data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hongbin Du' _publ_contact_author_email HBDU@NJU.EDU.CN _publ_section_title ; A 3-dimensional highly porous coordination polymer with a fluorite structure constructed from a semi-rigid tetrahedral ligand ; loop_ _publ_author_name 'Hongbin Du.' 'Yi-Zhi Li.' 'Li-Li Liang.' 'Shi-Bin Ren.' 'Jun Wang.' ; Xiao-Zeng You ; 'Jun Zhang.' # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 765419' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H50 Co3 O24' _chemical_formula_sum 'C66 H50 Co3 O24' _chemical_formula_weight 1403.85 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.036(3) _cell_length_b 15.301(4) _cell_length_c 16.906(5) _cell_angle_alpha 108.300(5) _cell_angle_beta 101.394(4) _cell_angle_gamma 102.280(5) _cell_volume 2768.6(13) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1172 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 18.302 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 719 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9081 _exptl_absorpt_correction_T_max 0.9168 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; The final structural model was refined without the guest molecules by using the SQUEEZE option of PLATON. The identity and number of the guest molecules were determined from the IR spectra, elemental analyses, and TGA data. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15137 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10665 _reflns_number_gt 7878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.2200P] 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 10665 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0175(2) 0.9078(2) 0.62814(18) 0.0449(6) Uani 1 1 d . . . C2 C 0.9994(2) 0.8523(2) 0.68737(18) 0.0448(6) Uani 1 1 d . . . H2A H 0.9601 0.8823 0.7286 0.054 Uiso 1 1 calc R . . H2B H 0.9507 0.7864 0.6535 0.054 Uiso 1 1 calc R . . C3 C 1.1213(2) 0.8075(2) 0.78825(18) 0.0425(6) Uani 1 1 d . . . C4 C 1.2327(3) 0.8112(2) 0.8305(2) 0.0548(8) Uani 1 1 d . . . H4 H 1.2980 0.8462 0.8204 0.066 Uiso 1 1 calc R . . C5 C 1.2511(3) 0.7639(2) 0.88842(18) 0.0469(7) Uani 1 1 d . . . H5 H 1.3273 0.7665 0.9160 0.056 Uiso 1 1 calc R . . C6 C 1.1539(3) 0.7136(2) 0.90354(19) 0.0493(7) Uani 1 1 d . . . C7 C 1.0462(3) 0.7062(2) 0.86088(18) 0.0473(7) Uani 1 1 d . . . H7 H 0.9825 0.6669 0.8689 0.057 Uiso 1 1 calc R . . C8 C 1.0206(2) 0.7555(2) 0.80226(18) 0.0446(6) Uani 1 1 d . . . H8 H 0.9439 0.7529 0.7759 0.054 Uiso 1 1 calc R . . C9 C 1.1691(2) 0.6603(2) 0.96308(18) 0.0422(6) Uani 1 1 d . . . C10 C 0.8956(3) 0.9092(2) 0.58159(19) 0.0503(7) Uani 1 1 d . . . H10A H 0.8626 0.9471 0.6232 0.060 Uiso 1 1 calc R . . H10B H 0.9030 0.9382 0.5388 0.060 Uiso 1 1 calc R . . C11 C 0.7366(2) 0.7856(2) 0.46392(19) 0.0514(7) Uani 1 1 d . . . C12 C 0.6813(3) 0.6873(2) 0.4199(2) 0.0569(8) Uani 1 1 d . . . H12 H 0.7041 0.6455 0.4450 0.068 Uiso 1 1 calc R . . C13 C 0.5958(3) 0.6486(2) 0.3420(2) 0.0551(8) Uani 1 1 d . . . H13 H 0.5578 0.5827 0.3156 0.066 Uiso 1 1 calc R . . C14 C 0.5681(2) 0.7126(2) 0.30402(18) 0.0461(6) Uani 1 1 d . . . C15 C 0.6174(2) 0.8100(2) 0.34556(19) 0.0469(7) Uani 1 1 d . . . H15 H 0.5943 0.8513 0.3199 0.056 Uiso 1 1 calc R . . C16 C 0.7001(2) 0.8466(2) 0.42423(18) 0.0472(7) Uani 1 1 d . . . H16 H 0.7330 0.9129 0.4521 0.057 Uiso 1 1 calc R . . C17 C 0.4795(3) 0.6712(2) 0.21407(18) 0.0454(7) Uani 1 1 d . . . C18 C 1.0729(3) 0.8553(2) 0.56200(18) 0.0427(6) Uani 1 1 d . . . H18A H 1.1511 0.8569 0.5922 0.051 Uiso 1 1 calc R . . H18B H 1.0252 0.7884 0.5340 0.051 Uiso 1 1 calc R . . C19 C 1.0838(3) 0.8269(2) 0.42290(19) 0.0485(7) Uani 1 1 d . . . C20 C 0.9878(3) 0.7490(2) 0.3665(2) 0.0522(7) Uani 1 1 d . . . H20 H 0.9169 0.7367 0.3809 0.063 Uiso 1 1 calc R . . C21 C 0.9977(3) 0.6894(2) 0.2887(2) 0.0604(9) Uani 1 1 d . . . H21 H 0.9335 0.6372 0.2510 0.073 Uiso 1 1 calc R . . C22 C 1.1037(2) 0.70772(19) 0.26727(16) 0.0401(6) Uani 1 1 d . . . C23 C 1.1998(3) 0.7857(2) 0.3236(2) 0.0581(9) Uani 1 1 d . . . H23 H 1.2707 0.7980 0.3093 0.070 Uiso 1 1 calc R . . C24 C 1.1898(3) 0.8453(2) 0.4015(2) 0.0576(8) Uani 1 1 d . . . H24 H 1.2541 0.8975 0.4392 0.069 Uiso 1 1 calc R . . C25 C 1.1270(2) 0.64719(19) 0.18649(17) 0.0405(6) Uani 1 1 d . . . C26 C 1.0938(2) 1.00779(18) 0.68036(16) 0.0399(6) Uani 1 1 d . . . H26A H 1.1728 1.0075 0.7070 0.048 Uiso 1 1 calc R . . H26B H 1.1000 1.0448 0.6434 0.048 Uiso 1 1 calc R . . C27 C 1.0943(2) 1.1416(2) 0.80131(18) 0.0462(6) Uani 1 1 d . . . C28 C 1.0357(2) 1.1784(2) 0.86148(18) 0.0439(6) Uani 1 1 d . . . H28 H 0.9645 1.1397 0.8612 0.053 Uiso 1 1 calc R . . C29 C 1.0818(2) 1.27137(19) 0.92128(17) 0.0412(6) Uani 1 1 d . . . H29 H 1.0421 1.2948 0.9614 0.049 Uiso 1 1 calc R . . C30 C 1.1885(2) 1.3309(2) 0.92198(18) 0.0450(6) Uani 1 1 d . . . C31 C 1.2485(2) 1.2920(2) 0.86337(18) 0.0435(6) Uani 1 1 d . . . H31 H 1.3220 1.3291 0.8656 0.052 Uiso 1 1 calc R . . C32 C 1.1994(2) 1.1974(2) 0.80087(18) 0.0513(8) Uani 1 1 d . . . H32 H 1.2378 1.1733 0.7600 0.062 Uiso 1 1 calc R . . C33 C 1.2354(2) 1.43197(19) 0.98231(16) 0.0385(6) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 1.0000 0.03580(13) Uani 1 2 d S . . Co2 Co 0.29708(3) 0.60374(3) 0.08920(2) 0.04034(11) Uani 1 1 d . . . O1 O 1.11353(17) 0.85407(14) 0.73171(12) 0.0472(5) Uani 1 1 d . . . O2 O 1.07729(15) 0.61891(12) 0.97565(11) 0.0380(4) Uani 1 1 d . . . O3 O 1.27418(16) 0.66131(14) 0.99725(13) 0.0464(4) Uani 1 1 d . . . O4 O 0.81976(18) 0.81335(14) 0.54031(13) 0.0557(6) Uani 1 1 d . . . O5 O 0.42236(17) 0.58659(14) 0.18511(13) 0.0567(6) Uani 1 1 d . . . O6 O 0.46043(17) 0.72713(15) 0.17453(13) 0.0531(5) Uani 1 1 d . . . O7 O 1.08313(18) 0.89274(13) 0.49955(12) 0.0484(5) Uani 1 1 d . . . O8 O 1.22477(16) 0.66933(13) 0.17530(12) 0.0429(4) Uani 1 1 d . . . O9 O 1.03197(16) 0.57788(13) 0.12968(12) 0.0432(4) Uani 1 1 d . . . H9C H 0.9792 0.6027 0.1134 0.052 Uiso 1 1 d R . . O10 O 1.04186(17) 1.04955(14) 0.74549(13) 0.0514(5) Uani 1 1 d . . . O11 O 1.17123(15) 1.47088(12) 1.02658(12) 0.0403(4) Uani 1 1 d . . . O12 O 1.33779(16) 1.48089(13) 0.98965(12) 0.0445(4) 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 0.0470(15) 0.0436(15) 0.0388(15) 0.0112(12) 0.0104(12) 0.0108(12) C2 0.0421(15) 0.0506(16) 0.0387(14) 0.0151(12) 0.0101(12) 0.0113(12) C3 0.0434(14) 0.0452(15) 0.0426(15) 0.0174(12) 0.0170(12) 0.0141(12) C4 0.0497(17) 0.0513(17) 0.0557(18) 0.0229(14) -0.0042(14) 0.0129(14) C5 0.0541(17) 0.0468(16) 0.0448(16) 0.0217(13) 0.0127(13) 0.0189(13) C6 0.0539(17) 0.0400(15) 0.0409(15) 0.0130(12) -0.0007(13) 0.0038(13) C7 0.0497(16) 0.0494(16) 0.0398(15) 0.0174(13) 0.0123(13) 0.0077(13) C8 0.0418(15) 0.0499(16) 0.0471(16) 0.0246(13) 0.0166(12) 0.0097(12) C9 0.0433(15) 0.0436(15) 0.0398(15) 0.0143(12) 0.0134(12) 0.0132(12) C10 0.0470(16) 0.0509(16) 0.0394(15) 0.0091(13) 0.0000(12) 0.0104(13) C11 0.0408(15) 0.0507(17) 0.0455(16) 0.0119(13) -0.0075(12) 0.0069(13) C12 0.0568(18) 0.0494(17) 0.0517(18) 0.0195(14) -0.0057(14) 0.0084(14) C13 0.0512(17) 0.0496(17) 0.0473(17) 0.0116(13) -0.0084(14) 0.0107(14) C14 0.0428(15) 0.0415(15) 0.0421(15) 0.0034(12) 0.0047(12) 0.0139(12) C15 0.0470(16) 0.0492(16) 0.0453(16) 0.0183(13) 0.0137(13) 0.0142(13) C16 0.0476(16) 0.0400(15) 0.0448(16) 0.0093(12) 0.0072(13) 0.0099(12) C17 0.0477(16) 0.0405(15) 0.0377(15) -0.0009(12) 0.0099(12) 0.0178(13) C18 0.0501(16) 0.0426(14) 0.0418(15) 0.0175(12) 0.0194(12) 0.0180(12) C19 0.0564(17) 0.0496(16) 0.0449(16) 0.0189(13) 0.0222(14) 0.0173(14) C20 0.0466(16) 0.0482(16) 0.0618(19) 0.0107(14) 0.0281(14) 0.0172(13) C21 0.0487(17) 0.0548(18) 0.0533(19) -0.0137(14) 0.0134(14) 0.0188(14) C22 0.0437(14) 0.0441(14) 0.0318(13) 0.0100(11) 0.0070(11) 0.0214(12) C23 0.0521(17) 0.0474(17) 0.0503(18) -0.0167(13) 0.0146(14) 0.0187(14) C24 0.0514(17) 0.0446(16) 0.0584(19) -0.0087(14) 0.0165(15) 0.0193(14) C25 0.0427(15) 0.0416(14) 0.0349(14) 0.0105(11) 0.0083(11) 0.0161(12) C26 0.0395(14) 0.0411(14) 0.0288(13) 0.0036(11) 0.0066(11) 0.0083(11) C27 0.0411(14) 0.0436(15) 0.0420(15) 0.0044(12) 0.0111(12) 0.0072(12) C28 0.0433(15) 0.0462(15) 0.0424(15) 0.0143(12) 0.0158(12) 0.0136(12) C29 0.0442(15) 0.0388(14) 0.0407(15) 0.0111(11) 0.0161(12) 0.0142(12) C30 0.0389(14) 0.0498(16) 0.0402(15) 0.0067(12) 0.0103(11) 0.0173(12) C31 0.0405(14) 0.0432(15) 0.0440(15) 0.0120(12) 0.0129(12) 0.0121(12) C32 0.0428(15) 0.0545(17) 0.0344(14) -0.0099(12) 0.0168(12) 0.0050(13) C33 0.0453(15) 0.0420(14) 0.0293(13) 0.0152(11) 0.0080(11) 0.0147(12) Co1 0.0365(3) 0.0372(3) 0.0343(3) 0.0134(2) 0.0108(2) 0.0113(2) Co2 0.0410(2) 0.03581(19) 0.0394(2) 0.00937(15) 0.00882(16) 0.01126(15) O1 0.0468(11) 0.0509(11) 0.0451(11) 0.0219(9) 0.0104(9) 0.0133(9) O2 0.0383(9) 0.0399(10) 0.0369(10) 0.0146(8) 0.0113(8) 0.0126(8) O3 0.0395(10) 0.0486(11) 0.0513(11) 0.0207(9) 0.0087(9) 0.0139(9) O4 0.0527(12) 0.0444(11) 0.0509(12) 0.0177(9) -0.0187(9) 0.0074(9) O5 0.0443(11) 0.0477(12) 0.0455(11) -0.0118(9) -0.0107(9) 0.0146(9) O6 0.0428(11) 0.0606(13) 0.0406(11) 0.0112(10) -0.0003(9) 0.0077(9) O7 0.0600(12) 0.0418(10) 0.0427(11) 0.0132(9) 0.0159(9) 0.0160(9) O8 0.0417(10) 0.0396(10) 0.0411(10) 0.0087(8) 0.0100(8) 0.0106(8) O9 0.0425(10) 0.0458(10) 0.0431(11) 0.0142(9) 0.0172(8) 0.0153(8) O10 0.0440(11) 0.0432(11) 0.0443(11) -0.0087(9) 0.0131(9) 0.0050(8) O11 0.0391(9) 0.0360(9) 0.0399(10) 0.0086(8) 0.0077(8) 0.0107(8) O12 0.0398(10) 0.0414(10) 0.0389(10) 0.0031(8) 0.0059(8) 0.0079(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C26 1.483(4) . ? C1 C18 1.516(4) . ? C1 C2 1.520(4) . ? C1 C10 1.530(4) . ? C2 O1 1.420(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O1 1.360(3) . ? C3 C4 1.369(4) . ? C3 C8 1.407(4) . ? C4 C5 1.400(4) . ? C4 H4 0.9300 . ? C5 C6 1.373(4) . ? C5 H5 0.9300 . ? C6 C7 1.316(4) . ? C6 C9 1.489(4) . ? C7 C8 1.446(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O2 1.243(3) . ? C9 O3 1.277(3) . ? C10 O4 1.416(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O4 1.347(3) . ? C11 C12 1.391(4) . ? C11 C16 1.402(4) . ? C12 C13 1.364(4) . ? C12 H12 0.9300 . ? C13 C14 1.389(4) . ? C13 H13 0.9300 . ? C14 C15 1.367(4) . ? C14 C17 1.522(4) . ? C15 C16 1.359(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O5 1.216(3) . ? C17 O6 1.271(4) . ? C17 Co2 2.486(3) . ? C18 O7 1.364(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O7 1.372(3) . ? C19 C20 1.390(4) . ? C19 C24 1.390(4) . ? C20 C21 1.390(4) . ? C20 H20 0.9300 . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.390(4) . ? C22 C25 1.506(4) . ? C23 C24 1.390(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O8 1.223(3) . ? C25 O9 1.329(3) . ? C26 O10 1.418(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O10 1.350(3) . ? C27 C32 1.371(4) . ? C27 C28 1.394(4) . ? C28 C29 1.376(4) . ? C28 H28 0.9300 . ? C29 C30 1.404(4) . ? C29 H29 0.9300 . ? C30 C31 1.398(4) . ? C30 C33 1.470(4) . ? C31 C32 1.411(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O12 1.258(3) . ? C33 O11 1.286(3) . ? Co1 O9 2.0507(19) 2_766 ? Co1 O9 2.0507(19) 1_556 ? Co1 O2 2.0608(18) . ? Co1 O2 2.0608(18) 2_767 ? Co1 O11 2.1906(18) 2_777 ? Co1 O11 2.1906(18) 1_545 ? Co2 O8 1.9591(19) 1_455 ? Co2 O3 2.016(2) 1_454 ? Co2 O11 2.0623(18) 1_444 ? Co2 O5 2.107(2) . ? Co2 O6 2.259(2) . ? Co2 O12 2.3101(19) 1_444 ? O3 Co2 2.016(2) 1_656 ? O8 Co2 1.9591(19) 1_655 ? O9 Co1 2.0507(19) 1_554 ? O9 H9C 0.8500 . ? O11 Co2 2.0623(18) 1_666 ? O11 Co1 2.1906(18) 1_565 ? O12 Co2 2.3101(19) 1_666 ? 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 C26 C1 C18 111.3(2) . . ? C26 C1 C2 109.9(2) . . ? C18 C1 C2 108.4(2) . . ? C26 C1 C10 109.7(2) . . ? C18 C1 C10 109.7(2) . . ? C2 C1 C10 107.8(2) . . ? O1 C2 C1 106.9(2) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? O1 C3 C4 117.0(3) . . ? O1 C3 C8 122.6(3) . . ? C4 C3 C8 120.4(3) . . ? C3 C4 C5 121.9(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 118.4(3) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 C9 119.2(3) . . ? C5 C6 C9 120.3(3) . . ? C6 C7 C8 124.1(3) . . ? C6 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C3 C8 C7 114.6(3) . . ? C3 C8 H8 122.7 . . ? C7 C8 H8 122.7 . . ? O2 C9 O3 125.6(3) . . ? O2 C9 C6 116.6(3) . . ? O3 C9 C6 117.8(2) . . ? O4 C10 C1 108.9(2) . . ? O4 C10 H10A 109.9 . . ? C1 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C1 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O4 C11 C12 117.3(3) . . ? O4 C11 C16 126.1(3) . . ? C12 C11 C16 116.5(3) . . ? C13 C12 C11 123.9(3) . . ? C13 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C12 C13 C14 116.6(3) . . ? C12 C13 H13 121.7 . . ? C14 C13 H13 121.7 . . ? C15 C14 C13 121.7(3) . . ? C15 C14 C17 120.3(3) . . ? C13 C14 C17 118.0(3) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.9(3) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O5 C17 O6 121.8(3) . . ? O5 C17 C14 118.6(3) . . ? O6 C17 C14 119.4(2) . . ? O5 C17 Co2 57.86(15) . . ? O6 C17 Co2 64.77(15) . . ? C14 C17 Co2 165.2(2) . . ? O7 C18 C1 114.1(2) . . ? O7 C18 H18A 108.7 . . ? C1 C18 H18A 108.7 . . ? O7 C18 H18B 108.7 . . ? C1 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O7 C19 C20 125.2(3) . . ? O7 C19 C24 114.7(3) . . ? C20 C19 C24 120.0(3) . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 C25 114.8(2) . . ? C21 C22 C25 125.2(3) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? O8 C25 O9 126.0(2) . . ? O8 C25 C22 119.4(2) . . ? O9 C25 C22 114.3(2) . . ? O10 C26 C1 108.2(2) . . ? O10 C26 H26A 110.1 . . ? C1 C26 H26A 110.1 . . ? O10 C26 H26B 110.1 . . ? C1 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? O10 C27 C32 123.3(2) . . ? O10 C27 C28 116.2(2) . . ? C32 C27 C28 120.5(3) . . ? C29 C28 C27 120.8(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 118.4(3) . . ? C31 C30 C33 120.8(3) . . ? C29 C30 C33 120.8(2) . . ? C30 C31 C32 121.0(3) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 119.0(2) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? O12 C33 O11 120.0(2) . . ? O12 C33 C30 119.9(2) . . ? O11 C33 C30 120.1(2) . . ? O9 Co1 O9 180.000(1) 2_766 1_556 ? O9 Co1 O2 86.87(7) 2_766 . ? O9 Co1 O2 93.13(7) 1_556 . ? O9 Co1 O2 93.13(7) 2_766 2_767 ? O9 Co1 O2 86.87(7) 1_556 2_767 ? O2 Co1 O2 180.000(1) . 2_767 ? O9 Co1 O11 90.34(7) 2_766 2_777 ? O9 Co1 O11 89.66(7) 1_556 2_777 ? O2 Co1 O11 89.78(7) . 2_777 ? O2 Co1 O11 90.22(7) 2_767 2_777 ? O9 Co1 O11 89.66(7) 2_766 1_545 ? O9 Co1 O11 90.34(7) 1_556 1_545 ? O2 Co1 O11 90.22(7) . 1_545 ? O2 Co1 O11 89.78(7) 2_767 1_545 ? O11 Co1 O11 180.000(1) 2_777 1_545 ? O8 Co2 O3 104.93(8) 1_455 1_454 ? O8 Co2 O11 101.42(8) 1_455 1_444 ? O3 Co2 O11 100.89(8) 1_454 1_444 ? O8 Co2 O5 91.83(8) 1_455 . ? O3 Co2 O5 145.26(9) 1_454 . ? O11 Co2 O5 105.36(8) 1_444 . ? O8 Co2 O6 82.49(8) 1_455 . ? O3 Co2 O6 92.19(8) 1_454 . ? O11 Co2 O6 164.75(8) 1_444 . ? O5 Co2 O6 59.57(8) . . ? O8 Co2 O12 160.12(7) 1_455 1_444 ? O3 Co2 O12 87.17(8) 1_454 1_444 ? O11 Co2 O12 60.21(7) 1_444 1_444 ? O5 Co2 O12 86.51(7) . 1_444 ? O6 Co2 O12 113.27(7) . 1_444 ? O8 Co2 C17 83.93(8) 1_455 . ? O3 Co2 C17 121.52(9) 1_454 . ? O11 Co2 C17 134.54(9) 1_444 . ? O5 Co2 C17 29.25(9) . . ? O6 Co2 C17 30.59(8) . . ? O12 Co2 C17 103.39(8) 1_444 . ? C3 O1 C2 118.4(2) . . ? C9 O2 Co1 143.00(18) . . ? C9 O3 Co2 117.81(17) . 1_656 ? C11 O4 C10 121.1(2) . . ? C17 O5 Co2 92.89(19) . . ? C17 O6 Co2 84.64(16) . . ? C18 O7 C19 113.7(2) . . ? C25 O8 Co2 132.38(18) . 1_655 ? C25 O9 Co1 130.66(16) . 1_554 ? C25 O9 H9C 109.5 . . ? Co1 O9 H9C 85.8 1_554 . ? C27 O10 C26 119.7(2) . . ? C33 O11 Co2 95.12(15) . 1_666 ? C33 O11 Co1 137.27(16) . 1_565 ? Co2 O11 Co1 105.93(8) 1_666 1_565 ? C33 O12 Co2 84.69(15) . 1_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C26 C1 C2 O1 -58.9(3) . . . . ? C18 C1 C2 O1 63.0(3) . . . . ? C10 C1 C2 O1 -178.4(2) . . . . ? O1 C3 C4 C5 -178.3(3) . . . . ? C8 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C7 3.5(5) . . . . ? C4 C5 C6 C9 178.6(3) . . . . ? C5 C6 C7 C8 -5.6(5) . . . . ? C9 C6 C7 C8 179.2(3) . . . . ? O1 C3 C8 C7 176.6(2) . . . . ? C4 C3 C8 C7 -1.9(4) . . . . ? C6 C7 C8 C3 4.7(4) . . . . ? C7 C6 C9 O2 -7.0(4) . . . . ? C5 C6 C9 O2 177.8(3) . . . . ? C7 C6 C9 O3 173.5(3) . . . . ? C5 C6 C9 O3 -1.7(4) . . . . ? C26 C1 C10 O4 -173.3(2) . . . . ? C18 C1 C10 O4 64.1(3) . . . . ? C2 C1 C10 O4 -53.7(3) . . . . ? O4 C11 C12 C13 -179.9(3) . . . . ? C16 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 3.2(5) . . . . ? C12 C13 C14 C15 -4.9(5) . . . . ? C12 C13 C14 C17 175.6(3) . . . . ? C13 C14 C15 C16 3.3(5) . . . . ? C17 C14 C15 C16 -177.3(3) . . . . ? C14 C15 C16 C11 0.2(5) . . . . ? O4 C11 C16 C15 178.1(3) . . . . ? C12 C11 C16 C15 -1.9(5) . . . . ? C15 C14 C17 O5 -167.7(3) . . . . ? C13 C14 C17 O5 11.8(4) . . . . ? C15 C14 C17 O6 6.7(4) . . . . ? C13 C14 C17 O6 -173.8(3) . . . . ? C15 C14 C17 Co2 -95.7(8) . . . . ? C13 C14 C17 Co2 83.8(8) . . . . ? C26 C1 C18 O7 -65.0(3) . . . . ? C2 C1 C18 O7 174.0(2) . . . . ? C10 C1 C18 O7 56.5(3) . . . . ? O7 C19 C20 C21 177.3(3) . . . . ? C24 C19 C20 C21 0.0(5) . . . . ? C19 C20 C21 C22 0.0(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C20 C21 C22 C25 178.2(3) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C25 C22 C23 C24 -178.3(3) . . . . ? C22 C23 C24 C19 0.0(5) . . . . ? O7 C19 C24 C23 -177.5(3) . . . . ? C20 C19 C24 C23 0.0(5) . . . . ? C23 C22 C25 O8 -0.3(4) . . . . ? C21 C22 C25 O8 -178.5(3) . . . . ? C23 C22 C25 O9 -174.6(3) . . . . ? C21 C22 C25 O9 7.2(4) . . . . ? C18 C1 C26 O10 -175.0(2) . . . . ? C2 C1 C26 O10 -54.9(3) . . . . ? C10 C1 C26 O10 63.4(3) . . . . ? O10 C27 C28 C29 179.9(3) . . . . ? C32 C27 C28 C29 0.2(5) . . . . ? C27 C28 C29 C30 0.6(4) . . . . ? C28 C29 C30 C31 -2.8(4) . . . . ? C28 C29 C30 C33 176.6(3) . . . . ? C29 C30 C31 C32 4.4(4) . . . . ? C33 C30 C31 C32 -175.1(3) . . . . ? O10 C27 C32 C31 -178.4(3) . . . . ? C28 C27 C32 C31 1.3(5) . . . . ? C30 C31 C32 C27 -3.6(5) . . . . ? C31 C30 C33 O12 -9.3(4) . . . . ? C29 C30 C33 O12 171.3(3) . . . . ? C31 C30 C33 O11 169.6(2) . . . . ? C29 C30 C33 O11 -9.8(4) . . . . ? O5 C17 Co2 O8 104.81(18) . . . 1_455 ? O6 C17 Co2 O8 -85.49(16) . . . 1_455 ? C14 C17 Co2 O8 24.3(8) . . . 1_455 ? O5 C17 Co2 O3 -151.38(16) . . . 1_454 ? O6 C17 Co2 O3 18.32(18) . . . 1_454 ? C14 C17 Co2 O3 128.1(8) . . . 1_454 ? O5 C17 Co2 O11 4.7(2) . . . 1_444 ? O6 C17 Co2 O11 174.45(13) . . . 1_444 ? C14 C17 Co2 O11 -75.7(8) . . . 1_444 ? O6 C17 Co2 O5 169.7(3) . . . . ? C14 C17 Co2 O5 -80.5(8) . . . . ? O5 C17 Co2 O6 -169.7(3) . . . . ? C14 C17 Co2 O6 109.8(8) . . . . ? O5 C17 Co2 O12 -56.42(18) . . . 1_444 ? O6 C17 Co2 O12 113.28(15) . . . 1_444 ? C14 C17 Co2 O12 -136.9(8) . . . 1_444 ? C4 C3 O1 C2 -179.5(3) . . . . ? C8 C3 O1 C2 2.0(4) . . . . ? C1 C2 O1 C3 -179.0(2) . . . . ? O3 C9 O2 Co1 -33.1(5) . . . . ? C6 C9 O2 Co1 147.4(2) . . . . ? O9 Co1 O2 C9 -77.7(3) 2_766 . . . ? O9 Co1 O2 C9 102.3(3) 1_556 . . . ? O11 Co1 O2 C9 -168.1(3) 2_777 . . . ? O11 Co1 O2 C9 11.9(3) 1_545 . . . ? O2 C9 O3 Co2 -7.0(4) . . . 1_656 ? C6 C9 O3 Co2 172.42(18) . . . 1_656 ? C12 C11 O4 C10 168.2(3) . . . . ? C16 C11 O4 C10 -11.8(5) . . . . ? C1 C10 O4 C11 -145.6(3) . . . . ? O6 C17 O5 Co2 -11.0(3) . . . . ? C14 C17 O5 Co2 163.3(2) . . . . ? O8 Co2 O5 C17 -74.13(18) 1_455 . . . ? O3 Co2 O5 C17 45.8(2) 1_454 . . . ? O11 Co2 O5 C17 -176.49(17) 1_444 . . . ? O6 Co2 O5 C17 6.06(16) . . . . ? O12 Co2 O5 C17 125.71(18) 1_444 . . . ? O5 C17 O6 Co2 10.3(3) . . . . ? C14 C17 O6 Co2 -164.0(2) . . . . ? O8 Co2 O6 C17 90.78(16) 1_455 . . . ? O3 Co2 O6 C17 -164.45(16) 1_454 . . . ? O11 Co2 O6 C17 -15.2(4) 1_444 . . . ? O5 Co2 O6 C17 -5.82(15) . . . . ? O12 Co2 O6 C17 -76.59(17) 1_444 . . . ? C1 C18 O7 C19 -153.7(2) . . . . ? C20 C19 O7 C18 68.1(4) . . . . ? C24 C19 O7 C18 -114.5(3) . . . . ? O9 C25 O8 Co2 -15.1(4) . . . 1_655 ? C22 C25 O8 Co2 171.39(17) . . . 1_655 ? O8 C25 O9 Co1 -12.2(4) . . . 1_554 ? C22 C25 O9 Co1 161.63(17) . . . 1_554 ? C32 C27 O10 C26 -2.4(4) . . . . ? C28 C27 O10 C26 177.9(2) . . . . ? C1 C26 O10 C27 -179.2(2) . . . . ? O12 C33 O11 Co2 -1.0(3) . . . 1_666 ? C30 C33 O11 Co2 -179.9(2) . . . 1_666 ? O12 C33 O11 Co1 119.2(2) . . . 1_565 ? C30 C33 O11 Co1 -59.7(3) . . . 1_565 ? O11 C33 O12 Co2 0.9(2) . . . 1_666 ? C30 C33 O12 Co2 179.8(2) . . . 1_666 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.232 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.051