6 . ? O13 Co2 O31 177.37(15) . . ? O12 Co2 O31 85.3(2) 6 . ? O17 Co2 O31 82.7(2) . . ? O13 Co2 O9 91.08(12) . . ? O12 Co2 O9 163.53(12) 6 . ? O17 Co2 O9 101.39(15) . . ? O31 Co2 O9 90.79(18) . . ? O13 Co2 O10 93.85(11) . . ? O12 Co2 O10 103.36(14) 6 . ? O17 Co2 O10 159.94(16) . . ? O31 Co2 O10 88.68(18) . . ? O9 Co2 O10 60.50(13) . . ? O13 Co2 C29 91.78(13) . . ? O12 Co2 C29 133.18(17) 6 . ? O17 Co2 C29 131.80(19) . . ? O31 Co2 C29 90.77(16) . . ? O9 Co2 C29 30.70(16) . . ? O10 Co2 C29 29.83(14) . . ? O8 Co3 O21 93.13(13) . . ? O8 Co3 O19 91.56(12) . . ? O21 Co3 O19 94.47(14) . . ? O8 Co3 O25 177.49(12) . . ? O21 Co3 O25 86.66(15) . . ? O19 Co3 O25 90.94(12) . . ? O8 Co3 O24 92.59(12) . . ? O21 Co3 O24 157.69(12) . . ? O19 Co3 O24 106.90(11) . . ? O25 Co3 O24 86.69(14) . . ? O8 Co3 O15 88.68(11) . . ? O21 Co3 O15 98.15(13) . . ? O19 Co3 O15 167.34(13) . . ? O25 Co3 O15 88.87(12) . . ? O24 Co3 O15 60.45(10) . . ? O11 Co4 O14 99.53(11) 6 . ? O11 Co4 O22 174.35(13) 6 . ? O14 Co4 O22 85.82(13) . . ? O11 Co4 O29 88.15(15) 6 . ? O14 Co4 O29 89.52(13) . . ? O22 Co4 O29 90.11(17) . . ? O11 Co4 O10 88.13(14) 6 . ? O14 Co4 O10 90.40(12) . . ? O22 Co4 O10 93.67(16) . . ? O29 Co4 O10 176.21(13) . . ? O11 Co4 O20 85.23(12) 6 . ? O14 Co4 O20 175.21(13) . . ? O22 Co4 O20 89.40(14) . . ? O29 Co4 O20 90.13(14) . . ? O10 Co4 O20 90.27(13) . . ? O3 Co5 O1 90.17(13) . . ? O3 Co5 O26 93.69(14) . . ? O1 Co5 O26 90.14(15) . . ? O3 Co5 O28 91.72(15) . . ? O1 Co5 O28 177.10(18) . . ? O26 Co5 O28 87.56(16) . . ? O3 Co5 O5 104.58(13) . . ? O1 Co5 O5 91.39(11) . . ? O26 Co5 O5 161.66(13) . . ? O28 Co5 O5 90.25(12) . . ? O3 Co5 O6 165.89(14) . . ? O1 Co5 O6 90.27(12) . . ? O26 Co5 O6 100.41(14) . . ? O28 Co5 O6 88.42(13) . . ? O5 Co5 O6 61.31(11) . . ? O3 Co5 C30 135.33(17) . . ? O1 Co5 C30 91.81(12) . . ? O26 Co5 C30 130.91(17) . . ? O28 Co5 C30 88.37(13) . . ? O5 Co5 C30 30.77(14) . . ? O6 Co5 C30 30.57(15) . . ? O16 Co6 O30 177.57(15) . . ? O16 Co6 O24 85.86(13) . . ? O30 Co6 O24 94.66(14) . . ? O16 Co6 O7 94.67(15) . . ? O30 Co6 O7 87.70(15) . . ? O24 Co6 O7 90.76(11) . . ? O16 Co6 O18 86.95(15) . . ? O30 Co6 O18 90.66(16) . . ? O24 Co6 O18 91.42(12) . . ? O7 Co6 O18 177.37(15) . . ? O16 Co6 O23 89.63(16) . . ? O30 Co6 O23 90.01(17) . . ? O24 Co6 O23 174.02(16) . . ? O7 Co6 O23 85.69(15) . . ? O18 Co6 O23 92.26(16) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.988 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.063 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.001 -0.009 0.000 41666.7 9499.1 _platon_squeeze_details ; ; # Attachment '- MOF-39-Co-CCDC-80202.cif' data_rg-68-ds1 _database_code_depnum_ccdc_archive 'CCDC 801202' #TrackingRef '- MOF-39-Co-CCDC-80202.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common Co3O(H2btb)2(H2O) _chemical_formula_moiety 'C54 H30 Co3 O14' _chemical_formula_sum 'C54 H30 Co3 O14' _chemical_properties_physical moisture-sensitive _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour violet _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100 _chemical_formula_weight 1079.57 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_int_tables_number 62 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.551(4) _cell_length_b 25.356(5) _cell_length_c 21.148(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9411(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3199 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 31.00 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56458 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 31.00 _reflns_number_total 7076 _reflns_number_gt 6506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement XDS _computing_data_reduction XDSCONV _computing_structure_solution 'SUPERFLIP (Palatinus, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.1687P)^2^+5.1686P] 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_number_reflns 7076 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2266 _refine_ls_wR_factor_gt 0.2221 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.007 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 Co01 Co 0.61277(3) 0.7500 0.66324(2) 0.0191(2) Uani 1 2 d S . . Co02 Co 0.50325(2) 0.680786(16) 0.56379(2) 0.0289(2) Uani 1 1 d . . . O7 O 0.60643(14) 0.66042(10) 0.53421(12) 0.0449(6) Uani 1 1 d . . . O4 O 0.51577(17) 0.7500 0.60699(14) 0.0262(6) Uani 1 2 d S . . O8 O 0.56122(14) 0.69148(8) 0.71655(9) 0.0365(5) Uani 1 1 d . . . O5 O 0.70046(19) 0.7500 0.73070(14) 0.0372(7) Uani 1 2 d S . . O9 O 0.50030(15) 0.63924(11) 0.64716(12) 0.0519(8) Uani 1 1 d . . . C008 C 0.0793(2) 0.57067(15) 0.45540(18) 0.0461(9) Uani 1 1 d . . . O6 O 0.67289(14) 0.69265(10) 0.61533(11) 0.0450(6) Uani 1 1 d . . . C010 C 0.3778(3) 0.64880(19) 0.53052(17) 0.0546(11) Uani 1 1 d . . . C011 C 0.56250(19) 0.61051(13) 0.80516(16) 0.0384(8) Uani 1 1 d . . . H011 H 0.5970 0.6379 0.8108 0.046 Uiso 1 1 calc R . . C012 C 1.00298(19) 0.51048(16) 0.39270(19) 0.0447(10) Uani 1 1 d . . . C013 C 0.0734(2) 0.53087(16) 0.41032(19) 0.0498(10) Uani 1 1 d . . . H013 H 0.1174 0.5177 0.3916 0.060 Uiso 1 1 calc R . . C014 C 0.5180(2) 0.60907(13) 0.75080(17) 0.0389(8) Uani 1 1 d . . . C015 C 0.8022(2) 0.59229(17) 0.4589(2) 0.0593(12) Uani 1 1 d . . . H015 H 0.8010 0.5760 0.4195 0.071 Uiso 1 1 calc R . . C016 C 0.1557(2) 0.59005(16) 0.47470(19) 0.0530(10) Uani 1 1 d . . . C017 C 0.2999(2) 0.62656(19) 0.51103(19) 0.0576(11) Uani 1 1 d . . . C018 C 0.5036(2) 0.53185(15) 0.84510(19) 0.0440(10) Uani 1 1 d . . . C019 C 1.0130(2) 0.59107(16) 0.4819(2) 0.0473(10) Uani 1 1 d . . . H019 H 1.0165 0.6184 0.5111 0.057 Uiso 1 1 calc R . . C020 C 0.7370(2) 0.63982(13) 0.54094(16) 0.0386(8) Uani 1 1 d . . . C021 C 0.4585(2) 0.52969(15) 0.78945(19) 0.0510(10) Uani 1 1 d . . . H021 H 0.4240 0.5022 0.7836 0.061 Uiso 1 1 calc R . . C022 C 0.8707(2) 0.59423(14) 0.49270(18) 0.0440(9) Uani 1 1 d . . . C023 C 0.5273(2) 0.65010(12) 0.70043(15) 0.0345(7) Uani 1 1 d . . . O3 O 0.37920(19) 0.68598(12) 0.56513(17) 0.0649(9) Uani 1 1 d . . . C025 C 0.4658(2) 0.56853(14) 0.74389(18) 0.0465(9) Uani 1 1 d . . . H025 H 0.4351 0.5674 0.7080 0.056 Uiso 1 1 calc R . . C026 C 0.7358(2) 0.61442(17) 0.48351(19) 0.0532(11) Uani 1 1 d . . . H026 H 0.6904 0.6120 0.4610 0.064 Uiso 1 1 calc R . . C027 C 0.5563(2) 0.57196(14) 0.85085(17) 0.0425(8) Uani 1 1 d . . . H027 H 0.5880 0.5730 0.8860 0.051 Uiso 1 1 calc R . . C028 C 0.6658(2) 0.66609(13) 0.56625(14) 0.0333(8) Uani 1 1 d . . . C029 C 0.9413(2) 0.57136(15) 0.46556(19) 0.0454(9) Uani 1 1 d . . . C030 C 0.8707(2) 0.61905(16) 0.55119(18) 0.0479(10) Uani 1 1 d . . . H030 H 0.9154 0.6203 0.5747 0.057 Uiso 1 1 calc R . . C031 C 0.8050(2) 0.64209(15) 0.57507(17) 0.0458(9) Uani 1 1 d . . . H031 H 0.8063 0.6591 0.6140 0.055 Uiso 1 1 calc R . . C033 C 0.2367(3) 0.65651(18) 0.5179(3) 0.0680(13) Uani 1 1 d . . . H033 H 0.2409 0.6896 0.5365 0.082 Uiso 1 1 calc R . . C035 C 0.9371(2) 0.53058(15) 0.42172(19) 0.0462(9) Uani 1 1 d . . . H035 H 0.8899 0.5164 0.4114 0.055 Uiso 1 1 calc R . . O1 O 0.4351(2) 0.6249(2) 0.51169(18) 0.1037(16) Uani 1 1 d . . . C037 C 0.1677(2) 0.63973(18) 0.4985(3) 0.0694(14) Uani 1 1 d . . . H037 H 0.1266 0.6627 0.5014 0.083 Uiso 1 1 calc R . . C038 C 0.2178(3) 0.5552(2) 0.4759(3) 0.099(2) Uani 1 1 d . . . H038 H 0.2109 0.5196 0.4667 0.119 Uiso 1 1 calc R . . C039 C 0.2883(3) 0.5739(3) 0.4907(3) 0.109(3) Uani 1 1 d . . . H039 H 0.3301 0.5514 0.4874 0.131 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 Co01 0.0144(4) 0.0197(3) 0.0232(3) 0.000 -0.00023(18) 0.000 Co02 0.0152(4) 0.0312(3) 0.0403(3) -0.00674(15) -0.00097(15) -0.00391(14) O7 0.0205(16) 0.0591(15) 0.0552(14) -0.0222(12) -0.0066(11) 0.0120(11) O4 0.0141(17) 0.0218(13) 0.0428(16) 0.000 -0.0073(12) 0.000 O8 0.0441(16) 0.0315(11) 0.0339(11) 0.0085(9) -0.0010(9) -0.0094(10) O5 0.027(2) 0.0450(17) 0.0392(16) 0.000 -0.0078(13) 0.000 O9 0.060(2) 0.0454(14) 0.0505(15) 0.0179(12) -0.0233(12) -0.0273(12) C008 0.020(2) 0.055(2) 0.064(2) -0.0327(18) -0.0061(16) -0.0043(15) O6 0.0235(16) 0.0659(15) 0.0456(13) -0.0262(12) -0.0090(10) 0.0198(11) C010 0.039(3) 0.087(3) 0.0379(18) -0.0033(19) 0.0016(16) 0.018(2) C011 0.020(2) 0.0432(17) 0.0522(19) 0.0196(15) -0.0023(13) -0.0101(13) C012 0.017(3) 0.051(2) 0.066(2) -0.0325(19) 0.0024(14) -0.0029(13) C013 0.019(2) 0.059(2) 0.072(2) -0.0384(19) 0.0047(16) 0.0032(15) C014 0.029(2) 0.0370(17) 0.0506(19) 0.0178(14) -0.0077(15) -0.0065(14) C015 0.034(3) 0.077(3) 0.067(2) -0.051(2) -0.0058(18) 0.0079(19) C016 0.029(3) 0.064(2) 0.066(2) -0.038(2) -0.0025(17) -0.0020(17) C017 0.021(3) 0.090(3) 0.062(2) -0.031(2) 0.0009(16) -0.018(2) C018 0.019(2) 0.048(2) 0.066(2) 0.0324(18) -0.0083(14) -0.0053(14) C019 0.019(2) 0.055(2) 0.068(2) -0.0380(19) -0.0019(16) 0.0013(15) C020 0.021(2) 0.0445(18) 0.0502(19) -0.0194(15) -0.0016(14) 0.0052(13) C021 0.019(2) 0.054(2) 0.081(3) 0.0345(19) -0.0134(17) -0.0171(15) C022 0.018(2) 0.051(2) 0.062(2) -0.0305(17) -0.0064(15) 0.0019(15) C023 0.024(2) 0.0350(16) 0.0449(17) 0.0154(13) -0.0043(14) -0.0078(13) O3 0.028(2) 0.0568(18) 0.110(3) -0.0229(17) -0.0167(14) -0.0114(12) C025 0.030(2) 0.0479(19) 0.062(2) 0.0269(17) -0.0150(16) -0.0134(15) C026 0.022(3) 0.076(3) 0.062(2) -0.036(2) -0.0069(16) 0.0105(17) C027 0.018(2) 0.054(2) 0.0559(19) 0.0263(16) -0.0073(14) -0.0036(14) C028 0.021(2) 0.0347(16) 0.0441(17) -0.0105(13) -0.0011(13) 0.0030(13) C029 0.017(2) 0.053(2) 0.066(2) -0.0357(18) -0.0013(15) 0.0021(15) C030 0.021(2) 0.063(2) 0.060(2) -0.0313(18) -0.0078(15) 0.0090(16) C031 0.028(2) 0.059(2) 0.0505(19) -0.0236(16) -0.0060(15) 0.0106(16) C033 0.036(3) 0.056(2) 0.112(4) -0.031(2) -0.017(2) -0.0053(19) C035 0.016(2) 0.053(2) 0.070(2) -0.0373(18) 0.0023(15) -0.0036(15) O1 0.043(3) 0.167(4) 0.101(3) -0.088(3) -0.0197(18) 0.006(2) C037 0.021(3) 0.065(3) 0.122(4) -0.054(3) -0.010(2) -0.0060(18) C038 0.029(3) 0.106(4) 0.162(6) -0.088(4) -0.012(3) 0.010(3) C039 0.030(4) 0.143(6) 0.156(6) -0.101(5) -0.011(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co01 O6 2.063(2) 8_575 ? Co01 O6 2.063(2) . ? Co01 O8 2.072(2) 8_575 ? Co01 O8 2.072(2) . ? Co01 O4 2.077(3) . ? Co01 O5 2.098(3) . ? Co02 O7 1.984(2) . ? Co02 O4 1.9907(14) . ? Co02 O9 2.054(2) . ? Co02 O1 2.158(3) . ? Co02 O3 2.182(3) . ? Co02 C010 2.449(5) . ? O7 C028 1.251(4) . ? O4 Co02 1.9907(14) 8_575 ? O8 C023 1.254(4) . ? O9 C023 1.253(4) . ? C008 C019 1.391(5) 1_455 ? C008 C013 1.392(5) . ? C008 C016 1.485(5) . ? O6 C028 1.244(4) . ? C010 O3 1.194(5) . ? C010 O1 1.239(5) . ? C010 C017 1.536(6) . ? C011 C027 1.379(5) . ? C011 C014 1.390(5) . ? C012 C013 1.390(5) 1_655 ? C012 C035 1.404(5) . ? C012 C018 1.476(5) 2_664 ? C013 C012 1.390(5) 1_455 ? C014 C025 1.385(5) . ? C014 C023 1.498(4) . ? C015 C026 1.395(5) . ? C015 C022 1.399(5) . ? C016 C037 1.373(5) . ? C016 C038 1.404(7) . ? C017 C033 1.352(6) . ? C017 C039 1.419(7) . ? C018 C027 1.380(5) . ? C018 C021 1.420(5) . ? C018 C012 1.476(5) 2_665 ? C019 C008 1.391(5) 1_655 ? C019 C029 1.397(5) . ? C020 C026 1.375(5) . ? C020 C031 1.396(5) . ? C020 C028 1.514(5) . ? C021 C025 1.384(5) . ? C022 C030 1.388(5) . ? C022 C029 1.484(5) . ? C029 C035 1.391(5) . ? C030 C031 1.388(5) . ? C033 C037 1.347(6) . ? C038 C039 1.361(7) . ? 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 O6 Co01 O6 89.66(17) 8_575 . ? O6 Co01 O8 89.18(11) 8_575 8_575 ? O6 Co01 O8 174.71(9) . 8_575 ? O6 Co01 O8 174.71(9) 8_575 . ? O6 Co01 O8 89.18(11) . . ? O8 Co01 O8 91.51(13) 8_575 . ? O6 Co01 O4 97.93(9) 8_575 . ? O6 Co01 O4 97.93(9) . . ? O8 Co01 O4 87.35(9) 8_575 . ? O8 Co01 O4 87.35(9) . . ? O6 Co01 O5 87.64(9) 8_575 . ? O6 Co01 O5 87.64(9) . . ? O8 Co01 O5 87.16(9) 8_575 . ? O8 Co01 O5 87.16(9) . . ? O4 Co01 O5 172.12(12) . . ? O7 Co02 O4 105.87(11) . . ? O7 Co02 O9 99.21(12) . . ? O4 Co02 O9 93.50(11) . . ? O7 Co02 O1 100.03(12) . . ? O4 Co02 O1 151.02(14) . . ? O9 Co02 O1 95.00(16) . . ? O7 Co02 O3 158.54(11) . . ? O4 Co02 O3 92.92(11) . . ? O9 Co02 O3 89.69(12) . . ? O1 Co02 O3 59.52(13) . . ? O7 Co02 C010 130.06(12) . . ? O4 Co02 C010 121.53(13) . . ? O9 Co02 C010 93.09(12) . . ? O1 Co02 C010 30.38(13) . . ? O3 Co02 C010 29.15(12) . . ? C028 O7 Co02 124.0(2) . . ? Co02 O4 Co02 123.68(15) 8_575 . ? Co02 O4 Co01 110.69(9) 8_575 . ? Co02 O4 Co01 110.69(9) . . ? C023 O8 Co01 131.22(19) . . ? C023 O9 Co02 130.5(2) . . ? C019 C008 C013 118.9(3) 1_455 . ? C019 C008 C016 121.4(3) 1_455 . ? C013 C008 C016 119.7(3) . . ? C028 O6 Co01 137.8(2) . . ? O3 C010 O1 124.5(4) . . ? O3 C010 C017 118.2(4) . . ? O1 C010 C017 117.1(4) . . ? O3 C010 Co02 62.9(3) . . ? O1 C010 Co02 61.7(2) . . ? C017 C010 Co02 177.6(3) . . ? C027 C011 C014 121.1(3) . . ? C013 C012 C035 118.6(3) 1_655 . ? C013 C012 C018 121.5(3) 1_655 2_664 ? C035 C012 C018 119.8(3) . 2_664 ? C012 C013 C008 121.3(3) 1_455 . ? C025 C014 C011 118.6(3) . . ? C025 C014 C023 120.8(3) . . ? C011 C014 C023 120.6(3) . . ? C026 C015 C022 120.9(3) . . ? C037 C016 C038 116.9(4) . . ? C037 C016 C008 122.9(4) . . ? C038 C016 C008 119.8(4) . . ? C033 C017 C039 116.4(4) . . ? C033 C017 C010 119.7(4) . . ? C039 C017 C010 123.7(4) . . ? C027 C018 C021 118.4(3) . . ? C027 C018 C012 121.9(3) . 2_665 ? C021 C018 C012 119.6(3) . 2_665 ? C008 C019 C029 121.3(3) 1_655 . ? C026 C020 C031 119.3(3) . . ? C026 C020 C028 120.3(3) . . ? C031 C020 C028 120.3(3) . . ? C025 C021 C018 119.9(3) . . ? C030 C022 C015 118.1(3) . . ? C030 C022 C029 121.5(3) . . ? C015 C022 C029 120.4(3) . . ? O9 C023 O8 127.5(3) . . ? O9 C023 C014 116.5(3) . . ? O8 C023 C014 116.1(3) . . ? C010 O3 Co02 88.0(3) . . ? C021 C025 C014 121.1(3) . . ? C020 C026 C015 120.3(3) . . ? C011 C027 C018 120.9(3) . . ? O6 C028 O7 126.7(3) . . ? O6 C028 C020 116.8(3) . . ? O7 C028 C020 116.5(3) . . ? C035 C029 C019 118.6(3) . . ? C035 C029 C022 120.3(3) . . ? C019 C029 C022 121.1(3) . . ? C022 C030 C031 121.0(3) . . ? C030 C031 C020 120.3(3) . . ? C037 C033 C017 121.8(4) . . ? C029 C035 C012 121.2(3) . . ? C010 O1 Co02 87.9(3) . . ? C033 C037 C016 122.6(4) . . ? C039 C038 C016 119.4(5) . . ? C038 C039 C017 121.8(5) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 1.676 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.133 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.000 -0.002 5741 1739 ' ' _platon_squeeze_details ; ;