# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 922854' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Co4 N4 O18 ' _chemical_formula_sum 'C36 H52 Co4 N4 O18' _chemical_formula_weight 1064.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.070(5) _cell_length_b 10.734(5) _cell_length_c 11.474(5) _cell_angle_alpha 115.129(5) _cell_angle_beta 109.861(5) _cell_angle_gamma 97.138(5) _cell_volume 1002.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4484 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.276 _exptl_crystal_size_mid 0.269 _exptl_crystal_size_min 0.261 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.640 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9787 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4484 _reflns_number_gt 3824 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.3194P] 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 4484 _refine_ls_number_parameters 296 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.066 _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 0.89086(3) 0.37720(3) 0.99067(3) 0.01589(11) Uani 1 1 d . . . Co2 Co 0.85799(4) 0.71316(4) 1.13546(3) 0.01984(11) Uani 1 1 d . . . C1 C 1.4825(4) 0.6436(4) 1.6475(4) 0.0498(9) Uani 1 1 d . . . H1A H 1.5719 0.7162 1.6779 0.075 Uiso 1 1 calc R . . H1B H 1.5001 0.5517 1.6219 0.075 Uiso 1 1 calc R . . H1C H 1.4535 0.6697 1.7240 0.075 Uiso 1 1 calc R . . C2 C 1.3600(3) 0.6325(3) 1.5194(3) 0.0324(6) Uani 1 1 d . . . C3 C 1.2189(3) 0.5367(3) 1.4535(3) 0.0298(6) Uani 1 1 d . . . H3 H 1.1989 0.4780 1.4901 0.036 Uiso 1 1 calc R . . C4 C 1.1044(3) 0.5237(3) 1.3341(3) 0.0223(5) Uani 1 1 d . . . C5 C 1.1356(3) 0.6095(3) 1.2765(2) 0.0191(5) Uani 1 1 d . . . C6 C 1.2734(3) 0.7168(3) 1.3489(2) 0.0227(5) Uani 1 1 d . . . C7 C 1.3838(3) 0.7237(3) 1.4665(3) 0.0295(6) Uani 1 1 d . . . H7 H 1.4771 0.7920 1.5114 0.035 Uiso 1 1 calc R . . C8 C 0.9479(3) 0.4353(3) 1.2824(3) 0.0252(5) Uani 1 1 d . . . H8A H 0.9458 0.4061 1.3512 0.030 Uiso 1 1 calc R . . H8B H 0.8854 0.4970 1.2815 0.030 Uiso 1 1 calc R . . C9 C 0.7257(3) 0.2390(3) 1.1052(3) 0.0274(6) Uani 1 1 d . . . H9A H 0.6731 0.3082 1.1021 0.033 Uiso 1 1 calc R . . H9B H 0.7255 0.2242 1.1829 0.033 Uiso 1 1 calc R . . C10 C 0.6394(3) 0.0946(3) 0.9644(3) 0.0319(6) Uani 1 1 d . . . H10A H 0.6621 0.0175 0.9825 0.038 Uiso 1 1 calc R . . H10B H 0.5340 0.0801 0.9374 0.038 Uiso 1 1 calc R . . C11 C 0.6672(3) 0.0772(3) 0.8366(3) 0.0285(6) Uani 1 1 d . . . H11A H 0.7559 0.0482 0.8440 0.034 Uiso 1 1 calc R . . H11B H 0.5845 -0.0011 0.7501 0.034 Uiso 1 1 calc R . . C12 C 0.7027(3) 0.1649(3) 0.6861(3) 0.0247(5) Uani 1 1 d . . . H12A H 0.6141 0.0866 0.6073 0.030 Uiso 1 1 calc R . . H12B H 0.7861 0.1274 0.6923 0.030 Uiso 1 1 calc R . . C13 C 0.9698(3) 0.2028(3) 1.1385(3) 0.0239(5) Uani 1 1 d . . . H13A H 0.9031 0.1041 1.0846 0.029 Uiso 1 1 calc R . . H13B H 1.0255 0.2250 1.2362 0.029 Uiso 1 1 calc R . . C14 C 1.0770(3) 0.2134(3) 1.0745(3) 0.0197(5) Uani 1 1 d . . . C15 C 0.5572(3) 0.2611(3) 0.8124(3) 0.0244(5) Uani 1 1 d . . . H15A H 0.5049 0.2276 0.8559 0.029 Uiso 1 1 calc R . . H15B H 0.4892 0.2213 0.7126 0.029 Uiso 1 1 calc R . . C16 C 0.6029(3) 0.4249(3) 0.8866(3) 0.0200(5) Uani 1 1 d . . . C17 C 0.8557(5) 1.0643(4) 1.3667(4) 0.0547(10) Uani 1 1 d . . . H17A H 0.8766 1.1624 1.4386 0.082 Uiso 1 1 calc R . . H17B H 0.8045 0.9987 1.3855 0.082 Uiso 1 1 calc R . . H17C H 0.7943 1.0497 1.2743 0.082 Uiso 1 1 calc R . . C18 C 0.9990(4) 1.0364(3) 1.3696(3) 0.0364(7) Uani 1 1 d . . . N1 N 0.8807(2) 0.3028(2) 1.1380(2) 0.0211(4) Uani 1 1 d . . . N2 N 0.6861(2) 0.2072(2) 0.8210(2) 0.0200(4) Uani 1 1 d . . . O1 O 1.0306(4) 0.5896(3) 1.1533(4) 0.0132(5) Uani 0.85 1 d PU . . O2 O 1.0551(2) 0.2819(2) 1.00466(19) 0.0219(4) Uani 1 1 d U . . O3 O 1.1731(2) 0.1541(2) 1.0878(2) 0.0320(4) Uani 1 1 d U . . O4 O 0.73862(19) 0.49184(19) 0.97954(18) 0.0221(4) Uani 1 1 d U . . O5 O 0.5081(2) 0.4842(2) 0.8604(2) 0.0287(4) Uani 1 1 d U . . O6 O 0.9935(2) 0.9147(2) 1.2821(2) 0.0382(5) Uani 1 1 d U . . O7 O 1.1197(3) 1.1347(3) 1.4572(3) 0.0638(9) Uani 1 1 d U . . O1' O 1.032(3) 0.618(3) 1.148(3) 0.022(2) Uiso 0.15 1 d PU . . O1W O 0.6721(2) 0.7675(2) 1.0329(2) 0.0291(4) Uani 1 1 d DU . . H1WA H 0.714(4) 0.803(4) 0.995(3) 0.044 Uiso 1 1 d D . . H1WB H 0.603(3) 0.689(3) 0.974(3) 0.044 Uiso 1 1 d D . . O2W O 0.7859(2) 0.6827(2) 1.2712(2) 0.0292(4) Uani 1 1 d DU . . H2WA H 0.694(2) 0.636(4) 1.241(3) 0.044 Uiso 1 1 d D . . H2WB H 0.825(3) 0.740(3) 1.3636(19) 0.044 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01445(18) 0.01585(18) 0.01706(18) 0.00786(13) 0.00686(13) 0.00534(13) Co2 0.01870(19) 0.01886(19) 0.01887(18) 0.00638(13) 0.00892(14) 0.00579(14) C1 0.046(2) 0.065(2) 0.0321(16) 0.0264(16) 0.0054(14) 0.0248(18) C2 0.0338(16) 0.0381(16) 0.0204(12) 0.0131(11) 0.0069(11) 0.0164(13) C3 0.0399(16) 0.0360(15) 0.0233(13) 0.0188(11) 0.0165(12) 0.0194(13) C4 0.0273(13) 0.0236(12) 0.0176(11) 0.0101(9) 0.0107(10) 0.0108(10) C5 0.0214(12) 0.0196(11) 0.0122(10) 0.0045(9) 0.0066(9) 0.0090(9) C6 0.0216(12) 0.0231(12) 0.0167(11) 0.0051(9) 0.0070(9) 0.0078(10) C7 0.0219(13) 0.0334(15) 0.0189(12) 0.0072(10) 0.0020(10) 0.0060(11) C8 0.0340(15) 0.0276(13) 0.0236(12) 0.0156(10) 0.0180(11) 0.0137(11) C9 0.0273(14) 0.0340(15) 0.0378(15) 0.0254(12) 0.0213(12) 0.0134(12) C10 0.0250(14) 0.0281(14) 0.0514(17) 0.0247(13) 0.0198(13) 0.0082(11) C11 0.0303(14) 0.0157(12) 0.0337(14) 0.0113(10) 0.0104(11) 0.0041(10) C12 0.0209(12) 0.0199(12) 0.0216(12) 0.0042(9) 0.0056(10) 0.0040(10) C13 0.0275(14) 0.0257(13) 0.0293(13) 0.0193(11) 0.0150(11) 0.0133(11) C14 0.0184(12) 0.0186(11) 0.0209(11) 0.0102(9) 0.0074(9) 0.0053(9) C15 0.0174(12) 0.0208(12) 0.0287(13) 0.0096(10) 0.0080(10) 0.0032(10) C16 0.0170(11) 0.0214(12) 0.0201(11) 0.0097(9) 0.0080(9) 0.0046(9) C17 0.076(3) 0.043(2) 0.058(2) 0.0245(17) 0.039(2) 0.033(2) C18 0.0511(19) 0.0253(14) 0.0281(14) 0.0109(11) 0.0176(13) 0.0056(13) N1 0.0223(11) 0.0231(11) 0.0266(10) 0.0158(9) 0.0145(9) 0.0101(9) N2 0.0182(10) 0.0162(10) 0.0239(10) 0.0088(8) 0.0090(8) 0.0054(8) O1 0.0146(9) 0.0131(14) 0.0140(9) 0.0091(9) 0.0053(7) 0.0049(10) O2 0.0234(9) 0.0269(9) 0.0269(9) 0.0180(7) 0.0155(7) 0.0143(7) O3 0.0283(10) 0.0362(11) 0.0476(12) 0.0296(10) 0.0196(9) 0.0189(9) O4 0.0158(8) 0.0205(9) 0.0220(8) 0.0062(7) 0.0051(7) 0.0063(7) O5 0.0192(9) 0.0268(10) 0.0350(10) 0.0155(8) 0.0059(8) 0.0079(8) O6 0.0316(11) 0.0279(11) 0.0333(10) 0.0007(8) 0.0119(9) 0.0039(9) O7 0.0717(19) 0.0424(15) 0.0358(12) -0.0056(11) 0.0237(12) -0.0166(14) O1W 0.0257(10) 0.0283(10) 0.0323(10) 0.0131(8) 0.0134(8) 0.0110(8) O2W 0.0241(10) 0.0327(11) 0.0212(9) 0.0067(8) 0.0109(8) 0.0023(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1' 2.01(2) 2_767 ? Co1 O2 2.046(2) . ? Co1 O4 2.086(2) . ? Co1 O1 2.113(3) . ? Co1 N2 2.166(2) . ? Co1 N1 2.179(2) . ? Co1 O1 2.191(3) 2_767 ? Co1 O1' 2.31(3) . ? Co2 O6 1.997(2) . ? Co2 O2W 2.050(2) . ? Co2 O2 2.0908(19) 2_767 ? Co2 O4 2.123(2) . ? Co2 O1' 2.13(3) . ? Co2 O1W 2.142(2) . ? Co2 O1 2.321(3) . ? C1 C2 1.510(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(4) . ? C2 C7 1.389(4) . ? C3 C4 1.396(4) . ? C3 H3 0.9300 . ? C4 C5 1.404(4) . ? C4 C8 1.500(4) . ? C5 O1 1.354(4) . ? C5 C6 1.396(4) . ? C5 O1' 1.53(2) . ? C6 C7 1.392(4) . ? C6 C12 1.501(4) 2_767 ? C7 H7 0.9300 . ? C8 N1 1.491(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.471(3) . ? C9 C10 1.534(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.524(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.478(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.492(3) . ? C12 C6 1.501(4) 2_767 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.483(3) . ? C13 C14 1.516(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.225(3) . ? C14 O2 1.285(3) . ? C15 N2 1.476(3) . ? C15 C16 1.512(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O5 1.235(3) . ? C16 O4 1.279(3) . ? C17 C18 1.502(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O6 1.244(4) . ? C18 O7 1.246(4) . ? O1 Co1 2.191(3) 2_767 ? O2 Co2 2.0908(18) 2_767 ? O1' Co1 2.01(2) 2_767 ? O1W H1WA 0.855(17) . ? O1W H1WB 0.841(17) . ? O2W H2WA 0.864(18) . ? O2W H2WB 0.872(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Co1 O2 72.8(7) 2_767 . ? O1' Co1 O4 103.6(7) 2_767 . ? O2 Co1 O4 174.28(7) . . ? O1' Co1 O1 92.9(7) 2_767 . ? O2 Co1 O1 96.17(11) . . ? O4 Co1 O1 79.41(10) . . ? O1' Co1 N2 92.6(8) 2_767 . ? O2 Co1 N2 106.48(9) . . ? O4 Co1 N2 77.91(8) . . ? O1 Co1 N2 157.32(10) . . ? O1' Co1 N1 150.6(7) 2_767 . ? O2 Co1 N1 78.16(8) . . ? O4 Co1 N1 105.68(8) . . ? O1 Co1 N1 94.84(10) . . ? N2 Co1 N1 91.02(9) . . ? O1' Co1 O1 7.6(7) 2_767 2_767 ? O2 Co1 O1 79.10(9) . 2_767 ? O4 Co1 O1 97.03(9) . 2_767 ? O1 Co1 O1 88.00(13) . 2_767 ? N2 Co1 O1 95.01(11) . 2_767 ? N1 Co1 O1 157.26(10) . 2_767 ? O1' Co1 O1' 88.7(10) 2_767 . ? O2 Co1 O1' 100.1(7) . . ? O4 Co1 O1' 75.1(7) . . ? O1 Co1 O1' 6.9(6) . . ? N2 Co1 O1' 152.5(6) . . ? N1 Co1 O1' 101.2(6) . . ? O1 Co1 O1' 83.2(6) 2_767 . ? O6 Co2 O2W 94.63(9) . . ? O6 Co2 O2 89.41(9) . 2_767 ? O2W Co2 O2 171.15(8) . 2_767 ? O6 Co2 O4 172.74(8) . . ? O2W Co2 O4 88.45(8) . . ? O2 Co2 O4 86.66(8) 2_767 . ? O6 Co2 O1' 94.7(7) . . ? O2W Co2 O1' 102.2(6) . . ? O2 Co2 O1' 69.5(6) 2_767 . ? O4 Co2 O1' 78.2(7) . . ? O6 Co2 O1W 97.90(10) . . ? O2W Co2 O1W 97.02(9) . . ? O2 Co2 O1W 90.19(8) 2_767 . ? O4 Co2 O1W 88.22(8) . . ? O1' Co2 O1W 156.0(7) . . ? O6 Co2 O1 99.00(11) . . ? O2W Co2 O1 96.30(10) . . ? O2 Co2 O1 75.27(9) 2_767 . ? O4 Co2 O1 74.10(10) . . ? O1' Co2 O1 7.0(6) . . ? O1W Co2 O1 157.50(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.0(3) . . ? C3 C2 C1 122.0(3) . . ? C7 C2 C1 121.0(3) . . ? C2 C3 C4 123.0(3) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 118.5(2) . . ? C3 C4 C8 120.0(2) . . ? C5 C4 C8 121.0(2) . . ? O1 C5 C6 120.8(2) . . ? O1 C5 C4 119.6(2) . . ? C6 C5 C4 119.5(2) . . ? O1 C5 O1' 11.1(9) . . ? C6 C5 O1' 110.7(9) . . ? C4 C5 O1' 129.4(10) . . ? C7 C6 C5 119.0(3) . . ? C7 C6 C12 119.6(2) . 2_767 ? C5 C6 C12 121.0(2) . 2_767 ? C2 C7 C6 122.5(3) . . ? C2 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? N1 C8 C4 116.3(2) . . ? N1 C8 H8A 108.2 . . ? C4 C8 H8A 108.2 . . ? N1 C8 H8B 108.2 . . ? C4 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? N1 C9 C10 115.3(2) . . ? N1 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N1 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 117.4(2) . . ? C11 C10 H10A 107.9 . . ? C9 C10 H10A 107.9 . . ? C11 C10 H10B 107.9 . . ? C9 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? N2 C11 C10 115.7(2) . . ? N2 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? N2 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? N2 C12 C6 115.9(2) . 2_767 ? N2 C12 H12A 108.3 . . ? C6 C12 H12A 108.3 2_767 . ? N2 C12 H12B 108.3 . . ? C6 C12 H12B 108.3 2_767 . ? H12A C12 H12B 107.4 . . ? N1 C13 C14 112.5(2) . . ? N1 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N1 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? O3 C14 O2 124.9(2) . . ? O3 C14 C13 119.4(2) . . ? O2 C14 C13 115.7(2) . . ? N2 C15 C16 112.2(2) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O5 C16 O4 124.8(2) . . ? O5 C16 C15 119.3(2) . . ? O4 C16 C15 115.8(2) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O6 C18 O7 121.4(3) . . ? O6 C18 C17 118.6(3) . . ? O7 C18 C17 120.0(3) . . ? C9 N1 C13 113.0(2) . . ? C9 N1 C8 107.1(2) . . ? C13 N1 C8 109.3(2) . . ? C9 N1 Co1 111.12(16) . . ? C13 N1 Co1 110.07(15) . . ? C8 N1 Co1 105.91(15) . . ? C15 N2 C11 112.1(2) . . ? C15 N2 C12 109.2(2) . . ? C11 N2 C12 107.2(2) . . ? C15 N2 Co1 110.89(15) . . ? C11 N2 Co1 111.53(16) . . ? C12 N2 Co1 105.62(15) . . ? C5 O1 Co1 119.14(17) . . ? C5 O1 Co1 116.8(2) . 2_767 ? Co1 O1 Co1 92.00(13) . 2_767 ? C5 O1 Co2 125.9(2) . . ? Co1 O1 Co2 99.43(14) . . ? Co1 O1 Co2 96.49(9) 2_767 . ? C14 O2 Co1 121.18(15) . . ? C14 O2 Co2 129.04(16) . 2_767 ? Co1 O2 Co2 108.96(8) . 2_767 ? C16 O4 Co1 119.71(16) . . ? C16 O4 Co2 133.21(17) . . ? Co1 O4 Co2 107.05(8) . . ? C18 O6 Co2 143.7(2) . . ? C5 O1' Co1 118.2(16) . 2_767 ? C5 O1' Co2 127.7(15) . . ? Co1 O1' Co2 108.7(10) 2_767 . ? C5 O1' Co1 101.4(10) . . ? Co1 O1' Co1 91.3(10) 2_767 . ? Co2 O1' Co1 99.2(11) . . ? Co2 O1W H1WA 96(3) . . ? Co2 O1W H1WB 106(3) . . ? H1WA O1W H1WB 114(3) . . ? Co2 O2W H2WA 121(2) . . ? Co2 O2W H2WB 125(2) . . ? H2WA O2W H2WB 109(2) . . ? 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 C7 C2 C3 C4 3.3(4) . . . . ? C1 C2 C3 C4 -179.3(3) . . . . ? C2 C3 C4 C5 1.7(4) . . . . ? C2 C3 C4 C8 -170.1(3) . . . . ? C3 C4 C5 O1 174.0(3) . . . . ? C8 C4 C5 O1 -14.3(4) . . . . ? C3 C4 C5 C6 -7.6(4) . . . . ? C8 C4 C5 C6 164.1(2) . . . . ? C3 C4 C5 O1' -179.6(13) . . . . ? C8 C4 C5 O1' -8.0(13) . . . . ? O1 C5 C6 C7 -173.2(3) . . . . ? C4 C5 C6 C7 8.4(4) . . . . ? O1' C5 C6 C7 -178.2(11) . . . . ? O1 C5 C6 C12 14.7(4) . . . 2_767 ? C4 C5 C6 C12 -163.7(2) . . . 2_767 ? O1' C5 C6 C12 9.7(11) . . . 2_767 ? C3 C2 C7 C6 -2.5(4) . . . . ? C1 C2 C7 C6 -179.9(3) . . . . ? C5 C6 C7 C2 -3.3(4) . . . . ? C12 C6 C7 C2 168.9(3) 2_767 . . . ? C3 C4 C8 N1 -115.0(3) . . . . ? C5 C4 C8 N1 73.5(3) . . . . ? N1 C9 C10 C11 -38.3(3) . . . . ? C9 C10 C11 N2 -38.8(4) . . . . ? N1 C13 C14 O3 168.8(2) . . . . ? N1 C13 C14 O2 -13.5(3) . . . . ? N2 C15 C16 O5 163.0(2) . . . . ? N2 C15 C16 O4 -20.8(3) . . . . ? C10 C9 N1 C13 -55.5(3) . . . . ? C10 C9 N1 C8 -176.0(2) . . . . ? C10 C9 N1 Co1 68.8(2) . . . . ? C14 C13 N1 C9 141.6(2) . . . . ? C14 C13 N1 C8 -99.2(2) . . . . ? C14 C13 N1 Co1 16.8(3) . . . . ? C4 C8 N1 C9 -176.3(2) . . . . ? C4 C8 N1 C13 60.9(3) . . . . ? C4 C8 N1 Co1 -57.6(2) . . . . ? O1' Co1 N1 C9 -128.5(15) 2_767 . . . ? O2 Co1 N1 C9 -137.99(18) . . . . ? O4 Co1 N1 C9 46.37(18) . . . . ? O1 Co1 N1 C9 126.70(19) . . . . ? N2 Co1 N1 C9 -31.36(17) . . . . ? O1 Co1 N1 C9 -136.9(3) 2_767 . . . ? O1' Co1 N1 C9 123.9(7) . . . . ? O1' Co1 N1 C13 -2.6(15) 2_767 . . . ? O2 Co1 N1 C13 -12.07(16) . . . . ? O4 Co1 N1 C13 172.29(16) . . . . ? O1 Co1 N1 C13 -107.38(19) . . . . ? N2 Co1 N1 C13 94.56(17) . . . . ? O1 Co1 N1 C13 -11.0(4) 2_767 . . . ? O1' Co1 N1 C13 -110.2(7) . . . . ? O1' Co1 N1 C8 115.5(15) 2_767 . . . ? O2 Co1 N1 C8 106.02(17) . . . . ? O4 Co1 N1 C8 -69.62(17) . . . . ? O1 Co1 N1 C8 10.72(18) . . . . ? N2 Co1 N1 C8 -147.34(16) . . . . ? O1 Co1 N1 C8 107.1(3) 2_767 . . . ? O1' Co1 N1 C8 7.9(7) . . . . ? C16 C15 N2 C11 144.0(2) . . . . ? C16 C15 N2 C12 -97.4(2) . . . . ? C16 C15 N2 Co1 18.6(2) . . . . ? C10 C11 N2 C15 -56.8(3) . . . . ? C10 C11 N2 C12 -176.6(2) . . . . ? C10 C11 N2 Co1 68.2(3) . . . . ? C6 C12 N2 C15 59.6(3) 2_767 . . . ? C6 C12 N2 C11 -178.8(2) 2_767 . . . ? C6 C12 N2 Co1 -59.8(2) 2_767 . . . ? O1' Co1 N2 C15 -113.3(7) 2_767 . . . ? O2 Co1 N2 C15 173.79(15) . . . . ? O4 Co1 N2 C15 -9.99(16) . . . . ? O1 Co1 N2 C15 -9.3(3) . . . . ? N1 Co1 N2 C15 95.83(17) . . . . ? O1 Co1 N2 C15 -106.12(17) 2_767 . . . ? O1' Co1 N2 C15 -21.1(14) . . . . ? O1' Co1 N2 C11 121.0(7) 2_767 . . . ? O2 Co1 N2 C11 48.11(18) . . . . ? O4 Co1 N2 C11 -135.67(18) . . . . ? O1 Co1 N2 C11 -135.0(3) . . . . ? N1 Co1 N2 C11 -29.85(17) . . . . ? O1 Co1 N2 C11 128.20(18) 2_767 . . . ? O1' Co1 N2 C11 -146.8(13) . . . . ? O1' Co1 N2 C12 4.9(7) 2_767 . . . ? O2 Co1 N2 C12 -67.98(16) . . . . ? O4 Co1 N2 C12 108.24(16) . . . . ? O1 Co1 N2 C12 108.9(3) . . . . ? N1 Co1 N2 C12 -145.93(16) . . . . ? O1 Co1 N2 C12 12.11(17) 2_767 . . . ? O1' Co1 N2 C12 97.1(13) . . . . ? C6 C5 O1 Co1 144.6(2) . . . . ? C4 C5 O1 Co1 -37.0(4) . . . . ? O1' C5 O1 Co1 170(6) . . . . ? C6 C5 O1 Co1 35.5(3) . . . 2_767 ? C4 C5 O1 Co1 -146.1(2) . . . 2_767 ? O1' C5 O1 Co1 60(6) . . . 2_767 ? C6 C5 O1 Co2 -86.0(3) . . . . ? C4 C5 O1 Co2 92.4(3) . . . . ? O1' C5 O1 Co2 -61(6) . . . . ? O1' Co1 O1 C5 -116.7(6) 2_767 . . . ? O2 Co1 O1 C5 -43.7(3) . . . . ? O4 Co1 O1 C5 140.0(3) . . . . ? N2 Co1 O1 C5 139.3(2) . . . . ? N1 Co1 O1 C5 34.9(3) . . . . ? O1 Co1 O1 C5 -122.5(3) 2_767 . . . ? O1' Co1 O1 C5 -169(6) . . . . ? O1' Co1 O1 Co1 5.8(8) 2_767 . . 2_767 ? O2 Co1 O1 Co1 78.80(10) . . . 2_767 ? O4 Co1 O1 Co1 -97.53(10) . . . 2_767 ? N2 Co1 O1 Co1 -98.2(3) . . . 2_767 ? N1 Co1 O1 Co1 157.39(10) . . . 2_767 ? O1 Co1 O1 Co1 0.0 2_767 . . 2_767 ? O1' Co1 O1 Co1 -46(6) . . . 2_767 ? O1' Co1 O1 Co2 102.7(7) 2_767 . . . ? O2 Co1 O1 Co2 175.73(9) . . . . ? O4 Co1 O1 Co2 -0.61(8) . . . . ? N2 Co1 O1 Co2 -1.3(3) . . . . ? N1 Co1 O1 Co2 -105.69(10) . . . . ? O1 Co1 O1 Co2 96.92(11) 2_767 . . . ? O1' Co1 O1 Co2 50(6) . . . . ? O6 Co2 O1 C5 46.1(3) . . . . ? O2W Co2 O1 C5 -49.6(2) . . . . ? O2 Co2 O1 C5 133.1(3) 2_767 . . . ? O4 Co2 O1 C5 -136.2(3) . . . . ? O1' Co2 O1 C5 99(6) . . . . ? O1W Co2 O1 C5 -175.7(2) . . . . ? O6 Co2 O1 Co1 -177.09(10) . . . . ? O2W Co2 O1 Co1 87.18(11) . . . . ? O2 Co2 O1 Co1 -90.09(11) 2_767 . . . ? O4 Co2 O1 Co1 0.61(8) . . . . ? O1' Co2 O1 Co1 -125(6) . . . . ? O1W Co2 O1 Co1 -38.8(3) . . . . ? O6 Co2 O1 Co1 -83.96(12) . . . 2_767 ? O2W Co2 O1 Co1 -179.69(10) . . . 2_767 ? O2 Co2 O1 Co1 3.04(9) 2_767 . . 2_767 ? O4 Co2 O1 Co1 93.74(12) . . . 2_767 ? O1' Co2 O1 Co1 -32(6) . . . 2_767 ? O1W Co2 O1 Co1 54.3(3) . . . 2_767 ? O3 C14 O2 Co1 -179.8(2) . . . . ? C13 C14 O2 Co1 2.7(3) . . . . ? O3 C14 O2 Co2 11.8(4) . . . 2_767 ? C13 C14 O2 Co2 -165.73(16) . . . 2_767 ? O1' Co1 O2 C14 -169.6(8) 2_767 . . . ? O4 Co1 O2 C14 138.3(6) . . . . ? O1 Co1 O2 C14 99.2(2) . . . . ? N2 Co1 O2 C14 -82.01(19) . . . . ? N1 Co1 O2 C14 5.52(18) . . . . ? O1 Co1 O2 C14 -174.1(2) 2_767 . . . ? O1' Co1 O2 C14 104.9(6) . . . . ? O1' Co1 O2 Co2 0.9(8) 2_767 . . 2_767 ? O4 Co1 O2 Co2 -51.2(7) . . . 2_767 ? O1 Co1 O2 Co2 -90.32(11) . . . 2_767 ? N2 Co1 O2 Co2 88.48(10) . . . 2_767 ? N1 Co1 O2 Co2 176.01(10) . . . 2_767 ? O1 Co1 O2 Co2 -3.56(10) 2_767 . . 2_767 ? O1' Co1 O2 Co2 -84.6(6) . . . 2_767 ? O5 C16 O4 Co1 -171.56(19) . . . . ? C15 C16 O4 Co1 12.5(3) . . . . ? O5 C16 O4 Co2 6.1(4) . . . . ? C15 C16 O4 Co2 -169.82(16) . . . . ? O1' Co1 O4 C16 88.5(8) 2_767 . . . ? O2 Co1 O4 C16 139.3(6) . . . . ? O1 Co1 O4 C16 178.9(2) . . . . ? N2 Co1 O4 C16 -1.33(18) . . . . ? N1 Co1 O4 C16 -88.97(19) . . . . ? O1 Co1 O4 C16 92.3(2) 2_767 . . . ? O1' Co1 O4 C16 173.4(7) . . . . ? O1' Co1 O4 Co2 -89.8(8) 2_767 . . . ? O2 Co1 O4 Co2 -38.9(7) . . . . ? O1 Co1 O4 Co2 0.68(10) . . . . ? N2 Co1 O4 Co2 -179.59(9) . . . . ? N1 Co1 O4 Co2 92.78(10) . . . . ? O1 Co1 O4 Co2 -85.94(11) 2_767 . . . ? O1' Co1 O4 Co2 -4.9(6) . . . . ? O6 Co2 O4 C16 -160.3(6) . . . . ? O2W Co2 O4 C16 84.4(2) . . . . ? O2 Co2 O4 C16 -102.9(2) 2_767 . . . ? O1' Co2 O4 C16 -172.7(7) . . . . ? O1W Co2 O4 C16 -12.6(2) . . . . ? O1 Co2 O4 C16 -178.6(2) . . . . ? O6 Co2 O4 Co1 17.6(7) . . . . ? O2W Co2 O4 Co1 -97.63(10) . . . . ? O2 Co2 O4 Co1 74.99(9) 2_767 . . . ? O1' Co2 O4 Co1 5.2(6) . . . . ? O1W Co2 O4 Co1 165.29(9) . . . . ? O1 Co2 O4 Co1 -0.64(9) . . . . ? O7 C18 O6 Co2 171.4(3) . . . . ? C17 C18 O6 Co2 -9.5(5) . . . . ? O2W Co2 O6 C18 -54.5(4) . . . . ? O2 Co2 O6 C18 133.4(4) 2_767 . . . ? O4 Co2 O6 C18 -169.4(5) . . . . ? O1' Co2 O6 C18 -157.2(7) . . . . ? O1W Co2 O6 C18 43.3(4) . . . . ? O1 Co2 O6 C18 -151.6(4) . . . . ? O1 C5 O1' Co1 -106(6) . . . 2_767 ? C6 C5 O1' Co1 51.0(15) . . . 2_767 ? C4 C5 O1' Co1 -136.4(9) . . . 2_767 ? O1 C5 O1' Co2 103(6) . . . . ? C6 C5 O1' Co2 -100.0(15) . . . . ? C4 C5 O1' Co2 72.6(18) . . . . ? O1 C5 O1' Co1 -8(5) . . . . ? C6 C5 O1' Co1 148.7(6) . . . . ? C4 C5 O1' Co1 -38.7(16) . . . . ? O6 Co2 O1' C5 64.8(16) . . . . ? O2W Co2 O1' C5 -31.0(17) . . . . ? O2 Co2 O1' C5 152.4(18) 2_767 . . . ? O4 Co2 O1' C5 -116.8(17) . . . . ? O1W Co2 O1' C5 -173.7(4) . . . . ? O1 Co2 O1' C5 -63(6) . . . . ? O6 Co2 O1' Co1 -88.5(10) . . . 2_767 ? O2W Co2 O1' Co1 175.8(8) . . . 2_767 ? O2 Co2 O1' Co1 -0.8(7) 2_767 . . 2_767 ? O4 Co2 O1' Co1 90.0(10) . . . 2_767 ? O1W Co2 O1' Co1 33(2) . . . 2_767 ? O1 Co2 O1' Co1 143(7) . . . 2_767 ? O6 Co2 O1' Co1 177.0(6) . . . . ? O2W Co2 O1' Co1 81.2(8) . . . . ? O2 Co2 O1' Co1 -95.4(8) 2_767 . . . ? O4 Co2 O1' Co1 -4.6(6) . . . . ? O1W Co2 O1' Co1 -61.4(18) . . . . ? O1 Co2 O1' Co1 49(6) . . . . ? O1' Co1 O1' C5 -119.2(17) 2_767 . . . ? O2 Co1 O1' C5 -46.9(12) . . . . ? O4 Co1 O1' C5 136.4(13) . . . . ? O1 Co1 O1' C5 9(5) . . . . ? N2 Co1 O1' C5 147.7(6) . . . . ? N1 Co1 O1' C5 32.9(13) . . . . ? O1 Co1 O1' C5 -124.5(12) 2_767 . . . ? O1' Co1 O1' Co1 0.0 2_767 . . 2_767 ? O2 Co1 O1' Co1 72.3(8) . . . 2_767 ? O4 Co1 O1' Co1 -104.4(8) . . . 2_767 ? O1 Co1 O1' Co1 128(7) . . . 2_767 ? N2 Co1 O1' Co1 -93.2(15) . . . 2_767 ? N1 Co1 O1' Co1 152.1(6) . . . 2_767 ? O1 Co1 O1' Co1 -5.3(7) 2_767 . . 2_767 ? O1' Co1 O1' Co2 109.1(11) 2_767 . . . ? O2 Co1 O1' Co2 -178.5(6) . . . . ? O4 Co1 O1' Co2 4.7(6) . . . . ? O1 Co1 O1' Co2 -123(7) . . . . ? N2 Co1 O1' Co2 16.0(19) . . . . ? N1 Co1 O1' Co2 -98.8(7) . . . . ? O1 Co1 O1' Co2 103.8(8) 2_767 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.855(17) 1.84(2) 2.681(3) 166(4) 2_767 O2W H2WA O5 0.864(18) 1.904(17) 2.757(3) 169(3) 2_667 O2W H2WB O7 0.872(17) 1.741(19) 2.606(3) 171(4) 2_778 O1W H1WB O5 0.841(17) 1.90(2) 2.704(3) 158(4) . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.203 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.107 data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 922855' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Mn4 N4 O18 ' _chemical_formula_sum 'C36 H52 Mn4 N4 O18' _chemical_formula_weight 1048.58 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.2072(9) _cell_length_b 10.7719(7) _cell_length_c 11.5617(8) _cell_angle_alpha 114.506(7) _cell_angle_beta 109.613(7) _cell_angle_gamma 97.489(6) _cell_volume 1034.30(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5099 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 29.9 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.346 _exptl_crystal_size_mid 0.242 _exptl_crystal_size_min 0.232 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11577 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 29.89 _reflns_number_total 5099 _reflns_number_gt 3107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+0.0000P] 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 5099 _refine_ls_number_parameters 292 _refine_ls_number_restraints 300 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.14457(5) 0.27998(5) 0.36045(5) 0.02907(15) Uani 1 1 d . . . Mn2 Mn 0.89026(5) 0.37638(5) 0.48954(5) 0.02420(14) Uani 1 1 d . . . C1 C 0.5315(5) 0.3659(6) -0.1394(4) 0.0659(13) Uani 1 1 d U . . H1A H 0.5684 0.4384 -0.1584 0.099 Uiso 1 1 calc R . . H1B H 0.4481 0.3807 -0.1211 0.099 Uiso 1 1 calc R . . H1C H 0.5029 0.2727 -0.2195 0.099 Uiso 1 1 calc R . . C2 C 0.6491(4) 0.3751(4) -0.0126(4) 0.0438(9) Uani 1 1 d U . . C3 C 0.7876(4) 0.4702(4) 0.0531(4) 0.0415(9) Uani 1 1 d U . . H3 H 0.8077 0.5310 0.0187 0.050 Uiso 1 1 calc R . . C4 C 0.9010(4) 0.4796(4) 0.1704(3) 0.0316(7) Uani 1 1 d U . . C5 C 0.8702(4) 0.3910(3) 0.2238(3) 0.0274(7) Uani 1 1 d U . . C6 C 0.7318(4) 0.2860(4) 0.1529(3) 0.0325(7) Uani 1 1 d U . . C7 C 0.6241(4) 0.2825(4) 0.0372(4) 0.0407(9) Uani 1 1 d U . . H7 H 0.5318 0.2149 -0.0079 0.049 Uiso 1 1 calc R . . C8 C 0.7041(4) 0.1669(3) 0.1856(3) 0.0333(8) Uani 1 1 d U . . H8A H 0.7866 0.1299 0.1943 0.040 Uiso 1 1 calc R . . H8B H 0.6182 0.0896 0.1061 0.040 Uiso 1 1 calc R . . C9 C 0.6648(4) 0.0770(4) 0.3345(4) 0.0378(8) Uani 1 1 d U . . H9A H 0.7525 0.0490 0.3412 0.045 Uiso 1 1 calc R . . H9B H 0.5834 -0.0012 0.2504 0.045 Uiso 1 1 calc R . . C10 C 0.6392(4) 0.0937(4) 0.4617(4) 0.0410(9) Uani 1 1 d U . . H10A H 0.6590 0.0150 0.4774 0.049 Uiso 1 1 calc R . . H10B H 0.5359 0.0817 0.4369 0.049 Uiso 1 1 calc R . . C11 C 0.7262(4) 0.2333(4) 0.6021(4) 0.0377(8) Uani 1 1 d U . . H11A H 0.6767 0.3041 0.6009 0.045 Uiso 1 1 calc R . . H11B H 0.7227 0.2152 0.6767 0.045 Uiso 1 1 calc R . . C12 C 0.9448(4) 0.4305(4) 0.7787(4) 0.0351(8) Uani 1 1 d U . . H12A H 0.9424 0.4033 0.8484 0.042 Uiso 1 1 calc R . . H12B H 0.8816 0.4899 0.7744 0.042 Uiso 1 1 calc R . . C13 C 0.9695(4) 0.1975(4) 0.6406(4) 0.0333(7) Uani 1 1 d U . . H13A H 0.9037 0.0995 0.5859 0.040 Uiso 1 1 calc R . . H13B H 1.0217 0.2174 0.7367 0.040 Uiso 1 1 calc R . . C14 C 1.0786(4) 0.2110(3) 0.5808(3) 0.0298(7) Uani 1 1 d U . . C15 C 0.5541(4) 0.2600(4) 0.3059(4) 0.0353(8) Uani 1 1 d U . . H15A H 0.4992 0.2235 0.3455 0.042 Uiso 1 1 calc R . . H15B H 0.4902 0.2233 0.2073 0.042 Uiso 1 1 calc R . . C16 C 0.5981(3) 0.4224(3) 0.3819(3) 0.0290(7) Uani 1 1 d U . . C17 C 1.0005(6) -0.0476(4) 0.1254(4) 0.0566(12) Uani 1 1 d U . . C18 C 1.1379(7) -0.0755(6) 0.1210(6) 0.0831(17) Uani 1 1 d U . . H18A H 1.1150 -0.1714 0.0471 0.125 Uiso 1 1 calc R . . H18B H 1.2005 -0.0655 0.2097 0.125 Uiso 1 1 calc R . . H18C H 1.1870 -0.0078 0.1033 0.125 Uiso 1 1 calc R . . N1 N 0.6813(3) 0.2059(3) 0.3162(3) 0.0293(6) Uani 1 1 d . . . N2 N 0.8819(3) 0.2974(3) 0.6391(3) 0.0303(6) Uani 1 1 d . . . O1 O 0.9734(2) 0.4030(2) 0.3448(2) 0.0221(5) Uani 1 1 d . . . O2 O 0.7305(2) 0.4900(2) 0.4776(2) 0.0318(5) Uani 1 1 d . . . O3 O 0.5053(2) 0.4808(2) 0.3545(3) 0.0372(6) Uani 1 1 d . . . O4 O 1.0127(3) 0.0730(3) 0.2160(3) 0.0535(8) Uani 1 1 d . . . O5 O 0.8815(5) -0.1433(4) 0.0430(3) 0.1015(16) Uani 1 1 d . . . O6 O 1.0568(2) 0.2752(2) 0.5075(2) 0.0322(5) Uani 1 1 d . . . O7 O 1.1760(3) 0.1572(3) 0.6003(3) 0.0425(6) Uani 1 1 d . . . O1W O 1.2188(3) 0.3172(3) 0.2232(2) 0.0397(6) Uani 1 1 d D . . H1WA H 1.179(4) 0.252(3) 0.1371(17) 0.059 Uiso 1 1 d D . . H1WB H 1.299(3) 0.378(3) 0.250(3) 0.059 Uiso 1 1 d D . . O2W O 1.3364(3) 0.2340(3) 0.4806(3) 0.0378(6) Uani 1 1 d D . . H2WA H 1.296(4) 0.200(4) 0.519(3) 0.057 Uiso 1 1 d D . . H2WB H 1.394(4) 0.319(2) 0.535(3) 0.057 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0288(3) 0.0304(3) 0.0263(3) 0.0126(2) 0.0109(2) 0.0115(2) Mn2 0.0234(3) 0.0266(3) 0.0239(2) 0.0145(2) 0.0082(2) 0.00992(19) C1 0.073(3) 0.089(3) 0.037(2) 0.037(2) 0.010(2) 0.041(3) C2 0.0472(19) 0.056(2) 0.0239(15) 0.0194(15) 0.0073(14) 0.0264(16) C3 0.057(2) 0.0482(19) 0.0277(15) 0.0245(15) 0.0165(15) 0.0256(16) C4 0.0396(17) 0.0385(16) 0.0235(14) 0.0173(13) 0.0153(13) 0.0206(14) C5 0.0330(16) 0.0349(16) 0.0182(13) 0.0138(12) 0.0114(12) 0.0187(13) C6 0.0325(16) 0.0379(16) 0.0232(14) 0.0123(12) 0.0095(12) 0.0154(13) C7 0.0367(17) 0.0440(18) 0.0285(15) 0.0125(14) 0.0061(14) 0.0142(14) C8 0.0293(16) 0.0293(15) 0.0281(15) 0.0085(12) 0.0058(13) 0.0067(13) C9 0.0345(17) 0.0291(16) 0.0458(18) 0.0184(14) 0.0130(15) 0.0099(13) C10 0.0377(18) 0.0401(18) 0.058(2) 0.0336(17) 0.0219(17) 0.0152(15) C11 0.0391(18) 0.0433(18) 0.0463(18) 0.0294(15) 0.0239(15) 0.0189(14) C12 0.0465(19) 0.0457(19) 0.0354(17) 0.0288(15) 0.0269(15) 0.0249(16) C13 0.0379(18) 0.0368(17) 0.0397(17) 0.0276(14) 0.0195(15) 0.0174(14) C14 0.0314(17) 0.0344(17) 0.0312(16) 0.0207(14) 0.0141(14) 0.0153(14) C15 0.0282(16) 0.0348(16) 0.0380(16) 0.0161(14) 0.0112(14) 0.0097(13) C16 0.0273(16) 0.0325(15) 0.0281(14) 0.0165(13) 0.0106(13) 0.0100(13) C17 0.094(4) 0.037(2) 0.040(2) 0.0183(19) 0.035(2) 0.009(2) C18 0.130(5) 0.068(3) 0.076(3) 0.038(3) 0.059(4) 0.054(3) N1 0.0276(14) 0.0235(13) 0.0330(14) 0.0130(11) 0.0104(12) 0.0078(11) N2 0.0345(15) 0.0358(15) 0.0345(15) 0.0241(13) 0.0190(13) 0.0174(12) O1 0.0193(10) 0.0265(11) 0.0185(10) 0.0115(9) 0.0053(8) 0.0073(8) O2 0.0230(11) 0.0310(12) 0.0298(11) 0.0103(10) 0.0045(10) 0.0086(9) O3 0.0266(12) 0.0392(13) 0.0422(13) 0.0221(11) 0.0068(11) 0.0148(10) O4 0.0475(16) 0.0310(14) 0.0490(16) 0.0004(13) 0.0151(14) -0.0024(12) O5 0.133(4) 0.063(2) 0.0415(18) -0.0055(17) 0.029(2) -0.035(2) O6 0.0341(13) 0.0419(13) 0.0356(12) 0.0269(11) 0.0175(11) 0.0219(11) O7 0.0380(14) 0.0561(16) 0.0588(16) 0.0440(14) 0.0233(13) 0.0287(12) O1W 0.0326(14) 0.0448(15) 0.0297(12) 0.0129(11) 0.0105(11) 0.0038(11) O2W 0.0361(14) 0.0392(14) 0.0436(14) 0.0234(12) 0.0177(12) 0.0169(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.047(2) . ? Mn1 O1W 2.123(3) . ? Mn1 O6 2.186(2) . ? Mn1 O2 2.235(2) 2_766 ? Mn1 O2W 2.237(3) . ? Mn1 O1 2.331(2) . ? Mn2 O6 2.135(2) . ? Mn2 O2 2.164(2) . ? Mn2 O1 2.197(2) 2_766 ? Mn2 O1 2.211(2) . ? Mn2 N1 2.235(3) . ? Mn2 N2 2.240(3) . ? Mn2 Mn2 3.1171(10) 2_766 ? C1 C2 1.506(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.372(6) . ? C2 C7 1.379(6) . ? C3 C4 1.411(5) . ? C3 H3 0.9300 . ? C4 C5 1.391(5) . ? C4 C12 1.506(5) 2_766 ? C5 O1 1.382(4) . ? C5 C6 1.408(5) . ? C6 C7 1.400(5) . ? C6 C8 1.499(5) . ? C7 H7 0.9300 . ? C8 N1 1.499(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.486(4) . ? C9 C10 1.522(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.531(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.483(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.489(4) . ? C12 C4 1.506(5) 2_766 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.488(4) . ? C13 C14 1.516(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O7 1.218(4) . ? C14 O6 1.282(4) . ? C15 N1 1.479(4) . ? C15 C16 1.513(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.230(4) . ? C16 O2 1.286(4) . ? C17 O5 1.235(5) . ? C17 O4 1.242(5) . ? C17 C18 1.485(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? O1 Mn2 2.1967(19) 2_766 ? O2 Mn1 2.235(2) 2_766 ? O1W H1WA 0.849(10) . ? O1W H1WB 0.847(10) . ? O2W H2WA 0.854(10) . ? O2W H2WB 0.848(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O1W 96.03(11) . . ? O4 Mn1 O6 89.80(10) . . ? O1W Mn1 O6 170.02(10) . . ? O4 Mn1 O2 174.31(10) . 2_766 ? O1W Mn1 O2 87.60(9) . 2_766 ? O6 Mn1 O2 86.00(9) . 2_766 ? O4 Mn1 O2W 98.80(11) . . ? O1W Mn1 O2W 100.18(10) . . ? O6 Mn1 O2W 86.87(9) . . ? O2 Mn1 O2W 84.81(9) 2_766 . ? O4 Mn1 O1 100.71(10) . . ? O1W Mn1 O1 96.13(9) . . ? O6 Mn1 O1 74.78(8) . . ? O2 Mn1 O1 74.48(7) 2_766 . ? O2W Mn1 O1 153.01(8) . . ? O6 Mn2 O2 176.92(9) . . ? O6 Mn2 O1 98.39(8) . 2_766 ? O2 Mn2 O1 78.66(8) . 2_766 ? O6 Mn2 O1 78.33(8) . . ? O2 Mn2 O1 100.66(9) . . ? O1 Mn2 O1 89.98(7) 2_766 . ? O6 Mn2 N1 106.98(9) . . ? O2 Mn2 N1 75.95(9) . . ? O1 Mn2 N1 154.61(9) 2_766 . ? O1 Mn2 N1 94.22(9) . . ? O6 Mn2 N2 75.56(9) . . ? O2 Mn2 N2 105.47(10) . . ? O1 Mn2 N2 95.01(9) 2_766 . ? O1 Mn2 N2 153.87(9) . . ? N1 Mn2 N2 92.16(10) . . ? O6 Mn2 Mn2 87.67(7) . 2_766 ? O2 Mn2 Mn2 89.58(7) . 2_766 ? O1 Mn2 Mn2 45.18(6) 2_766 2_766 ? O1 Mn2 Mn2 44.81(5) . 2_766 ? N1 Mn2 Mn2 133.54(8) . 2_766 ? N2 Mn2 Mn2 134.29(8) . 2_766 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.2(3) . . ? C3 C2 C1 121.5(4) . . ? C7 C2 C1 121.2(4) . . ? C2 C3 C4 122.9(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 C12 121.7(3) . 2_766 ? C3 C4 C12 119.2(3) . 2_766 ? O1 C5 C4 121.2(3) . . ? O1 C5 C6 119.1(3) . . ? C4 C5 C6 119.6(3) . . ? C7 C6 C5 118.7(3) . . ? C7 C6 C8 119.2(3) . . ? C5 C6 C8 121.6(3) . . ? C2 C7 C6 122.7(4) . . ? C2 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C6 C8 N1 116.0(3) . . ? C6 C8 H8A 108.3 . . ? N1 C8 H8A 108.3 . . ? C6 C8 H8B 108.3 . . ? N1 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? N1 C9 C10 116.1(3) . . ? N1 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? N1 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C9 C10 H10B 107.6 . . ? C11 C10 H10B 107.6 . . ? H10A C10 H10B 107.0 . . ? N2 C11 C10 116.9(3) . . ? N2 C11 H11A 108.1 . . ? C10 C11 H11A 108.1 . . ? N2 C11 H11B 108.1 . . ? C10 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? N2 C12 C4 116.3(3) . 2_766 ? N2 C12 H12A 108.2 . . ? C4 C12 H12A 108.2 2_766 . ? N2 C12 H12B 108.2 . . ? C4 C12 H12B 108.2 2_766 . ? H12A C12 H12B 107.4 . . ? N2 C13 C14 112.3(3) . . ? N2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? O7 C14 O6 124.6(3) . . ? O7 C14 C13 119.1(3) . . ? O6 C14 C13 116.2(3) . . ? N1 C15 C16 112.8(3) . . ? N1 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O3 C16 O2 124.3(3) . . ? O3 C16 C15 119.1(3) . . ? O2 C16 C15 116.5(3) . . ? O5 C17 O4 123.1(5) . . ? O5 C17 C18 120.0(4) . . ? O4 C17 C18 116.9(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 N1 C9 113.4(3) . . ? C15 N1 C8 110.1(3) . . ? C9 N1 C8 107.7(3) . . ? C15 N1 Mn2 111.74(18) . . ? C9 N1 Mn2 109.4(2) . . ? C8 N1 Mn2 104.09(19) . . ? C11 N2 C13 113.4(3) . . ? C11 N2 C12 107.8(3) . . ? C13 N2 C12 111.0(3) . . ? C11 N2 Mn2 108.5(2) . . ? C13 N2 Mn2 111.4(2) . . ? C12 N2 Mn2 104.2(2) . . ? C5 O1 Mn2 115.15(18) . 2_766 ? C5 O1 Mn2 116.18(18) . . ? Mn2 O1 Mn2 90.02(7) 2_766 . ? C5 O1 Mn1 127.26(18) . . ? Mn2 O1 Mn1 101.32(8) 2_766 . ? Mn2 O1 Mn1 99.73(8) . . ? C16 O2 Mn2 119.7(2) . . ? C16 O2 Mn1 134.6(2) . 2_766 ? Mn2 O2 Mn1 105.52(9) . 2_766 ? C17 O4 Mn1 147.3(3) . . ? C14 O6 Mn2 121.6(2) . . ? C14 O6 Mn1 130.8(2) . . ? Mn2 O6 Mn1 107.00(10) . . ? Mn1 O1W H1WA 117(2) . . ? Mn1 O1W H1WB 124(2) . . ? H1WA O1W H1WB 116.2(18) . . ? Mn1 O2W H2WA 98(3) . . ? Mn1 O2W H2WB 99(3) . . ? H2WA O2W H2WB 114.4(18) . . ? 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 C7 C2 C3 C4 -2.4(6) . . . . ? C1 C2 C3 C4 -178.8(4) . . . . ? C2 C3 C4 C5 -1.5(5) . . . . ? C2 C3 C4 C12 170.3(3) . . . 2_766 ? C3 C4 C5 O1 -175.0(3) . . . . ? C12 C4 C5 O1 13.5(5) 2_766 . . . ? C3 C4 C5 C6 5.6(5) . . . . ? C12 C4 C5 C6 -165.9(3) 2_766 . . . ? O1 C5 C6 C7 174.8(3) . . . . ? C4 C5 C6 C7 -5.8(5) . . . . ? O1 C5 C6 C8 -13.6(4) . . . . ? C4 C5 C6 C8 165.8(3) . . . . ? C3 C2 C7 C6 2.2(6) . . . . ? C1 C2 C7 C6 178.6(4) . . . . ? C5 C6 C7 C2 1.8(5) . . . . ? C8 C6 C7 C2 -169.9(3) . . . . ? C7 C6 C8 N1 -109.9(4) . . . . ? C5 C6 C8 N1 78.5(4) . . . . ? N1 C9 C10 C11 -41.0(5) . . . . ? C9 C10 C11 N2 -39.1(5) . . . . ? N2 C13 C14 O7 165.8(3) . . . . ? N2 C13 C14 O6 -16.8(4) . . . . ? N1 C15 C16 O3 162.9(3) . . . . ? N1 C15 C16 O2 -20.8(5) . . . . ? C16 C15 N1 C9 141.3(3) . . . . ? C16 C15 N1 C8 -98.1(3) . . . . ? C16 C15 N1 Mn2 17.1(4) . . . . ? C10 C9 N1 C15 -57.5(4) . . . . ? C10 C9 N1 C8 -179.5(3) . . . . ? C10 C9 N1 Mn2 67.9(3) . . . . ? C6 C8 N1 C15 59.3(4) . . . . ? C6 C8 N1 C9 -176.6(3) . . . . ? C6 C8 N1 Mn2 -60.6(3) . . . . ? O6 Mn2 N1 C15 172.9(2) . . . . ? O2 Mn2 N1 C15 -8.1(2) . . . . ? O1 Mn2 N1 C15 -9.1(4) 2_766 . . . ? O1 Mn2 N1 C15 -108.1(2) . . . . ? N2 Mn2 N1 C15 97.3(2) . . . . ? Mn2 Mn2 N1 C15 -83.7(2) 2_766 . . . ? O6 Mn2 N1 C9 46.5(2) . . . . ? O2 Mn2 N1 C9 -134.5(2) . . . . ? O1 Mn2 N1 C9 -135.5(2) 2_766 . . . ? O1 Mn2 N1 C9 125.6(2) . . . . ? N2 Mn2 N1 C9 -29.1(2) . . . . ? Mn2 Mn2 N1 C9 149.87(18) 2_766 . . . ? O6 Mn2 N1 C8 -68.4(2) . . . . ? O2 Mn2 N1 C8 110.7(2) . . . . ? O1 Mn2 N1 C8 109.6(3) 2_766 . . . ? O1 Mn2 N1 C8 10.73(19) . . . . ? N2 Mn2 N1 C8 -143.9(2) . . . . ? Mn2 Mn2 N1 C8 35.0(2) 2_766 . . . ? C10 C11 N2 C13 -56.3(4) . . . . ? C10 C11 N2 C12 -179.6(3) . . . . ? C10 C11 N2 Mn2 68.0(3) . . . . ? C14 C13 N2 C11 141.2(3) . . . . ? C14 C13 N2 C12 -97.3(3) . . . . ? C14 C13 N2 Mn2 18.5(3) . . . . ? C4 C12 N2 C11 -174.3(3) 2_766 . . . ? C4 C12 N2 C13 61.0(4) 2_766 . . . ? C4 C12 N2 Mn2 -59.1(3) 2_766 . . . ? O6 Mn2 N2 C11 -137.4(2) . . . . ? O2 Mn2 N2 C11 45.6(2) . . . . ? O1 Mn2 N2 C11 125.2(2) 2_766 . . . ? O1 Mn2 N2 C11 -134.6(2) . . . . ? N1 Mn2 N2 C11 -30.4(2) . . . . ? Mn2 Mn2 N2 C11 150.61(17) 2_766 . . . ? O6 Mn2 N2 C13 -11.9(2) . . . . ? O2 Mn2 N2 C13 171.1(2) . . . . ? O1 Mn2 N2 C13 -109.3(2) 2_766 . . . ? O1 Mn2 N2 C13 -9.1(3) . . . . ? N1 Mn2 N2 C13 95.0(2) . . . . ? Mn2 Mn2 N2 C13 -83.9(2) 2_766 . . . ? O6 Mn2 N2 C12 107.9(2) . . . . ? O2 Mn2 N2 C12 -69.1(2) . . . . ? O1 Mn2 N2 C12 10.5(2) 2_766 . . . ? O1 Mn2 N2 C12 110.8(2) . . . . ? N1 Mn2 N2 C12 -145.1(2) . . . . ? Mn2 Mn2 N2 C12 35.9(2) 2_766 . . . ? C4 C5 O1 Mn2 38.0(3) . . . 2_766 ? C6 C5 O1 Mn2 -142.6(2) . . . 2_766 ? C4 C5 O1 Mn2 141.4(2) . . . . ? C6 C5 O1 Mn2 -39.3(3) . . . . ? C4 C5 O1 Mn1 -91.0(3) . . . . ? C6 C5 O1 Mn1 88.4(3) . . . . ? O6 Mn2 O1 C5 143.2(2) . . . . ? O2 Mn2 O1 C5 -39.8(2) . . . . ? O1 Mn2 O1 C5 -118.3(2) 2_766 . . . ? N1 Mn2 O1 C5 36.7(2) . . . . ? N2 Mn2 O1 C5 140.3(2) . . . . ? Mn2 Mn2 O1 C5 -118.3(2) 2_766 . . . ? O6 Mn2 O1 Mn2 -98.57(8) . . . 2_766 ? O2 Mn2 O1 Mn2 78.46(8) . . . 2_766 ? O1 Mn2 O1 Mn2 0.0 2_766 . . 2_766 ? N1 Mn2 O1 Mn2 154.94(9) . . . 2_766 ? N2 Mn2 O1 Mn2 -101.4(2) . . . 2_766 ? O6 Mn2 O1 Mn1 2.92(8) . . . . ? O2 Mn2 O1 Mn1 179.95(7) . . . . ? O1 Mn2 O1 Mn1 101.49(8) 2_766 . . . ? N1 Mn2 O1 Mn1 -103.57(9) . . . . ? N2 Mn2 O1 Mn1 0.1(2) . . . . ? Mn2 Mn2 O1 Mn1 101.49(8) 2_766 . . . ? O4 Mn1 O1 C5 -49.9(3) . . . . ? O1W Mn1 O1 C5 47.4(2) . . . . ? O6 Mn1 O1 C5 -136.7(2) . . . . ? O2 Mn1 O1 C5 133.2(3) 2_766 . . . ? O2W Mn1 O1 C5 174.5(2) . . . . ? O4 Mn1 O1 Mn2 175.93(10) . . . 2_766 ? O1W Mn1 O1 Mn2 -86.73(9) . . . 2_766 ? O6 Mn1 O1 Mn2 89.09(9) . . . 2_766 ? O2 Mn1 O1 Mn2 -0.94(9) 2_766 . . 2_766 ? O2W Mn1 O1 Mn2 40.3(2) . . . 2_766 ? O4 Mn1 O1 Mn2 83.95(11) . . . . ? O1W Mn1 O1 Mn2 -178.71(8) . . . . ? O6 Mn1 O1 Mn2 -2.89(8) . . . . ? O2 Mn1 O1 Mn2 -92.92(9) 2_766 . . . ? O2W Mn1 O1 Mn2 -51.7(2) . . . . ? O3 C16 O2 Mn2 -169.7(3) . . . . ? C15 C16 O2 Mn2 14.2(4) . . . . ? O3 C16 O2 Mn1 3.8(6) . . . 2_766 ? C15 C16 O2 Mn1 -172.3(2) . . . 2_766 ? O6 Mn2 O2 C16 159.1(16) . . . . ? O1 Mn2 O2 C16 176.2(3) 2_766 . . . ? O1 Mn2 O2 C16 88.4(2) . . . . ? N1 Mn2 O2 C16 -3.3(2) . . . . ? N2 Mn2 O2 C16 -91.7(3) . . . . ? Mn2 Mn2 O2 C16 132.0(2) 2_766 . . . ? O6 Mn2 O2 Mn1 -16.1(18) . . . 2_766 ? O1 Mn2 O2 Mn1 1.01(9) 2_766 . . 2_766 ? O1 Mn2 O2 Mn1 -86.81(10) . . . 2_766 ? N1 Mn2 O2 Mn1 -178.53(13) . . . 2_766 ? N2 Mn2 O2 Mn1 93.13(11) . . . 2_766 ? Mn2 Mn2 O2 Mn1 -43.14(9) 2_766 . . 2_766 ? O5 C17 O4 Mn1 -167.9(4) . . . . ? C18 C17 O4 Mn1 13.5(8) . . . . ? O1W Mn1 O4 C17 48.8(6) . . . . ? O6 Mn1 O4 C17 -139.3(6) . . . . ? O2 Mn1 O4 C17 178.3(9) 2_766 . . . ? O2W Mn1 O4 C17 -52.5(6) . . . . ? O1 Mn1 O4 C17 146.3(5) . . . . ? O7 C14 O6 Mn2 -176.5(3) . . . . ? C13 C14 O6 Mn2 6.3(4) . . . . ? O7 C14 O6 Mn1 13.4(5) . . . . ? C13 C14 O6 Mn1 -163.8(2) . . . . ? O2 Mn2 O6 C14 113.3(17) . . . . ? O1 Mn2 O6 C14 96.4(2) 2_766 . . . ? O1 Mn2 O6 C14 -175.4(2) . . . . ? N1 Mn2 O6 C14 -84.5(2) . . . . ? N2 Mn2 O6 C14 3.3(2) . . . . ? Mn2 Mn2 O6 C14 140.4(2) 2_766 . . . ? O2 Mn2 O6 Mn1 -74.5(17) . . . . ? O1 Mn2 O6 Mn1 -91.45(10) 2_766 . . . ? O1 Mn2 O6 Mn1 -3.21(8) . . . . ? N1 Mn2 O6 Mn1 87.68(12) . . . . ? N2 Mn2 O6 Mn1 175.50(12) . . . . ? Mn2 Mn2 O6 Mn1 -47.43(8) 2_766 . . . ? O4 Mn1 O6 C14 73.1(3) . . . . ? O1W Mn1 O6 C14 -161.0(5) . . . . ? O2 Mn1 O6 C14 -110.7(3) 2_766 . . . ? O2W Mn1 O6 C14 -25.7(3) . . . . ? O1 Mn1 O6 C14 174.3(3) . . . . ? O4 Mn1 O6 Mn2 -98.07(12) . . . . ? O1W Mn1 O6 Mn2 27.8(6) . . . . ? O2 Mn1 O6 Mn2 78.09(10) 2_766 . . . ? O2W Mn1 O6 Mn2 163.10(11) . . . . ? O1 Mn1 O6 Mn2 3.09(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O3 0.847(10) 1.921(19) 2.724(3) 158(4) 1_655 O2W H2WB O3 0.848(10) 1.893(13) 2.732(3) 170(4) 2_766 O1W H1WA O5 0.849(10) 1.737(14) 2.575(4) 169(4) 2_755 O2W H2WA O7 0.854(10) 1.887(16) 2.721(4) 165(4) . _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.833 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.101 data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 922856' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H48 Co4 N4 O17), H2 O ' _chemical_formula_sum 'C80 H98 Co8 N8 O35' _chemical_formula_weight 2203.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.706(5) _cell_length_b 13.774(5) _cell_length_c 14.198(5) _cell_angle_alpha 79.814(5) _cell_angle_beta 69.227(5) _cell_angle_gamma 79.861(5) _cell_volume 2269.3(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10243 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.261 _exptl_crystal_size_mid 0.257 _exptl_crystal_size_min 0.246 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1130 _exptl_absorpt_coefficient_mu 1.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22444 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10243 _reflns_number_gt 6600 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+2.9195P] 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 10243 _refine_ls_number_parameters 595 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _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 0.26998(5) 0.35090(4) 0.75775(4) 0.02579(14) Uani 1 1 d . . . Co2 Co 0.14412(5) 0.20470(4) 0.96994(4) 0.02786(15) Uani 1 1 d . . . Co3 Co 0.43644(5) 0.26143(4) 0.54594(4) 0.02963(15) Uani 1 1 d . . . Co4 Co 0.30857(5) 0.12059(4) 0.75204(4) 0.02584(14) Uani 1 1 d . . . C1 C -0.1573(6) 0.2733(6) 0.5928(6) 0.087(2) Uani 1 1 d . . . H1A H -0.1933 0.3408 0.5916 0.131 Uiso 1 1 calc R . . H1B H -0.2039 0.2327 0.6489 0.131 Uiso 1 1 calc R . . H1C H -0.1474 0.2491 0.5305 0.131 Uiso 1 1 calc R . . C2 C -0.0421(5) 0.2694(5) 0.6047(5) 0.0577(15) Uani 1 1 d . . . C3 C -0.0017(4) 0.3544(4) 0.6121(4) 0.0468(12) Uani 1 1 d . . . H3 H -0.0451 0.4157 0.6067 0.056 Uiso 1 1 calc R . . C4 C 0.1009(4) 0.3506(3) 0.6271(3) 0.0371(10) Uani 1 1 d . . . C5 C 0.1655(4) 0.2584(3) 0.6386(3) 0.0303(9) Uani 1 1 d . . . C6 C 0.1318(4) 0.1720(3) 0.6223(3) 0.0374(10) Uani 1 1 d . . . C7 C 0.0277(5) 0.1789(4) 0.6083(4) 0.0511(13) Uani 1 1 d . . . H7 H 0.0037 0.1215 0.6011 0.061 Uiso 1 1 calc R . . C8 C 0.2127(4) 0.0771(3) 0.6074(4) 0.0391(11) Uani 1 1 d . . . H8A H 0.1840 0.0338 0.5778 0.047 Uiso 1 1 calc R . . H8B H 0.2853 0.0932 0.5589 0.047 Uiso 1 1 calc R . . C9 C 0.3093(4) -0.0714(3) 0.6719(4) 0.0418(11) Uani 1 1 d . . . H9A H 0.3784 -0.0526 0.6194 0.050 Uiso 1 1 calc R . . H9B H 0.2736 -0.1089 0.6424 0.050 Uiso 1 1 calc R . . C10 C 0.3413(5) -0.1395(3) 0.7572(4) 0.0463(12) Uani 1 1 d . . . H10A H 0.4091 -0.1832 0.7262 0.056 Uiso 1 1 calc R . . H10B H 0.2811 -0.1809 0.7921 0.056 Uiso 1 1 calc R . . C11 C 0.3632(4) -0.0923(3) 0.8378(4) 0.0404(11) Uani 1 1 d . . . H11A H 0.2911 -0.0766 0.8900 0.048 Uiso 1 1 calc R . . H11B H 0.4094 -0.1413 0.8694 0.048 Uiso 1 1 calc R . . C12 C 0.4416(4) 0.0269(3) 0.8875(3) 0.0336(10) Uani 1 1 d . . . H12A H 0.4940 -0.0256 0.9076 0.040 Uiso 1 1 calc R . . H12B H 0.3707 0.0298 0.9439 0.040 Uiso 1 1 calc R . . C13 C 0.4890(4) 0.1246(3) 0.8691(3) 0.0330(10) Uani 1 1 d . . . C14 C 0.5970(4) 0.1248(4) 0.8740(4) 0.0418(11) Uani 1 1 d . . . H14 H 0.6441 0.0650 0.8750 0.050 Uiso 1 1 calc R . . C15 C 0.6360(4) 0.2121(4) 0.8774(4) 0.0468(12) Uani 1 1 d . . . C16 C 0.7538(5) 0.2111(5) 0.8813(6) 0.074(2) Uani 1 1 d . . . H16A H 0.7933 0.1450 0.8767 0.111 Uiso 1 1 calc R . . H16B H 0.7481 0.2321 0.9441 0.111 Uiso 1 1 calc R . . H16C H 0.7948 0.2556 0.8255 0.111 Uiso 1 1 calc R . . C17 C 0.5617(4) 0.2979(4) 0.8824(4) 0.0442(12) Uani 1 1 d . . . H17 H 0.5847 0.3559 0.8893 0.053 Uiso 1 1 calc R . . C18 C 0.4540(4) 0.3020(3) 0.8778(3) 0.0330(10) Uani 1 1 d . . . C19 C 0.4192(3) 0.2152(3) 0.8639(3) 0.0281(9) Uani 1 1 d . . . C20 C 0.3714(4) 0.3948(3) 0.8969(3) 0.0372(10) Uani 1 1 d . . . H20A H 0.3008 0.3765 0.9473 0.045 Uiso 1 1 calc R . . H20B H 0.4010 0.4379 0.9261 0.045 Uiso 1 1 calc R . . C21 C 0.2644(4) 0.5413(3) 0.8435(4) 0.0406(11) Uani 1 1 d . . . H21A H 0.2985 0.5780 0.8751 0.049 Uiso 1 1 calc R . . H21B H 0.1968 0.5185 0.8952 0.049 Uiso 1 1 calc R . . C22 C 0.2290(5) 0.6122(3) 0.7607(4) 0.0477(13) Uani 1 1 d . . . H22A H 0.1580 0.6514 0.7934 0.057 Uiso 1 1 calc R . . H22B H 0.2855 0.6577 0.7288 0.057 Uiso 1 1 calc R . . C23 C 0.2139(4) 0.5660(3) 0.6776(4) 0.0401(11) Uani 1 1 d . . . H23A H 0.1685 0.6148 0.6450 0.048 Uiso 1 1 calc R . . H23B H 0.2879 0.5530 0.6270 0.048 Uiso 1 1 calc R . . C24 C 0.1477(4) 0.4462(3) 0.6166(4) 0.0386(11) Uani 1 1 d . . . H24A H 0.2217 0.4434 0.5641 0.046 Uiso 1 1 calc R . . H24B H 0.0988 0.4999 0.5931 0.046 Uiso 1 1 calc R . . C25 C 0.5303(4) -0.0163(3) 0.7166(3) 0.0357(10) Uani 1 1 d . . . H25A H 0.5304 -0.0725 0.6839 0.043 Uiso 1 1 calc R . . H25B H 0.5912 -0.0319 0.7450 0.043 Uiso 1 1 calc R . . C26 C 0.5514(4) 0.0743(3) 0.6385(3) 0.0362(10) Uani 1 1 d . . . C27 C 0.4519(4) 0.4797(3) 0.7270(4) 0.0381(11) Uani 1 1 d . . . H27A H 0.5076 0.4823 0.7584 0.046 Uiso 1 1 calc R . . H27B H 0.4374 0.5453 0.6924 0.046 Uiso 1 1 calc R . . C28 C 0.4997(4) 0.4067(3) 0.6501(4) 0.0351(10) Uani 1 1 d . . . C29 C 0.0492(4) 0.4827(3) 0.7899(4) 0.0422(11) Uani 1 1 d . . . H29A H -0.0100 0.4882 0.7602 0.051 Uiso 1 1 calc R . . H29B H 0.0409 0.5440 0.8179 0.051 Uiso 1 1 calc R . . C30 C 0.0318(4) 0.3980(3) 0.8753(3) 0.0343(10) Uani 1 1 d . . . C31 C 0.1219(4) -0.0023(3) 0.7781(3) 0.0387(11) Uani 1 1 d . . . H31A H 0.1315 -0.0686 0.8134 0.046 Uiso 1 1 calc R . . H31B H 0.0676 -0.0015 0.7441 0.046 Uiso 1 1 calc R . . C32 C 0.0762(4) 0.0715(3) 0.8542(3) 0.0304(9) Uani 1 1 d . . . C33 C 0.3680(4) 0.3041(3) 0.4007(3) 0.0298(9) Uani 1 1 d . . . C34 C 0.3165(4) 0.3389(3) 0.3199(3) 0.0313(9) Uani 1 1 d . . . C35 C 0.2953(4) 0.2720(3) 0.2680(3) 0.0377(11) Uani 1 1 d . . . H35 H 0.3122 0.2041 0.2848 0.045 Uiso 1 1 calc R . . C36 C 0.2489(4) 0.3061(3) 0.1907(3) 0.0357(10) Uani 1 1 d . . . C37 C 0.2255(4) 0.4070(3) 0.1661(3) 0.0347(10) Uani 1 1 d . . . H37 H 0.1969 0.4304 0.1133 0.042 Uiso 1 1 calc R . . C38 C 0.2441(4) 0.4740(3) 0.2190(4) 0.0381(11) Uani 1 1 d . . . H38 H 0.2266 0.5419 0.2025 0.046 Uiso 1 1 calc R . . C39 C 0.2882(4) 0.4404(3) 0.2954(3) 0.0340(10) Uani 1 1 d . . . H39 H 0.2994 0.4856 0.3314 0.041 Uiso 1 1 calc R . . C40 C 0.2243(5) 0.2328(4) 0.1366(4) 0.0446(12) Uani 1 1 d . . . N1 N 0.2321(3) 0.0207(3) 0.7016(3) 0.0322(8) Uani 1 1 d . . . N2 N 0.1601(3) 0.4721(3) 0.7088(3) 0.0347(8) Uani 1 1 d . . . N3 N 0.4203(3) -0.0005(3) 0.7996(3) 0.0320(8) Uani 1 1 d . . . N4 N 0.3455(3) 0.4531(3) 0.8069(3) 0.0309(8) Uani 1 1 d . . . O1 O 0.2621(2) 0.2520(2) 0.6616(2) 0.0273(6) Uani 1 1 d . . . O2 O 0.3189(2) 0.2175(2) 0.8488(2) 0.0264(6) Uani 1 1 d . . . O3 O 0.1457(2) 0.1270(2) 0.8565(2) 0.0319(7) Uani 1 1 d . . . O4 O -0.0234(3) 0.0731(2) 0.9125(3) 0.0406(8) Uani 1 1 d . . . O5 O 0.1214(2) 0.3373(2) 0.8771(2) 0.0323(7) Uani 1 1 d . . . O6 O -0.0622(3) 0.3917(3) 0.9384(3) 0.0618(11) Uani 1 1 d . . . O7 O 0.4609(2) 0.1330(2) 0.6343(2) 0.0338(7) Uani 1 1 d . . . O8 O 0.6477(3) 0.0859(3) 0.5804(3) 0.0511(9) Uani 1 1 d . . . O9 O 0.4278(2) 0.3520(2) 0.6483(2) 0.0328(7) Uani 1 1 d . . . O10 O 0.5983(3) 0.4037(3) 0.5933(3) 0.0540(10) Uani 1 1 d . . . O11 O 0.3835(3) 0.3679(2) 0.4463(2) 0.0400(8) Uani 1 1 d . . . O12 O 0.3948(3) 0.2130(2) 0.4255(2) 0.0358(7) Uani 1 1 d . . . O14 O 0.2466(5) 0.1414(3) 0.1622(4) 0.0921(18) Uani 1 1 d . . . O13 O 0.1801(3) 0.2686(2) 0.0697(2) 0.0377(7) Uani 1 1 d . . . O1W O -0.0366(3) 0.2077(2) 1.0390(2) 0.0428(8) Uani 1 1 d D . . H1WA H -0.0609 0.2651 1.0125 0.064 Uiso 1 1 d RD . . H1WB H -0.0524 0.1642 1.0116 0.064 Uiso 1 1 d RD . . O2W O 0.1732(3) 0.0640(2) 1.0473(2) 0.0372(7) Uani 1 1 d D . . H2WA H 0.1849 0.0809 1.0945 0.056 Uiso 1 1 d RD . . H2WB H 0.1155 0.0389 1.0608 0.056 Uiso 1 1 d RD . . O3W O 0.6132(3) 0.2667(2) 0.4726(2) 0.0413(8) Uani 1 1 d D . . H3WA H 0.6258 0.3191 0.4860 0.062 Uiso 1 1 d RD . . H3WB H 0.6383 0.2167 0.5056 0.062 Uiso 1 1 d RD . . O4W O 0.8524(9) 0.9823(9) 0.6333(9) 0.110(4) Uani 0.50 1 d PD . . H4WA H 0.9000 0.9629 0.6713 0.165 Uiso 1 1 d RD . . 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 0.0240(3) 0.0276(3) 0.0262(3) -0.0032(2) -0.0080(2) -0.0054(2) Co2 0.0300(3) 0.0323(3) 0.0245(3) -0.0040(2) -0.0105(2) -0.0086(2) Co3 0.0338(3) 0.0343(3) 0.0225(3) -0.0025(2) -0.0105(2) -0.0075(3) Co4 0.0274(3) 0.0271(3) 0.0245(3) -0.0039(2) -0.0091(2) -0.0055(2) C1 0.064(4) 0.105(6) 0.120(6) 0.007(5) -0.067(5) -0.021(4) C2 0.047(3) 0.073(4) 0.067(4) 0.003(3) -0.038(3) -0.016(3) C3 0.038(3) 0.055(3) 0.049(3) 0.002(2) -0.023(2) -0.001(2) C4 0.040(3) 0.039(2) 0.037(3) 0.002(2) -0.021(2) -0.007(2) C5 0.029(2) 0.040(2) 0.026(2) -0.0047(18) -0.0134(18) -0.0056(18) C6 0.038(3) 0.045(3) 0.034(2) -0.002(2) -0.015(2) -0.013(2) C7 0.052(3) 0.058(3) 0.060(3) -0.006(3) -0.035(3) -0.017(3) C8 0.048(3) 0.041(3) 0.035(3) -0.004(2) -0.021(2) -0.011(2) C9 0.051(3) 0.038(3) 0.037(3) -0.016(2) -0.012(2) -0.003(2) C10 0.052(3) 0.030(2) 0.057(3) -0.010(2) -0.017(3) -0.003(2) C11 0.050(3) 0.028(2) 0.040(3) 0.0028(19) -0.014(2) -0.007(2) C12 0.039(3) 0.036(2) 0.026(2) -0.0017(18) -0.0129(19) 0.000(2) C13 0.031(2) 0.039(2) 0.026(2) -0.0011(18) -0.0091(18) -0.0025(19) C14 0.028(2) 0.053(3) 0.043(3) -0.001(2) -0.017(2) 0.004(2) C15 0.028(2) 0.061(3) 0.054(3) 0.010(3) -0.022(2) -0.012(2) C16 0.043(3) 0.087(5) 0.100(5) 0.018(4) -0.042(4) -0.019(3) C17 0.043(3) 0.049(3) 0.053(3) 0.001(2) -0.028(2) -0.018(2) C18 0.033(2) 0.038(2) 0.033(2) -0.0012(19) -0.0160(19) -0.0099(19) C19 0.026(2) 0.038(2) 0.024(2) -0.0020(17) -0.0109(17) -0.0069(18) C20 0.039(3) 0.043(3) 0.037(3) -0.012(2) -0.014(2) -0.014(2) C21 0.039(3) 0.038(3) 0.047(3) -0.013(2) -0.013(2) -0.005(2) C22 0.052(3) 0.030(2) 0.058(3) -0.008(2) -0.015(3) 0.000(2) C23 0.047(3) 0.027(2) 0.042(3) 0.0017(19) -0.011(2) -0.006(2) C24 0.041(3) 0.036(2) 0.039(3) 0.004(2) -0.019(2) -0.003(2) C25 0.039(3) 0.031(2) 0.034(2) -0.0066(19) -0.013(2) 0.0069(19) C26 0.037(3) 0.036(2) 0.033(2) -0.0091(19) -0.009(2) -0.001(2) C27 0.033(2) 0.038(2) 0.044(3) -0.010(2) -0.006(2) -0.016(2) C28 0.031(2) 0.033(2) 0.041(3) -0.0053(19) -0.009(2) -0.0070(19) C29 0.030(2) 0.039(3) 0.050(3) -0.005(2) -0.010(2) 0.004(2) C30 0.026(2) 0.035(2) 0.036(2) -0.0017(19) -0.0062(19) -0.0007(18) C31 0.048(3) 0.036(2) 0.037(3) -0.004(2) -0.013(2) -0.019(2) C32 0.035(2) 0.031(2) 0.030(2) 0.0022(17) -0.0169(19) -0.0090(18) C33 0.030(2) 0.041(2) 0.022(2) -0.0074(18) -0.0085(17) -0.0086(19) C34 0.031(2) 0.039(2) 0.029(2) -0.0064(18) -0.0163(19) -0.0036(19) C35 0.051(3) 0.031(2) 0.041(3) -0.0088(19) -0.026(2) -0.001(2) C36 0.042(3) 0.035(2) 0.040(3) -0.012(2) -0.023(2) 0.000(2) C37 0.037(3) 0.037(2) 0.035(2) -0.0056(19) -0.019(2) 0.000(2) C38 0.043(3) 0.033(2) 0.046(3) -0.005(2) -0.025(2) -0.002(2) C39 0.030(2) 0.037(2) 0.040(2) -0.013(2) -0.013(2) -0.0056(19) C40 0.062(3) 0.039(3) 0.047(3) -0.010(2) -0.037(3) 0.000(2) N1 0.038(2) 0.0299(18) 0.0318(19) -0.0078(15) -0.0112(16) -0.0093(16) N2 0.033(2) 0.0333(19) 0.035(2) -0.0003(16) -0.0103(17) -0.0014(16) N3 0.035(2) 0.0291(18) 0.0300(19) -0.0038(15) -0.0094(16) -0.0035(16) N4 0.0304(19) 0.0301(18) 0.033(2) -0.0068(15) -0.0079(16) -0.0080(15) O1 0.0277(15) 0.0306(15) 0.0289(15) -0.0028(12) -0.0156(12) -0.0047(12) O2 0.0212(14) 0.0334(15) 0.0276(15) -0.0046(12) -0.0107(12) -0.0045(12) O3 0.0313(16) 0.0384(16) 0.0308(16) -0.0084(13) -0.0109(13) -0.0118(13) O4 0.0303(17) 0.0475(19) 0.048(2) -0.0093(15) -0.0119(15) -0.0146(14) O5 0.0263(15) 0.0347(16) 0.0334(16) -0.0026(13) -0.0086(13) -0.0019(13) O6 0.0308(19) 0.060(2) 0.067(3) 0.007(2) 0.0039(18) 0.0063(17) O7 0.0290(16) 0.0370(16) 0.0297(16) 0.0008(13) -0.0067(13) -0.0011(13) O8 0.0324(19) 0.055(2) 0.048(2) 0.0054(17) 0.0003(16) 0.0018(16) O9 0.0286(16) 0.0421(17) 0.0314(16) -0.0090(13) -0.0087(13) -0.0124(13) O10 0.0287(18) 0.057(2) 0.071(3) -0.0290(19) 0.0039(17) -0.0150(16) O11 0.059(2) 0.0357(17) 0.0357(17) -0.0069(14) -0.0267(16) -0.0074(15) O12 0.049(2) 0.0333(16) 0.0314(16) -0.0021(13) -0.0222(15) -0.0040(14) O14 0.170(5) 0.041(2) 0.121(4) -0.014(2) -0.124(4) 0.005(3) O13 0.049(2) 0.0383(17) 0.0355(17) -0.0049(14) -0.0241(16) -0.0088(15) O1W 0.0354(18) 0.0475(19) 0.0423(19) -0.0061(15) -0.0071(15) -0.0090(15) O2W 0.0424(19) 0.0368(17) 0.0377(17) -0.0005(13) -0.0168(15) -0.0157(14) O3W 0.0398(19) 0.0465(19) 0.0330(17) -0.0040(14) -0.0049(15) -0.0097(15) O4W 0.071(7) 0.145(10) 0.114(9) 0.032(7) -0.036(7) -0.053(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.053(3) . ? Co1 O9 2.057(3) . ? Co1 O1 2.128(3) . ? Co1 N2 2.163(4) . ? Co1 N4 2.165(3) . ? Co1 O2 2.182(3) . ? Co2 O13 2.008(3) 1_556 ? Co2 O3 2.078(3) . ? Co2 O2W 2.093(3) . ? Co2 O5 2.095(3) . ? Co2 O1W 2.149(3) . ? Co2 O2 2.290(3) . ? Co3 O7 2.025(3) . ? Co3 O9 2.040(3) . ? Co3 O11 2.049(3) . ? Co3 O3W 2.123(3) . ? Co3 O12 2.196(3) . ? Co3 O1 2.250(3) . ? Co3 C33 2.453(4) . ? Co4 O7 2.071(3) . ? Co4 O3 2.072(3) . ? Co4 O2 2.127(3) . ? Co4 O1 2.148(3) . ? Co4 N1 2.159(3) . ? Co4 N3 2.168(4) . ? C1 C2 1.522(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.392(8) . ? C2 C7 1.401(8) . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.403(6) . ? C4 C24 1.501(6) . ? C5 O1 1.364(5) . ? C5 C6 1.414(6) . ? C6 C7 1.390(7) . ? C6 C8 1.510(7) . ? C7 H7 0.9300 . ? C8 N1 1.500(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.486(6) . ? C9 C10 1.525(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.536(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N3 1.492(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.488(5) . ? C12 C13 1.513(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.399(6) . ? C13 C19 1.406(6) . ? C14 C15 1.393(7) . ? C14 H14 0.9300 . ? C15 C17 1.372(7) . ? C15 C16 1.515(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.384(6) . ? C17 H17 0.9300 . ? C18 C19 1.413(6) . ? C18 C20 1.502(6) . ? C19 O2 1.360(5) . ? C20 N4 1.493(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.487(6) . ? C21 C22 1.534(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.517(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N2 1.493(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N2 1.483(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N3 1.484(5) . ? C25 C26 1.508(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O8 1.229(5) . ? C26 O7 1.297(5) . ? C27 N4 1.479(5) . ? C27 C28 1.508(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O10 1.224(5) . ? C28 O9 1.292(5) . ? C29 N2 1.472(6) . ? C29 C30 1.511(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O6 1.219(5) . ? C30 O5 1.294(5) . ? C31 N1 1.482(6) . ? C31 C32 1.507(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O4 1.241(5) . ? C32 O3 1.278(5) . ? C33 O11 1.259(5) . ? C33 O12 1.262(5) . ? C33 C34 1.484(6) . ? C34 C35 1.389(6) . ? C34 C39 1.395(6) . ? C35 C36 1.397(6) . ? C35 H35 0.9300 . ? C36 C37 1.377(6) . ? C36 C40 1.503(6) . ? C37 C38 1.387(6) . ? C37 H37 0.9300 . ? C38 C39 1.366(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O13 1.255(5) . ? C40 O14 1.259(6) . ? O13 Co2 2.008(3) 1_554 ? O1W H1WA 0.8682 . ? O1W H1WB 0.8563 . ? O2W H2WA 0.8151 . ? O2W H2WB 0.8117 . ? O3W H3WA 0.8329 . ? O3W H3WB 0.8426 . ? O4W H4WA 0.9221 . ? 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 O9 173.19(12) . . ? O5 Co1 O1 102.20(11) . . ? O9 Co1 O1 78.48(11) . . ? O5 Co1 N2 79.79(13) . . ? O9 Co1 N2 106.95(13) . . ? O1 Co1 N2 95.19(13) . . ? O5 Co1 N4 101.47(13) . . ? O9 Co1 N4 77.77(12) . . ? O1 Co1 N4 156.24(12) . . ? N2 Co1 N4 91.06(14) . . ? O5 Co1 O2 78.84(11) . . ? O9 Co1 O2 94.49(11) . . ? O1 Co1 O2 85.75(10) . . ? N2 Co1 O2 158.32(12) . . ? N4 Co1 O2 96.76(12) . . ? O13 Co2 O3 167.05(13) 1_556 . ? O13 Co2 O2W 90.43(12) 1_556 . ? O3 Co2 O2W 84.99(12) . . ? O13 Co2 O5 95.40(12) 1_556 . ? O3 Co2 O5 88.60(12) . . ? O2W Co2 O5 173.27(12) . . ? O13 Co2 O1W 100.77(13) 1_556 . ? O3 Co2 O1W 91.51(12) . . ? O2W Co2 O1W 92.02(13) . . ? O5 Co2 O1W 90.19(12) . . ? O13 Co2 O2 93.68(12) 1_556 . ? O3 Co2 O2 75.35(11) . . ? O2W Co2 O2 100.75(11) . . ? O5 Co2 O2 75.57(11) . . ? O1W Co2 O2 160.64(12) . . ? O7 Co3 O9 95.28(13) . . ? O7 Co3 O11 163.45(13) . . ? O9 Co3 O11 97.65(12) . . ? O7 Co3 O3W 92.72(12) . . ? O9 Co3 O3W 92.51(12) . . ? O11 Co3 O3W 96.98(13) . . ? O7 Co3 O12 103.52(12) . . ? O9 Co3 O12 156.90(12) . . ? O11 Co3 O12 61.66(11) . . ? O3W Co3 O12 99.80(12) . . ? O7 Co3 O1 78.14(11) . . ? O9 Co3 O1 76.04(11) . . ? O11 Co3 O1 94.99(12) . . ? O3W Co3 O1 164.44(11) . . ? O12 Co3 O1 94.62(11) . . ? O7 Co3 C33 133.74(13) . . ? O9 Co3 C33 127.48(13) . . ? O11 Co3 C33 30.83(12) . . ? O3W Co3 C33 101.07(13) . . ? O12 Co3 C33 30.88(12) . . ? O1 Co3 C33 94.30(12) . . ? O7 Co4 O3 170.89(12) . . ? O7 Co4 O2 101.03(12) . . ? O3 Co4 O2 79.12(11) . . ? O7 Co4 O1 79.56(11) . . ? O3 Co4 O1 91.37(12) . . ? O2 Co4 O1 86.62(11) . . ? O7 Co4 N1 102.25(13) . . ? O3 Co4 N1 77.65(12) . . ? O2 Co4 N1 156.67(13) . . ? O1 Co4 N1 96.06(12) . . ? O7 Co4 N3 77.84(13) . . ? O3 Co4 N3 111.27(13) . . ? O2 Co4 N3 94.22(12) . . ? O1 Co4 N3 157.12(12) . . ? N1 Co4 N3 92.15(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.4(5) . . ? C3 C2 C1 121.9(6) . . ? C7 C2 C1 120.7(5) . . ? C4 C3 C2 122.2(5) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 C24 118.8(4) . . ? C5 C4 C24 121.2(4) . . ? O1 C5 C4 120.6(4) . . ? O1 C5 C6 120.0(4) . . ? C4 C5 C6 119.4(4) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 C8 120.1(4) . . ? C5 C6 C8 120.8(4) . . ? C6 C7 C2 122.2(5) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? N1 C8 C6 115.6(4) . . ? N1 C8 H8A 108.4 . . ? C6 C8 H8A 108.4 . . ? N1 C8 H8B 108.4 . . ? C6 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? N1 C9 C10 115.7(4) . . ? N1 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? N1 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C9 C10 H10B 107.6 . . ? C11 C10 H10B 107.6 . . ? H10A C10 H10B 107.1 . . ? N3 C11 C10 115.4(4) . . ? N3 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? N3 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? N3 C12 C13 115.5(3) . . ? N3 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? N3 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C19 119.2(4) . . ? C14 C13 C12 119.5(4) . . ? C19 C13 C12 120.4(4) . . ? C15 C14 C13 121.9(4) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C17 C15 C14 117.4(4) . . ? C17 C15 C16 121.3(5) . . ? C14 C15 C16 121.2(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 C18 123.0(4) . . ? C15 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 C20 120.4(4) . . ? C19 C18 C20 120.2(4) . . ? O2 C19 C13 119.9(4) . . ? O2 C19 C18 121.4(4) . . ? C13 C19 C18 118.6(4) . . ? N4 C20 C18 116.4(4) . . ? N4 C20 H20A 108.2 . . ? C18 C20 H20A 108.2 . . ? N4 C20 H20B 108.2 . . ? C18 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? N4 C21 C22 114.6(4) . . ? N4 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N4 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 117.3(4) . . ? C23 C22 H22A 108.0 . . ? C21 C22 H22A 108.0 . . ? C23 C22 H22B 108.0 . . ? C21 C22 H22B 108.0 . . ? H22A C22 H22B 107.2 . . ? N2 C23 C22 116.9(4) . . ? N2 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? N2 C23 H23B 108.1 . . ? C22 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? N2 C24 C4 116.8(4) . . ? N2 C24 H24A 108.1 . . ? C4 C24 H24A 108.1 . . ? N2 C24 H24B 108.1 . . ? C4 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? N3 C25 C26 111.7(3) . . ? N3 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N3 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? O8 C26 O7 124.2(4) . . ? O8 C26 C25 120.7(4) . . ? O7 C26 C25 115.0(4) . . ? N4 C27 C28 112.6(3) . . ? N4 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N4 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? O10 C28 O9 124.4(4) . . ? O10 C28 C27 121.0(4) . . ? O9 C28 C27 114.5(4) . . ? N2 C29 C30 114.4(4) . . ? N2 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? N2 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O6 C30 O5 124.3(4) . . ? O6 C30 C29 119.7(4) . . ? O5 C30 C29 116.0(4) . . ? N1 C31 C32 111.5(3) . . ? N1 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? N1 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? O4 C32 O3 123.8(4) . . ? O4 C32 C31 119.5(4) . . ? O3 C32 C31 116.6(4) . . ? O11 C33 O12 119.6(4) . . ? O11 C33 C34 118.4(4) . . ? O12 C33 C34 121.9(4) . . ? O11 C33 Co3 56.6(2) . . ? O12 C33 Co3 63.2(2) . . ? C34 C33 Co3 173.2(3) . . ? C35 C34 C39 119.1(4) . . ? C35 C34 C33 121.2(4) . . ? C39 C34 C33 119.7(4) . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 118.9(4) . . ? C37 C36 C40 121.2(4) . . ? C35 C36 C40 119.9(4) . . ? C36 C37 C38 120.9(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 120.0(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.5(4) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? O13 C40 O14 124.7(4) . . ? O13 C40 C36 116.4(4) . . ? O14 C40 C36 118.8(4) . . ? C31 N1 C9 111.4(3) . . ? C31 N1 C8 109.4(4) . . ? C9 N1 C8 107.2(3) . . ? C31 N1 Co4 111.5(2) . . ? C9 N1 Co4 112.6(3) . . ? C8 N1 Co4 104.4(2) . . ? C29 N2 C24 110.6(4) . . ? C29 N2 C23 112.4(4) . . ? C24 N2 C23 106.5(3) . . ? C29 N2 Co1 109.5(3) . . ? C24 N2 Co1 106.7(3) . . ? C23 N2 Co1 111.0(3) . . ? C25 N3 C12 108.9(3) . . ? C25 N3 C11 112.4(3) . . ? C12 N3 C11 106.2(3) . . ? C25 N3 Co4 110.9(3) . . ? C12 N3 Co4 107.7(2) . . ? C11 N3 Co4 110.4(3) . . ? C27 N4 C21 113.1(3) . . ? C27 N4 C20 109.7(4) . . ? C21 N4 C20 106.8(3) . . ? C27 N4 Co1 110.6(2) . . ? C21 N4 Co1 112.5(3) . . ? C20 N4 Co1 103.6(2) . . ? C5 O1 Co1 119.0(2) . . ? C5 O1 Co4 118.7(2) . . ? Co1 O1 Co4 94.28(11) . . ? C5 O1 Co3 124.5(2) . . ? Co1 O1 Co3 97.94(11) . . ? Co4 O1 Co3 96.04(11) . . ? C19 O2 Co4 118.8(2) . . ? C19 O2 Co1 115.3(2) . . ? Co4 O2 Co1 93.34(11) . . ? C19 O2 Co2 127.4(2) . . ? Co4 O2 Co2 97.92(11) . . ? Co1 O2 Co2 97.23(11) . . ? C32 O3 Co4 120.3(3) . . ? C32 O3 Co2 131.1(3) . . ? Co4 O3 Co2 106.85(13) . . ? C30 O5 Co1 119.2(3) . . ? C30 O5 Co2 131.9(3) . . ? Co1 O5 Co2 107.99(13) . . ? C26 O7 Co3 132.7(3) . . ? C26 O7 Co4 120.1(3) . . ? Co3 O7 Co4 105.95(13) . . ? C28 O9 Co3 131.1(3) . . ? C28 O9 Co1 121.3(3) . . ? Co3 O9 Co1 107.53(13) . . ? C33 O11 Co3 92.6(3) . . ? C33 O12 Co3 85.9(2) . . ? C40 O13 Co2 131.7(3) . 1_554 ? Co2 O1W H1WA 101.9 . . ? Co2 O1W H1WB 103.7 . . ? H1WA O1W H1WB 106.1 . . ? Co2 O2W H2WA 99.0 . . ? Co2 O2W H2WB 105.2 . . ? H2WA O2W H2WB 116.6 . . ? Co3 O3W H3WA 105.1 . . ? Co3 O3W H3WB 99.6 . . ? H3WA O3W H3WB 111.0 . . ? 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 C7 C2 C3 C4 -3.0(9) . . . . ? C1 C2 C3 C4 177.3(6) . . . . ? C2 C3 C4 C5 -2.1(8) . . . . ? C2 C3 C4 C24 169.8(5) . . . . ? C3 C4 C5 O1 -174.6(4) . . . . ? C24 C4 C5 O1 13.7(7) . . . . ? C3 C4 C5 C6 7.7(7) . . . . ? C24 C4 C5 C6 -163.9(4) . . . . ? O1 C5 C6 C7 174.1(4) . . . . ? C4 C5 C6 C7 -8.3(7) . . . . ? O1 C5 C6 C8 -13.4(6) . . . . ? C4 C5 C6 C8 164.3(4) . . . . ? C5 C6 C7 C2 3.2(8) . . . . ? C8 C6 C7 C2 -169.3(5) . . . . ? C3 C2 C7 C6 2.3(9) . . . . ? C1 C2 C7 C6 -177.9(6) . . . . ? C7 C6 C8 N1 -112.5(5) . . . . ? C5 C6 C8 N1 75.1(6) . . . . ? N1 C9 C10 C11 -38.7(6) . . . . ? C9 C10 C11 N3 -36.4(6) . . . . ? N3 C12 C13 C14 -116.4(5) . . . . ? N3 C12 C13 C19 74.2(5) . . . . ? C19 C13 C14 C15 2.3(7) . . . . ? C12 C13 C14 C15 -167.3(4) . . . . ? C13 C14 C15 C17 4.1(8) . . . . ? C13 C14 C15 C16 -179.2(5) . . . . ? C14 C15 C17 C18 -4.1(8) . . . . ? C16 C15 C17 C18 179.1(5) . . . . ? C15 C17 C18 C19 -2.2(8) . . . . ? C15 C17 C18 C20 172.2(5) . . . . ? C14 C13 C19 O2 173.4(4) . . . . ? C12 C13 C19 O2 -17.2(6) . . . . ? C14 C13 C19 C18 -8.6(6) . . . . ? C12 C13 C19 C18 160.9(4) . . . . ? C17 C18 C19 O2 -173.4(4) . . . . ? C20 C18 C19 O2 12.2(6) . . . . ? C17 C18 C19 C13 8.6(6) . . . . ? C20 C18 C19 C13 -165.9(4) . . . . ? C17 C18 C20 N4 109.2(5) . . . . ? C19 C18 C20 N4 -76.5(5) . . . . ? N4 C21 C22 C23 36.8(6) . . . . ? C21 C22 C23 N2 39.1(6) . . . . ? C3 C4 C24 N2 116.6(5) . . . . ? C5 C4 C24 N2 -71.7(6) . . . . ? N3 C25 C26 O8 160.4(4) . . . . ? N3 C25 C26 O7 -23.7(6) . . . . ? N4 C27 C28 O10 -163.2(4) . . . . ? N4 C27 C28 O9 18.9(6) . . . . ? N2 C29 C30 O6 -169.3(4) . . . . ? N2 C29 C30 O5 12.5(6) . . . . ? N1 C31 C32 O4 167.8(4) . . . . ? N1 C31 C32 O3 -14.7(6) . . . . ? O7 Co3 C33 O11 170.2(2) . . . . ? O9 Co3 C33 O11 16.8(3) . . . . ? O3W Co3 C33 O11 -85.1(3) . . . . ? O12 Co3 C33 O11 -175.7(4) . . . . ? O1 Co3 C33 O11 92.5(3) . . . . ? O7 Co3 C33 O12 -14.1(3) . . . . ? O9 Co3 C33 O12 -167.5(2) . . . . ? O11 Co3 C33 O12 175.7(4) . . . . ? O3W Co3 C33 O12 90.6(3) . . . . ? O1 Co3 C33 O12 -91.8(2) . . . . ? O7 Co3 C33 C34 126(3) . . . . ? O9 Co3 C33 C34 -27(3) . . . . ? O11 Co3 C33 C34 -44(3) . . . . ? O3W Co3 C33 C34 -129(3) . . . . ? O12 Co3 C33 C34 140(3) . . . . ? O1 Co3 C33 C34 48(3) . . . . ? O11 C33 C34 C35 -178.8(4) . . . . ? O12 C33 C34 C35 0.2(7) . . . . ? Co3 C33 C34 C35 -137(2) . . . . ? O11 C33 C34 C39 0.9(6) . . . . ? O12 C33 C34 C39 179.9(4) . . . . ? Co3 C33 C34 C39 42(3) . . . . ? C39 C34 C35 C36 1.5(7) . . . . ? C33 C34 C35 C36 -178.7(4) . . . . ? C34 C35 C36 C37 0.6(7) . . . . ? C34 C35 C36 C40 -178.8(4) . . . . ? C35 C36 C37 C38 -2.1(7) . . . . ? C40 C36 C37 C38 177.4(4) . . . . ? C36 C37 C38 C39 1.2(7) . . . . ? C37 C38 C39 C34 1.0(7) . . . . ? C35 C34 C39 C38 -2.4(7) . . . . ? C33 C34 C39 C38 177.9(4) . . . . ? C37 C36 C40 O13 -1.1(7) . . . . ? C35 C36 C40 O13 178.3(5) . . . . ? C37 C36 C40 O14 -179.6(5) . . . . ? C35 C36 C40 O14 -0.2(8) . . . . ? C32 C31 N1 C9 143.8(4) . . . . ? C32 C31 N1 C8 -97.8(4) . . . . ? C32 C31 N1 Co4 17.1(5) . . . . ? C10 C9 N1 C31 -61.0(5) . . . . ? C10 C9 N1 C8 179.3(4) . . . . ? C10 C9 N1 Co4 65.0(5) . . . . ? C6 C8 N1 C31 56.6(5) . . . . ? C6 C8 N1 C9 177.5(4) . . . . ? C6 C8 N1 Co4 -62.8(4) . . . . ? O7 Co4 N1 C31 177.6(3) . . . . ? O3 Co4 N1 C31 -11.8(3) . . . . ? O2 Co4 N1 C31 -6.3(5) . . . . ? O1 Co4 N1 C31 -101.8(3) . . . . ? N3 Co4 N1 C31 99.6(3) . . . . ? O7 Co4 N1 C9 51.5(3) . . . . ? O3 Co4 N1 C9 -137.8(3) . . . . ? O2 Co4 N1 C9 -132.3(3) . . . . ? O1 Co4 N1 C9 132.1(3) . . . . ? N3 Co4 N1 C9 -26.5(3) . . . . ? O7 Co4 N1 C8 -64.4(3) . . . . ? O3 Co4 N1 C8 106.3(3) . . . . ? O2 Co4 N1 C8 111.7(4) . . . . ? O1 Co4 N1 C8 16.2(3) . . . . ? N3 Co4 N1 C8 -142.4(3) . . . . ? C30 C29 N2 C24 106.4(5) . . . . ? C30 C29 N2 C23 -134.7(4) . . . . ? C30 C29 N2 Co1 -10.9(5) . . . . ? C4 C24 N2 C29 -60.8(5) . . . . ? C4 C24 N2 C23 176.8(4) . . . . ? C4 C24 N2 Co1 58.1(4) . . . . ? C22 C23 N2 C29 54.9(6) . . . . ? C22 C23 N2 C24 176.2(4) . . . . ? C22 C23 N2 Co1 -68.1(5) . . . . ? O5 Co1 N2 C29 5.7(3) . . . . ? O9 Co1 N2 C29 -173.3(3) . . . . ? O1 Co1 N2 C29 107.2(3) . . . . ? N4 Co1 N2 C29 -95.8(3) . . . . ? O2 Co1 N2 C29 15.6(5) . . . . ? O5 Co1 N2 C24 -114.0(3) . . . . ? O9 Co1 N2 C24 67.0(3) . . . . ? O1 Co1 N2 C24 -12.5(3) . . . . ? N4 Co1 N2 C24 144.5(3) . . . . ? O2 Co1 N2 C24 -104.1(4) . . . . ? O5 Co1 N2 C23 130.3(3) . . . . ? O9 Co1 N2 C23 -48.7(3) . . . . ? O1 Co1 N2 C23 -128.2(3) . . . . ? N4 Co1 N2 C23 28.8(3) . . . . ? O2 Co1 N2 C23 140.2(3) . . . . ? C26 C25 N3 C12 -98.2(4) . . . . ? C26 C25 N3 C11 144.4(4) . . . . ? C26 C25 N3 Co4 20.2(4) . . . . ? C13 C12 N3 C25 64.5(5) . . . . ? C13 C12 N3 C11 -174.2(4) . . . . ? C13 C12 N3 Co4 -55.9(4) . . . . ? C10 C11 N3 C25 -56.3(5) . . . . ? C10 C11 N3 C12 -175.3(4) . . . . ? C10 C11 N3 Co4 68.2(4) . . . . ? O7 Co4 N3 C25 -10.0(3) . . . . ? O3 Co4 N3 C25 169.6(3) . . . . ? O2 Co4 N3 C25 -110.4(3) . . . . ? O1 Co4 N3 C25 -19.1(5) . . . . ? N1 Co4 N3 C25 92.0(3) . . . . ? O7 Co4 N3 C12 109.1(3) . . . . ? O3 Co4 N3 C12 -71.3(3) . . . . ? O2 Co4 N3 C12 8.7(3) . . . . ? O1 Co4 N3 C12 100.0(4) . . . . ? N1 Co4 N3 C12 -148.9(3) . . . . ? O7 Co4 N3 C11 -135.4(3) . . . . ? O3 Co4 N3 C11 44.2(3) . . . . ? O2 Co4 N3 C11 124.2(3) . . . . ? O1 Co4 N3 C11 -144.5(3) . . . . ? N1 Co4 N3 C11 -33.3(3) . . . . ? C28 C27 N4 C21 -146.1(4) . . . . ? C28 C27 N4 C20 94.8(4) . . . . ? C28 C27 N4 Co1 -18.9(5) . . . . ? C22 C21 N4 C27 58.1(5) . . . . ? C22 C21 N4 C20 178.8(4) . . . . ? C22 C21 N4 Co1 -68.2(4) . . . . ? C18 C20 N4 C27 -56.3(5) . . . . ? C18 C20 N4 C21 -179.1(4) . . . . ? C18 C20 N4 Co1 61.9(4) . . . . ? O5 Co1 N4 C27 -175.8(3) . . . . ? O9 Co1 N4 C27 11.2(3) . . . . ? O1 Co1 N4 C27 9.5(5) . . . . ? N2 Co1 N4 C27 -96.0(3) . . . . ? O2 Co1 N4 C27 104.3(3) . . . . ? O5 Co1 N4 C21 -48.2(3) . . . . ? O9 Co1 N4 C21 138.7(3) . . . . ? O1 Co1 N4 C21 137.0(3) . . . . ? N2 Co1 N4 C21 31.6(3) . . . . ? O2 Co1 N4 C21 -128.1(3) . . . . ? O5 Co1 N4 C20 66.8(3) . . . . ? O9 Co1 N4 C20 -106.3(3) . . . . ? O1 Co1 N4 C20 -108.0(3) . . . . ? N2 Co1 N4 C20 146.5(3) . . . . ? O2 Co1 N4 C20 -13.2(3) . . . . ? C4 C5 O1 Co1 34.5(5) . . . . ? C6 C5 O1 Co1 -147.9(3) . . . . ? C4 C5 O1 Co4 148.1(3) . . . . ? C6 C5 O1 Co4 -34.3(5) . . . . ? C4 C5 O1 Co3 -90.5(4) . . . . ? C6 C5 O1 Co3 87.2(4) . . . . ? O5 Co1 O1 C5 49.2(3) . . . . ? O9 Co1 O1 C5 -137.7(3) . . . . ? N2 Co1 O1 C5 -31.4(3) . . . . ? N4 Co1 O1 C5 -136.1(3) . . . . ? O2 Co1 O1 C5 126.8(3) . . . . ? O5 Co1 O1 Co4 -77.05(12) . . . . ? O9 Co1 O1 Co4 96.02(12) . . . . ? N2 Co1 O1 Co4 -157.71(12) . . . . ? N4 Co1 O1 Co4 97.7(3) . . . . ? O2 Co1 O1 Co4 0.56(10) . . . . ? O5 Co1 O1 Co3 -173.77(10) . . . . ? O9 Co1 O1 Co3 -0.70(11) . . . . ? N2 Co1 O1 Co3 105.58(13) . . . . ? N4 Co1 O1 Co3 1.0(3) . . . . ? O2 Co1 O1 Co3 -96.16(11) . . . . ? O7 Co4 O1 C5 131.1(3) . . . . ? O3 Co4 O1 C5 -48.1(3) . . . . ? O2 Co4 O1 C5 -127.1(3) . . . . ? N1 Co4 O1 C5 29.7(3) . . . . ? N3 Co4 O1 C5 140.1(3) . . . . ? O7 Co4 O1 Co1 -102.44(12) . . . . ? O3 Co4 O1 Co1 78.45(11) . . . . ? O2 Co4 O1 Co1 -0.57(11) . . . . ? N1 Co4 O1 Co1 156.17(12) . . . . ? N3 Co4 O1 Co1 -93.4(3) . . . . ? O7 Co4 O1 Co3 -3.98(11) . . . . ? O3 Co4 O1 Co3 176.91(11) . . . . ? O2 Co4 O1 Co3 97.90(11) . . . . ? N1 Co4 O1 Co3 -105.36(12) . . . . ? N3 Co4 O1 Co3 5.0(3) . . . . ? O7 Co3 O1 C5 -127.1(3) . . . . ? O9 Co3 O1 C5 134.3(3) . . . . ? O11 Co3 O1 C5 37.7(3) . . . . ? O3W Co3 O1 C5 177.9(4) . . . . ? O12 Co3 O1 C5 -24.2(3) . . . . ? C33 Co3 O1 C5 6.7(3) . . . . ? O7 Co3 O1 Co1 99.28(13) . . . . ? O9 Co3 O1 Co1 0.71(11) . . . . ? O11 Co3 O1 Co1 -95.95(12) . . . . ? O3W Co3 O1 Co1 44.3(5) . . . . ? O12 Co3 O1 Co1 -157.85(11) . . . . ? C33 Co3 O1 Co1 -126.88(13) . . . . ? O7 Co3 O1 Co4 4.09(11) . . . . ? O9 Co3 O1 Co4 -94.48(13) . . . . ? O11 Co3 O1 Co4 168.85(11) . . . . ? O3W Co3 O1 Co4 -50.9(5) . . . . ? O12 Co3 O1 Co4 106.95(11) . . . . ? C33 Co3 O1 Co4 137.93(12) . . . . ? C13 C19 O2 Co4 -35.9(5) . . . . ? C18 C19 O2 Co4 146.1(3) . . . . ? C13 C19 O2 Co1 -145.3(3) . . . . ? C18 C19 O2 Co1 36.6(5) . . . . ? C13 C19 O2 Co2 92.2(4) . . . . ? C18 C19 O2 Co2 -85.8(4) . . . . ? O7 Co4 O2 C19 -42.1(3) . . . . ? O3 Co4 O2 C19 147.2(3) . . . . ? O1 Co4 O2 C19 -120.8(3) . . . . ? N1 Co4 O2 C19 141.7(3) . . . . ? N3 Co4 O2 C19 36.3(3) . . . . ? O7 Co4 O2 Co1 79.22(12) . . . . ? O3 Co4 O2 Co1 -91.50(12) . . . . ? O1 Co4 O2 Co1 0.56(10) . . . . ? N1 Co4 O2 Co1 -96.9(3) . . . . ? N3 Co4 O2 Co1 157.64(12) . . . . ? O7 Co4 O2 Co2 177.01(10) . . . . ? O3 Co4 O2 Co2 6.29(11) . . . . ? O1 Co4 O2 Co2 98.34(11) . . . . ? N1 Co4 O2 Co2 0.9(4) . . . . ? N3 Co4 O2 Co2 -104.57(13) . . . . ? O5 Co1 O2 C19 -133.1(3) . . . . ? O9 Co1 O2 C19 45.5(3) . . . . ? O1 Co1 O2 C19 123.6(3) . . . . ? N2 Co1 O2 C19 -143.1(4) . . . . ? N4 Co1 O2 C19 -32.7(3) . . . . ? O5 Co1 O2 Co4 102.77(12) . . . . ? O9 Co1 O2 Co4 -78.63(11) . . . . ? O1 Co1 O2 Co4 -0.56(10) . . . . ? N2 Co1 O2 Co4 92.8(3) . . . . ? N4 Co1 O2 Co4 -156.82(12) . . . . ? O5 Co1 O2 Co2 4.34(10) . . . . ? O9 Co1 O2 Co2 -177.06(10) . . . . ? O1 Co1 O2 Co2 -98.99(11) . . . . ? N2 Co1 O2 Co2 -5.6(4) . . . . ? N4 Co1 O2 Co2 104.75(12) . . . . ? O13 Co2 O2 C19 30.7(3) 1_556 . . . ? O3 Co2 O2 C19 -142.3(3) . . . . ? O2W Co2 O2 C19 -60.4(3) . . . . ? O5 Co2 O2 C19 125.4(3) . . . . ? O1W Co2 O2 C19 169.2(3) . . . . ? O13 Co2 O2 Co4 166.65(12) 1_556 . . . ? O3 Co2 O2 Co4 -6.37(11) . . . . ? O2W Co2 O2 Co4 75.50(13) . . . . ? O5 Co2 O2 Co4 -98.72(13) . . . . ? O1W Co2 O2 Co4 -54.9(4) . . . . ? O13 Co2 O2 Co1 -98.94(12) 1_556 . . . ? O3 Co2 O2 Co1 88.05(12) . . . . ? O2W Co2 O2 Co1 169.92(11) . . . . ? O5 Co2 O2 Co1 -4.31(10) . . . . ? O1W Co2 O2 Co1 39.5(4) . . . . ? O4 C32 O3 Co4 -178.1(3) . . . . ? C31 C32 O3 Co4 4.6(5) . . . . ? O4 C32 O3 Co2 19.3(6) . . . . ? C31 C32 O3 Co2 -158.1(3) . . . . ? O7 Co4 O3 C32 94.6(8) . . . . ? O2 Co4 O3 C32 -173.6(3) . . . . ? O1 Co4 O3 C32 100.1(3) . . . . ? N1 Co4 O3 C32 4.2(3) . . . . ? N3 Co4 O3 C32 -83.3(3) . . . . ? O7 Co4 O3 Co2 -99.0(7) . . . . ? O2 Co4 O3 Co2 -7.18(12) . . . . ? O1 Co4 O3 Co2 -93.47(14) . . . . ? N1 Co4 O3 Co2 170.63(17) . . . . ? N3 Co4 O3 Co2 83.15(16) . . . . ? O13 Co2 O3 C32 138.3(5) 1_556 . . . ? O2W Co2 O3 C32 68.7(4) . . . . ? O5 Co2 O3 C32 -113.4(4) . . . . ? O1W Co2 O3 C32 -23.2(4) . . . . ? O2 Co2 O3 C32 171.2(4) . . . . ? O13 Co2 O3 Co4 -26.0(6) 1_556 . . . ? O2W Co2 O3 Co4 -95.73(14) . . . . ? O5 Co2 O3 Co4 82.22(14) . . . . ? O1W Co2 O3 Co4 172.37(14) . . . . ? O2 Co2 O3 Co4 6.77(12) . . . . ? O6 C30 O5 Co1 174.4(4) . . . . ? C29 C30 O5 Co1 -7.5(5) . . . . ? O6 C30 O5 Co2 6.7(7) . . . . ? C29 C30 O5 Co2 -175.1(3) . . . . ? O9 Co1 O5 C30 172.8(9) . . . . ? O1 Co1 O5 C30 -92.2(3) . . . . ? N2 Co1 O5 C30 0.9(3) . . . . ? N4 Co1 O5 C30 89.9(3) . . . . ? O2 Co1 O5 C30 -175.3(3) . . . . ? O9 Co1 O5 Co2 -16.8(10) . . . . ? O1 Co1 O5 Co2 78.16(14) . . . . ? N2 Co1 O5 Co2 171.32(16) . . . . ? N4 Co1 O5 Co2 -99.67(15) . . . . ? O2 Co1 O5 Co2 -4.95(12) . . . . ? O13 Co2 O5 C30 -94.1(4) 1_556 . . . ? O3 Co2 O5 C30 98.2(4) . . . . ? O2W Co2 O5 C30 116.0(10) . . . . ? O1W Co2 O5 C30 6.7(4) . . . . ? O2 Co2 O5 C30 173.5(4) . . . . ? O13 Co2 O5 Co1 97.20(15) 1_556 . . . ? O3 Co2 O5 Co1 -70.45(14) . . . . ? O2W Co2 O5 Co1 -52.7(11) . . . . ? O1W Co2 O5 Co1 -161.96(14) . . . . ? O2 Co2 O5 Co1 4.78(11) . . . . ? O8 C26 O7 Co3 -3.4(7) . . . . ? C25 C26 O7 Co3 -179.1(3) . . . . ? O8 C26 O7 Co4 -168.5(4) . . . . ? C25 C26 O7 Co4 15.7(5) . . . . ? O9 Co3 O7 C26 -96.5(4) . . . . ? O11 Co3 O7 C26 122.2(5) . . . . ? O3W Co3 O7 C26 -3.8(4) . . . . ? O12 Co3 O7 C26 97.0(4) . . . . ? O1 Co3 O7 C26 -171.0(4) . . . . ? C33 Co3 O7 C26 104.4(4) . . . . ? O9 Co3 O7 Co4 70.13(15) . . . . ? O11 Co3 O7 Co4 -71.1(5) . . . . ? O3W Co3 O7 Co4 162.91(14) . . . . ? O12 Co3 O7 Co4 -96.34(15) . . . . ? O1 Co3 O7 Co4 -4.38(12) . . . . ? C33 Co3 O7 Co4 -88.9(2) . . . . ? O3 Co4 O7 C26 178.9(6) . . . . ? O2 Co4 O7 C26 88.8(3) . . . . ? O1 Co4 O7 C26 173.3(3) . . . . ? N1 Co4 O7 C26 -92.7(3) . . . . ? N3 Co4 O7 C26 -3.2(3) . . . . ? O3 Co4 O7 Co3 10.2(8) . . . . ? O2 Co4 O7 Co3 -79.87(15) . . . . ? O1 Co4 O7 Co3 4.57(12) . . . . ? N1 Co4 O7 Co3 98.57(15) . . . . ? N3 Co4 O7 Co3 -171.86(17) . . . . ? O10 C28 O9 Co3 -10.5(7) . . . . ? C27 C28 O9 Co3 167.4(3) . . . . ? O10 C28 O9 Co1 172.7(4) . . . . ? C27 C28 O9 Co1 -9.4(5) . . . . ? O7 Co3 O9 C28 105.8(4) . . . . ? O11 Co3 O9 C28 -84.6(4) . . . . ? O3W Co3 O9 C28 12.8(4) . . . . ? O12 Co3 O9 C28 -109.7(4) . . . . ? O1 Co3 O9 C28 -177.9(4) . . . . ? C33 Co3 O9 C28 -93.2(4) . . . . ? O7 Co3 O9 Co1 -77.14(15) . . . . ? O11 Co3 O9 Co1 92.50(16) . . . . ? O3W Co3 O9 Co1 -170.10(15) . . . . ? O12 Co3 O9 Co1 67.4(3) . . . . ? O1 Co3 O9 Co1 -0.77(12) . . . . ? C33 Co3 O9 Co1 83.89(19) . . . . ? O5 Co1 O9 C28 -85.3(10) . . . . ? O1 Co1 O9 C28 178.3(3) . . . . ? N2 Co1 O9 C28 86.3(3) . . . . ? N4 Co1 O9 C28 -1.1(3) . . . . ? O2 Co1 O9 C28 -97.0(3) . . . . ? O5 Co1 O9 Co3 97.2(10) . . . . ? O1 Co1 O9 Co3 0.80(13) . . . . ? N2 Co1 O9 Co3 -91.17(16) . . . . ? N4 Co1 O9 Co3 -178.52(17) . . . . ? O2 Co1 O9 Co3 85.53(14) . . . . ? O12 C33 O11 Co3 -4.4(4) . . . . ? C34 C33 O11 Co3 174.6(3) . . . . ? O7 Co3 O11 C33 -25.5(6) . . . . ? O9 Co3 O11 C33 -166.6(3) . . . . ? O3W Co3 O11 C33 99.9(3) . . . . ? O12 Co3 O11 C33 2.5(2) . . . . ? O1 Co3 O11 C33 -90.0(3) . . . . ? O11 C33 O12 Co3 4.2(4) . . . . ? C34 C33 O12 Co3 -174.8(4) . . . . ? O7 Co3 O12 C33 169.6(2) . . . . ? O9 Co3 O12 C33 26.0(4) . . . . ? O11 Co3 O12 C33 -2.5(2) . . . . ? O3W Co3 O12 C33 -95.2(3) . . . . ? O1 Co3 O12 C33 90.7(2) . . . . ? O14 C40 O13 Co2 -7.7(9) . . . 1_554 ? C36 C40 O13 Co2 174.0(3) . . . 1_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2WA O14 0.82 1.81 2.591(5) 159.7 1_556 O2W H2WB O4 0.81 2.00 2.762(4) 155.7 2_557 O1W H1WA O6 0.87 1.87 2.707(5) 161.1 . O1W H1WB O4 0.86 1.94 2.747(5) 155.7 . O3W H3WA O10 0.83 1.98 2.706(5) 145.7 . O3W H3WB O8 0.84 1.93 2.734(5) 159.4 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.940 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.097 data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 922857' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H48 N4 O17 Zn4), 2(O0.50) ' _chemical_formula_sum 'C80 H96 N8 O35 Zn8' _chemical_formula_weight 2252.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 12.722(3) _cell_length_b 13.796(3) _cell_length_c 14.181(3) _cell_angle_alpha 79.70(3) _cell_angle_beta 68.75(3) _cell_angle_gamma 80.00(3) _cell_volume 2266.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10153 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2863 _exptl_crystal_size_mid 0.271 _exptl_crystal_size_min 0.262 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.567 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22207 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10153 _reflns_number_gt 6532 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+5.8102P] 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 10153 _refine_ls_number_parameters 613 _refine_ls_number_restraints 1019 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.017 _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 Zn1 Zn 0.77197(5) 0.35344(4) 0.75966(4) 0.02531(14) Uani 1 1 d . . . Zn2 Zn 0.80939(5) 0.12095(4) 0.75317(4) 0.02581(14) Uani 1 1 d . . . Zn4 Zn 0.94666(5) 0.26443(4) 0.54465(4) 0.03068(15) Uani 1 1 d . . . Zn3 Zn 0.63928(5) 0.20520(4) 0.97666(4) 0.03013(15) Uani 1 1 d D . . C1 C 0.3517(6) 0.2771(6) 0.5884(7) 0.076(2) Uani 1 1 d U . . H1A H 0.3387 0.2115 0.5850 0.114 Uiso 1 1 calc R . . H1B H 0.3531 0.3186 0.5260 0.114 Uiso 1 1 calc R . . H1C H 0.2918 0.3041 0.6446 0.114 Uiso 1 1 calc R . . C2 C 0.4652(5) 0.2723(5) 0.6036(5) 0.0477(12) Uani 1 1 d U . . C3 C 0.5050(5) 0.3555(4) 0.6114(4) 0.0429(11) Uani 1 1 d U . . H3 H 0.4619 0.4167 0.6063 0.052 Uiso 1 1 calc R . . C4 C 0.6074(5) 0.3519(4) 0.6267(4) 0.0350(10) Uani 1 1 d U . . C5 C 0.6705(4) 0.2593(4) 0.6394(4) 0.0322(9) Uani 1 1 d U . . C6 C 0.6368(5) 0.1748(4) 0.6219(4) 0.0368(10) Uani 1 1 d U . . C7 C 0.5332(5) 0.1814(4) 0.6068(4) 0.0431(11) Uani 1 1 d U . . H7 H 0.5091 0.1245 0.5988 0.052 Uiso 1 1 calc R . . C8 C 0.6541(5) 0.4473(4) 0.6168(4) 0.0375(10) Uani 1 1 d U . . H8A H 0.7292 0.4444 0.5651 0.045 Uiso 1 1 calc R . . H8B H 0.6064 0.5009 0.5922 0.045 Uiso 1 1 calc R . . C9 C 0.7159(5) 0.0798(4) 0.6075(4) 0.0358(10) Uani 1 1 d U . . H9A H 0.6870 0.0371 0.5775 0.043 Uiso 1 1 calc R . . H9B H 0.7894 0.0951 0.5592 0.043 Uiso 1 1 calc R . . C10 C 0.8108(5) -0.0691(4) 0.6724(4) 0.0374(11) Uani 1 1 d U . . H10A H 0.8806 -0.0501 0.6201 0.045 Uiso 1 1 calc R . . H10B H 0.7760 -0.1066 0.6423 0.045 Uiso 1 1 calc R . . C11 C 0.8407(5) -0.1368(4) 0.7587(4) 0.0401(11) Uani 1 1 d U . . H11A H 0.9084 -0.1810 0.7282 0.048 Uiso 1 1 calc R . . H11B H 0.7797 -0.1776 0.7939 0.048 Uiso 1 1 calc R . . C12 C 0.8621(5) -0.0893(4) 0.8394(4) 0.0373(11) Uani 1 1 d U . . H12A H 0.7895 -0.0724 0.8912 0.045 Uiso 1 1 calc R . . H12B H 0.9067 -0.1383 0.8721 0.045 Uiso 1 1 calc R . . C13 C 0.7173(5) 0.5665(4) 0.6803(4) 0.0384(11) Uani 1 1 d U . . H13A H 0.6726 0.6155 0.6475 0.046 Uiso 1 1 calc R . . H13B H 0.7919 0.5537 0.6296 0.046 Uiso 1 1 calc R . . C14 C 0.7308(5) 0.6114(4) 0.7642(4) 0.0422(12) Uani 1 1 d U . . H14A H 0.6591 0.6494 0.7976 0.051 Uiso 1 1 calc R . . H14B H 0.7866 0.6580 0.7326 0.051 Uiso 1 1 calc R . . C15 C 0.7664(5) 0.5412(4) 0.8466(4) 0.0378(11) Uani 1 1 d U . . H15A H 0.8005 0.5781 0.8778 0.045 Uiso 1 1 calc R . . H15B H 0.6988 0.5181 0.8991 0.045 Uiso 1 1 calc R . . C16 C 0.8716(5) 0.3953(4) 0.9002(4) 0.0345(10) Uani 1 1 d U . . H16A H 0.8005 0.3771 0.9509 0.041 Uiso 1 1 calc R . . H16B H 0.9016 0.4376 0.9297 0.041 Uiso 1 1 calc R . . C17 C 0.9405(5) 0.0295(4) 0.8882(4) 0.0354(10) Uani 1 1 d U . . H17A H 0.9916 -0.0230 0.9097 0.042 Uiso 1 1 calc R . . H17B H 0.8686 0.0329 0.9442 0.042 Uiso 1 1 calc R . . C18 C 0.9887(4) 0.1263(4) 0.8701(4) 0.0331(10) Uani 1 1 d U . . C19 C 0.9190(4) 0.2172(4) 0.8651(4) 0.0296(9) Uani 1 1 d U . . C20 C 0.9528(4) 0.3034(4) 0.8797(4) 0.0344(10) Uani 1 1 d U . . C21 C 1.0608(5) 0.2996(4) 0.8844(4) 0.0395(11) Uani 1 1 d U . . H21 H 1.0834 0.3573 0.8925 0.047 Uiso 1 1 calc R . . C22 C 1.1360(5) 0.2135(5) 0.8776(5) 0.0432(12) Uani 1 1 d U . . C23 C 1.0966(5) 0.1274(4) 0.8740(4) 0.0400(11) Uani 1 1 d U . . H23 H 1.1438 0.0678 0.8742 0.048 Uiso 1 1 calc R . . C24 C 1.2536(5) 0.2112(5) 0.8815(6) 0.0638(18) Uani 1 1 d U . . H24A H 1.2928 0.1453 0.8751 0.096 Uiso 1 1 calc R . . H24B H 1.2477 0.2301 0.9453 0.096 Uiso 1 1 calc R . . H24C H 1.2951 0.2566 0.8264 0.096 Uiso 1 1 calc R . . C25 C 0.5515(4) 0.4829(4) 0.7905(4) 0.0375(11) Uani 1 1 d U . . H25A H 0.4938 0.4880 0.7596 0.045 Uiso 1 1 calc R . . H25B H 0.5421 0.5443 0.8186 0.045 Uiso 1 1 calc R . . C26 C 0.5318(4) 0.3980(4) 0.8772(4) 0.0352(10) Uani 1 1 d U . . C27 C 0.6219(5) 0.0007(4) 0.7792(4) 0.0345(10) Uani 1 1 d U . . H27A H 0.6308 -0.0656 0.8144 0.041 Uiso 1 1 calc R . . H27B H 0.5681 0.0018 0.7449 0.041 Uiso 1 1 calc R . . C28 C 0.5745(4) 0.0740(4) 0.8569(4) 0.0314(10) Uani 1 1 d U . . C29 C 0.9540(4) 0.4818(4) 0.7303(4) 0.0339(10) Uani 1 1 d U . . H29A H 1.0092 0.4843 0.7621 0.041 Uiso 1 1 calc R . . H29B H 0.9396 0.5475 0.6960 0.041 Uiso 1 1 calc R . . C30 C 1.0032(4) 0.4085(4) 0.6517(4) 0.0333(10) Uani 1 1 d U . . C31 C 1.0307(4) -0.0140(4) 0.7170(4) 0.0356(11) Uani 1 1 d U . . H31A H 1.0305 -0.0704 0.6849 0.043 Uiso 1 1 calc R . . H31B H 1.0914 -0.0296 0.7453 0.043 Uiso 1 1 calc R . . C32 C 1.0542(4) 0.0766(4) 0.6362(4) 0.0309(10) Uani 1 1 d U . . C33 C 0.7232(5) 0.2320(4) 1.1384(4) 0.0414(11) Uani 1 1 d U . . C34 C 0.7479(5) 0.3044(4) 1.1935(4) 0.0335(10) Uani 1 1 d U . . C35 C 0.7963(5) 0.2696(4) 1.2678(4) 0.0353(10) Uani 1 1 d U . . H35 H 0.8147 0.2017 1.2824 0.042 Uiso 1 1 calc R . . C36 C 0.8176(4) 0.3341(4) 1.3208(4) 0.0302(10) Uani 1 1 d U . . C37 C 0.7880(4) 0.4352(4) 1.3005(4) 0.0327(10) Uani 1 1 d U . . H37 H 0.7997 0.4791 1.3374 0.039 Uiso 1 1 calc R . . C38 C 0.7411(5) 0.4706(4) 1.2256(4) 0.0358(10) Uani 1 1 d U . . H38 H 0.7217 0.5384 1.2119 0.043 Uiso 1 1 calc R . . C39 C 0.7227(4) 0.4056(4) 1.1706(4) 0.0335(10) Uani 1 1 d U . . H39 H 0.6935 0.4300 1.1184 0.040 Uiso 1 1 calc R . . C88 C 0.8710(4) 0.2959(4) 1.4009(4) 0.0318(10) Uani 1 1 d U . . N1 N 0.6630(3) 0.4728(3) 0.7111(3) 0.0311(9) Uani 1 1 d . . . N2 N 0.7326(4) 0.0232(3) 0.7023(3) 0.0325(9) Uani 1 1 d . . . N3 N 0.8475(4) 0.4537(3) 0.8098(3) 0.0303(9) Uani 1 1 d . . . N4 N 0.9216(4) 0.0015(3) 0.8002(3) 0.0300(9) Uani 1 1 d . . . O1 O 0.7662(3) 0.2528(2) 0.6638(2) 0.0256(7) Uani 1 1 d . . . O2 O 0.8192(3) 0.2200(2) 0.8496(2) 0.0269(7) Uani 1 1 d . . . O3 O 0.6202(3) 0.3383(2) 0.8805(2) 0.0302(8) Uani 1 1 d . . . O4 O 0.4359(3) 0.3926(3) 0.9389(3) 0.0559(12) Uani 1 1 d . . . O5 O 0.6454(3) 0.1270(3) 0.8614(2) 0.0305(8) Uani 1 1 d . . . O6 O 0.4749(3) 0.0751(3) 0.9143(3) 0.0394(9) Uani 1 1 d . . . O7 O 0.9315(3) 0.3577(3) 0.6462(2) 0.0308(8) Uani 1 1 d . . . O8 O 1.1028(3) 0.4053(3) 0.5971(3) 0.0477(10) Uani 1 1 d . . . O9 O 0.9645(3) 0.1339(2) 0.6306(2) 0.0307(8) Uani 1 1 d . . . O10 O 1.1506(3) 0.0879(3) 0.5817(3) 0.0488(10) Uani 1 1 d . . . O11 O 0.8887(3) 0.3592(3) 1.4457(3) 0.0406(9) Uani 1 1 d . . . O12 O 0.8998(3) 0.2061(3) 1.4207(3) 0.0385(9) Uani 1 1 d . . . O13 O 0.6766(3) 0.2695(3) 1.0727(3) 0.0364(9) Uani 1 1 d . . . O14 O 0.7464(6) 0.1417(3) 1.1611(5) 0.099(2) Uani 1 1 d . . . O1W O 0.6692(3) 0.0636(3) 1.0513(3) 0.0378(9) Uani 1 1 d D . . H1WB H 0.687(4) 0.067(5) 1.102(3) 0.057 Uiso 1 1 d D . . H1WA H 0.601(2) 0.0599(18) 1.067(3) 0.057 Uiso 1 1 d D . . O2W O 0.4595(3) 0.2099(3) 1.0398(3) 0.0413(9) Uani 1 1 d D . . H2WA H 0.430(5) 0.267(2) 1.022(5) 0.062 Uiso 1 1 d D . . H2WB H 0.453(5) 0.169(3) 1.004(4) 0.062 Uiso 1 1 d D . . O3W O 1.1214(3) 0.2686(3) 0.4766(3) 0.0415(9) Uani 1 1 d D . . H3WA H 1.135(6) 0.312(3) 0.504(4) 0.062 Uiso 1 1 d D . . H3WB H 1.144(6) 0.2119(18) 0.500(5) 0.062 Uiso 1 1 d D . . O4W O 0.6457(10) 0.0129(10) 0.3615(11) 0.111(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0227(3) 0.0270(3) 0.0268(3) -0.0039(2) -0.0079(2) -0.0051(2) Zn2 0.0268(3) 0.0266(3) 0.0253(3) -0.0034(2) -0.0091(2) -0.0057(2) Zn4 0.0370(3) 0.0327(3) 0.0238(3) -0.0012(2) -0.0121(3) -0.0068(3) Zn3 0.0350(3) 0.0335(3) 0.0263(3) -0.0038(2) -0.0133(3) -0.0095(3) C1 0.053(4) 0.090(5) 0.101(5) 0.005(4) -0.049(4) -0.017(4) C2 0.041(2) 0.059(3) 0.053(3) 0.000(2) -0.030(2) -0.008(2) C3 0.036(2) 0.049(2) 0.049(2) -0.001(2) -0.022(2) -0.006(2) C4 0.034(2) 0.038(2) 0.038(2) -0.0041(19) -0.0194(18) -0.0048(18) C5 0.032(2) 0.039(2) 0.032(2) -0.0015(18) -0.0191(17) -0.0081(18) C6 0.036(2) 0.042(2) 0.038(2) 0.0015(19) -0.0185(18) -0.0129(18) C7 0.039(2) 0.049(2) 0.050(2) -0.002(2) -0.024(2) -0.015(2) C8 0.035(2) 0.038(2) 0.042(2) 0.001(2) -0.0201(19) -0.0037(19) C9 0.040(2) 0.039(2) 0.035(2) -0.0078(19) -0.0167(19) -0.0101(19) C10 0.042(2) 0.035(2) 0.037(2) -0.0117(19) -0.0115(19) -0.0067(19) C11 0.044(2) 0.032(2) 0.042(2) -0.003(2) -0.012(2) -0.007(2) C12 0.040(2) 0.030(2) 0.037(2) 0.0038(19) -0.011(2) -0.0044(19) C13 0.041(2) 0.028(2) 0.044(2) -0.001(2) -0.014(2) -0.0042(19) C14 0.043(2) 0.033(2) 0.047(2) -0.005(2) -0.011(2) -0.005(2) C15 0.039(2) 0.032(2) 0.043(2) -0.010(2) -0.012(2) -0.0066(19) C16 0.038(2) 0.039(2) 0.034(2) -0.0086(18) -0.0167(17) -0.0095(18) C17 0.036(2) 0.039(2) 0.031(2) -0.0024(19) -0.0140(18) -0.0010(19) C18 0.032(2) 0.040(2) 0.031(2) -0.0024(18) -0.0157(17) -0.0027(18) C19 0.0279(19) 0.037(2) 0.0304(19) -0.0053(17) -0.0157(16) -0.0061(17) C20 0.034(2) 0.039(2) 0.036(2) -0.0052(18) -0.0165(17) -0.0086(18) C21 0.038(2) 0.046(2) 0.043(2) -0.003(2) -0.0206(19) -0.012(2) C22 0.033(2) 0.053(3) 0.046(2) 0.003(2) -0.020(2) -0.007(2) C23 0.034(2) 0.046(2) 0.038(2) 0.004(2) -0.0167(19) 0.002(2) C24 0.041(3) 0.074(4) 0.081(4) 0.016(4) -0.034(3) -0.016(3) C25 0.032(2) 0.035(2) 0.041(2) 0.000(2) -0.0110(19) 0.0004(19) C26 0.031(2) 0.034(2) 0.039(2) -0.0036(19) -0.0116(19) -0.0024(19) C27 0.038(2) 0.036(2) 0.034(2) -0.0070(19) -0.0136(19) -0.0108(19) C28 0.033(2) 0.034(2) 0.032(2) 0.0008(18) -0.0153(18) -0.0116(18) C29 0.035(2) 0.034(2) 0.037(2) -0.0104(19) -0.0097(19) -0.0126(18) C30 0.032(2) 0.037(2) 0.033(2) -0.0024(19) -0.0117(18) -0.0102(19) C31 0.033(2) 0.037(2) 0.034(2) -0.0034(19) -0.0099(18) 0.0005(19) C32 0.030(2) 0.033(2) 0.030(2) -0.0075(18) -0.0111(18) -0.0013(18) C33 0.048(2) 0.040(2) 0.046(2) -0.008(2) -0.027(2) -0.003(2) C34 0.042(2) 0.033(2) 0.035(2) -0.0079(19) -0.0230(19) -0.0018(19) C35 0.043(2) 0.034(2) 0.038(2) -0.0082(19) -0.023(2) -0.0020(19) C36 0.031(2) 0.036(2) 0.031(2) -0.0076(19) -0.0186(18) -0.0020(18) C37 0.034(2) 0.036(2) 0.035(2) -0.012(2) -0.0160(19) -0.0046(19) C38 0.037(2) 0.034(2) 0.041(2) -0.007(2) -0.019(2) 0.0000(19) C39 0.036(2) 0.036(2) 0.037(2) -0.0078(19) -0.0215(19) -0.0011(19) C88 0.030(2) 0.041(2) 0.027(2) -0.003(2) -0.0115(19) -0.006(2) N1 0.027(2) 0.027(2) 0.036(2) -0.0013(18) -0.0072(18) -0.0054(17) N2 0.037(2) 0.033(2) 0.029(2) -0.0033(18) -0.0103(19) -0.0100(19) N3 0.032(2) 0.029(2) 0.030(2) -0.0075(18) -0.0066(18) -0.0069(18) N4 0.033(2) 0.027(2) 0.029(2) -0.0060(18) -0.0092(18) -0.0001(17) O1 0.0260(17) 0.0275(17) 0.0282(17) -0.0040(14) -0.0136(14) -0.0058(13) O2 0.0268(18) 0.0313(18) 0.0262(17) -0.0040(14) -0.0132(14) -0.0035(14) O3 0.0242(18) 0.0358(19) 0.0281(18) 0.0005(15) -0.0087(14) -0.0027(14) O4 0.029(2) 0.053(3) 0.059(3) 0.010(2) 0.005(2) 0.0030(19) O5 0.0277(18) 0.0393(19) 0.0270(17) -0.0082(15) -0.0063(14) -0.0129(15) O6 0.027(2) 0.045(2) 0.046(2) -0.0091(18) -0.0067(17) -0.0126(16) O7 0.0248(18) 0.042(2) 0.0287(18) -0.0129(16) -0.0057(14) -0.0098(15) O8 0.027(2) 0.050(2) 0.062(3) -0.024(2) 0.0016(19) -0.0142(17) O9 0.0282(19) 0.0316(18) 0.0277(17) 0.0013(15) -0.0074(15) -0.0015(14) O10 0.029(2) 0.052(2) 0.048(2) 0.004(2) -0.0009(18) 0.0019(18) O11 0.054(3) 0.050(2) 0.0287(19) -0.0065(17) -0.0244(18) -0.0107(19) O12 0.048(2) 0.037(2) 0.035(2) -0.0019(17) -0.0221(18) -0.0027(17) O13 0.046(2) 0.041(2) 0.0340(19) -0.0063(17) -0.0272(18) -0.0059(17) O14 0.199(7) 0.033(2) 0.134(5) -0.016(3) -0.145(5) 0.008(3) O1W 0.044(2) 0.036(2) 0.042(2) -0.0019(18) -0.0240(19) -0.0113(17) O2W 0.033(2) 0.051(2) 0.036(2) -0.0067(19) -0.0049(17) -0.0113(19) O3W 0.043(2) 0.045(2) 0.032(2) -0.0028(18) -0.0055(17) -0.0127(19) O4W 0.061(8) 0.129(11) 0.139(12) 0.037(9) -0.040(8) -0.045(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.079(3) . ? Zn1 O7 2.086(3) . ? Zn1 O1 2.137(3) . ? Zn1 N1 2.145(4) . ? Zn1 N3 2.156(4) . ? Zn1 O2 2.170(3) . ? Zn2 O5 2.092(3) . ? Zn2 O9 2.115(3) . ? Zn2 O1 2.133(3) . ? Zn2 O2 2.146(3) . ? Zn2 N2 2.146(4) . ? Zn2 N4 2.163(4) . ? Zn4 O11 1.995(4) 1_554 ? Zn4 O9 2.013(3) . ? Zn4 O7 2.035(3) . ? Zn4 O3W 2.084(4) . ? Zn4 O1 2.317(3) . ? Zn4 O12 2.350(4) 1_554 ? Zn4 C88 2.496(5) 1_554 ? Zn3 O13 1.978(3) . ? Zn3 O5 2.085(3) . ? Zn3 O1W 2.091(4) . ? Zn3 O3 2.116(3) . ? Zn3 O2W 2.126(4) . ? Zn3 O2 2.359(3) . ? C1 C2 1.524(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.369(8) . ? C2 C7 1.399(8) . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C4 C5 1.405(7) . ? C4 C8 1.500(7) . ? C5 O1 1.366(6) . ? C5 C6 1.399(7) . ? C6 C7 1.394(7) . ? C6 C9 1.505(7) . ? C7 H7 0.9300 . ? C8 N1 1.489(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.495(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.496(6) . ? C10 C11 1.523(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.539(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.492(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.494(6) . ? C13 C14 1.509(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.528(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N3 1.482(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N3 1.489(7) . ? C16 C20 1.489(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N4 1.479(6) . ? C17 C18 1.507(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.396(7) . ? C18 C19 1.412(7) . ? C19 O2 1.358(6) . ? C19 C20 1.403(7) . ? C20 C21 1.392(7) . ? C21 C22 1.384(8) . ? C21 H21 0.9300 . ? C22 C23 1.383(8) . ? C22 C24 1.512(8) . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N1 1.459(6) . ? C25 C26 1.519(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O4 1.222(6) . ? C26 O3 1.285(6) . ? C27 N2 1.479(7) . ? C27 C28 1.517(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O6 1.232(6) . ? C28 O5 1.281(6) . ? C29 N3 1.475(6) . ? C29 C30 1.527(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O8 1.220(6) . ? C30 O7 1.274(6) . ? C31 N4 1.471(6) . ? C31 C32 1.528(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O10 1.209(6) . ? C32 O9 1.290(6) . ? C33 O14 1.241(7) . ? C33 O13 1.269(6) . ? C33 C34 1.507(7) . ? C34 C35 1.382(7) . ? C34 C39 1.384(7) . ? C35 C36 1.379(7) . ? C35 H35 0.9300 . ? C36 C37 1.387(7) . ? C36 C88 1.500(7) . ? C37 C38 1.376(7) . ? C37 H37 0.9300 . ? C38 C39 1.387(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C88 O12 1.240(6) . ? C88 O11 1.261(6) . ? C88 Zn4 2.496(5) 1_556 ? O11 Zn4 1.995(4) 1_556 ? O12 Zn4 2.350(4) 1_556 ? O1W H1WB 0.843(18) . ? O1W H1WA 0.819(18) . ? O2W H2WA 0.852(19) . ? O2W H2WB 0.855(19) . ? O3W H3WA 0.847(19) . ? O3W H3WB 0.839(19) . ? 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 O3 Zn1 O7 174.47(13) . . ? O3 Zn1 O1 101.67(13) . . ? O7 Zn1 O1 78.42(13) . . ? O3 Zn1 N1 79.66(15) . . ? O7 Zn1 N1 105.85(15) . . ? O1 Zn1 N1 95.80(14) . . ? O3 Zn1 N3 101.95(15) . . ? O7 Zn1 N3 77.72(14) . . ? O1 Zn1 N3 156.10(14) . . ? N1 Zn1 N3 91.99(16) . . ? O3 Zn1 O2 78.80(13) . . ? O7 Zn1 O2 95.74(14) . . ? O1 Zn1 O2 84.34(12) . . ? N1 Zn1 O2 158.01(14) . . ? N3 Zn1 O2 96.68(14) . . ? O5 Zn2 O9 170.99(13) . . ? O5 Zn2 O1 92.35(13) . . ? O9 Zn2 O1 78.70(13) . . ? O5 Zn2 O2 78.56(13) . . ? O9 Zn2 O2 101.37(13) . . ? O1 Zn2 O2 85.01(12) . . ? O5 Zn2 N2 78.27(15) . . ? O9 Zn2 N2 101.61(15) . . ? O1 Zn2 N2 96.51(14) . . ? O2 Zn2 N2 156.82(15) . . ? O5 Zn2 N4 111.04(15) . . ? O9 Zn2 N4 77.97(15) . . ? O1 Zn2 N4 156.08(15) . . ? O2 Zn2 N4 94.48(14) . . ? N2 Zn2 N4 93.24(16) . . ? O11 Zn4 O9 155.50(15) 1_554 . ? O11 Zn4 O7 99.62(14) 1_554 . ? O9 Zn4 O7 99.02(14) . . ? O11 Zn4 O3W 101.43(16) 1_554 . ? O9 Zn4 O3W 93.30(15) . . ? O7 Zn4 O3W 93.09(15) . . ? O11 Zn4 O1 92.96(14) 1_554 . ? O9 Zn4 O1 76.56(13) . . ? O7 Zn4 O1 75.36(12) . . ? O3W Zn4 O1 162.96(13) . . ? O11 Zn4 O12 59.42(14) 1_554 1_554 ? O9 Zn4 O12 98.43(14) . 1_554 ? O7 Zn4 O12 155.66(14) . 1_554 ? O3W Zn4 O12 102.71(15) . 1_554 ? O1 Zn4 O12 92.42(12) . 1_554 ? O11 Zn4 C88 30.04(15) 1_554 1_554 ? O9 Zn4 C88 126.79(16) . 1_554 ? O7 Zn4 C88 128.18(16) . 1_554 ? O3W Zn4 C88 105.50(16) . 1_554 ? O1 Zn4 C88 91.53(14) . 1_554 ? O12 Zn4 C88 29.46(14) 1_554 1_554 ? O13 Zn3 O5 165.09(15) . . ? O13 Zn3 O1W 92.11(15) . . ? O5 Zn3 O1W 83.66(14) . . ? O13 Zn3 O3 94.81(14) . . ? O5 Zn3 O3 88.32(13) . . ? O1W Zn3 O3 171.30(14) . . ? O13 Zn3 O2W 103.35(15) . . ? O5 Zn3 O2W 91.24(14) . . ? O1W Zn3 O2W 94.16(16) . . ? O3 Zn3 O2W 89.36(15) . . ? O13 Zn3 O2 92.86(14) . . ? O5 Zn3 O2 73.98(12) . . ? O1W Zn3 O2 100.52(14) . . ? O3 Zn3 O2 73.90(12) . . ? O2W Zn3 O2 157.70(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 118.2(5) . . ? C3 C2 C1 121.9(6) . . ? C7 C2 C1 119.8(6) . . ? C2 C3 C4 122.4(6) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 C8 118.8(5) . . ? C5 C4 C8 121.7(5) . . ? O1 C5 C6 120.7(5) . . ? O1 C5 C4 120.3(4) . . ? C6 C5 C4 119.0(5) . . ? C7 C6 C5 119.6(5) . . ? C7 C6 C9 119.1(5) . . ? C5 C6 C9 120.9(5) . . ? C6 C7 C2 121.0(5) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? N1 C8 C4 116.4(4) . . ? N1 C8 H8A 108.2 . . ? C4 C8 H8A 108.2 . . ? N1 C8 H8B 108.2 . . ? C4 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? N2 C9 C6 115.4(4) . . ? N2 C9 H9A 108.4 . . ? C6 C9 H9A 108.4 . . ? N2 C9 H9B 108.4 . . ? C6 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C11 115.4(4) . . ? N2 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? N2 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C10 C11 C12 118.6(4) . . ? C10 C11 H11A 107.7 . . ? C12 C11 H11A 107.7 . . ? C10 C11 H11B 107.7 . . ? C12 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? N4 C12 C11 115.4(4) . . ? N4 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? N4 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C14 116.6(5) . . ? N1 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? N1 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C15 117.9(4) . . ? C13 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C13 C14 H14B 107.8 . . ? C15 C14 H14B 107.8 . . ? H14A C14 H14B 107.2 . . ? N3 C15 C14 114.8(4) . . ? N3 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? N3 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? N3 C16 C20 115.4(4) . . ? N3 C16 H16A 108.4 . . ? C20 C16 H16A 108.4 . . ? N3 C16 H16B 108.4 . . ? C20 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? N4 C17 C18 116.0(4) . . ? N4 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? N4 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C23 C18 C19 118.7(5) . . ? C23 C18 C17 120.4(5) . . ? C19 C18 C17 120.2(5) . . ? O2 C19 C20 120.9(4) . . ? O2 C19 C18 120.1(4) . . ? C20 C19 C18 119.0(5) . . ? C21 C20 C19 119.0(5) . . ? C21 C20 C16 119.5(5) . . ? C19 C20 C16 121.2(5) . . ? C22 C21 C20 122.7(5) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C23 C22 C21 117.2(5) . . ? C23 C22 C24 120.8(6) . . ? C21 C22 C24 121.9(6) . . ? C22 C23 C18 122.6(5) . . ? C22 C23 H23 118.7 . . ? C18 C23 H23 118.7 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 114.5(4) . . ? N1 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N1 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? O4 C26 O3 125.1(5) . . ? O4 C26 C25 119.0(5) . . ? O3 C26 C25 115.9(5) . . ? N2 C27 C28 112.4(4) . . ? N2 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N2 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? O6 C28 O5 124.5(5) . . ? O6 C28 C27 119.4(4) . . ? O5 C28 C27 115.9(4) . . ? N3 C29 C30 111.9(4) . . ? N3 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? N3 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? O8 C30 O7 125.2(5) . . ? O8 C30 C29 120.0(5) . . ? O7 C30 C29 114.7(4) . . ? N4 C31 C32 112.7(4) . . ? N4 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N4 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? O10 C32 O9 125.4(5) . . ? O10 C32 C31 120.1(5) . . ? O9 C32 C31 114.5(4) . . ? O14 C33 O13 124.7(5) . . ? O14 C33 C34 119.2(5) . . ? O13 C33 C34 116.1(5) . . ? C35 C34 C39 119.4(5) . . ? C35 C34 C33 119.7(5) . . ? C39 C34 C33 120.9(5) . . ? C36 C35 C34 120.9(5) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.5(5) . . ? C35 C36 C88 120.7(5) . . ? C37 C36 C88 119.9(4) . . ? C38 C37 C36 120.0(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.4(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C34 C39 C38 119.8(5) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? O12 C88 O11 120.9(5) . . ? O12 C88 C36 121.9(5) . . ? O11 C88 C36 117.2(5) . . ? O12 C88 Zn4 68.7(3) . 1_556 ? O11 C88 Zn4 52.4(2) . 1_556 ? C36 C88 Zn4 169.0(4) . 1_556 ? C25 N1 C8 110.9(4) . . ? C25 N1 C13 112.6(4) . . ? C8 N1 C13 106.0(4) . . ? C25 N1 Zn1 110.3(3) . . ? C8 N1 Zn1 106.4(3) . . ? C13 N1 Zn1 110.4(3) . . ? C27 N2 C9 110.1(4) . . ? C27 N2 C10 111.9(4) . . ? C9 N2 C10 107.1(4) . . ? C27 N2 Zn2 111.3(3) . . ? C9 N2 Zn2 104.4(3) . . ? C10 N2 Zn2 111.8(3) . . ? C29 N3 C15 112.4(4) . . ? C29 N3 C16 110.1(4) . . ? C15 N3 C16 106.6(4) . . ? C29 N3 Zn1 111.3(3) . . ? C15 N3 Zn1 112.0(3) . . ? C16 N3 Zn1 103.9(3) . . ? C31 N4 C17 109.9(4) . . ? C31 N4 C12 113.3(4) . . ? C17 N4 C12 106.0(4) . . ? C31 N4 Zn2 111.1(3) . . ? C17 N4 Zn2 107.2(3) . . ? C12 N4 Zn2 109.0(3) . . ? C5 O1 Zn2 118.1(3) . . ? C5 O1 Zn1 118.7(3) . . ? Zn2 O1 Zn1 95.99(12) . . ? C5 O1 Zn4 124.1(3) . . ? Zn2 O1 Zn4 96.72(13) . . ? Zn1 O1 Zn4 97.47(13) . . ? C19 O2 Zn2 118.5(3) . . ? C19 O2 Zn1 115.3(3) . . ? Zn2 O2 Zn1 94.64(12) . . ? C19 O2 Zn3 126.5(3) . . ? Zn2 O2 Zn3 97.82(13) . . ? Zn1 O2 Zn3 97.91(13) . . ? C26 O3 Zn1 118.4(3) . . ? C26 O3 Zn3 131.5(3) . . ? Zn1 O3 Zn3 109.15(15) . . ? C28 O5 Zn3 130.7(3) . . ? C28 O5 Zn2 119.5(3) . . ? Zn3 O5 Zn2 108.87(15) . . ? C30 O7 Zn4 130.6(3) . . ? C30 O7 Zn1 120.5(3) . . ? Zn4 O7 Zn1 108.75(15) . . ? C32 O9 Zn4 131.1(3) . . ? C32 O9 Zn2 119.0(3) . . ? Zn4 O9 Zn2 107.43(15) . . ? C88 O11 Zn4 97.6(3) . 1_556 ? C88 O12 Zn4 81.8(3) . 1_556 ? C33 O13 Zn3 130.0(3) . . ? Zn3 O1W H1WB 111(4) . . ? Zn3 O1W H1WA 86.9(9) . . ? H1WB O1W H1WA 112(3) . . ? Zn3 O2W H2WA 109(5) . . ? Zn3 O2W H2WB 97(4) . . ? H2WA O2W H2WB 108(2) . . ? Zn4 O3W H3WA 104(5) . . ? Zn4 O3W H3WB 99(5) . . ? H3WA O3W H3WB 110(3) . . ? 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 C7 C2 C3 C4 -2.8(9) . . . . ? C1 C2 C3 C4 179.1(6) . . . . ? C2 C3 C4 C5 -3.0(9) . . . . ? C2 C3 C4 C8 169.8(6) . . . . ? C3 C4 C5 O1 -174.0(5) . . . . ? C8 C4 C5 O1 13.4(8) . . . . ? C3 C4 C5 C6 9.0(8) . . . . ? C8 C4 C5 C6 -163.6(5) . . . . ? O1 C5 C6 C7 173.8(5) . . . . ? C4 C5 C6 C7 -9.2(8) . . . . ? O1 C5 C6 C9 -13.0(8) . . . . ? C4 C5 C6 C9 164.0(5) . . . . ? C5 C6 C7 C2 3.4(9) . . . . ? C9 C6 C7 C2 -169.9(5) . . . . ? C3 C2 C7 C6 2.7(9) . . . . ? C1 C2 C7 C6 -179.2(6) . . . . ? C3 C4 C8 N1 115.5(6) . . . . ? C5 C4 C8 N1 -71.9(7) . . . . ? C7 C6 C9 N2 -112.4(6) . . . . ? C5 C6 C9 N2 74.4(7) . . . . ? N2 C10 C11 C12 -39.5(7) . . . . ? C10 C11 C12 N4 -36.8(7) . . . . ? N1 C13 C14 C15 40.2(7) . . . . ? C13 C14 C15 N3 35.8(7) . . . . ? N4 C17 C18 C23 -114.9(5) . . . . ? N4 C17 C18 C19 75.1(6) . . . . ? C23 C18 C19 O2 172.5(5) . . . . ? C17 C18 C19 O2 -17.3(7) . . . . ? C23 C18 C19 C20 -9.5(8) . . . . ? C17 C18 C19 C20 160.6(5) . . . . ? O2 C19 C20 C21 -173.2(5) . . . . ? C18 C19 C20 C21 8.9(8) . . . . ? O2 C19 C20 C16 12.9(8) . . . . ? C18 C19 C20 C16 -165.0(5) . . . . ? N3 C16 C20 C21 109.4(6) . . . . ? N3 C16 C20 C19 -76.7(6) . . . . ? C19 C20 C21 C22 -1.5(9) . . . . ? C16 C20 C21 C22 172.5(5) . . . . ? C20 C21 C22 C23 -5.1(9) . . . . ? C20 C21 C22 C24 179.1(6) . . . . ? C21 C22 C23 C18 4.4(9) . . . . ? C24 C22 C23 C18 -179.8(6) . . . . ? C19 C18 C23 C22 2.9(8) . . . . ? C17 C18 C23 C22 -167.3(5) . . . . ? N1 C25 C26 O4 -169.2(5) . . . . ? N1 C25 C26 O3 12.4(7) . . . . ? N2 C27 C28 O6 167.5(5) . . . . ? N2 C27 C28 O5 -16.7(6) . . . . ? N3 C29 C30 O8 -161.3(5) . . . . ? N3 C29 C30 O7 22.0(6) . . . . ? N4 C31 C32 O10 157.6(5) . . . . ? N4 C31 C32 O9 -24.9(6) . . . . ? O14 C33 C34 C35 0.3(9) . . . . ? O13 C33 C34 C35 178.6(5) . . . . ? O14 C33 C34 C39 -179.7(6) . . . . ? O13 C33 C34 C39 -1.4(8) . . . . ? C39 C34 C35 C36 1.3(8) . . . . ? C33 C34 C35 C36 -178.7(5) . . . . ? C34 C35 C36 C37 1.3(8) . . . . ? C34 C35 C36 C88 -179.5(5) . . . . ? C35 C36 C37 C38 -2.1(8) . . . . ? C88 C36 C37 C38 178.6(5) . . . . ? C36 C37 C38 C39 0.3(8) . . . . ? C35 C34 C39 C38 -3.1(8) . . . . ? C33 C34 C39 C38 176.9(5) . . . . ? C37 C38 C39 C34 2.3(8) . . . . ? C35 C36 C88 O12 1.5(8) . . . . ? C37 C36 C88 O12 -179.3(5) . . . . ? C35 C36 C88 O11 179.5(5) . . . . ? C37 C36 C88 O11 -1.3(7) . . . . ? C35 C36 C88 Zn4 -163.7(17) . . . 1_556 ? C37 C36 C88 Zn4 15(2) . . . 1_556 ? C26 C25 N1 C8 106.9(5) . . . . ? C26 C25 N1 C13 -134.5(5) . . . . ? C26 C25 N1 Zn1 -10.7(6) . . . . ? C4 C8 N1 C25 -60.7(6) . . . . ? C4 C8 N1 C13 176.8(4) . . . . ? C4 C8 N1 Zn1 59.2(5) . . . . ? C14 C13 N1 C25 55.7(6) . . . . ? C14 C13 N1 C8 177.0(5) . . . . ? C14 C13 N1 Zn1 -68.1(5) . . . . ? O3 Zn1 N1 C25 5.4(3) . . . . ? O7 Zn1 N1 C25 -174.2(3) . . . . ? O1 Zn1 N1 C25 106.3(3) . . . . ? N3 Zn1 N1 C25 -96.3(3) . . . . ? O2 Zn1 N1 C25 17.0(6) . . . . ? O3 Zn1 N1 C8 -114.8(3) . . . . ? O7 Zn1 N1 C8 65.6(3) . . . . ? O1 Zn1 N1 C8 -14.0(3) . . . . ? N3 Zn1 N1 C8 143.4(3) . . . . ? O2 Zn1 N1 C8 -103.2(4) . . . . ? O3 Zn1 N1 C13 130.5(3) . . . . ? O7 Zn1 N1 C13 -49.1(3) . . . . ? O1 Zn1 N1 C13 -128.6(3) . . . . ? N3 Zn1 N1 C13 28.7(3) . . . . ? O2 Zn1 N1 C13 142.1(4) . . . . ? C28 C27 N2 C9 -97.8(5) . . . . ? C28 C27 N2 C10 143.3(4) . . . . ? C28 C27 N2 Zn2 17.4(5) . . . . ? C6 C9 N2 C27 56.6(6) . . . . ? C6 C9 N2 C10 178.5(4) . . . . ? C6 C9 N2 Zn2 -62.8(5) . . . . ? C11 C10 N2 C27 -60.4(6) . . . . ? C11 C10 N2 C9 178.9(4) . . . . ? C11 C10 N2 Zn2 65.1(5) . . . . ? O5 Zn2 N2 C27 -10.9(3) . . . . ? O9 Zn2 N2 C27 178.3(3) . . . . ? O1 Zn2 N2 C27 -101.9(3) . . . . ? O2 Zn2 N2 C27 -9.4(6) . . . . ? N4 Zn2 N2 C27 100.0(3) . . . . ? O5 Zn2 N2 C9 107.8(3) . . . . ? O9 Zn2 N2 C9 -63.0(3) . . . . ? O1 Zn2 N2 C9 16.8(3) . . . . ? O2 Zn2 N2 C9 109.3(4) . . . . ? N4 Zn2 N2 C9 -141.4(3) . . . . ? O5 Zn2 N2 C10 -136.8(3) . . . . ? O9 Zn2 N2 C10 52.4(3) . . . . ? O1 Zn2 N2 C10 132.2(3) . . . . ? O2 Zn2 N2 C10 -135.3(4) . . . . ? N4 Zn2 N2 C10 -26.0(3) . . . . ? C30 C29 N3 C15 -146.1(4) . . . . ? C30 C29 N3 C16 95.1(5) . . . . ? C30 C29 N3 Zn1 -19.5(5) . . . . ? C14 C15 N3 C29 59.1(6) . . . . ? C14 C15 N3 C16 179.8(4) . . . . ? C14 C15 N3 Zn1 -67.1(5) . . . . ? C20 C16 N3 C29 -57.5(5) . . . . ? C20 C16 N3 C15 -179.7(4) . . . . ? C20 C16 N3 Zn1 61.8(5) . . . . ? O3 Zn1 N3 C29 -175.3(3) . . . . ? O7 Zn1 N3 C29 10.3(3) . . . . ? O1 Zn1 N3 C29 13.7(6) . . . . ? N1 Zn1 N3 C29 -95.5(3) . . . . ? O2 Zn1 N3 C29 104.7(3) . . . . ? O3 Zn1 N3 C15 -48.5(3) . . . . ? O7 Zn1 N3 C15 137.1(4) . . . . ? O1 Zn1 N3 C15 140.5(4) . . . . ? N1 Zn1 N3 C15 31.3(3) . . . . ? O2 Zn1 N3 C15 -128.4(3) . . . . ? O3 Zn1 N3 C16 66.2(3) . . . . ? O7 Zn1 N3 C16 -108.2(3) . . . . ? O1 Zn1 N3 C16 -104.8(4) . . . . ? N1 Zn1 N3 C16 146.1(3) . . . . ? O2 Zn1 N3 C16 -13.7(3) . . . . ? C32 C31 N4 C17 -98.0(5) . . . . ? C32 C31 N4 C12 143.7(4) . . . . ? C32 C31 N4 Zn2 20.5(5) . . . . ? C18 C17 N4 C31 63.6(5) . . . . ? C18 C17 N4 C12 -173.7(4) . . . . ? C18 C17 N4 Zn2 -57.3(5) . . . . ? C11 C12 N4 C31 -55.3(6) . . . . ? C11 C12 N4 C17 -175.8(4) . . . . ? C11 C12 N4 Zn2 69.0(5) . . . . ? O5 Zn2 N4 C31 170.1(3) . . . . ? O9 Zn2 N4 C31 -9.7(3) . . . . ? O1 Zn2 N4 C31 -22.6(6) . . . . ? O2 Zn2 N4 C31 -110.4(3) . . . . ? N2 Zn2 N4 C31 91.5(3) . . . . ? O5 Zn2 N4 C17 -69.8(3) . . . . ? O9 Zn2 N4 C17 110.4(3) . . . . ? O1 Zn2 N4 C17 97.5(4) . . . . ? O2 Zn2 N4 C17 9.7(3) . . . . ? N2 Zn2 N4 C17 -148.5(3) . . . . ? O5 Zn2 N4 C12 44.6(3) . . . . ? O9 Zn2 N4 C12 -135.2(3) . . . . ? O1 Zn2 N4 C12 -148.1(3) . . . . ? O2 Zn2 N4 C12 124.1(3) . . . . ? N2 Zn2 N4 C12 -34.0(3) . . . . ? C6 C5 O1 Zn2 -33.8(6) . . . . ? C4 C5 O1 Zn2 149.2(4) . . . . ? C6 C5 O1 Zn1 -149.1(4) . . . . ? C4 C5 O1 Zn1 33.9(6) . . . . ? C6 C5 O1 Zn4 87.6(5) . . . . ? C4 C5 O1 Zn4 -89.4(5) . . . . ? O5 Zn2 O1 C5 -49.9(3) . . . . ? O9 Zn2 O1 C5 129.2(3) . . . . ? O2 Zn2 O1 C5 -128.2(3) . . . . ? N2 Zn2 O1 C5 28.6(3) . . . . ? N4 Zn2 O1 C5 142.0(4) . . . . ? O5 Zn2 O1 Zn1 77.25(13) . . . . ? O9 Zn2 O1 Zn1 -103.71(14) . . . . ? O2 Zn2 O1 Zn1 -1.05(13) . . . . ? N2 Zn2 O1 Zn1 155.70(15) . . . . ? N4 Zn2 O1 Zn1 -90.9(3) . . . . ? O5 Zn2 O1 Zn4 175.52(12) . . . . ? O9 Zn2 O1 Zn4 -5.44(12) . . . . ? O2 Zn2 O1 Zn4 97.23(13) . . . . ? N2 Zn2 O1 Zn4 -106.02(14) . . . . ? N4 Zn2 O1 Zn4 7.4(4) . . . . ? O3 Zn1 O1 C5 50.4(3) . . . . ? O7 Zn1 O1 C5 -135.2(4) . . . . ? N1 Zn1 O1 C5 -30.2(4) . . . . ? N3 Zn1 O1 C5 -138.6(4) . . . . ? O2 Zn1 O1 C5 127.7(3) . . . . ? O3 Zn1 O1 Zn2 -76.26(14) . . . . ? O7 Zn1 O1 Zn2 98.10(15) . . . . ? N1 Zn1 O1 Zn2 -156.87(14) . . . . ? N3 Zn1 O1 Zn2 94.7(4) . . . . ? O2 Zn1 O1 Zn2 1.04(13) . . . . ? O3 Zn1 O1 Zn4 -173.87(12) . . . . ? O7 Zn1 O1 Zn4 0.49(12) . . . . ? N1 Zn1 O1 Zn4 105.53(14) . . . . ? N3 Zn1 O1 Zn4 -2.9(4) . . . . ? O2 Zn1 O1 Zn4 -96.57(13) . . . . ? O11 Zn4 O1 C5 32.6(4) 1_554 . . . ? O9 Zn4 O1 C5 -125.0(4) . . . . ? O7 Zn4 O1 C5 131.8(4) . . . . ? O3W Zn4 O1 C5 -179.7(5) . . . . ? O12 Zn4 O1 C5 -26.9(3) 1_554 . . . ? C88 Zn4 O1 C5 2.6(4) 1_554 . . . ? O11 Zn4 O1 Zn2 163.35(13) 1_554 . . . ? O9 Zn4 O1 Zn2 5.76(13) . . . . ? O7 Zn4 O1 Zn2 -97.48(14) . . . . ? O3W Zn4 O1 Zn2 -48.9(5) . . . . ? O12 Zn4 O1 Zn2 103.85(13) 1_554 . . . ? C88 Zn4 O1 Zn2 133.32(15) 1_554 . . . ? O11 Zn4 O1 Zn1 -99.68(14) 1_554 . . . ? O9 Zn4 O1 Zn1 102.74(14) . . . . ? O7 Zn4 O1 Zn1 -0.51(13) . . . . ? O3W Zn4 O1 Zn1 48.0(5) . . . . ? O12 Zn4 O1 Zn1 -159.17(13) 1_554 . . . ? C88 Zn4 O1 Zn1 -129.71(15) 1_554 . . . ? C20 C19 O2 Zn2 147.4(4) . . . . ? C18 C19 O2 Zn2 -34.7(6) . . . . ? C20 C19 O2 Zn1 36.4(6) . . . . ? C18 C19 O2 Zn1 -145.7(4) . . . . ? C20 C19 O2 Zn3 -86.1(5) . . . . ? C18 C19 O2 Zn3 91.8(5) . . . . ? O5 Zn2 O2 C19 145.5(3) . . . . ? O9 Zn2 O2 C19 -43.7(3) . . . . ? O1 Zn2 O2 C19 -121.1(3) . . . . ? N2 Zn2 O2 C19 144.0(4) . . . . ? N4 Zn2 O2 C19 34.9(3) . . . . ? O5 Zn2 O2 Zn1 -92.39(14) . . . . ? O9 Zn2 O2 Zn1 78.43(14) . . . . ? O1 Zn2 O2 Zn1 1.03(12) . . . . ? N2 Zn2 O2 Zn1 -93.9(4) . . . . ? N4 Zn2 O2 Zn1 157.03(14) . . . . ? O5 Zn2 O2 Zn3 6.27(12) . . . . ? O9 Zn2 O2 Zn3 177.08(12) . . . . ? O1 Zn2 O2 Zn3 99.68(13) . . . . ? N2 Zn2 O2 Zn3 4.8(4) . . . . ? N4 Zn2 O2 Zn3 -104.31(15) . . . . ? O3 Zn1 O2 C19 -133.3(3) . . . . ? O7 Zn1 O2 C19 45.8(3) . . . . ? O1 Zn1 O2 C19 123.6(3) . . . . ? N1 Zn1 O2 C19 -145.0(4) . . . . ? N3 Zn1 O2 C19 -32.4(3) . . . . ? O3 Zn1 O2 Zn2 102.08(14) . . . . ? O7 Zn1 O2 Zn2 -78.74(13) . . . . ? O1 Zn1 O2 Zn2 -1.03(12) . . . . ? N1 Zn1 O2 Zn2 90.4(4) . . . . ? N3 Zn1 O2 Zn2 -157.01(14) . . . . ? O3 Zn1 O2 Zn3 3.51(12) . . . . ? O7 Zn1 O2 Zn3 -177.32(12) . . . . ? O1 Zn1 O2 Zn3 -99.60(13) . . . . ? N1 Zn1 O2 Zn3 -8.1(4) . . . . ? N3 Zn1 O2 Zn3 104.42(14) . . . . ? O13 Zn3 O2 C19 32.0(4) . . . . ? O5 Zn3 O2 C19 -140.9(4) . . . . ? O1W Zn3 O2 C19 -60.7(4) . . . . ? O3 Zn3 O2 C19 126.2(4) . . . . ? O2W Zn3 O2 C19 169.0(4) . . . . ? O13 Zn3 O2 Zn2 166.47(14) . . . . ? O5 Zn3 O2 Zn2 -6.41(13) . . . . ? O1W Zn3 O2 Zn2 73.79(15) . . . . ? O3 Zn3 O2 Zn2 -99.34(14) . . . . ? O2W Zn3 O2 Zn2 -56.6(4) . . . . ? O13 Zn3 O2 Zn1 -97.70(14) . . . . ? O5 Zn3 O2 Zn1 89.41(14) . . . . ? O1W Zn3 O2 Zn1 169.62(13) . . . . ? O3 Zn3 O2 Zn1 -3.52(12) . . . . ? O2W Zn3 O2 Zn1 39.3(4) . . . . ? O4 C26 O3 Zn1 174.1(5) . . . . ? C25 C26 O3 Zn1 -7.7(6) . . . . ? O4 C26 O3 Zn3 6.5(8) . . . . ? C25 C26 O3 Zn3 -175.3(3) . . . . ? O7 Zn1 O3 C26 177.1(12) . . . . ? O1 Zn1 O3 C26 -92.6(4) . . . . ? N1 Zn1 O3 C26 1.3(4) . . . . ? N3 Zn1 O3 C26 91.1(4) . . . . ? O2 Zn1 O3 C26 -174.3(4) . . . . ? O7 Zn1 O3 Zn3 -12.7(14) . . . . ? O1 Zn1 O3 Zn3 77.64(16) . . . . ? N1 Zn1 O3 Zn3 171.49(18) . . . . ? N3 Zn1 O3 Zn3 -98.65(17) . . . . ? O2 Zn1 O3 Zn3 -4.10(14) . . . . ? O13 Zn3 O3 C26 -96.1(4) . . . . ? O5 Zn3 O3 C26 98.5(4) . . . . ? O1W Zn3 O3 C26 121.3(9) . . . . ? O2W Zn3 O3 C26 7.3(4) . . . . ? O2 Zn3 O3 C26 172.3(5) . . . . ? O13 Zn3 O3 Zn1 95.44(17) . . . . ? O5 Zn3 O3 Zn1 -69.96(16) . . . . ? O1W Zn3 O3 Zn1 -47.1(10) . . . . ? O2W Zn3 O3 Zn1 -161.21(17) . . . . ? O2 Zn3 O3 Zn1 3.85(13) . . . . ? O6 C28 O5 Zn3 15.6(8) . . . . ? C27 C28 O5 Zn3 -160.0(3) . . . . ? O6 C28 O5 Zn2 -177.0(4) . . . . ? C27 C28 O5 Zn2 7.4(6) . . . . ? O13 Zn3 O5 C28 146.6(6) . . . . ? O1W Zn3 O5 C28 72.4(4) . . . . ? O3 Zn3 O5 C28 -111.0(4) . . . . ? O2W Zn3 O5 C28 -21.7(4) . . . . ? O2 Zn3 O5 C28 175.3(4) . . . . ? O13 Zn3 O5 Zn2 -21.8(6) . . . . ? O1W Zn3 O5 Zn2 -96.00(18) . . . . ? O3 Zn3 O5 Zn2 80.62(17) . . . . ? O2W Zn3 O5 Zn2 169.95(17) . . . . ? O2 Zn3 O5 Zn2 6.89(13) . . . . ? O9 Zn2 O5 C28 92.2(9) . . . . ? O1 Zn2 O5 C28 98.2(4) . . . . ? O2 Zn2 O5 C28 -177.3(4) . . . . ? N2 Zn2 O5 C28 2.1(4) . . . . ? N4 Zn2 O5 C28 -86.9(4) . . . . ? O9 Zn2 O5 Zn3 -97.9(8) . . . . ? O1 Zn2 O5 Zn3 -91.86(16) . . . . ? O2 Zn2 O5 Zn3 -7.43(15) . . . . ? N2 Zn2 O5 Zn3 172.0(2) . . . . ? N4 Zn2 O5 Zn3 83.00(19) . . . . ? O8 C30 O7 Zn4 -5.2(8) . . . . ? C29 C30 O7 Zn4 171.3(3) . . . . ? O8 C30 O7 Zn1 169.8(4) . . . . ? C29 C30 O7 Zn1 -13.7(6) . . . . ? O11 Zn4 O7 C30 -93.4(4) 1_554 . . . ? O9 Zn4 O7 C30 102.5(4) . . . . ? O3W Zn4 O7 C30 8.7(5) . . . . ? O1 Zn4 O7 C30 176.0(5) . . . . ? O12 Zn4 O7 C30 -122.1(5) 1_554 . . . ? C88 Zn4 O7 C30 -103.8(5) 1_554 . . . ? O11 Zn4 O7 Zn1 91.11(19) 1_554 . . . ? O9 Zn4 O7 Zn1 -72.91(18) . . . . ? O3W Zn4 O7 Zn1 -166.75(17) . . . . ? O1 Zn4 O7 Zn1 0.54(14) . . . . ? O12 Zn4 O7 Zn1 62.4(4) 1_554 . . . ? C88 Zn4 O7 Zn1 80.7(2) 1_554 . . . ? O3 Zn1 O7 C30 -85.1(14) . . . . ? O1 Zn1 O7 C30 -176.6(4) . . . . ? N1 Zn1 O7 C30 90.6(4) . . . . ? N3 Zn1 O7 C30 2.0(4) . . . . ? O2 Zn1 O7 C30 -93.6(4) . . . . ? O3 Zn1 O7 Zn4 90.9(13) . . . . ? O1 Zn1 O7 Zn4 -0.58(15) . . . . ? N1 Zn1 O7 Zn4 -93.39(19) . . . . ? N3 Zn1 O7 Zn4 178.0(2) . . . . ? O2 Zn1 O7 Zn4 82.42(17) . . . . ? O10 C32 O9 Zn4 -6.2(8) . . . . ? C31 C32 O9 Zn4 176.5(3) . . . . ? O10 C32 O9 Zn2 -165.8(4) . . . . ? C31 C32 O9 Zn2 16.9(5) . . . . ? O11 Zn4 O9 C32 126.0(5) 1_554 . . . ? O7 Zn4 O9 C32 -94.9(4) . . . . ? O3W Zn4 O9 C32 -1.2(4) . . . . ? O1 Zn4 O9 C32 -167.4(4) . . . . ? O12 Zn4 O9 C32 102.1(4) 1_554 . . . ? C88 Zn4 O9 C32 110.9(4) 1_554 . . . ? O11 Zn4 O9 Zn2 -72.7(4) 1_554 . . . ? O7 Zn4 O9 Zn2 66.43(17) . . . . ? O3W Zn4 O9 Zn2 160.09(17) . . . . ? O1 Zn4 O9 Zn2 -6.05(13) . . . . ? O12 Zn4 O9 Zn2 -96.54(16) 1_554 . . . ? C88 Zn4 O9 Zn2 -87.7(2) 1_554 . . . ? O5 Zn2 O9 C32 176.6(7) . . . . ? O1 Zn2 O9 C32 170.5(4) . . . . ? O2 Zn2 O9 C32 88.0(4) . . . . ? N2 Zn2 O9 C32 -95.1(4) . . . . ? N4 Zn2 O9 C32 -4.2(3) . . . . ? O5 Zn2 O9 Zn4 12.7(9) . . . . ? O1 Zn2 O9 Zn4 6.52(14) . . . . ? O2 Zn2 O9 Zn4 -75.98(17) . . . . ? N2 Zn2 O9 Zn4 100.93(18) . . . . ? N4 Zn2 O9 Zn4 -168.19(19) . . . . ? O12 C88 O11 Zn4 -5.9(6) . . . 1_556 ? C36 C88 O11 Zn4 176.0(4) . . . 1_556 ? O11 C88 O12 Zn4 5.0(5) . . . 1_556 ? C36 C88 O12 Zn4 -177.0(5) . . . 1_556 ? O14 C33 O13 Zn3 -6.7(10) . . . . ? C34 C33 O13 Zn3 175.1(3) . . . . ? O5 Zn3 O13 C33 -60.7(8) . . . . ? O1W Zn3 O13 C33 12.4(5) . . . . ? O3 Zn3 O13 C33 -162.3(5) . . . . ? O2W Zn3 O13 C33 107.2(5) . . . . ? O2 Zn3 O13 C33 -88.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O6 0.819(18) 2.18(2) 2.738(5) 126(3) 2_657 O1W H1WA O2W 0.819(18) 2.57(2) 3.089(6) 122.6(12) . O2W H2WA O4 0.852(19) 1.91(4) 2.692(6) 152(7) . O2W H2WB O6 0.855(19) 1.89(2) 2.733(5) 167(6) . O3W H3WA O8 0.847(19) 1.89(3) 2.691(5) 157(7) . O3W H3WB O10 0.839(19) 1.89(3) 2.706(6) 163(7) . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.122 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.115 data_Compound-5 _database_code_depnum_ccdc_archive 'CCDC 922858' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H21 Co2 N2 O8), 2(H O0.50)' _chemical_formula_sum 'C34 H44 Co4 N4 O17' _chemical_formula_weight 1016.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m ' _symmetry_space_group_name_hall '-C 2y ' 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 14.726(5) _cell_length_b 16.062(5) _cell_length_c 10.163(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 123.115(5) _cell_angle_gamma 90.000(5) _cell_volume 2013.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2377 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.253 _exptl_crystal_size_mid 0.246 _exptl_crystal_size_min 0.235 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_T_max 0.671 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9967 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2377 _reflns_number_gt 1756 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+4.3186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2377 _refine_ls_number_parameters 154 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Co1 Co 0.89596(6) 0.5000 0.18341(8) 0.0350(2) Uani 1 2 d S . . Co2 Co 1.0000 0.40131(4) 0.0000 0.0243(2) Uani 1 2 d S . . C1 C 1.4928(6) 0.5000 0.6796(10) 0.106(4) Uani 1 2 d S . . H1A H 1.5189 0.5563 0.7041 0.159 Uiso 0.50 1 calc PR . . H1B H 1.5342 0.4693 0.6487 0.159 Uiso 0.50 1 calc PR . . H1C H 1.5005 0.4744 0.7706 0.159 Uiso 0.50 1 calc PR . . C2 C 1.3731(5) 0.5000 0.5449(8) 0.069(2) Uani 1 2 d S . . C3 C 1.3154(4) 0.5737(3) 0.4831(5) 0.0646(14) Uani 1 1 d . . . H3 H 1.3513 0.6240 0.5239 0.077 Uiso 1 1 calc R . . C4 C 1.2059(4) 0.5751(3) 0.3626(4) 0.0482(11) Uani 1 1 d . . . C5 C 1.1520(4) 0.5000 0.2951(6) 0.0382(13) Uani 1 2 d S . . C6 C 0.7865(3) 0.3587(3) -0.0610(5) 0.0433(10) Uani 1 1 d . . . C7 C 0.8009(3) 0.2928(3) -0.1528(5) 0.0490(11) Uani 1 1 d . . . H7A H 0.8107 0.2394 -0.1021 0.059 Uiso 1 1 calc R . . H7B H 0.7354 0.2896 -0.2572 0.059 Uiso 1 1 calc R . . C8 C 0.9555(4) 0.2318(3) -0.1504(5) 0.0540(12) Uani 1 1 d . . . H8A H 1.0158 0.2472 -0.1590 0.065 Uiso 1 1 calc R . . H8B H 0.9085 0.1955 -0.2382 0.065 Uiso 1 1 calc R . . C9 C 1.0000 0.1825(4) 0.0000 0.0570(17) Uani 1 2 d S . . H9A H 0.9426 0.1467 -0.0128 0.068 Uiso 0.50 1 calc PR . . H9B H 1.0574 0.1467 0.0128 0.068 Uiso 0.50 1 calc PR . . C10 C 0.8556(4) 0.3444(3) -0.3240(5) 0.0506(11) Uani 1 1 d . . . H10A H 0.8095 0.3037 -0.4034 0.061 Uiso 1 1 calc R . . H10B H 0.9180 0.3533 -0.3310 0.061 Uiso 1 1 calc R . . C11 C 1.0000 0.5476(4) 0.5000 0.0451(14) Uani 1 2 d S . . N1 N 0.8942(3) 0.3085(2) -0.1667(4) 0.0431(8) Uani 1 1 d . . . O1 O 1.0472(3) 0.5000 0.1691(4) 0.0367(9) Uani 1 2 d S . . O2 O 0.8687(2) 0.40668(18) 0.0247(3) 0.0435(7) Uani 1 1 d . . . O4 O 0.9553(3) 0.58369(19) 0.3687(3) 0.0559(8) Uani 1 1 d . . . O3 O 0.7009(2) 0.3630(2) -0.0658(4) 0.0655(9) Uani 1 1 d . . . O1W O 0.7345(5) 0.5000 0.1140(7) 0.0701(14) Uani 1 2 d SD . . H1WA H 0.706(5) 0.544(3) 0.058(6) 0.105 Uiso 1 1 d D . . O2W O 0.5000 0.7328(8) 0.5000 0.124(6) Uani 0.50 2 d SPD . . H2WA H 0.542(11) 0.774(6) 0.53(2) 0.187 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0454(5) 0.0391(5) 0.0283(4) 0.000 0.0252(4) 0.000 Co2 0.0241(3) 0.0280(4) 0.0213(3) 0.000 0.0127(3) 0.000 C1 0.049(5) 0.134(9) 0.077(6) 0.000 -0.003(4) 0.000 C2 0.043(4) 0.079(5) 0.045(4) 0.000 -0.001(3) 0.000 C3 0.048(3) 0.074(3) 0.045(3) -0.011(2) 0.008(2) -0.012(2) C4 0.049(2) 0.055(3) 0.031(2) -0.0029(18) 0.0158(19) 0.001(2) C5 0.036(3) 0.049(3) 0.019(2) 0.000 0.009(2) 0.000 C6 0.037(2) 0.044(2) 0.047(2) 0.0044(19) 0.0220(19) -0.0040(18) C7 0.045(2) 0.043(2) 0.055(3) -0.0038(19) 0.025(2) -0.0117(19) C8 0.059(3) 0.045(3) 0.057(3) -0.012(2) 0.031(2) -0.004(2) C9 0.057(4) 0.038(3) 0.073(4) 0.000 0.034(4) 0.000 C10 0.060(3) 0.048(3) 0.037(2) -0.0124(19) 0.022(2) -0.005(2) C11 0.063(4) 0.047(4) 0.041(3) 0.000 0.038(3) 0.000 N1 0.0464(19) 0.041(2) 0.0446(19) -0.0056(15) 0.0269(16) -0.0061(16) O1 0.037(2) 0.043(2) 0.0267(18) 0.000 0.0153(16) 0.000 O2 0.0396(15) 0.0509(17) 0.0447(16) -0.0081(13) 0.0261(13) -0.0087(13) O4 0.083(2) 0.0509(19) 0.0476(17) 0.0042(14) 0.0440(17) 0.0040(16) O3 0.0475(18) 0.064(2) 0.096(3) 0.0002(19) 0.0460(19) -0.0056(16) O1W 0.070(3) 0.073(4) 0.092(4) 0.000 0.060(3) 0.000 O2W 0.148(14) 0.047(7) 0.231(19) 0.000 0.137(15) 0.000 _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 O2 2.074(3) . ? Co1 O2 2.074(3) 6_565 ? Co1 O4 2.078(3) . ? Co1 O4 2.078(3) 6_565 ? Co1 O1W 2.079(6) . ? Co1 O1 2.309(4) . ? Co2 O2 2.083(3) . ? Co2 O2 2.083(3) 2_755 ? Co2 N1 2.153(3) . ? Co2 N1 2.153(3) 2_755 ? Co2 O1 2.155(2) . ? Co2 O1 2.155(2) 5_765 ? C1 C2 1.531(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.391(6) 6_565 ? C2 C3 1.391(6) . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C5 1.400(5) . ? C4 C10 1.503(6) 5_765 ? C5 O1 1.365(6) . ? C5 C4 1.400(5) 6_565 ? C6 O3 1.238(5) . ? C6 O2 1.291(5) . ? C6 C7 1.499(6) . ? C7 N1 1.477(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.482(6) . ? C8 C9 1.516(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C8 1.516(6) 2_755 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.491(5) . ? C10 C4 1.503(6) 5_765 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O4 1.261(4) 2_756 ? C11 O4 1.261(4) . ? C11 C11 1.530(12) 5_766 ? O1 Co2 2.155(2) 5_765 ? O1W H1WA 0.865(19) . ? O2W H2WA 0.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 92.55(16) . 6_565 ? O2 Co1 O4 168.25(13) . . ? O2 Co1 O4 92.53(12) 6_565 . ? O2 Co1 O4 92.53(12) . 6_565 ? O2 Co1 O4 168.25(13) 6_565 6_565 ? O4 Co1 O4 80.61(17) . 6_565 ? O2 Co1 O1W 92.11(13) . . ? O2 Co1 O1W 92.11(13) 6_565 . ? O4 Co1 O1W 98.28(16) . . ? O4 Co1 O1W 98.28(16) 6_565 . ? O2 Co1 O1 74.60(10) . . ? O2 Co1 O1 74.60(10) 6_565 . ? O4 Co1 O1 96.59(12) . . ? O4 Co1 O1 96.59(12) 6_565 . ? O1W Co1 O1 160.46(18) . . ? O2 Co2 O2 175.25(16) . 2_755 ? O2 Co2 N1 78.63(12) . . ? O2 Co2 N1 104.75(12) 2_755 . ? O2 Co2 N1 104.75(12) . 2_755 ? O2 Co2 N1 78.63(12) 2_755 2_755 ? N1 Co2 N1 92.35(19) . 2_755 ? O2 Co2 O1 77.84(12) . . ? O2 Co2 O1 98.61(13) 2_755 . ? N1 Co2 O1 156.34(14) . . ? N1 Co2 O1 95.90(12) 2_755 . ? O2 Co2 O1 98.61(13) . 5_765 ? O2 Co2 O1 77.84(12) 2_755 5_765 ? N1 Co2 O1 95.90(12) . 5_765 ? N1 Co2 O1 156.34(14) 2_755 5_765 ? O1 Co2 O1 85.29(14) . 5_765 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C3 116.6(6) 6_565 . ? C3 C2 C1 121.7(3) 6_565 . ? C3 C2 C1 121.7(3) . . ? C2 C3 C4 122.6(5) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 C10 119.1(4) . 5_765 ? C5 C4 C10 120.9(4) . 5_765 ? O1 C5 C4 120.5(2) . . ? O1 C5 C4 120.5(2) . 6_565 ? C4 C5 C4 118.9(5) . 6_565 ? O3 C6 O2 123.6(4) . . ? O3 C6 C7 120.1(4) . . ? O2 C6 C7 116.2(4) . . ? N1 C7 C6 113.2(3) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 116.6(4) . . ? N1 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? N1 C8 H8B 108.1 . . ? C9 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C8 117.0(5) 2_755 . ? C8 C9 H9A 108.1 2_755 . ? C8 C9 H9A 108.1 . . ? C8 C9 H9B 108.1 2_755 . ? C8 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? N1 C10 C4 115.8(4) . 5_765 ? N1 C10 H10A 108.3 . . ? C4 C10 H10A 108.3 5_765 . ? N1 C10 H10B 108.3 . . ? C4 C10 H10B 108.3 5_765 . ? H10A C10 H10B 107.4 . . ? O4 C11 O4 125.3(6) 2_756 . ? O4 C11 C11 117.3(3) 2_756 5_766 ? O4 C11 C11 117.3(3) . 5_766 ? C7 N1 C8 113.0(3) . . ? C7 N1 C10 109.9(3) . . ? C8 N1 C10 107.0(3) . . ? C7 N1 Co2 110.7(2) . . ? C8 N1 Co2 110.6(3) . . ? C10 N1 Co2 105.3(2) . . ? C5 O1 Co2 117.1(2) . . ? C5 O1 Co2 117.1(2) . 5_765 ? Co2 O1 Co2 94.71(14) . 5_765 ? C5 O1 Co1 125.1(3) . . ? Co2 O1 Co1 98.54(12) . . ? Co2 O1 Co1 98.54(12) 5_765 . ? C6 O2 Co1 131.9(3) . . ? C6 O2 Co2 118.9(3) . . ? Co1 O2 Co2 109.01(12) . . ? C11 O4 Co1 112.3(3) . . ? Co1 O1W H1WA 106(5) . . ? 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 C3 C2 C3 C4 -1.6(12) 6_565 . . . ? C1 C2 C3 C4 -178.7(7) . . . . ? C2 C3 C4 C5 -2.9(9) . . . . ? C2 C3 C4 C10 168.2(6) . . . 5_765 ? C3 C4 C5 O1 -174.9(5) . . . . ? C10 C4 C5 O1 14.1(7) 5_765 . . . ? C3 C4 C5 C4 7.4(9) . . . 6_565 ? C10 C4 C5 C4 -163.6(3) 5_765 . . 6_565 ? O3 C6 C7 N1 165.7(4) . . . . ? O2 C6 C7 N1 -16.8(5) . . . . ? N1 C8 C9 C8 -38.5(3) . . . 2_755 ? C6 C7 N1 C8 139.9(4) . . . . ? C6 C7 N1 C10 -100.7(4) . . . . ? C6 C7 N1 Co2 15.2(4) . . . . ? C9 C8 N1 C7 -57.0(5) . . . . ? C9 C8 N1 C10 -178.1(3) . . . . ? C9 C8 N1 Co2 67.8(4) . . . . ? C4 C10 N1 C7 59.0(5) 5_765 . . . ? C4 C10 N1 C8 -178.0(4) 5_765 . . . ? C4 C10 N1 Co2 -60.3(4) 5_765 . . . ? O2 Co2 N1 C7 -8.2(3) . . . . ? O2 Co2 N1 C7 175.2(3) 2_755 . . . ? N1 Co2 N1 C7 96.4(3) 2_755 . . . ? O1 Co2 N1 C7 -14.1(5) . . . . ? O1 Co2 N1 C7 -105.8(3) 5_765 . . . ? O2 Co2 N1 C8 -134.2(3) . . . . ? O2 Co2 N1 C8 49.2(3) 2_755 . . . ? N1 Co2 N1 C8 -29.7(2) 2_755 . . . ? O1 Co2 N1 C8 -140.2(3) . . . . ? O1 Co2 N1 C8 128.1(3) 5_765 . . . ? O2 Co2 N1 C10 110.5(3) . . . . ? O2 Co2 N1 C10 -66.1(3) 2_755 . . . ? N1 Co2 N1 C10 -144.9(3) 2_755 . . . ? O1 Co2 N1 C10 104.6(3) . . . . ? O1 Co2 N1 C10 12.9(3) 5_765 . . . ? C4 C5 O1 Co2 146.9(4) . . . . ? C4 C5 O1 Co2 -35.5(6) 6_565 . . . ? C4 C5 O1 Co2 35.5(6) . . . 5_765 ? C4 C5 O1 Co2 -146.9(4) 6_565 . . 5_765 ? C4 C5 O1 Co1 -88.8(5) . . . . ? C4 C5 O1 Co1 88.8(5) 6_565 . . . ? O2 Co2 O1 C5 136.4(3) . . . . ? O2 Co2 O1 C5 -46.8(3) 2_755 . . . ? N1 Co2 O1 C5 142.4(3) . . . . ? N1 Co2 O1 C5 32.6(3) 2_755 . . . ? O1 Co2 O1 C5 -123.7(3) 5_765 . . . ? O2 Co2 O1 Co2 -99.87(14) . . . 5_765 ? O2 Co2 O1 Co2 76.92(13) 2_755 . . 5_765 ? N1 Co2 O1 Co2 -93.9(3) . . . 5_765 ? N1 Co2 O1 Co2 156.27(14) 2_755 . . 5_765 ? O1 Co2 O1 Co2 0.0 5_765 . . 5_765 ? O2 Co2 O1 Co1 -0.49(10) . . . . ? O2 Co2 O1 Co1 176.31(9) 2_755 . . . ? N1 Co2 O1 Co1 5.4(3) . . . . ? N1 Co2 O1 Co1 -104.34(12) 2_755 . . . ? O1 Co2 O1 Co1 99.39(14) 5_765 . . . ? O2 Co1 O1 C5 -131.45(9) . . . . ? O2 Co1 O1 C5 131.45(9) 6_565 . . . ? O4 Co1 O1 C5 40.63(9) . . . . ? O4 Co1 O1 C5 -40.63(9) 6_565 . . . ? O1W Co1 O1 C5 180.000(2) . . . . ? O2 Co1 O1 Co2 0.49(10) . . . . ? O2 Co1 O1 Co2 -96.61(13) 6_565 . . . ? O4 Co1 O1 Co2 172.57(10) . . . . ? O4 Co1 O1 Co2 91.31(13) 6_565 . . . ? O1W Co1 O1 Co2 -48.06(8) . . . . ? O2 Co1 O1 Co2 96.61(13) . . . 5_765 ? O2 Co1 O1 Co2 -0.49(10) 6_565 . . 5_765 ? O4 Co1 O1 Co2 -91.31(13) . . . 5_765 ? O4 Co1 O1 Co2 -172.57(10) 6_565 . . 5_765 ? O1W Co1 O1 Co2 48.06(8) . . . 5_765 ? O3 C6 O2 Co1 2.5(6) . . . . ? C7 C6 O2 Co1 -175.0(3) . . . . ? O3 C6 O2 Co2 -172.7(3) . . . . ? C7 C6 O2 Co2 9.8(5) . . . . ? O2 Co1 O2 C6 -102.9(3) 6_565 . . . ? O4 Co1 O2 C6 141.6(5) . . . . ? O4 Co1 O2 C6 87.7(4) 6_565 . . . ? O1W Co1 O2 C6 -10.6(4) . . . . ? O1 Co1 O2 C6 -176.1(4) . . . . ? O2 Co1 O2 Co2 72.73(15) 6_565 . . . ? O4 Co1 O2 Co2 -42.8(6) . . . . ? O4 Co1 O2 Co2 -96.68(15) 6_565 . . . ? O1W Co1 O2 Co2 164.94(16) . . . . ? O1 Co1 O2 Co2 -0.53(11) . . . . ? O2 Co2 O2 C6 134.9(3) 2_755 . . . ? N1 Co2 O2 C6 -0.8(3) . . . . ? N1 Co2 O2 C6 -90.2(3) 2_755 . . . ? O1 Co2 O2 C6 176.8(3) . . . . ? O1 Co2 O2 C6 93.6(3) 5_765 . . . ? O2 Co2 O2 Co1 -41.35(11) 2_755 . . . ? N1 Co2 O2 Co1 -177.01(16) . . . . ? N1 Co2 O2 Co1 93.54(15) 2_755 . . . ? O1 Co2 O2 Co1 0.57(11) . . . . ? O1 Co2 O2 Co1 -82.68(14) 5_765 . . . ? O4 C11 O4 Co1 178.3(2) 2_756 . . . ? C11 C11 O4 Co1 -1.7(3) 5_766 . . . ? O2 Co1 O4 C11 -52.9(7) . . . . ? O2 Co1 O4 C11 -168.5(2) 6_565 . . . ? O4 Co1 O4 C11 1.9(3) 6_565 . . . ? O1W Co1 O4 C11 99.0(2) . . . . ? O1 Co1 O4 C11 -93.7(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.865(19) 1.92(3) 2.727(5) 154(6) 6_565 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.556 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.094 data_Compound-6 _database_code_depnum_ccdc_archive 'CCDC 922859' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H21 N2 O8 Zn2), 2(H O0.50)' _chemical_formula_sum 'C34 H44 N4 O17 Zn4' _chemical_formula_weight 1042.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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_space_group_name_hall '-C 2y ' 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 14.719(5) _cell_length_b 16.064(5) _cell_length_c 10.160(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 123.156(5) _cell_angle_gamma 90.000(5) _cell_volume 2011.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2390 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.281 _exptl_crystal_size_mid 0.273 _exptl_crystal_size_min 0.262 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9941 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2390 _reflns_number_gt 1971 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.9867P] 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 2390 _refine_ls_number_parameters 153 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.063 _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 Zn1 Zn 0.0000 0.40135(2) 0.0000 0.02476(11) Uani 1 2 d S . . Zn2 Zn -0.10412(4) 0.5000 0.18334(5) 0.03572(13) Uani 1 2 d SD . . C1 C 0.4924(4) 0.5000 0.6768(6) 0.0902(19) Uani 1 2 d S . . H1A H 0.5180 0.5563 0.7029 0.135 Uiso 0.50 1 calc PR . . H1B H 0.5335 0.4706 0.6440 0.135 Uiso 0.50 1 calc PR . . H1C H 0.5010 0.4731 0.7673 0.135 Uiso 0.50 1 calc PR . . C2 C 0.3726(3) 0.5000 0.5434(5) 0.0578(12) Uani 1 2 d S . . C3 C 0.3157(2) 0.42671(19) 0.4835(3) 0.0506(7) Uani 1 1 d . . . H3 H 0.3519 0.3766 0.5250 0.061 Uiso 1 1 calc R . . C4 C 0.2061(2) 0.42482(16) 0.3630(3) 0.0362(6) Uani 1 1 d . . . C5 C 0.1520(3) 0.5000 0.2957(3) 0.0288(7) Uani 1 2 d S . . C6 C 0.1448(2) 0.34419(15) 0.3246(3) 0.0383(6) Uani 1 1 d . . . H6A H 0.1912 0.3035 0.4038 0.046 Uiso 1 1 calc R . . H6B H 0.0824 0.3529 0.3318 0.046 Uiso 1 1 calc R . . C7 C 0.0441(2) 0.23186(16) 0.1508(3) 0.0418(6) Uani 1 1 d . . . H7A H -0.0163 0.2473 0.1590 0.050 Uiso 1 1 calc R . . H7B H 0.0910 0.1955 0.2387 0.050 Uiso 1 1 calc R . . C8 C 0.0000 0.1829(2) 0.0000 0.0462(9) Uani 1 2 d S . . H8A H -0.0575 0.1471 -0.0133 0.055 Uiso 0.50 1 calc PR . . H8B H 0.0575 0.1471 0.0133 0.055 Uiso 0.50 1 calc PR . . C9 C 0.1987(2) 0.29260(16) 0.1522(3) 0.0387(6) Uani 1 1 d . . . H9A H 0.1882 0.2394 0.1004 0.046 Uiso 1 1 calc R . . H9B H 0.2644 0.2888 0.2565 0.046 Uiso 1 1 calc R . . C10 C 0.2135(2) 0.35951(15) 0.0603(3) 0.0336(5) Uani 1 1 d . . . C11 C 0.0000 0.5481(2) 0.5000 0.0353(8) Uani 1 2 d S . . N1 N 0.10601(17) 0.30854(12) 0.1668(2) 0.0321(4) Uani 1 1 d . . . O1 O 0.04722(17) 0.5000 0.1691(2) 0.0259(5) Uani 1 2 d S . . O2 O 0.13121(14) 0.40684(10) -0.02471(19) 0.0338(4) Uani 1 1 d . . . O3 O 0.29853(15) 0.36252(12) 0.0654(3) 0.0506(5) Uani 1 1 d . . . O4 O -0.04455(18) 0.58316(11) 0.3691(2) 0.0437(5) Uani 1 1 d . . . O1W O -0.2665(3) 0.5000 0.1137(4) 0.0583(8) Uani 1 2 d SD . . H1WA H -0.2795(17) 0.5395(17) 0.057(3) 0.087 Uiso 1 1 d D . . O2W O 0.0000 0.7671(5) 0.5000 0.110(3) Uani 0.50 2 d SPD . . H2WA H 0.051(8) 0.755(8) 0.587(8) 0.164 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0234(2) 0.0290(2) 0.02165(18) 0.000 0.01218(16) 0.000 Zn2 0.0459(3) 0.0404(2) 0.0289(2) 0.000 0.0256(2) 0.000 C1 0.039(3) 0.116(5) 0.057(3) 0.000 -0.011(2) 0.000 C2 0.033(2) 0.078(3) 0.031(2) 0.000 -0.0024(18) 0.000 C3 0.0394(17) 0.0602(18) 0.0305(13) 0.0097(13) 0.0051(12) 0.0110(14) C4 0.0345(14) 0.0443(14) 0.0204(11) 0.0044(10) 0.0090(10) 0.0039(11) C5 0.0293(18) 0.0367(17) 0.0148(13) 0.000 0.0084(13) 0.000 C6 0.0459(16) 0.0374(13) 0.0265(12) 0.0109(10) 0.0166(12) 0.0092(11) C7 0.0465(17) 0.0346(13) 0.0447(15) 0.0091(11) 0.0253(14) 0.0006(11) C8 0.051(3) 0.0273(17) 0.064(3) 0.000 0.034(2) 0.000 C9 0.0330(14) 0.0373(13) 0.0427(14) 0.0051(11) 0.0187(12) 0.0106(11) C10 0.0283(13) 0.0346(12) 0.0360(13) -0.0067(10) 0.0163(11) 0.0008(10) C11 0.050(2) 0.0349(18) 0.0358(18) 0.000 0.0334(18) 0.000 N1 0.0337(11) 0.0310(10) 0.0314(10) 0.0047(8) 0.0176(9) 0.0034(8) O1 0.0242(12) 0.0309(11) 0.0175(10) 0.000 0.0081(9) 0.000 O2 0.0288(9) 0.0444(9) 0.0328(9) 0.0086(7) 0.0197(8) 0.0070(7) O3 0.0332(11) 0.0482(11) 0.0772(14) -0.0005(10) 0.0345(11) 0.0040(9) O4 0.0686(14) 0.0384(9) 0.0343(9) 0.0036(8) 0.0346(10) 0.0032(9) O1W 0.060(2) 0.064(2) 0.076(2) 0.000 0.0528(19) 0.000 O2W 0.125(10) 0.046(4) 0.193(12) 0.000 0.109(9) 0.000 _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 Zn1 O2 2.0810(17) 2 ? Zn1 O2 2.0810(17) . ? Zn1 N1 2.153(2) 2 ? Zn1 N1 2.153(2) . ? Zn1 O1 2.1539(15) . ? Zn1 O1 2.1539(15) 5_565 ? Zn2 O2 2.0720(17) 2 ? Zn2 O2 2.0720(17) 5_565 ? Zn2 O4 2.0750(19) . ? Zn2 O4 2.0750(19) 6_565 ? Zn2 O1W 2.089(3) . ? Zn2 O1 2.310(2) . ? C1 C2 1.527(6) . ? C2 C3 1.379(4) . ? C2 C3 1.379(4) 6_565 ? C3 C4 1.393(4) . ? C4 C5 1.402(3) . ? C4 C6 1.503(4) . ? C5 O1 1.365(4) . ? C5 C4 1.402(3) 6_565 ? C6 N1 1.491(3) . ? C7 N1 1.487(3) . ? C7 C8 1.516(3) . ? C8 C7 1.516(3) 2 ? C9 N1 1.474(3) . ? C9 C10 1.516(4) . ? C10 O3 1.224(3) . ? C10 O2 1.284(3) . ? C11 O4 1.250(2) 2_556 ? C11 O4 1.250(2) . ? C11 C11 1.546(7) 5_566 ? O1 Zn1 2.1539(15) 5_565 ? O2 Zn2 2.0720(17) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O2 175.13(9) 2 . ? O2 Zn1 N1 78.66(7) 2 2 ? O2 Zn1 N1 104.79(7) . 2 ? O2 Zn1 N1 104.79(7) 2 . ? O2 Zn1 N1 78.66(7) . . ? N1 Zn1 N1 92.36(11) 2 . ? O2 Zn1 O1 77.79(7) 2 . ? O2 Zn1 O1 98.57(8) . . ? N1 Zn1 O1 156.33(8) 2 . ? N1 Zn1 O1 95.91(7) . . ? O2 Zn1 O1 98.57(8) 2 5_565 ? O2 Zn1 O1 77.79(7) . 5_565 ? N1 Zn1 O1 95.91(7) 2 5_565 ? N1 Zn1 O1 156.33(8) . 5_565 ? O1 Zn1 O1 85.26(8) . 5_565 ? O2 Zn2 O2 92.48(10) 2 5_565 ? O2 Zn2 O4 168.05(8) 2 . ? O2 Zn2 O4 92.77(7) 5_565 . ? O2 Zn2 O4 92.77(7) 2 6_565 ? O2 Zn2 O4 168.05(8) 5_565 6_565 ? O4 Zn2 O4 80.15(10) . 6_565 ? O2 Zn2 O1W 92.22(8) 2 . ? O2 Zn2 O1W 92.22(8) 5_565 . ? O4 Zn2 O1W 98.29(9) . . ? O4 Zn2 O1W 98.29(9) 6_565 . ? O2 Zn2 O1 74.52(6) 2 . ? O2 Zn2 O1 74.52(6) 5_565 . ? O4 Zn2 O1 96.59(7) . . ? O4 Zn2 O1 96.59(7) 6_565 . ? O1W Zn2 O1 160.51(11) . . ? C3 C2 C3 117.3(4) . 6_565 ? C3 C2 C1 121.31(18) . . ? C3 C2 C1 121.31(18) 6_565 . ? C2 C3 C4 122.6(3) . . ? C3 C4 C5 119.1(3) . . ? C3 C4 C6 119.3(2) . . ? C5 C4 C6 121.0(2) . . ? O1 C5 C4 120.51(16) . 6_565 ? O1 C5 C4 120.51(16) . . ? C4 C5 C4 119.0(3) 6_565 . ? N1 C6 C4 115.6(2) . . ? N1 C7 C8 116.0(2) . . ? C7 C8 C7 117.5(3) . 2 ? N1 C9 C10 113.07(19) . . ? O3 C10 O2 124.9(2) . . ? O3 C10 C9 119.3(2) . . ? O2 C10 C9 115.7(2) . . ? O4 C11 O4 126.4(3) 2_556 . ? O4 C11 C11 116.78(16) 2_556 5_566 ? O4 C11 C11 116.78(16) . 5_566 ? C9 N1 C7 113.00(19) . . ? C9 N1 C6 110.1(2) . . ? C7 N1 C6 106.67(18) . . ? C9 N1 Zn1 110.70(14) . . ? C7 N1 Zn1 110.53(16) . . ? C6 N1 Zn1 105.46(14) . . ? C5 O1 Zn1 117.20(11) . . ? C5 O1 Zn1 117.20(11) . 5_565 ? Zn1 O1 Zn1 94.74(8) . 5_565 ? C5 O1 Zn2 124.89(18) . . ? Zn1 O1 Zn2 98.54(7) . . ? Zn1 O1 Zn2 98.54(7) 5_565 . ? C10 O2 Zn2 131.32(16) . 5_565 ? C10 O2 Zn1 119.39(15) . . ? Zn2 O2 Zn1 109.15(7) 5_565 . ? C11 O4 Zn2 113.12(17) . . ? 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 C3 C2 C3 C4 2.4(7) 6_565 . . . ? C1 C2 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 2.4(5) . . . . ? C2 C3 C4 C6 -168.7(3) . . . . ? C3 C4 C5 O1 174.6(3) . . . . ? C6 C4 C5 O1 -14.5(4) . . . . ? C3 C4 C5 C4 -7.2(5) . . . 6_565 ? C6 C4 C5 C4 163.75(19) . . . 6_565 ? C3 C4 C6 N1 -114.0(3) . . . . ? C5 C4 C6 N1 75.2(3) . . . . ? N1 C7 C8 C7 -38.55(15) . . . 2 ? N1 C9 C10 O3 165.9(2) . . . . ? N1 C9 C10 O2 -17.5(3) . . . . ? C10 C9 N1 C7 140.4(2) . . . . ? C10 C9 N1 C6 -100.4(2) . . . . ? C10 C9 N1 Zn1 15.8(3) . . . . ? C8 C7 N1 C9 -56.7(3) . . . . ? C8 C7 N1 C6 -177.8(2) . . . . ? C8 C7 N1 Zn1 68.0(2) . . . . ? C4 C6 N1 C9 59.4(3) . . . . ? C4 C6 N1 C7 -177.6(2) . . . . ? C4 C6 N1 Zn1 -60.1(2) . . . . ? O2 Zn1 N1 C9 174.94(15) 2 . . . ? O2 Zn1 N1 C9 -8.58(15) . . . . ? N1 Zn1 N1 C9 96.04(16) 2 . . . ? O1 Zn1 N1 C9 -106.16(16) . . . . ? O1 Zn1 N1 C9 -14.5(3) 5_565 . . . ? O2 Zn1 N1 C7 48.96(16) 2 . . . ? O2 Zn1 N1 C7 -134.56(16) . . . . ? N1 Zn1 N1 C7 -29.94(13) 2 . . . ? O1 Zn1 N1 C7 127.86(16) . . . . ? O1 Zn1 N1 C7 -140.47(17) 5_565 . . . ? O2 Zn1 N1 C6 -65.97(16) 2 . . . ? O2 Zn1 N1 C6 110.52(16) . . . . ? N1 Zn1 N1 C6 -144.86(18) 2 . . . ? O1 Zn1 N1 C6 12.93(16) . . . . ? O1 Zn1 N1 C6 104.6(2) 5_565 . . . ? C4 C5 O1 Zn1 146.7(2) 6_565 . . . ? C4 C5 O1 Zn1 -35.1(3) . . . . ? C4 C5 O1 Zn1 35.1(3) 6_565 . . 5_565 ? C4 C5 O1 Zn1 -146.7(2) . . . 5_565 ? C4 C5 O1 Zn2 -89.1(3) 6_565 . . . ? C4 C5 O1 Zn2 89.1(3) . . . . ? O2 Zn1 O1 C5 136.21(17) 2 . . . ? O2 Zn1 O1 C5 -47.07(17) . . . . ? N1 Zn1 O1 C5 142.1(2) 2 . . . ? N1 Zn1 O1 C5 32.31(17) . . . . ? O1 Zn1 O1 C5 -123.9(2) 5_565 . . . ? O2 Zn1 O1 Zn1 -99.84(8) 2 . . 5_565 ? O2 Zn1 O1 Zn1 76.87(8) . . . 5_565 ? N1 Zn1 O1 Zn1 -93.91(17) 2 . . 5_565 ? N1 Zn1 O1 Zn1 156.26(8) . . . 5_565 ? O1 Zn1 O1 Zn1 0.0 5_565 . . 5_565 ? O2 Zn1 O1 Zn2 -0.46(6) 2 . . . ? O2 Zn1 O1 Zn2 176.26(6) . . . . ? N1 Zn1 O1 Zn2 5.48(18) 2 . . . ? N1 Zn1 O1 Zn2 -104.36(7) . . . . ? O1 Zn1 O1 Zn2 99.38(8) 5_565 . . . ? O2 Zn2 O1 C5 -131.46(5) 2 . . . ? O2 Zn2 O1 C5 131.46(5) 5_565 . . . ? O4 Zn2 O1 C5 40.40(5) . . . . ? O4 Zn2 O1 C5 -40.40(5) 6_565 . . . ? O1W Zn2 O1 C5 180.000(2) . . . . ? O2 Zn2 O1 Zn1 0.47(6) 2 . . . ? O2 Zn2 O1 Zn1 -96.61(8) 5_565 . . . ? O4 Zn2 O1 Zn1 172.33(6) . . . . ? O4 Zn2 O1 Zn1 91.53(8) 6_565 . . . ? O1W Zn2 O1 Zn1 -48.07(5) . . . . ? O2 Zn2 O1 Zn1 96.61(8) 2 . . 5_565 ? O2 Zn2 O1 Zn1 -0.47(6) 5_565 . . 5_565 ? O4 Zn2 O1 Zn1 -91.53(8) . . . 5_565 ? O4 Zn2 O1 Zn1 -172.33(6) 6_565 . . 5_565 ? O1W Zn2 O1 Zn1 48.07(5) . . . 5_565 ? O3 C10 O2 Zn2 1.8(4) . . . 5_565 ? C9 C10 O2 Zn2 -174.64(15) . . . 5_565 ? O3 C10 O2 Zn1 -173.41(19) . . . . ? C9 C10 O2 Zn1 10.2(3) . . . . ? O2 Zn1 O2 C10 134.78(17) 2 . . . ? N1 Zn1 O2 C10 -90.34(18) 2 . . . ? N1 Zn1 O2 C10 -0.89(17) . . . . ? O1 Zn1 O2 C10 93.47(17) . . . . ? O1 Zn1 O2 C10 176.69(18) 5_565 . . . ? O2 Zn1 O2 Zn2 -41.37(7) 2 . . 5_565 ? N1 Zn1 O2 Zn2 93.51(9) 2 . . 5_565 ? N1 Zn1 O2 Zn2 -177.04(9) . . . 5_565 ? O1 Zn1 O2 Zn2 -82.68(9) . . . 5_565 ? O1 Zn1 O2 Zn2 0.54(7) 5_565 . . 5_565 ? O4 C11 O4 Zn2 178.39(15) 2_556 . . . ? C11 C11 O4 Zn2 -1.61(15) 5_566 . . . ? O2 Zn2 O4 C11 -52.5(4) 2 . . . ? O2 Zn2 O4 C11 -168.43(13) 5_565 . . . ? O4 Zn2 O4 C11 1.88(18) 6_565 . . . ? O1W Zn2 O4 C11 98.92(14) . . . . ? O1 Zn2 O4 C11 -93.70(13) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.496 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.070 data_Compound-7 _database_code_depnum_ccdc_archive 'CCDC 922860' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H24 Co2 N2 O9), 2(O0.50)' _chemical_formula_sum 'C36 H48 Co4 N4 O19' _chemical_formula_weight 1076.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.507(5) _cell_length_b 10.580(5) _cell_length_c 10.725(5) _cell_angle_alpha 101.281(5) _cell_angle_beta 108.121(5) _cell_angle_gamma 90.551(5) _cell_volume 1108.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5026 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.276 _exptl_crystal_size_mid 0.265 _exptl_crystal_size_min 0.253 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.676 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10916 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5026 _reflns_number_gt 4012 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.3462P] 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 5026 _refine_ls_number_parameters 301 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 0.93329(4) 0.38170(4) 0.02834(4) 0.02876(15) Uani 1 1 d . . . Co2 Co 0.81011(4) 0.66836(4) 0.09378(4) 0.02976(15) Uani 1 1 d . . . C1 C 1.4387(5) 0.6192(7) 0.6201(5) 0.0809(17) Uani 1 1 d . . . H1A H 1.4288 0.5501 0.6634 0.121 Uiso 1 1 calc R . . H1B H 1.4424 0.7006 0.6798 0.121 Uiso 1 1 calc R . . H1C H 1.5201 0.6127 0.5972 0.121 Uiso 1 1 calc R . . C2 C 1.3207(4) 0.6099(5) 0.4946(4) 0.0535(11) Uani 1 1 d . . . C3 C 1.2167(4) 0.5168(5) 0.4585(3) 0.0482(10) Uani 1 1 d . . . H3 H 1.2197 0.4586 0.5138 0.058 Uiso 1 1 calc R . . C4 C 1.1068(3) 0.5056(3) 0.3423(3) 0.0354(7) Uani 1 1 d . . . C5 C 1.1051(3) 0.5899(3) 0.2556(3) 0.0308(7) Uani 1 1 d . . . C6 C 0.9852(4) 0.4206(4) 0.3220(4) 0.0399(8) Uani 1 1 d . . . H6A H 0.9089 0.4731 0.3102 0.048 Uiso 1 1 calc R . . H6B H 0.9968 0.3888 0.4035 0.048 Uiso 1 1 calc R . . C7 C 0.8212(4) 0.2448(4) 0.2013(4) 0.0489(9) Uani 1 1 d . . . H7A H 0.7533 0.3063 0.1843 0.059 Uiso 1 1 calc R . . H7B H 0.8305 0.2265 0.2887 0.059 Uiso 1 1 calc R . . C8 C 0.7706(5) 0.1194(4) 0.0956(5) 0.0562(11) Uani 1 1 d . . . H8A H 0.8116 0.0485 0.1347 0.067 Uiso 1 1 calc R . . H8B H 0.6746 0.1063 0.0777 0.067 Uiso 1 1 calc R . . C9 C 0.7956(5) 0.1095(4) -0.0383(4) 0.0511(10) Uani 1 1 d . . . H9A H 0.8857 0.0830 -0.0286 0.061 Uiso 1 1 calc R . . H9B H 0.7334 0.0420 -0.1040 0.061 Uiso 1 1 calc R . . C10 C 0.8085(4) 0.1987(3) -0.2218(4) 0.0406(8) Uani 1 1 d . . . H10A H 0.7471 0.1264 -0.2793 0.049 Uiso 1 1 calc R . . H10B H 0.8989 0.1710 -0.2054 0.049 Uiso 1 1 calc R . . C11 C 1.2045(4) 0.6925(4) 0.2956(3) 0.0381(8) Uani 1 1 d . . . C12 C 1.3113(4) 0.6996(4) 0.4146(4) 0.0481(9) Uani 1 1 d . . . H12 H 1.3780 0.7668 0.4406 0.058 Uiso 1 1 calc R . . C13 C 1.0608(4) 0.2203(4) 0.2294(4) 0.0438(9) Uani 1 1 d . . . H13A H 1.0227 0.1316 0.2037 0.053 Uiso 1 1 calc R . . H13B H 1.1115 0.2372 0.3243 0.053 Uiso 1 1 calc R . . C14 C 1.1551(4) 0.2363(3) 0.1511(3) 0.0347(7) Uani 1 1 d . . . C15 C 0.6455(4) 0.2749(3) -0.1127(4) 0.0404(8) Uani 1 1 d . . . H15A H 0.6056 0.2433 -0.0533 0.048 Uiso 1 1 calc R . . H15B H 0.5900 0.2395 -0.2043 0.048 Uiso 1 1 calc R . . C16 C 0.6480(3) 0.4207(3) -0.0866(3) 0.0335(7) Uani 1 1 d . . . C17 C 0.9934(5) 0.9743(4) 0.4374(4) 0.0520(11) Uani 1 1 d . . . H17 H 1.0449 1.0119 0.3958 0.062 Uiso 1 1 calc R . . C19 C 0.9006(4) 0.8591(4) 0.3579(4) 0.0466(9) Uani 1 1 d . . . N1 N 0.9510(3) 0.3072(3) 0.2072(3) 0.0378(7) Uani 1 1 d . . . N2 N 0.7812(3) 0.2301(3) -0.0916(3) 0.0351(6) Uani 1 1 d . . . O1 O 1.0064(2) 0.5728(2) 0.1349(2) 0.0289(5) Uani 1 1 d . . . O2 O 1.1067(2) 0.2873(2) 0.0482(2) 0.0347(5) Uani 1 1 d . . . O3 O 1.2663(3) 0.1957(3) 0.1834(3) 0.0482(7) Uani 1 1 d . . . O4 O 0.7615(2) 0.4810(2) -0.0213(2) 0.0340(5) Uani 1 1 d . . . O5 O 0.5422(2) 0.4728(3) -0.1242(3) 0.0449(6) Uani 1 1 d . . . O8 O 0.8920(3) 0.8297(2) 0.2347(2) 0.0374(5) Uani 1 1 d . . . O9 O 0.8409(5) 0.7997(4) 0.4137(3) 0.0926(15) Uani 1 1 d . . . O1W O 0.6369(10) -0.1118(10) -0.4520(12) 0.117(3) Uani 0.50 1 d P . . O2W O 0.7243(3) 0.6048(2) 0.2235(3) 0.0380(5) Uani 1 1 d D . . H2WA H 0.641(2) 0.585(4) 0.193(4) 0.057 Uiso 1 1 d D . . H2WB H 0.752(4) 0.665(3) 0.290(3) 0.057 Uiso 1 1 d D . . O3W O 0.6207(3) 0.7288(3) -0.0117(3) 0.0443(6) Uani 1 1 d D . . H3WA H 0.579(4) 0.656(3) -0.051(4) 0.066 Uiso 1 1 d D . . H3WB H 0.662(5) 0.762(4) -0.054(4) 0.066 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0311(3) 0.0280(2) 0.0224(2) 0.00125(17) 0.00425(18) 0.00339(17) Co2 0.0302(3) 0.0297(2) 0.0223(2) -0.00264(17) 0.00334(18) 0.00236(17) C1 0.049(3) 0.144(5) 0.035(2) 0.022(3) -0.009(2) -0.001(3) C2 0.038(2) 0.091(3) 0.0227(18) 0.0065(19) -0.0005(15) 0.006(2) C3 0.045(2) 0.077(3) 0.0210(17) 0.0128(17) 0.0060(15) 0.017(2) C4 0.0350(18) 0.0450(18) 0.0233(16) 0.0037(13) 0.0068(13) 0.0101(14) C5 0.0279(16) 0.0382(16) 0.0191(14) -0.0025(12) 0.0024(12) 0.0056(12) C6 0.045(2) 0.0471(19) 0.0290(17) 0.0089(15) 0.0125(15) 0.0095(16) C7 0.053(2) 0.052(2) 0.049(2) 0.0150(19) 0.0239(19) -0.0010(18) C8 0.065(3) 0.046(2) 0.062(3) 0.021(2) 0.020(2) -0.005(2) C9 0.066(3) 0.0308(17) 0.051(2) 0.0058(17) 0.012(2) 0.0013(17) C10 0.039(2) 0.0368(17) 0.0350(19) -0.0096(15) 0.0077(15) -0.0033(14) C11 0.0357(18) 0.0455(19) 0.0243(16) -0.0038(14) 0.0038(14) 0.0018(14) C12 0.0336(19) 0.068(3) 0.0287(18) -0.0056(17) -0.0001(15) -0.0057(17) C13 0.058(2) 0.0410(19) 0.038(2) 0.0157(16) 0.0180(18) 0.0140(17) C14 0.0428(19) 0.0267(15) 0.0292(17) 0.0019(13) 0.0061(14) 0.0047(13) C15 0.0365(19) 0.0376(17) 0.041(2) -0.0007(15) 0.0095(16) -0.0059(14) C16 0.0316(17) 0.0380(17) 0.0238(16) -0.0020(13) 0.0040(13) -0.0025(13) C17 0.074(3) 0.044(2) 0.0329(19) -0.0053(16) 0.0188(19) -0.0241(19) C19 0.061(3) 0.045(2) 0.0274(18) -0.0069(15) 0.0134(17) -0.0134(18) N1 0.0451(17) 0.0377(15) 0.0303(15) 0.0064(12) 0.0118(13) 0.0060(13) N2 0.0391(16) 0.0283(13) 0.0333(15) 0.0004(11) 0.0089(13) -0.0019(11) O1 0.0307(12) 0.0303(11) 0.0187(10) -0.0006(8) 0.0013(9) 0.0029(9) O2 0.0357(13) 0.0402(12) 0.0262(12) 0.0072(10) 0.0070(10) 0.0110(10) O3 0.0466(16) 0.0471(15) 0.0494(16) 0.0194(13) 0.0071(13) 0.0140(12) O4 0.0287(12) 0.0309(11) 0.0314(12) -0.0046(9) 0.0005(10) 0.0018(9) O5 0.0299(13) 0.0469(14) 0.0473(16) 0.0042(12) 0.0010(11) 0.0015(11) O8 0.0462(14) 0.0327(12) 0.0259(12) -0.0062(9) 0.0088(10) -0.0033(10) O9 0.143(4) 0.087(2) 0.0372(17) -0.0227(17) 0.038(2) -0.074(3) O1W 0.090(7) 0.120(8) 0.140(9) 0.032(7) 0.032(6) 0.002(6) O2W 0.0327(13) 0.0406(13) 0.0335(13) -0.0010(10) 0.0061(10) -0.0044(10) O3W 0.0376(15) 0.0505(15) 0.0403(15) 0.0062(12) 0.0079(12) 0.0104(12) _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 O2 2.060(2) . ? Co1 O4 2.074(2) . ? Co1 O1 2.122(2) . ? Co1 N2 2.155(3) . ? Co1 N1 2.170(3) . ? Co1 O1 2.171(2) 2_765 ? Co2 O8 2.023(2) . ? Co2 O2W 2.082(3) . ? Co2 O4 2.085(2) . ? Co2 O2 2.098(3) 2_765 ? Co2 O3W 2.135(3) . ? Co2 O1 2.263(2) . ? C1 C2 1.506(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.371(6) . ? C2 C12 1.384(6) . ? C3 C4 1.395(5) . ? C3 H3 0.9300 . ? C4 C5 1.405(5) . ? C4 C6 1.489(5) . ? C5 O1 1.361(4) . ? C5 C11 1.404(5) . ? C6 N1 1.491(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N1 1.487(5) . ? C7 C8 1.534(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.522(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.488(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.488(5) . ? C10 C11 1.504(6) 2_765 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.401(5) . ? C11 C10 1.504(6) 2_765 ? C12 H12 0.9300 . ? C13 N1 1.472(5) . ? C13 C14 1.511(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.219(4) . ? C14 O2 1.287(4) . ? C15 N2 1.470(5) . ? C15 C16 1.511(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O5 1.234(4) . ? C16 O4 1.269(4) . ? C17 C17 1.310(7) 2_776 ? C17 C19 1.489(5) . ? C17 H17 0.9300 . ? C19 O9 1.232(5) . ? C19 O8 1.271(4) . ? O1 Co1 2.171(2) 2_765 ? O2 Co2 2.098(3) 2_765 ? O2W H2WA 0.842(18) . ? O2W H2WB 0.831(18) . ? O3W H3WA 0.848(18) . ? O3W H3WB 0.834(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O4 170.62(10) . . ? O2 Co1 O1 102.73(10) . . ? O4 Co1 O1 78.21(9) . . ? O2 Co1 N2 101.98(11) . . ? O4 Co1 N2 77.28(10) . . ? O1 Co1 N2 155.27(10) . . ? O2 Co1 N1 78.90(10) . . ? O4 Co1 N1 110.41(11) . . ? O1 Co1 N1 94.53(10) . . ? N2 Co1 N1 90.96(12) . . ? O2 Co1 O1 78.57(9) . 2_765 ? O4 Co1 O1 92.20(10) . 2_765 ? O1 Co1 O1 87.25(9) . 2_765 ? N2 Co1 O1 96.88(10) . 2_765 ? N1 Co1 O1 157.23(10) . 2_765 ? O8 Co2 O2W 90.21(10) . . ? O8 Co2 O4 166.21(10) . . ? O2W Co2 O4 85.93(10) . . ? O8 Co2 O2 95.41(10) . 2_765 ? O2W Co2 O2 174.10(9) . 2_765 ? O4 Co2 O2 88.20(10) . 2_765 ? O8 Co2 O3W 101.71(11) . . ? O2W Co2 O3W 89.94(11) . . ? O4 Co2 O3W 91.53(10) . . ? O2 Co2 O3W 90.67(10) 2_765 . ? O8 Co2 O1 93.07(10) . . ? O2W Co2 O1 102.23(10) . . ? O4 Co2 O1 74.89(9) . . ? O2 Co2 O1 75.73(9) 2_765 . ? O3W Co2 O1 160.85(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C12 117.7(3) . . ? C3 C2 C1 121.7(4) . . ? C12 C2 C1 120.5(4) . . ? C2 C3 C4 122.8(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 118.6(4) . . ? C3 C4 C6 120.2(3) . . ? C5 C4 C6 120.5(3) . . ? O1 C5 C11 120.6(3) . . ? O1 C5 C4 120.0(3) . . ? C11 C5 C4 119.4(3) . . ? C4 C6 N1 117.0(3) . . ? C4 C6 H6A 108.1 . . ? N1 C6 H6A 108.1 . . ? C4 C6 H6B 108.1 . . ? N1 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? N1 C7 C8 115.9(3) . . ? N1 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 117.9(3) . . ? C9 C8 H8A 107.8 . . ? C7 C8 H8A 107.8 . . ? C9 C8 H8B 107.8 . . ? C7 C8 H8B 107.8 . . ? H8A C8 H8B 107.2 . . ? N2 C9 C8 115.3(3) . . ? N2 C9 H9A 108.4 . . ? C8 C9 H9A 108.4 . . ? N2 C9 H9B 108.4 . . ? C8 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C11 115.3(3) . 2_765 ? N2 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 2_765 . ? N2 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 2_765 . ? H10A C10 H10B 107.5 . . ? C12 C11 C5 118.8(4) . . ? C12 C11 C10 119.4(3) . 2_765 ? C5 C11 C10 121.5(3) . 2_765 ? C2 C12 C11 122.1(4) . . ? C2 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N1 C13 C14 112.8(3) . . ? N1 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N1 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O3 C14 O2 124.5(3) . . ? O3 C14 C13 119.7(3) . . ? O2 C14 C13 115.6(3) . . ? N2 C15 C16 111.7(3) . . ? N2 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N2 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O5 C16 O4 124.6(3) . . ? O5 C16 C15 119.5(3) . . ? O4 C16 C15 115.9(3) . . ? C17 C17 C19 123.6(5) 2_776 . ? C17 C17 H17 118.2 2_776 . ? C19 C17 H17 118.2 . . ? O9 C19 O8 125.5(4) . . ? O9 C19 C17 119.6(3) . . ? O8 C19 C17 114.9(3) . . ? C13 N1 C7 112.7(3) . . ? C13 N1 C6 108.8(3) . . ? C7 N1 C6 106.7(3) . . ? C13 N1 Co1 109.9(2) . . ? C7 N1 Co1 111.7(2) . . ? C6 N1 Co1 106.9(2) . . ? C15 N2 C10 109.8(3) . . ? C15 N2 C9 111.8(3) . . ? C10 N2 C9 106.4(3) . . ? C15 N2 Co1 111.5(2) . . ? C10 N2 Co1 103.8(2) . . ? C9 N2 Co1 113.1(2) . . ? C5 O1 Co1 118.75(19) . . ? C5 O1 Co1 115.7(2) . 2_765 ? Co1 O1 Co1 92.75(9) . 2_765 ? C5 O1 Co2 125.77(19) . . ? Co1 O1 Co2 99.28(9) . . ? Co1 O1 Co2 98.11(9) 2_765 . ? C14 O2 Co1 119.2(2) . . ? C14 O2 Co2 132.1(2) . 2_765 ? Co1 O2 Co2 107.32(10) . 2_765 ? C16 O4 Co1 120.7(2) . . ? C16 O4 Co2 130.5(2) . . ? Co1 O4 Co2 106.99(10) . . ? C19 O8 Co2 130.5(2) . . ? Co2 O2W H2WA 116(3) . . ? Co2 O2W H2WB 100(3) . . ? H2WA O2W H2WB 118(3) . . ? Co2 O3W H3WA 100(4) . . ? Co2 O3W H3WB 86(4) . . ? H3WA O3W H3WB 116(3) . . ? 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 C12 C2 C3 C4 3.2(6) . . . . ? C1 C2 C3 C4 -179.6(5) . . . . ? C2 C3 C4 C5 2.7(6) . . . . ? C2 C3 C4 C6 -167.9(4) . . . . ? C3 C4 C5 O1 173.1(3) . . . . ? C6 C4 C5 O1 -16.3(5) . . . . ? C3 C4 C5 C11 -7.8(5) . . . . ? C6 C4 C5 C11 162.8(3) . . . . ? C3 C4 C6 N1 -115.9(4) . . . . ? C5 C4 C6 N1 73.6(4) . . . . ? N1 C7 C8 C9 -36.4(6) . . . . ? C7 C8 C9 N2 -38.4(6) . . . . ? O1 C5 C11 C12 -174.0(3) . . . . ? C4 C5 C11 C12 6.9(5) . . . . ? O1 C5 C11 C10 12.4(5) . . . 2_765 ? C4 C5 C11 C10 -166.7(3) . . . 2_765 ? C3 C2 C12 C11 -4.2(7) . . . . ? C1 C2 C12 C11 178.6(4) . . . . ? C5 C11 C12 C2 -0.9(6) . . . . ? C10 C11 C12 C2 172.8(4) 2_765 . . . ? N1 C13 C14 O3 162.0(3) . . . . ? N1 C13 C14 O2 -21.5(4) . . . . ? N2 C15 C16 O5 166.1(3) . . . . ? N2 C15 C16 O4 -16.5(5) . . . . ? C17 C17 C19 O9 -7.1(9) 2_776 . . . ? C17 C17 C19 O8 173.9(6) 2_776 . . . ? C14 C13 N1 C7 142.1(3) . . . . ? C14 C13 N1 C6 -99.8(4) . . . . ? C14 C13 N1 Co1 16.9(4) . . . . ? C8 C7 N1 C13 -56.7(4) . . . . ? C8 C7 N1 C6 -176.0(3) . . . . ? C8 C7 N1 Co1 67.6(4) . . . . ? C4 C6 N1 C13 62.8(4) . . . . ? C4 C6 N1 C7 -175.4(3) . . . . ? C4 C6 N1 Co1 -55.8(3) . . . . ? O2 Co1 N1 C13 -7.6(2) . . . . ? O4 Co1 N1 C13 171.2(2) . . . . ? O1 Co1 N1 C13 -109.7(2) . . . . ? N2 Co1 N1 C13 94.4(3) . . . . ? O1 Co1 N1 C13 -16.0(4) 2_765 . . . ? O2 Co1 N1 C7 -133.4(2) . . . . ? O4 Co1 N1 C7 45.4(3) . . . . ? O1 Co1 N1 C7 124.5(2) . . . . ? N2 Co1 N1 C7 -31.3(2) . . . . ? O1 Co1 N1 C7 -141.8(3) 2_765 . . . ? O2 Co1 N1 C6 110.3(2) . . . . ? O4 Co1 N1 C6 -70.9(2) . . . . ? O1 Co1 N1 C6 8.2(2) . . . . ? N2 Co1 N1 C6 -147.6(2) . . . . ? O1 Co1 N1 C6 101.9(3) 2_765 . . . ? C16 C15 N2 C10 -95.6(3) . . . . ? C16 C15 N2 C9 146.5(3) . . . . ? C16 C15 N2 Co1 18.9(4) . . . . ? C11 C10 N2 C15 57.2(4) 2_765 . . . ? C11 C10 N2 C9 178.4(3) 2_765 . . . ? C11 C10 N2 Co1 -62.1(3) 2_765 . . . ? C8 C9 N2 C15 -59.8(4) . . . . ? C8 C9 N2 C10 -179.6(3) . . . . ? C8 C9 N2 Co1 67.1(4) . . . . ? O2 Co1 N2 C15 176.9(2) . . . . ? O4 Co1 N2 C15 -12.7(2) . . . . ? O1 Co1 N2 C15 -4.9(4) . . . . ? N1 Co1 N2 C15 98.1(2) . . . . ? O1 Co1 N2 C15 -103.4(2) 2_765 . . . ? O2 Co1 N2 C10 -65.0(2) . . . . ? O4 Co1 N2 C10 105.5(2) . . . . ? O1 Co1 N2 C10 113.2(3) . . . . ? N1 Co1 N2 C10 -143.8(2) . . . . ? O1 Co1 N2 C10 14.8(2) 2_765 . . . ? O2 Co1 N2 C9 49.9(3) . . . . ? O4 Co1 N2 C9 -139.7(3) . . . . ? O1 Co1 N2 C9 -132.0(3) . . . . ? N1 Co1 N2 C9 -29.0(3) . . . . ? O1 Co1 N2 C9 129.6(3) 2_765 . . . ? C11 C5 O1 Co1 145.1(3) . . . . ? C4 C5 O1 Co1 -35.9(4) . . . . ? C11 C5 O1 Co1 36.1(4) . . . 2_765 ? C4 C5 O1 Co1 -144.8(3) . . . 2_765 ? C11 C5 O1 Co2 -86.5(4) . . . . ? C4 C5 O1 Co2 92.5(3) . . . . ? O2 Co1 O1 C5 -43.8(2) . . . . ? O4 Co1 O1 C5 145.8(2) . . . . ? N2 Co1 O1 C5 138.1(3) . . . . ? N1 Co1 O1 C5 35.9(2) . . . . ? O1 Co1 O1 C5 -121.4(3) 2_765 . . . ? O2 Co1 O1 Co1 77.63(10) . . . 2_765 ? O4 Co1 O1 Co1 -92.82(10) . . . 2_765 ? N2 Co1 O1 Co1 -100.5(2) . . . 2_765 ? N1 Co1 O1 Co1 157.25(10) . . . 2_765 ? O1 Co1 O1 Co1 0.0 2_765 . . 2_765 ? O2 Co1 O1 Co2 176.31(8) . . . . ? O4 Co1 O1 Co2 5.86(9) . . . . ? N2 Co1 O1 Co2 -1.8(3) . . . . ? N1 Co1 O1 Co2 -104.07(11) . . . . ? O1 Co1 O1 Co2 98.68(10) 2_765 . . . ? O8 Co2 O1 C5 31.4(3) . . . . ? O2W Co2 O1 C5 -59.5(3) . . . . ? O4 Co2 O1 C5 -141.8(3) . . . . ? O2 Co2 O1 C5 126.2(3) 2_765 . . . ? O3W Co2 O1 C5 172.1(3) . . . . ? O8 Co2 O1 Co1 167.28(10) . . . . ? O2W Co2 O1 Co1 76.40(11) . . . . ? O4 Co2 O1 Co1 -5.91(9) . . . . ? O2 Co2 O1 Co1 -97.92(11) 2_765 . . . ? O3W Co2 O1 Co1 -52.0(3) . . . . ? O8 Co2 O1 Co1 -98.57(10) . . . 2_765 ? O2W Co2 O1 Co1 170.54(8) . . . 2_765 ? O4 Co2 O1 Co1 88.24(10) . . . 2_765 ? O2 Co2 O1 Co1 -3.77(8) 2_765 . . 2_765 ? O3W Co2 O1 Co1 42.1(3) . . . 2_765 ? O3 C14 O2 Co1 -168.4(3) . . . . ? C13 C14 O2 Co1 15.4(4) . . . . ? O3 C14 O2 Co2 -3.8(5) . . . 2_765 ? C13 C14 O2 Co2 180.0(2) . . . 2_765 ? O4 Co1 O2 C14 -177.5(5) . . . . ? O1 Co1 O2 C14 87.8(2) . . . . ? N2 Co1 O2 C14 -93.0(2) . . . . ? N1 Co1 O2 C14 -4.4(2) . . . . ? O1 Co1 O2 C14 172.3(3) 2_765 . . . ? O4 Co1 O2 Co2 14.4(6) . . . 2_765 ? O1 Co1 O2 Co2 -80.25(12) . . . 2_765 ? N2 Co1 O2 Co2 98.95(12) . . . 2_765 ? N1 Co1 O2 Co2 -172.44(13) . . . 2_765 ? O1 Co1 O2 Co2 4.25(9) 2_765 . . 2_765 ? O5 C16 O4 Co1 -177.1(3) . . . . ? C15 C16 O4 Co1 5.6(4) . . . . ? O5 C16 O4 Co2 20.5(5) . . . . ? C15 C16 O4 Co2 -156.8(2) . . . . ? O2 Co1 O4 C16 90.6(6) . . . . ? O1 Co1 O4 C16 -172.6(3) . . . . ? N2 Co1 O4 C16 4.1(3) . . . . ? N1 Co1 O4 C16 -82.2(3) . . . . ? O1 Co1 O4 C16 100.6(3) 2_765 . . . ? O2 Co1 O4 Co2 -103.3(5) . . . . ? O1 Co1 O4 Co2 -6.56(10) . . . . ? N2 Co1 O4 Co2 170.14(14) . . . . ? N1 Co1 O4 Co2 83.91(14) . . . . ? O1 Co1 O4 Co2 -93.30(11) 2_765 . . . ? O8 Co2 O4 C16 140.7(4) . . . . ? O2W Co2 O4 C16 66.6(3) . . . . ? O2 Co2 O4 C16 -113.8(3) 2_765 . . . ? O3W Co2 O4 C16 -23.2(3) . . . . ? O1 Co2 O4 C16 170.5(3) . . . . ? O8 Co2 O4 Co1 -23.5(5) . . . . ? O2W Co2 O4 Co1 -97.60(12) . . . . ? O2 Co2 O4 Co1 81.94(12) 2_765 . . . ? O3W Co2 O4 Co1 172.56(12) . . . . ? O1 Co2 O4 Co1 6.24(9) . . . . ? O9 C19 O8 Co2 -11.5(7) . . . . ? C17 C19 O8 Co2 167.4(3) . . . . ? O2W Co2 O8 C19 10.2(4) . . . . ? O4 Co2 O8 C19 -63.3(6) . . . . ? O2 Co2 O8 C19 -168.0(4) 2_765 . . . ? O3W Co2 O8 C19 100.2(4) . . . . ? O1 Co2 O8 C19 -92.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2WA O5 0.842(18) 1.881(18) 2.722(4) 176(4) 2_665 O3W H3WB O3 0.834(18) 1.90(2) 2.712(4) 166(4) 2_765 O3W H3WB O2 0.834(18) 2.48(5) 3.011(4) 123(4) 2_765 O2W H2WB O9 0.831(18) 1.766(19) 2.582(4) 166(4) . O3W H3WA O5 0.848(18) 1.93(2) 2.744(4) 161(5) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.774 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.119 data_Compound-8 _database_code_depnum_ccdc_archive 'CCDC 922861' #TrackingRef 'crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 Co2 N2 O8, 0.5(H2 O), 0.2(O)' _chemical_formula_sum 'C19 H26 Co2 N2 O8.70' _chemical_formula_weight 539.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_hall '-C 2yc ' 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 23.5790(11) _cell_length_b 9.9671(2) _cell_length_c 20.2015(18) _cell_angle_alpha 90.00 _cell_angle_beta 114.428(4) _cell_angle_gamma 90.00 _cell_volume 4322.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5346 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 35.1 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.243 _exptl_crystal_size_min 0.232 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2221 _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.692 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13432 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 35.14 _reflns_number_total 5346 _reflns_number_gt 3383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+0.0000P] 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 5346 _refine_ls_number_parameters 297 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 1.532 _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 Co2 Co 0.89978(5) 0.19945(10) 0.39217(5) 0.0271(3) Uani 1 1 d D . . Co1 Co 0.94846(4) -0.11622(9) 0.44481(4) 0.0229(3) Uani 1 1 d D . . C1 C 1.1950(5) -0.0191(12) 0.3863(5) 0.069(3) Uani 1 1 d . . . H1A H 1.1871 -0.0933 0.3533 0.103 Uiso 1 1 calc R . . H1B H 1.2284 -0.0416 0.4319 0.103 Uiso 1 1 calc R . . H1C H 1.2063 0.0584 0.3662 0.103 Uiso 1 1 calc R . . C2 C 1.1394(4) 0.0096(9) 0.3974(4) 0.0399(19) Uani 1 1 d . . . C3 C 1.0751(4) -0.0619(8) 0.3614(4) 0.0386(19) Uani 1 1 d . . . H3 H 1.0723 -0.1283 0.3278 0.046 Uiso 1 1 calc R . . C4 C 1.0235(3) -0.0413(7) 0.3720(3) 0.0275(16) Uani 1 1 d D . . C5 C 1.0421(3) 0.0537(7) 0.4252(3) 0.0257(15) Uani 1 1 d . . . C6 C 1.1026(3) 0.1373(7) 0.4568(3) 0.0284(16) Uani 1 1 d . . . C7 C 1.1517(3) 0.1130(6) 0.4433(3) 0.0385(19) Uani 1 1 d . . . H7 H 1.1891 0.1603 0.4627 0.046 Uiso 1 1 calc R . . C9 C 0.8582(3) -0.2577(6) 0.2984(3) 0.0340(17) Uani 1 1 d R . . H9A H 0.8316 -0.1807 0.2938 0.041 Uiso 1 1 calc R . . H9B H 0.8568 -0.2758 0.2506 0.041 Uiso 1 1 calc R . . C10 C 0.8321(4) -0.3717(7) 0.3200(4) 0.0325(17) Uani 1 1 d . . . H10A H 0.7871 -0.3635 0.3011 0.039 Uiso 1 1 calc R . . H10B H 0.8421 -0.4541 0.3016 0.039 Uiso 1 1 calc R . . C11 C 0.8589(4) -0.3724(7) 0.3975(4) 0.0317(17) Uani 1 1 d . . . H11A H 0.9003 -0.4114 0.4152 0.038 Uiso 1 1 calc R . . H11B H 0.8338 -0.4283 0.4142 0.038 Uiso 1 1 calc R . . C12 C 0.8877(4) -0.2624(7) 0.5028(3) 0.0296(16) Uani 1 1 d . . . H12A H 0.9271 -0.3095 0.5179 0.036 Uiso 1 1 calc R . . H12B H 0.8593 -0.3190 0.5138 0.036 Uiso 1 1 calc R . . C13 C 0.7919(4) -0.1679(8) 0.3832(4) 0.0327(17) Uani 1 1 d . . . H13A H 0.7719 -0.2041 0.3343 0.039 Uiso 1 1 calc R . . H13B H 0.7658 -0.1875 0.4086 0.039 Uiso 1 1 calc R . . C14 C 0.8002(3) -0.0193(8) 0.3802(3) 0.0297(16) Uani 1 1 d . . . C15 C 0.9898(4) -0.3215(7) 0.3833(3) 0.0317(17) Uani 1 1 d D . . H15A H 1.0051 -0.3264 0.3456 0.038 Uiso 1 1 calc R . . H15B H 0.9708 -0.4077 0.3835 0.038 Uiso 1 1 calc R . . C16 C 1.0529(4) -0.3106(7) 0.4627(4) 0.0307(17) Uani 1 1 d D . . C17 C 0.9934(4) 0.3200(11) 0.2776(4) 0.054(3) Uani 1 1 d D . . H17A H 1.0112 0.3983 0.3075 0.065 Uiso 1 1 calc R . . H17B H 1.0102 0.2403 0.3068 0.065 Uiso 1 1 calc R . . C18 C 0.9164(4) 0.3222(11) 0.2466(4) 0.057(3) Uani 1 1 d D . . H18A H 0.9004 0.4121 0.2316 0.068 Uiso 1 1 calc R . . H18B H 0.8977 0.2622 0.2053 0.068 Uiso 1 1 calc R . . C19 C 0.9045(4) 0.2830(8) 0.2996(4) 0.0341(18) Uani 1 1 d . . . N1 N 0.9343(3) -0.2142(6) 0.3560(3) 0.0273(13) Uani 1 1 d D . . N2 N 0.8633(3) -0.2389(6) 0.4277(3) 0.0265(13) Uani 1 1 d . . . O1 O 0.9980(2) 0.0642(5) 0.4443(2) 0.0258(11) Uani 1 1 d . . . O2 O 0.8622(2) 0.0183(5) 0.3973(2) 0.0293(11) Uani 1 1 d . . . O3 O 0.7494(3) 0.0567(6) 0.3597(3) 0.0437(14) Uani 1 1 d . . . O4 O 1.0401(2) -0.2391(5) 0.4999(2) 0.0323(12) Uani 1 1 d . . . O5 O 1.1110(3) -0.3687(6) 0.4903(3) 0.0470(15) Uani 1 1 d . . . O6 O 0.9398(3) 0.3412(6) 0.3600(3) 0.0404(14) Uani 1 1 d . . . O7 O 0.8622(3) 0.1883(6) 0.2849(3) 0.0446(15) Uani 1 1 d . . . C8 C 0.9515(4) -0.1002(7) 0.3215(3) 0.0327(17) Uani 1 1 d D . . H8A H 0.9216 -0.0284 0.3132 0.039 Uiso 1 1 calc R . . H8B H 0.9493 -0.1284 0.2745 0.039 Uiso 1 1 calc R . . O1W O 0.8067(3) 0.3009(5) 0.3660(3) 0.0369(13) Uani 1 1 d D . . H1WB H 0.8205(16) 0.347(6) 0.405(2) 0.055 Uiso 1 1 d D . . H1WA H 0.780(3) 0.241(7) 0.362(4) 0.055 Uiso 1 1 d D . . O2W O 1.1400(9) -0.430(3) 0.3855(11) 0.132(10) Uani 0.50 1 d PD . . H2WA H 1.148(11) -0.351(9) 0.376(12) 0.198 Uiso 1 1 d D . . O3W O 1.0000 -0.347(4) 0.2500 0.106(11) Uiso 0.40 2 d SP . . 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 Co2 0.0407(6) 0.0268(5) 0.0250(4) 0.0028(4) 0.0248(4) 0.0011(4) Co1 0.0342(6) 0.0225(5) 0.0224(4) -0.0005(3) 0.0221(4) -0.0004(4) C1 0.088(7) 0.081(7) 0.080(6) -0.027(6) 0.077(6) -0.020(6) C2 0.048(5) 0.051(5) 0.040(4) -0.006(4) 0.038(4) -0.003(4) C3 0.058(5) 0.041(4) 0.034(3) -0.007(3) 0.036(4) -0.002(4) C4 0.037(4) 0.031(4) 0.027(3) 0.004(3) 0.025(3) 0.000(3) C5 0.036(4) 0.030(4) 0.023(3) 0.003(3) 0.025(3) 0.003(3) C6 0.043(4) 0.028(4) 0.026(3) 0.002(3) 0.026(3) -0.001(3) C7 0.045(5) 0.050(5) 0.036(4) -0.005(3) 0.033(4) -0.009(4) C9 0.043(5) 0.038(4) 0.029(3) -0.006(3) 0.023(4) -0.004(4) C10 0.044(5) 0.031(4) 0.033(3) -0.012(3) 0.026(3) -0.009(4) C11 0.048(5) 0.022(4) 0.039(4) -0.006(3) 0.032(4) -0.004(3) C12 0.044(5) 0.029(4) 0.029(3) 0.002(3) 0.029(3) -0.004(3) C13 0.045(5) 0.030(4) 0.036(4) -0.003(3) 0.030(4) -0.001(4) C14 0.040(4) 0.033(4) 0.025(3) 0.000(3) 0.021(3) 0.002(4) C15 0.050(5) 0.026(4) 0.033(3) -0.002(3) 0.031(4) 0.001(3) C16 0.050(5) 0.022(4) 0.033(3) -0.001(3) 0.031(4) 0.002(3) C17 0.072(6) 0.074(7) 0.038(4) 0.000(4) 0.045(5) -0.004(5) C18 0.068(6) 0.086(7) 0.036(4) 0.014(4) 0.042(4) 0.008(6) C19 0.040(5) 0.042(5) 0.033(4) 0.013(3) 0.028(4) 0.013(4) N1 0.043(4) 0.026(3) 0.025(3) -0.002(2) 0.026(3) -0.002(3) N2 0.042(4) 0.024(3) 0.026(3) -0.002(2) 0.026(3) -0.004(3) O1 0.041(3) 0.027(2) 0.025(2) -0.0008(18) 0.029(2) -0.002(2) O2 0.038(3) 0.026(3) 0.038(2) 0.004(2) 0.030(2) 0.001(2) O3 0.047(3) 0.039(3) 0.065(3) 0.010(3) 0.043(3) 0.007(3) O4 0.051(3) 0.036(3) 0.024(2) 0.001(2) 0.029(2) 0.010(3) O5 0.062(4) 0.054(4) 0.040(3) 0.000(3) 0.036(3) 0.020(3) O6 0.065(4) 0.041(3) 0.035(3) 0.000(2) 0.040(3) -0.007(3) O7 0.074(4) 0.043(3) 0.034(3) 0.001(2) 0.040(3) -0.004(3) C8 0.050(5) 0.032(4) 0.025(3) 0.001(3) 0.025(3) 0.005(4) O1W 0.052(4) 0.035(3) 0.037(3) -0.001(2) 0.031(3) 0.003(3) O2W 0.100(12) 0.22(2) 0.134(14) -0.136(17) 0.104(12) -0.083(15) _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 Co2 O6 1.954(5) . ? Co2 O7 1.976(5) . ? Co2 O2 2.033(5) . ? Co2 O4 2.090(5) 5_756 ? Co2 C19 2.093(6) . ? Co2 O1W 2.271(6) . ? Co1 N1 1.946(5) . ? Co1 O1 2.131(4) 5_756 ? Co1 O1 2.147(5) . ? Co1 N2 2.253(6) . ? Co1 O2 2.290(5) . ? Co1 O4 2.327(5) . ? C1 C2 1.447(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.336(9) . ? C2 C3 1.556(11) . ? C3 C4 1.336(9) . ? C3 H3 0.9300 . ? C4 C5 1.362(9) . ? C4 C8 1.684(10) . ? C5 O1 1.256(7) . ? C5 C6 1.544(10) . ? C6 C7 1.316(8) . ? C6 C12 1.456(10) 5_756 ? C7 H7 0.9300 . ? C9 C10 1.442(9) . ? C9 N1 1.743(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.426(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.450(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.402(8) . ? C12 C6 1.456(10) 5_756 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.499(10) . ? C13 N2 1.700(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.331(9) . ? C14 O2 1.407(9) . ? C15 N1 1.600(10) . ? C15 C16 1.681(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O4 1.162(7) . ? C16 O5 1.376(9) . ? C17 C17 1.275(12) 2_755 ? C17 C18 1.659(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.274(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O6 1.295(10) . ? C19 O7 1.316(10) . ? N1 C8 1.476(8) . ? O1 Co1 2.131(4) 5_756 ? O4 Co2 2.090(5) 5_756 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O1W H1WB 0.845(16) . ? O1W H1WA 0.848(16) . ? O2W H2WA 0.844(17) . ? 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 Co2 O7 74.6(2) . . ? O6 Co2 O2 160.05(19) . . ? O7 Co2 O2 89.9(2) . . ? O6 Co2 O4 89.9(2) . 5_756 ? O7 Co2 O4 163.4(2) . 5_756 ? O2 Co2 O4 103.70(19) . 5_756 ? O6 Co2 C19 37.1(3) . . ? O7 Co2 C19 37.6(3) . . ? O2 Co2 C19 125.8(3) . . ? O4 Co2 C19 126.4(3) 5_756 . ? O6 Co2 O1W 98.8(2) . . ? O7 Co2 O1W 79.5(2) . . ? O2 Co2 O1W 90.4(2) . . ? O4 Co2 O1W 109.39(18) 5_756 . ? C19 Co2 O1W 91.1(2) . . ? N1 Co1 O1 153.1(2) . 5_756 ? N1 Co1 O1 107.60(19) . . ? O1 Co1 O1 73.37(17) 5_756 . ? N1 Co1 N2 77.5(2) . . ? O1 Co1 N2 113.36(17) 5_756 . ? O1 Co1 N2 155.0(2) . . ? N1 Co1 O2 97.1(2) . . ? O1 Co1 O2 109.62(17) 5_756 . ? O1 Co1 O2 84.17(17) . . ? N2 Co1 O2 70.86(19) . . ? N1 Co1 O4 87.0(2) . . ? O1 Co1 O4 66.20(16) 5_756 . ? O1 Co1 O4 92.49(18) . . ? N2 Co1 O4 112.4(2) . . ? O2 Co1 O4 175.34(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C1 108.0(7) . . ? C7 C2 C3 124.6(6) . . ? C1 C2 C3 127.3(7) . . ? C4 C3 C2 129.1(7) . . ? C4 C3 H3 115.5 . . ? C2 C3 H3 115.5 . . ? C3 C4 C5 102.4(6) . . ? C3 C4 C8 127.3(6) . . ? C5 C4 C8 129.5(6) . . ? O1 C5 C4 105.2(6) . . ? O1 C5 C6 124.7(6) . . ? C4 C5 C6 130.0(5) . . ? C7 C6 C12 109.0(6) . 5_756 ? C7 C6 C5 123.8(6) . . ? C12 C6 C5 126.7(6) 5_756 . ? C6 C7 C2 109.1(6) . . ? C6 C7 H7 125.4 . . ? C2 C7 H7 125.4 . . ? C10 C9 N1 116.4(5) . . ? C10 C9 H9A 108.2 . . ? N1 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? N1 C9 H9B 108.2 . . ? H9A C9 H9B 107.3 . . ? C11 C10 C9 106.6(6) . . ? C11 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C10 C11 N2 112.3(6) . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? N2 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N2 C12 C6 111.3(6) . 5_756 ? N2 C12 H12A 109.4 . . ? C6 C12 H12A 109.4 5_756 . ? N2 C12 H12B 109.4 . . ? C6 C12 H12B 109.4 5_756 . ? H12A C12 H12B 108.0 . . ? C14 C13 N2 108.4(6) . . ? C14 C13 H13A 110.0 . . ? N2 C13 H13A 110.0 . . ? C14 C13 H13B 110.0 . . ? N2 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O3 C14 O2 129.5(6) . . ? O3 C14 C13 117.3(6) . . ? O2 C14 C13 113.2(6) . . ? N1 C15 C16 124.0(5) . . ? N1 C15 H15A 106.3 . . ? C16 C15 H15A 106.3 . . ? N1 C15 H15B 106.3 . . ? C16 C15 H15B 106.3 . . ? H15A C15 H15B 106.4 . . ? O4 C16 O5 118.5(7) . . ? O4 C16 C15 107.0(6) . . ? O5 C16 C15 134.4(5) . . ? C17 C17 C18 107.1(10) 2_755 . ? C17 C17 H17A 110.3 2_755 . ? C18 C17 H17A 110.3 . . ? C17 C17 H17B 110.3 2_755 . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C19 C18 C17 105.3(7) . . ? C19 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? C19 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C18 C19 O6 112.1(8) . . ? C18 C19 O7 116.1(8) . . ? O6 C19 O7 131.7(6) . . ? C18 C19 Co2 169.9(7) . . ? O6 C19 Co2 65.6(3) . . ? O7 C19 Co2 66.4(3) . . ? C8 N1 C15 109.4(5) . . ? C8 N1 C9 106.5(5) . . ? C15 N1 C9 122.2(5) . . ? C8 N1 Co1 94.2(4) . . ? C15 N1 Co1 102.4(4) . . ? C9 N1 Co1 118.5(3) . . ? C12 N2 C11 103.2(6) . . ? C12 N2 C13 121.1(5) . . ? C11 N2 C13 106.1(5) . . ? C12 N2 Co1 89.0(4) . . ? C11 N2 Co1 117.8(4) . . ? C13 N2 Co1 118.7(4) . . ? C5 O1 Co1 97.9(4) . 5_756 ? C5 O1 Co1 117.0(4) . . ? Co1 O1 Co1 106.63(17) 5_756 . ? C14 O2 Co2 130.9(4) . . ? C14 O2 Co1 126.9(4) . . ? Co2 O2 Co1 102.2(2) . . ? C16 O4 Co2 123.0(5) . 5_756 ? C16 O4 Co1 116.8(5) . . ? Co2 O4 Co1 119.6(2) 5_756 . ? C19 O6 Co2 77.2(4) . . ? C19 O7 Co2 76.0(4) . . ? N1 C8 C4 112.8(5) . . ? N1 C8 H8A 109.0 . . ? C4 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C4 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? Co2 O1W H1WB 94(2) . . ? Co2 O1W H1WA 109(7) . . ? H1WB O1W H1WA 117(3) . . ? 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 C7 C2 C3 C4 -4.4(13) . . . . ? C1 C2 C3 C4 177.6(9) . . . . ? C2 C3 C4 C5 -3.0(10) . . . . ? C2 C3 C4 C8 167.9(7) . . . . ? C3 C4 C5 O1 -171.4(6) . . . . ? C8 C4 C5 O1 18.0(9) . . . . ? C3 C4 C5 C6 10.0(10) . . . . ? C8 C4 C5 C6 -160.5(6) . . . . ? O1 C5 C6 C7 170.5(6) . . . . ? C4 C5 C6 C7 -11.2(11) . . . . ? O1 C5 C6 C12 -17.8(10) . . . 5_756 ? C4 C5 C6 C12 160.4(7) . . . 5_756 ? C12 C6 C7 C2 -171.0(6) 5_756 . . . ? C5 C6 C7 C2 1.9(9) . . . . ? C1 C2 C7 C6 -177.3(7) . . . . ? C3 C2 C7 C6 4.4(10) . . . . ? N1 C9 C10 C11 32.3(7) . . . . ? C9 C10 C11 N2 41.1(8) . . . . ? N2 C13 C14 O3 -167.7(5) . . . . ? N2 C13 C14 O2 14.7(6) . . . . ? N1 C15 C16 O4 20.0(8) . . . . ? N1 C15 C16 O5 -162.5(7) . . . . ? C17 C17 C18 C19 161.5(7) 2_755 . . . ? C17 C18 C19 O6 45.6(10) . . . . ? C17 C18 C19 O7 -131.1(8) . . . . ? C17 C18 C19 Co2 -29(5) . . . . ? O6 Co2 C19 C18 79(5) . . . . ? O7 Co2 C19 C18 -107(5) . . . . ? O2 Co2 C19 C18 -86(5) . . . . ? O4 Co2 C19 C18 67(5) 5_756 . . . ? O1W Co2 C19 C18 -178(5) . . . . ? O7 Co2 C19 O6 174.4(7) . . . . ? O2 Co2 C19 O6 -165.4(4) . . . . ? O4 Co2 C19 O6 -12.0(5) 5_756 . . . ? O1W Co2 C19 O6 103.3(4) . . . . ? O6 Co2 C19 O7 -174.4(7) . . . . ? O2 Co2 C19 O7 20.2(5) . . . . ? O4 Co2 C19 O7 173.6(4) 5_756 . . . ? O1W Co2 C19 O7 -71.2(4) . . . . ? C16 C15 N1 C8 83.2(7) . . . . ? C16 C15 N1 C9 -151.5(5) . . . . ? C16 C15 N1 Co1 -15.9(6) . . . . ? C10 C9 N1 C8 177.6(5) . . . . ? C10 C9 N1 C15 51.0(6) . . . . ? C10 C9 N1 Co1 -78.0(6) . . . . ? O1 Co1 N1 C8 -100.9(5) 5_756 . . . ? O1 Co1 N1 C8 -13.0(5) . . . . ? N2 Co1 N1 C8 141.6(4) . . . . ? O2 Co1 N1 C8 73.1(4) . . . . ? O4 Co1 N1 C8 -104.7(4) . . . . ? O1 Co1 N1 C15 10.1(6) 5_756 . . . ? O1 Co1 N1 C15 97.9(4) . . . . ? N2 Co1 N1 C15 -107.5(4) . . . . ? O2 Co1 N1 C15 -176.0(3) . . . . ? O4 Co1 N1 C15 6.2(4) . . . . ? O1 Co1 N1 C9 147.8(4) 5_756 . . . ? O1 Co1 N1 C9 -124.4(4) . . . . ? N2 Co1 N1 C9 30.2(4) . . . . ? O2 Co1 N1 C9 -38.3(4) . . . . ? O4 Co1 N1 C9 143.9(4) . . . . ? C6 C12 N2 C11 178.2(6) 5_756 . . . ? C6 C12 N2 C13 -63.5(8) 5_756 . . . ? C6 C12 N2 Co1 59.9(6) 5_756 . . . ? C10 C11 N2 C12 177.4(6) . . . . ? C10 C11 N2 C13 49.2(7) . . . . ? C10 C11 N2 Co1 -86.6(7) . . . . ? C14 C13 N2 C12 93.1(7) . . . . ? C14 C13 N2 C11 -150.1(5) . . . . ? C14 C13 N2 Co1 -14.8(6) . . . . ? N1 Co1 N2 C12 139.9(4) . . . . ? O1 Co1 N2 C12 -14.2(4) 5_756 . . . ? O1 Co1 N2 C12 -115.1(5) . . . . ? O2 Co1 N2 C12 -117.9(4) . . . . ? O4 Co1 N2 C12 58.5(4) . . . . ? N1 Co1 N2 C11 35.5(5) . . . . ? O1 Co1 N2 C11 -118.6(5) 5_756 . . . ? O1 Co1 N2 C11 140.5(5) . . . . ? O2 Co1 N2 C11 137.7(5) . . . . ? O4 Co1 N2 C11 -45.9(5) . . . . ? N1 Co1 N2 C13 -94.7(4) . . . . ? O1 Co1 N2 C13 111.2(4) 5_756 . . . ? O1 Co1 N2 C13 10.3(6) . . . . ? O2 Co1 N2 C13 7.4(3) . . . . ? O4 Co1 N2 C13 -176.1(3) . . . . ? C4 C5 O1 Co1 149.1(4) . . . 5_756 ? C6 C5 O1 Co1 -32.2(7) . . . 5_756 ? C4 C5 O1 Co1 35.9(6) . . . . ? C6 C5 O1 Co1 -145.5(5) . . . . ? N1 Co1 O1 C5 -43.6(5) . . . . ? O1 Co1 O1 C5 108.3(5) 5_756 . . . ? N2 Co1 O1 C5 -142.0(5) . . . . ? O2 Co1 O1 C5 -139.2(4) . . . . ? O4 Co1 O1 C5 44.0(4) . . . . ? N1 Co1 O1 Co1 -151.9(2) . . . 5_756 ? O1 Co1 O1 Co1 0.0 5_756 . . 5_756 ? N2 Co1 O1 Co1 109.8(4) . . . 5_756 ? O2 Co1 O1 Co1 112.5(2) . . . 5_756 ? O4 Co1 O1 Co1 -64.24(19) . . . 5_756 ? O3 C14 O2 Co2 -4.4(9) . . . . ? C13 C14 O2 Co2 172.9(4) . . . . ? O3 C14 O2 Co1 172.3(5) . . . . ? C13 C14 O2 Co1 -10.5(7) . . . . ? O6 Co2 O2 C14 -110.7(7) . . . . ? O7 Co2 O2 C14 -72.1(5) . . . . ? O4 Co2 O2 C14 117.5(5) 5_756 . . . ? C19 Co2 O2 C14 -84.2(5) . . . . ? O1W Co2 O2 C14 7.4(5) . . . . ? O6 Co2 O2 Co1 72.1(7) . . . . ? O7 Co2 O2 Co1 110.7(2) . . . . ? O4 Co2 O2 Co1 -59.7(2) 5_756 . . . ? C19 Co2 O2 Co1 98.5(3) . . . . ? O1W Co2 O2 Co1 -169.82(18) . . . . ? N1 Co1 O2 C14 75.5(5) . . . . ? O1 Co1 O2 C14 -107.4(4) 5_756 . . . ? O1 Co1 O2 C14 -177.4(4) . . . . ? N2 Co1 O2 C14 1.4(4) . . . . ? O4 Co1 O2 C14 -133.1(18) . . . . ? N1 Co1 O2 Co2 -107.1(2) . . . . ? O1 Co1 O2 Co2 70.0(2) 5_756 . . . ? O1 Co1 O2 Co2 -0.02(17) . . . . ? N2 Co1 O2 Co2 178.8(2) . . . . ? O4 Co1 O2 Co2 44.3(19) . . . . ? O5 C16 O4 Co2 -2.0(9) . . . 5_756 ? C15 C16 O4 Co2 176.0(4) . . . 5_756 ? O5 C16 O4 Co1 170.0(5) . . . . ? C15 C16 O4 Co1 -12.0(7) . . . . ? N1 Co1 O4 C16 4.3(5) . . . . ? O1 Co1 O4 C16 -173.8(6) 5_756 . . . ? O1 Co1 O4 C16 -103.2(5) . . . . ? N2 Co1 O4 C16 79.5(5) . . . . ? O2 Co1 O4 C16 -147.3(17) . . . . ? N1 Co1 O4 Co2 176.5(3) . . . 5_756 ? O1 Co1 O4 Co2 -1.6(2) 5_756 . . 5_756 ? O1 Co1 O4 Co2 69.0(2) . . . 5_756 ? N2 Co1 O4 Co2 -108.2(3) . . . 5_756 ? O2 Co1 O4 Co2 25(2) . . . 5_756 ? C18 C19 O6 Co2 -169.3(8) . . . . ? O7 C19 O6 Co2 6.8(8) . . . . ? O7 Co2 O6 C19 -3.5(4) . . . . ? O2 Co2 O6 C19 36.8(9) . . . . ? O4 Co2 O6 C19 170.4(4) 5_756 . . . ? O1W Co2 O6 C19 -80.0(4) . . . . ? C18 C19 O7 Co2 169.2(8) . . . . ? O6 C19 O7 Co2 -6.8(8) . . . . ? O6 Co2 O7 C19 3.5(4) . . . . ? O2 Co2 O7 C19 -163.8(4) . . . . ? O4 Co2 O7 C19 -18.3(10) 5_756 . . . ? O1W Co2 O7 C19 105.8(4) . . . . ? C15 N1 C8 C4 -48.2(6) . . . . ? C9 N1 C8 C4 177.8(4) . . . . ? Co1 N1 C8 C4 56.5(5) . . . . ? C3 C4 C8 N1 103.4(8) . . . . ? C5 C4 C8 N1 -88.2(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O5 0.845(16) 2.08(3) 2.826(8) 147(4) 5_756 O1W H1WA O3 0.848(16) 1.97(4) 2.762(8) 156(9) . _diffrn_measured_fraction_theta_max 0.555 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.462 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.121 #=========================END