# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Feifei Xing' _publ_contact_author_email xff@shu.edu.cn _publ_author_name 'Feifei Xing' data_090510c_0m _database_code_depnum_ccdc_archive 'CCDC 848873' #TrackingRef 'web_deposit_cif_file_0_xingfeifei_1318817696.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 O25 Zn3' _chemical_formula_weight 772.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8113(10) _cell_length_b 16.3344(14) _cell_length_c 13.8479(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.8510(10) _cell_angle_gamma 90.00 _cell_volume 2462.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4075 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.20 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 3.014 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5840 _exptl_absorpt_correction_T_max 0.6606 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12622 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4347 _reflns_number_gt 3541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.9458P] 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 4347 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.39669(3) 0.54738(2) 0.40022(3) 0.01548(11) Uani 1 1 d . . . Zn2 Zn 0.25546(4) 0.54509(2) 0.71655(3) 0.01908(11) Uani 1 1 d . . . Zn3 Zn 0.05188(3) 0.36869(2) 0.12724(3) 0.01546(11) Uani 1 1 d . . . C1 C 0.2438(3) 0.46616(19) 0.5072(2) 0.0134(7) Uani 1 1 d . . . C2 C 0.1669(3) 0.39501(19) 0.5189(2) 0.0118(7) Uani 1 1 d . . . H2 H 0.1034 0.4193 0.5390 0.014 Uiso 1 1 calc R . . C3 C 0.2341(3) 0.33016(19) 0.6050(2) 0.0124(7) Uani 1 1 d . . . H3 H 0.1668 0.2952 0.6054 0.015 Uiso 1 1 calc R . . C4 C 0.3171(3) 0.27011(19) 0.5775(2) 0.0123(7) Uani 1 1 d . . . H4 H 0.3336 0.2255 0.6285 0.015 Uiso 1 1 calc R . . C5 C 0.2437(3) 0.23032(18) 0.4693(2) 0.0108(7) Uani 1 1 d . . . H5 H 0.1762 0.2026 0.4805 0.013 Uiso 1 1 calc R . . C6 C 0.1764(3) 0.28973(19) 0.3788(2) 0.0117(7) Uani 1 1 d . . . H6 H 0.1182 0.2563 0.3227 0.014 Uiso 1 1 calc R . . C7 C 0.0976(3) 0.34746(19) 0.4157(2) 0.0114(7) Uani 1 1 d . . . H7 H 0.0492 0.3084 0.4376 0.014 Uiso 1 1 calc R . . C8 C 0.2942(3) 0.3589(2) 0.7187(3) 0.0157(7) Uani 1 1 d . . . C9 C 0.4422(3) 0.30611(19) 0.5952(2) 0.0122(7) Uani 1 1 d . . . C10 C 0.3071(3) 0.1606(2) 0.4366(2) 0.0147(7) Uani 1 1 d . . . C11 C 0.2643(3) 0.32649(18) 0.3341(2) 0.0124(7) Uani 1 1 d . . . C12 C -0.0029(3) 0.39632(19) 0.3314(2) 0.0130(7) Uani 1 1 d . . . O1 O 0.2658(2) 0.47163(13) 0.42608(16) 0.0154(5) Uani 1 1 d . . . O2 O 0.2779(2) 0.52129(13) 0.57862(17) 0.0169(5) Uani 1 1 d . . . O3 O 0.2559(2) 0.42397(14) 0.74600(18) 0.0239(6) Uani 1 1 d . . . O4 O 0.3700(2) 0.31233(15) 0.78228(18) 0.0280(6) Uani 1 1 d . . . O5 O 0.4579(2) 0.38218(13) 0.60547(17) 0.0156(5) Uani 1 1 d . . . O6 O 0.5300(2) 0.25669(13) 0.60497(18) 0.0174(5) Uani 1 1 d . . . O7 O 0.3821(2) 0.11459(13) 0.50508(17) 0.0201(5) Uani 1 1 d . . . O8 O 0.2717(2) 0.14629(15) 0.34071(18) 0.0286(6) Uani 1 1 d . . . O9 O 0.37710(19) 0.31732(14) 0.38602(17) 0.0161(5) Uani 1 1 d . . . O10 O 0.2226(2) 0.36094(13) 0.24513(16) 0.0160(5) Uani 1 1 d . . . O11 O -0.0261(2) 0.38516(14) 0.23638(16) 0.0189(5) Uani 1 1 d . . . O12 O -0.0684(2) 0.44046(15) 0.36377(17) 0.0231(6) Uani 1 1 d . . . O13 O 0.3401(2) 0.50621(14) 0.24766(17) 0.0194(5) Uani 1 1 d . . . H13A H 0.2999 0.5421 0.2075 0.029 Uiso 1 1 calc R . . O14 O 0.2820(2) 0.65076(14) 0.36674(18) 0.0215(6) Uani 1 1 d . . . H14A H 0.3237 0.6923 0.3749 0.032 Uiso 1 1 calc R . . O15 O 0.4817(2) 0.55891(13) 0.56307(17) 0.0164(5) Uani 1 1 d . . . O16 O 0.2657(3) 0.67375(17) 0.6931(3) 0.0496(9) Uani 1 1 d . . . H16A H 0.2076 0.6967 0.7001 0.074 Uiso 1 1 calc R . . O17 O 0.4547(2) 0.55277(19) 0.7885(2) 0.0430(8) Uani 1 1 d . . . H17A H 0.4844 0.5257 0.7542 0.065 Uiso 1 1 calc R . . O18 O 0.2680(2) 0.5653(2) 0.8697(2) 0.0421(8) Uani 1 1 d . . . H18A H 0.1996 0.5754 0.8687 0.063 Uiso 1 1 calc R . . O19 O 0.0677(2) 0.49656(14) 0.12748(19) 0.0261(6) Uani 1 1 d . . . H19A H 0.0808 0.5111 0.0761 0.039 Uiso 1 1 calc R . . O20 O 0.1457(3) 0.36688(18) 0.0245(2) 0.0355(7) Uani 1 1 d . . . H20A H 0.1143 0.3326 -0.0214 0.053 Uiso 1 1 calc R . . O21 O 0.1021(3) 0.6591(2) 0.4512(2) 0.0578(9) Uani 1 1 d . . . O22 O 0.5992(4) 0.6685(3) 0.9264(3) 0.0920(14) Uani 1 1 d . . . O23 O 0.5100(4) 0.4121(3) 0.9475(3) 0.0838(13) Uani 1 1 d . . . O24 O 0.0633(3) 0.26063(19) 0.8522(3) 0.0507(8) Uani 1 1 d . . . O25 O 0.0206(3) 0.40522(17) 0.7511(2) 0.0508(8) Uani 1 1 d . . . H13B H 0.2992 0.4619 0.2385 0.061 Uiso 1 1 d R . . H15B H 0.4178 0.5521 0.5765 0.061 Uiso 1 1 d R . . H16B H 0.3259 0.6929 0.6815 0.061 Uiso 1 1 d R . . H14B H 0.2461 0.6505 0.3000 0.061 Uiso 1 1 d R . . H18B H 0.3287 0.5684 0.9273 0.061 Uiso 1 1 d R . . H19B H 0.0437 0.5239 0.1676 0.061 Uiso 1 1 d R . . H20B H 0.2231 0.3664 0.0470 0.061 Uiso 1 1 d R . . H17B H 0.4889 0.5934 0.8258 0.061 Uiso 1 1 d R . . H15A H 0.5211 0.6033 0.5815 0.061 Uiso 1 1 d R . . H24A H 0.0229 0.2469 0.7876 0.061 Uiso 1 1 d R . . H21A H 0.1607 0.6624 0.4304 0.061 Uiso 1 1 d R . . H23A H 0.4464 0.4330 0.9531 0.061 Uiso 1 1 d R . . H25A H -0.0161 0.3953 0.6860 0.061 Uiso 1 1 d R . . H22A H 0.5940 0.6830 0.8658 0.061 Uiso 1 1 d R . . H22B H 0.5943 0.6530 0.9832 0.061 Uiso 1 1 d R . . H24B H -0.0016 0.2421 0.8572 0.061 Uiso 1 1 d R . . H23B H 0.4752 0.3812 0.8938 0.061 Uiso 1 1 d R . . H21B H 0.1324 0.6410 0.5132 0.061 Uiso 1 1 d R . . H25B H 0.0941 0.4115 0.7948 0.061 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0157(2) 0.0143(2) 0.0151(2) 0.00067(16) 0.00455(17) -0.00073(17) Zn2 0.0183(2) 0.0187(2) 0.0192(2) -0.00301(17) 0.00619(18) 0.00293(18) Zn3 0.0153(2) 0.0136(2) 0.0153(2) 0.00015(16) 0.00345(16) -0.00181(16) C1 0.0095(16) 0.0098(17) 0.0185(17) 0.0031(14) 0.0028(14) 0.0057(13) C2 0.0100(16) 0.0125(17) 0.0131(16) 0.0003(13) 0.0046(14) 0.0001(13) C3 0.0130(17) 0.0085(17) 0.0166(16) 0.0013(13) 0.0065(14) -0.0002(13) C4 0.0154(17) 0.0101(17) 0.0121(16) 0.0032(13) 0.0059(14) 0.0022(14) C5 0.0101(16) 0.0098(17) 0.0128(16) 0.0024(13) 0.0048(13) -0.0002(13) C6 0.0098(16) 0.0095(17) 0.0137(16) 0.0000(13) 0.0023(14) -0.0002(13) C7 0.0097(16) 0.0096(17) 0.0142(16) 0.0015(13) 0.0039(14) -0.0002(13) C8 0.0180(18) 0.0118(18) 0.0188(17) 0.0012(14) 0.0087(15) -0.0051(15) C9 0.0173(18) 0.0108(18) 0.0077(15) 0.0018(13) 0.0040(14) -0.0011(14) C10 0.0142(17) 0.0100(17) 0.0180(18) -0.0007(14) 0.0043(15) -0.0018(14) C11 0.0168(18) 0.0037(16) 0.0160(17) -0.0037(13) 0.0055(15) 0.0012(13) C12 0.0084(16) 0.0121(17) 0.0168(17) -0.0010(13) 0.0028(14) -0.0012(14) O1 0.0192(13) 0.0146(13) 0.0139(12) -0.0006(9) 0.0078(10) -0.0019(10) O2 0.0192(13) 0.0137(13) 0.0206(12) -0.0068(10) 0.0107(11) -0.0045(10) O3 0.0391(16) 0.0153(13) 0.0203(13) -0.0021(10) 0.0146(12) 0.0053(12) O4 0.0357(16) 0.0268(15) 0.0144(12) 0.0012(11) 0.0020(12) 0.0127(13) O5 0.0159(12) 0.0104(13) 0.0206(12) 0.0008(9) 0.0071(10) -0.0009(10) O6 0.0135(12) 0.0108(12) 0.0269(13) 0.0022(10) 0.0068(11) 0.0035(10) O7 0.0218(13) 0.0107(12) 0.0198(12) -0.0006(10) -0.0006(11) 0.0062(10) O8 0.0435(17) 0.0207(15) 0.0155(13) -0.0029(10) 0.0048(12) 0.0109(12) O9 0.0080(12) 0.0181(13) 0.0188(12) 0.0003(10) 0.0013(10) -0.0003(10) O10 0.0158(12) 0.0180(13) 0.0128(11) 0.0034(10) 0.0041(10) -0.0032(10) O11 0.0175(13) 0.0265(14) 0.0110(12) 0.0007(10) 0.0036(10) 0.0060(11) O12 0.0192(13) 0.0298(15) 0.0176(12) -0.0025(11) 0.0041(11) 0.0108(11) O13 0.0198(14) 0.0191(14) 0.0175(12) 0.0013(10) 0.0053(11) -0.0007(11) O14 0.0201(13) 0.0187(14) 0.0249(13) 0.0013(11) 0.0078(11) -0.0022(10) O15 0.0164(12) 0.0139(13) 0.0189(12) -0.0012(10) 0.0069(10) -0.0036(10) O16 0.055(2) 0.0225(17) 0.091(3) -0.0054(16) 0.050(2) -0.0011(15) O17 0.0247(16) 0.057(2) 0.0482(18) -0.0264(15) 0.0148(14) -0.0058(14) O18 0.0231(15) 0.071(2) 0.0284(16) -0.0189(14) 0.0053(13) 0.0089(15) O19 0.0354(16) 0.0176(14) 0.0254(14) -0.0015(11) 0.0119(13) -0.0073(12) O20 0.0341(17) 0.0477(19) 0.0288(15) -0.0049(13) 0.0168(14) -0.0086(14) O21 0.0407(19) 0.092(3) 0.0423(19) 0.0155(18) 0.0184(16) 0.0196(18) O22 0.075(3) 0.104(4) 0.099(3) -0.023(3) 0.036(3) -0.027(3) O23 0.080(3) 0.090(3) 0.051(2) -0.019(2) -0.007(2) 0.028(2) O24 0.0441(19) 0.050(2) 0.067(2) 0.0016(16) 0.0319(18) -0.0040(16) O25 0.056(2) 0.044(2) 0.061(2) -0.0025(16) 0.0337(18) -0.0039(16) _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 O13 2.065(2) . ? Zn1 O15 2.091(2) . ? Zn1 O5 2.094(2) 3_666 ? Zn1 O14 2.101(2) . ? Zn1 O1 2.116(2) . ? Zn1 O15 2.184(2) 3_666 ? Zn2 O3 2.020(2) . ? Zn2 O2 2.065(2) . ? Zn2 O12 2.066(2) 3_566 ? Zn2 O18 2.094(3) . ? Zn2 O16 2.137(3) . ? Zn2 O17 2.174(3) . ? Zn3 O10 2.047(2) . ? Zn3 O11 2.070(2) . ? Zn3 O6 2.072(2) 4_565 ? Zn3 O7 2.079(2) 4_565 ? Zn3 O19 2.097(2) . ? Zn3 O20 2.116(3) . ? C1 O1 1.251(4) . ? C1 O2 1.282(4) . ? C1 C2 1.522(4) . ? C2 C7 1.552(4) . ? C2 C3 1.561(4) . ? C2 H2 0.9800 . ? C3 C8 1.528(4) . ? C3 C4 1.536(4) . ? C3 H3 0.9800 . ? C4 C9 1.519(4) . ? C4 C5 1.553(4) . ? C4 H4 0.9800 . ? C5 C10 1.526(4) . ? C5 C6 1.539(4) . ? C5 H5 0.9800 . ? C6 C11 1.524(4) . ? C6 C7 1.544(4) . ? C6 H6 0.9800 . ? C7 C12 1.527(4) . ? C7 H7 0.9800 . ? C8 O4 1.243(4) . ? C8 O3 1.269(4) . ? C9 O5 1.256(4) . ? C9 O6 1.279(4) . ? C10 O8 1.250(4) . ? C10 O7 1.263(4) . ? C11 O9 1.253(4) . ? C11 O10 1.267(4) . ? C12 O11 1.249(4) . ? C12 O12 1.260(4) . ? O5 Zn1 2.094(2) 3_666 ? O6 Zn3 2.072(2) 4_666 ? O7 Zn3 2.079(2) 4_666 ? O12 Zn2 2.066(2) 3_566 ? O13 H13A 0.8200 . ? O13 H13B 0.8525 . ? O14 H14A 0.8200 . ? O14 H14B 0.8541 . ? O15 Zn1 2.184(2) 3_666 ? O15 H15B 0.8521 . ? O15 H15A 0.8450 . ? O16 H16A 0.8200 . ? O16 H16B 0.8472 . ? O17 H17A 0.8200 . ? O17 H17B 0.8419 . ? O18 H18A 0.8200 . ? O18 H18B 0.8419 . ? O19 H19A 0.8200 . ? O19 H19B 0.8438 . ? O20 H20A 0.8200 . ? O20 H20B 0.8438 . ? O21 H21A 0.8491 . ? O21 H21B 0.8442 . ? O22 H22A 0.8511 . ? O22 H22B 0.8495 . ? O23 H23A 0.8562 . ? O23 H23B 0.8595 . ? O24 H24A 0.8639 . ? O24 H24B 0.8518 . ? O25 H25A 0.8500 . ? O25 H25B 0.8500 . ? 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 O13 Zn1 O15 164.12(9) . . ? O13 Zn1 O5 94.86(9) . 3_666 ? O15 Zn1 O5 86.20(8) . 3_666 ? O13 Zn1 O14 96.38(9) . . ? O15 Zn1 O14 99.44(9) . . ? O5 Zn1 O14 91.05(9) 3_666 . ? O13 Zn1 O1 90.87(9) . . ? O15 Zn1 O1 86.94(8) . . ? O5 Zn1 O1 172.42(8) 3_666 . ? O14 Zn1 O1 93.23(9) . . ? O13 Zn1 O15 84.35(9) . 3_666 ? O15 Zn1 O15 79.84(9) . 3_666 ? O5 Zn1 O15 88.32(8) 3_666 3_666 ? O14 Zn1 O15 179.07(9) . 3_666 ? O1 Zn1 O15 87.33(8) . 3_666 ? O3 Zn2 O2 90.64(9) . . ? O3 Zn2 O12 97.99(10) . 3_566 ? O2 Zn2 O12 91.04(9) . 3_566 ? O3 Zn2 O18 87.52(11) . . ? O2 Zn2 O18 169.31(10) . . ? O12 Zn2 O18 99.64(10) 3_566 . ? O3 Zn2 O16 176.50(12) . . ? O2 Zn2 O16 90.55(11) . . ? O12 Zn2 O16 85.28(11) 3_566 . ? O18 Zn2 O16 90.70(13) . . ? O3 Zn2 O17 92.67(11) . . ? O2 Zn2 O17 85.96(10) . . ? O12 Zn2 O17 168.96(12) 3_566 . ? O18 Zn2 O17 83.61(11) . . ? O16 Zn2 O17 84.13(12) . . ? O10 Zn3 O11 90.32(9) . . ? O10 Zn3 O6 94.88(9) . 4_565 ? O11 Zn3 O6 99.90(9) . 4_565 ? O10 Zn3 O7 175.64(9) . 4_565 ? O11 Zn3 O7 90.86(9) . 4_565 ? O6 Zn3 O7 89.05(9) 4_565 4_565 ? O10 Zn3 O19 90.03(9) . . ? O11 Zn3 O19 86.23(9) . . ? O6 Zn3 O19 172.10(9) 4_565 . ? O7 Zn3 O19 85.86(9) 4_565 . ? O10 Zn3 O20 85.66(10) . . ? O11 Zn3 O20 172.00(10) . . ? O6 Zn3 O20 87.36(10) 4_565 . ? O7 Zn3 O20 92.65(10) 4_565 . ? O19 Zn3 O20 86.85(11) . . ? O1 C1 O2 122.0(3) . . ? O1 C1 C2 119.4(3) . . ? O2 C1 C2 118.4(3) . . ? C1 C2 C7 114.0(3) . . ? C1 C2 C3 116.9(3) . . ? C7 C2 C3 107.1(3) . . ? C1 C2 H2 106.0 . . ? C7 C2 H2 106.0 . . ? C3 C2 H2 106.0 . . ? C8 C3 C4 111.5(3) . . ? C8 C3 C2 118.2(3) . . ? C4 C3 C2 115.4(3) . . ? C8 C3 H3 103.1 . . ? C4 C3 H3 103.1 . . ? C2 C3 H3 103.1 . . ? C9 C4 C3 112.8(3) . . ? C9 C4 C5 117.5(2) . . ? C3 C4 C5 109.6(2) . . ? C9 C4 H4 105.3 . . ? C3 C4 H4 105.3 . . ? C5 C4 H4 105.3 . . ? C10 C5 C6 112.7(2) . . ? C10 C5 C4 116.4(3) . . ? C6 C5 C4 116.1(3) . . ? C10 C5 H5 103.0 . . ? C6 C5 H5 103.0 . . ? C4 C5 H5 103.0 . . ? C11 C6 C5 111.2(2) . . ? C11 C6 C7 119.1(3) . . ? C5 C6 C7 107.6(2) . . ? C11 C6 H6 106.0 . . ? C5 C6 H6 106.0 . . ? C7 C6 H6 106.0 . . ? C12 C7 C6 117.2(3) . . ? C12 C7 C2 114.7(3) . . ? C6 C7 C2 116.1(3) . . ? C12 C7 H7 101.7 . . ? C6 C7 H7 101.7 . . ? C2 C7 H7 101.7 . . ? O4 C8 O3 122.9(3) . . ? O4 C8 C3 117.4(3) . . ? O3 C8 C3 119.2(3) . . ? O5 C9 O6 122.4(3) . . ? O5 C9 C4 119.5(3) . . ? O6 C9 C4 118.1(3) . . ? O8 C10 O7 122.3(3) . . ? O8 C10 C5 117.1(3) . . ? O7 C10 C5 120.2(3) . . ? O9 C11 O10 122.4(3) . . ? O9 C11 C6 117.4(3) . . ? O10 C11 C6 120.1(3) . . ? O11 C12 O12 123.0(3) . . ? O11 C12 C7 121.1(3) . . ? O12 C12 C7 115.4(3) . . ? C1 O1 Zn1 127.9(2) . . ? C1 O2 Zn2 137.0(2) . . ? C8 O3 Zn2 137.2(2) . . ? C9 O5 Zn1 128.7(2) . 3_666 ? C9 O6 Zn3 133.5(2) . 4_666 ? C10 O7 Zn3 134.9(2) . 4_666 ? C11 O10 Zn3 133.9(2) . . ? C12 O11 Zn3 144.1(2) . . ? C12 O12 Zn2 123.4(2) . 3_566 ? Zn1 O13 H13A 109.5 . . ? Zn1 O13 H13B 111.6 . . ? H13A O13 H13B 111.2 . . ? Zn1 O14 H14A 109.5 . . ? Zn1 O14 H14B 104.0 . . ? H14A O14 H14B 99.9 . . ? Zn1 O15 Zn1 100.16(9) . 3_666 ? Zn1 O15 H15B 97.4 . . ? Zn1 O15 H15B 113.8 3_666 . ? Zn1 O15 H15A 112.4 . . ? Zn1 O15 H15A 112.1 3_666 . ? H15B O15 H15A 118.4 . . ? Zn2 O16 H16A 109.5 . . ? Zn2 O16 H16B 119.5 . . ? H16A O16 H16B 130.9 . . ? Zn2 O17 H17A 109.5 . . ? Zn2 O17 H17B 120.2 . . ? H17A O17 H17B 124.7 . . ? Zn2 O18 H18A 109.5 . . ? Zn2 O18 H18B 131.9 . . ? H18A O18 H18B 118.4 . . ? Zn3 O19 H19A 109.5 . . ? Zn3 O19 H19B 118.4 . . ? H19A O19 H19B 130.1 . . ? Zn3 O20 H20A 109.5 . . ? Zn3 O20 H20B 121.8 . . ? H20A O20 H20B 112.3 . . ? H21A O21 H21B 106.7 . . ? H22A O22 H22B 172.5 . . ? H23A O23 H23B 99.8 . . ? H24A O24 H24B 80.8 . . ? H25A O25 H25B 137.6 . . ? 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 O25 H25B O3 0.85 2.27 2.824(4) 122.9 . O21 H21B O2 0.84 2.53 3.106(4) 126.6 . O21 H21B O12 0.84 2.50 3.187(4) 139.3 3_566 O21 H21B O16 0.84 2.43 3.160(5) 144.5 . O23 H23B O4 0.86 1.92 2.772(4) 168.5 . O24 H24B O9 0.85 1.90 2.735(4) 167.6 4_566 O22 H22B O23 0.85 2.12 2.863(6) 146.1 3_667 O25 H25A O21 0.85 1.98 2.811(4) 164.1 3_566 O21 H21A O14 0.85 1.96 2.799(4) 168.9 . O15 H15A O9 0.84 1.71 2.540(3) 168.6 3_666 O17 H17B O22 0.84 1.93 2.756(5) 166.3 . O20 H20B O22 0.84 2.06 2.878(5) 161.6 3_666 O19 H19B O25 0.84 1.96 2.803(4) 174.3 3_566 O18 H18B O23 0.84 2.04 2.875(4) 169.8 3_667 O14 H14B O8 0.85 1.88 2.692(3) 158.6 2 O16 H16B O24 0.85 1.91 2.733(4) 165.4 2_556 O15 H15B O2 0.85 1.74 2.573(3) 165.9 . O13 H13B O10 0.85 1.90 2.742(3) 169.5 . O20 H20A O24 0.82 2.00 2.802(4) 166.7 1_554 O19 H19A O7 0.82 2.17 2.878(3) 145.1 2 O18 H18A O7 0.82 2.39 3.031(4) 135.8 2_556 O18 H18A O11 0.82 2.10 2.778(3) 139.7 3_566 O17 H17A O13 0.82 2.15 2.827(4) 140.3 3_666 O16 H16A O4 0.82 2.15 2.869(4) 145.8 2_556 O14 H14A O6 0.82 1.84 2.588(3) 150.9 3_666 O13 H13A O8 0.82 1.90 2.687(3) 159.8 2 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.087 # Attachment 'web_deposit_cif_file_1_xingfeifei_1318817696.2.cif' data_11a _database_code_depnum_ccdc_archive 'CCDC 848874' #TrackingRef 'web_deposit_cif_file_1_xingfeifei_1318817696.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Co3 O25' _chemical_formula_weight 753.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8151(13) _cell_length_b 16.3216(19) _cell_length_c 13.8362(16) _cell_angle_alpha 90.00 _cell_angle_beta 112.7660(10) _cell_angle_gamma 90.00 _cell_volume 2460.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4011 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.16 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 2.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6772 _exptl_absorpt_correction_T_max 0.6772 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12508 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4323 _reflns_number_gt 3496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+20.0915P] 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 4323 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 -0.10152(6) 0.04589(4) 0.90086(5) 0.01635(18) Uani 1 1 d . . . Co2 Co 0.24033(7) -0.04652(5) 0.78217(6) 0.02113(19) Uani 1 1 d . . . Co3 Co -0.05133(6) 0.36891(4) 0.87331(5) 0.01640(18) Uani 1 1 d . . . C1 C 0.0577(5) 0.1936(3) 0.9049(4) 0.0166(11) Uani 1 1 d . . . C2 C 0.1922(5) 0.3386(3) 1.0640(4) 0.0172(11) Uani 1 1 d . . . C3 C 0.2355(5) 0.1727(3) 1.1667(4) 0.0153(11) Uani 1 1 d . . . C4 C 0.5023(5) 0.1035(3) 1.1690(4) 0.0166(11) Uani 1 1 d . . . C5 C 0.2557(4) 0.0334(3) 0.9929(4) 0.0144(11) Uani 1 1 d . . . C6 C 0.2073(5) 0.1401(3) 0.7823(4) 0.0172(11) Uani 1 1 d . . . C7 C 0.2663(5) 0.1694(3) 0.8950(4) 0.0147(11) Uani 1 1 d . . . H7 H 0.3336 0.2044 0.8946 0.018 Uiso 1 1 calc R . . C8 C 0.1826(5) 0.2296(3) 0.9225(4) 0.0134(11) Uani 1 1 d . . . H8 H 0.1662 0.2743 0.8716 0.016 Uiso 1 1 calc R . . C9 C 0.2558(5) 0.2696(3) 1.0310(4) 0.0155(11) Uani 1 1 d . . . H9 H 0.3230 0.2978 1.0197 0.019 Uiso 1 1 calc R . . C10 C 0.3235(5) 0.2105(3) 1.1215(4) 0.0132(10) Uani 1 1 d . . . H10 H 0.3815 0.2441 1.1776 0.016 Uiso 1 1 calc R . . C11 C 0.4024(5) 0.1520(3) 1.0845(4) 0.0140(11) Uani 1 1 d . . . H11 H 0.4510 0.1909 1.0625 0.017 Uiso 1 1 calc R . . C12 C 0.3329(4) 0.1043(3) 0.9812(4) 0.0137(11) Uani 1 1 d . . . H12 H 0.3964 0.0798 0.9611 0.016 Uiso 1 1 calc R . . O1 O 0.1169(3) 0.3845(2) 0.9957(3) 0.0231(9) Uani 1 1 d . . . O2 O 0.2266(4) 0.3531(2) 1.1588(3) 0.0312(10) Uani 1 1 d . . . O3 O 0.1236(3) 0.1827(2) 1.1154(3) 0.0191(8) Uani 1 1 d . . . O4 O 0.2776(3) 0.1388(2) 1.2557(3) 0.0188(8) Uani 1 1 d . . . O5 O 0.5261(3) 0.1150(2) 1.2637(3) 0.0208(8) Uani 1 1 d . . . O6 O 0.5690(4) 0.0590(3) 1.1370(3) 0.0267(9) Uani 1 1 d . . . O7 O 0.2334(3) 0.0285(2) 1.0743(3) 0.0182(8) Uani 1 1 d . . . O8 O 0.2215(3) -0.0214(2) 0.9215(3) 0.0186(8) Uani 1 1 d . . . O9 O 0.2432(4) 0.0744(2) 0.7550(3) 0.0281(9) Uani 1 1 d . . . O10 O 0.1324(4) 0.1875(3) 0.7176(3) 0.0332(10) Uani 1 1 d . . . O11 O 0.0419(3) 0.1179(2) 0.8946(3) 0.0182(8) Uani 1 1 d . . . O12 O -0.0296(3) 0.2431(2) 0.8945(3) 0.0182(8) Uani 1 1 d . . . O13 O -0.1611(3) 0.0078(2) 0.7461(3) 0.0233(9) Uani 1 1 d . . . H13A H -0.1987 -0.0376 0.7264 0.028 Uiso 1 1 d R . . H13B H -0.2039 0.0436 0.7077 0.028 Uiso 1 1 d R . . O14 O -0.2170(3) 0.1501(2) 0.8686(3) 0.0239(9) Uani 1 1 d . . . H14A H -0.1762 0.1915 0.8720 0.036 Uiso 1 1 calc R . . H14B H -0.2333 0.1462 0.8029 0.029 Uiso 1 1 d R . . O15 O -0.0176(3) 0.0591(2) 1.0634(3) 0.0169(8) Uani 1 1 d . . . H15A H 0.0206 0.1039 1.0846 0.020 Uiso 1 1 d R . . H15B H -0.0619 0.0516 1.0984 0.020 Uiso 1 1 d R . . O16 O 0.2322(5) -0.1737(3) 0.8057(4) 0.0477(13) Uani 1 1 d . . . H16A H 0.1719 -0.1840 0.8190 0.057 Uiso 1 1 calc R . . H16B H 0.2837 -0.2108 0.8076 0.057 Uiso 1 1 d R . . O17 O 0.2330(4) -0.0667(3) 0.6303(3) 0.0467(13) Uani 1 1 d . . . H17B H 0.1614 -0.0654 0.5885 0.056 Uiso 1 1 calc R . . H17A H 0.2893 -0.0798 0.6078 0.056 Uiso 1 1 d R . . O18 O 0.0427(4) -0.0515(3) 0.7106(4) 0.0500(14) Uani 1 1 d . . . H18A H 0.0138 -0.0143 0.7337 0.060 Uiso 1 1 calc R . . H18B H 0.0211 -0.0955 0.6802 0.060 Uiso 1 1 d R . . O19 O -0.1440(4) 0.3656(3) 0.9772(4) 0.0395(11) Uani 1 1 d . . . H19A H -0.1109 0.3319 1.0236 0.047 Uiso 1 1 calc R . . H19B H -0.2211 0.3662 0.9451 0.047 Uiso 1 1 d R . . O20 O -0.0672(4) 0.4965(2) 0.8732(3) 0.0300(10) Uani 1 1 d . . . H20A H -0.0435 0.5193 0.8287 0.036 Uiso 1 1 d R . . H20B H -0.1219 0.5333 0.8596 0.036 Uiso 1 1 d R . . O21 O 0.8986(7) 0.8320(5) 0.5708(7) 0.105(3) Uani 1 1 d . . . H21A H 0.9662 0.8253 0.5618 0.126 Uiso 1 1 d R . . H21B H 0.8989 0.8216 0.6319 0.126 Uiso 1 1 d R . . O22 O 0.6036(5) 0.1596(4) 0.9518(4) 0.0637(17) Uani 1 1 d . . . H22A H 0.6266 0.1307 1.0081 0.076 Uiso 1 1 d R . . H22B H 0.6710 0.1522 0.9430 0.076 Uiso 1 1 d R . . O23 O -0.0100(6) 0.0893(4) 0.5512(5) 0.091(2) Uani 1 1 d . . . H23A H 0.0224 0.1179 0.6070 0.109 Uiso 1 1 d R . . H23B H 0.0359 0.0496 0.5464 0.109 Uiso 1 1 d R . . O24 O 0.9795(5) 0.4055(3) 0.2495(5) 0.0560(15) Uani 1 1 d . . . H24A H 1.0175 0.3976 0.3151 0.067 Uiso 1 1 d R . . H24B H 0.9113 0.4102 0.2561 0.067 Uiso 1 1 d R . . O25 O 0.9384(5) 0.2598(3) 0.1506(4) 0.0519(14) Uani 1 1 d . . . H25A H 0.9546 0.2997 0.1932 0.062 Uiso 1 1 d R . . H25B H 1.0020 0.2314 0.1558 0.062 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0155(4) 0.0155(4) 0.0174(4) 0.0008(3) 0.0056(3) -0.0012(3) Co2 0.0191(4) 0.0217(4) 0.0222(4) -0.0039(3) 0.0076(3) 0.0019(3) Co3 0.0158(4) 0.0158(4) 0.0153(4) -0.0004(3) 0.0034(3) 0.0018(3) C1 0.016(3) 0.021(3) 0.010(2) 0.003(2) 0.002(2) 0.004(2) C2 0.015(3) 0.015(3) 0.021(3) -0.001(2) 0.006(2) -0.003(2) C3 0.016(3) 0.013(3) 0.017(3) -0.001(2) 0.007(2) 0.001(2) C4 0.012(3) 0.014(3) 0.021(3) -0.004(2) 0.004(2) -0.001(2) C5 0.010(2) 0.016(3) 0.017(3) 0.003(2) 0.005(2) 0.004(2) C6 0.016(3) 0.016(3) 0.021(3) 0.001(2) 0.008(2) 0.000(2) C7 0.011(3) 0.015(3) 0.017(3) 0.004(2) 0.005(2) 0.002(2) C8 0.020(3) 0.011(3) 0.010(2) 0.002(2) 0.006(2) 0.000(2) C9 0.015(3) 0.012(3) 0.017(3) 0.002(2) 0.004(2) 0.001(2) C10 0.013(3) 0.011(3) 0.015(3) 0.000(2) 0.004(2) 0.000(2) C11 0.014(3) 0.014(3) 0.013(2) 0.001(2) 0.003(2) -0.003(2) C12 0.010(2) 0.017(3) 0.015(3) 0.001(2) 0.005(2) 0.000(2) O1 0.024(2) 0.018(2) 0.019(2) -0.0021(16) -0.0015(17) 0.0077(16) O2 0.047(3) 0.022(2) 0.020(2) -0.0082(17) 0.008(2) 0.0096(19) O3 0.014(2) 0.019(2) 0.022(2) 0.0020(16) 0.0045(16) -0.0004(15) O4 0.019(2) 0.021(2) 0.0149(18) 0.0029(16) 0.0052(16) -0.0042(16) O5 0.0168(19) 0.025(2) 0.018(2) 0.0008(16) 0.0051(16) 0.0039(16) O6 0.022(2) 0.034(2) 0.020(2) -0.0030(18) 0.0033(17) 0.0108(18) O7 0.020(2) 0.020(2) 0.0159(19) -0.0003(15) 0.0074(16) -0.0047(15) O8 0.0168(19) 0.019(2) 0.021(2) -0.0055(16) 0.0083(16) -0.0036(15) O9 0.041(3) 0.021(2) 0.021(2) -0.0005(17) 0.0114(19) 0.0052(18) O10 0.041(3) 0.030(2) 0.022(2) -0.0002(19) 0.004(2) 0.011(2) O11 0.019(2) 0.012(2) 0.023(2) -0.0005(15) 0.0087(16) -0.0010(15) O12 0.0135(19) 0.0151(19) 0.024(2) 0.0013(15) 0.0052(16) 0.0026(15) O13 0.025(2) 0.023(2) 0.019(2) -0.0015(16) 0.0052(17) -0.0025(17) O14 0.023(2) 0.021(2) 0.029(2) -0.0010(17) 0.0117(18) -0.0024(16) O15 0.0190(19) 0.0154(19) 0.0196(19) -0.0018(15) 0.0109(16) -0.0038(15) O16 0.052(3) 0.020(2) 0.087(4) -0.008(2) 0.044(3) -0.002(2) O17 0.030(3) 0.077(4) 0.032(3) -0.018(3) 0.012(2) 0.008(3) O18 0.029(3) 0.063(4) 0.057(3) -0.029(3) 0.017(2) -0.002(2) O19 0.036(3) 0.050(3) 0.036(3) 0.008(2) 0.018(2) 0.007(2) O20 0.033(2) 0.019(2) 0.036(2) -0.0017(18) 0.011(2) 0.0077(18) O21 0.070(5) 0.115(7) 0.132(7) -0.044(6) 0.041(5) -0.026(4) O22 0.049(3) 0.093(5) 0.052(3) 0.014(3) 0.023(3) 0.021(3) O23 0.082(5) 0.093(5) 0.064(4) -0.017(4) -0.009(4) 0.026(4) O24 0.066(4) 0.044(3) 0.075(4) -0.002(3) 0.047(3) 0.002(3) O25 0.051(3) 0.041(3) 0.076(4) -0.010(3) 0.037(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O13 2.073(4) . ? Co1 O15 2.089(4) . ? Co1 O11 2.092(4) . ? Co1 O7 2.106(4) 3_557 ? Co1 O14 2.117(4) . ? Co1 O15 2.150(4) 3_557 ? Co2 O9 2.012(4) . ? Co2 O8 2.065(4) . ? Co2 O17 2.096(4) . ? Co2 O6 2.102(4) 3_657 ? Co2 O16 2.109(5) . ? Co2 O18 2.156(5) . ? Co3 O4 2.051(4) 4_565 ? Co3 O1 2.068(4) . ? Co3 O5 2.068(4) 4_565 ? Co3 O12 2.075(4) . ? Co3 O20 2.090(4) . ? Co3 O19 2.117(4) . ? C1 O11 1.249(6) . ? C1 O12 1.274(6) . ? C1 C8 1.518(7) . ? C2 O2 1.237(6) . ? C2 O1 1.263(6) . ? C2 C9 1.519(7) . ? C3 O3 1.245(6) . ? C3 O4 1.264(6) . ? C3 C10 1.535(7) . ? C4 O5 1.244(6) . ? C4 O6 1.270(6) . ? C4 C11 1.523(7) . ? C5 O7 1.255(6) . ? C5 O8 1.277(6) . ? C5 C12 1.521(7) . ? C6 O10 1.254(7) . ? C6 O9 1.263(7) . ? C6 C7 1.518(7) . ? C7 C8 1.543(7) . ? C7 C12 1.563(7) . ? C7 H7 0.9800 . ? C8 C9 1.556(7) . ? C8 H8 0.9800 . ? C9 C10 1.537(7) . ? C9 H9 0.9800 . ? C10 C11 1.554(7) . ? C10 H10 0.9800 . ? C11 C12 1.554(7) . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? O4 Co3 2.051(4) 4_666 ? O5 Co3 2.068(4) 4_666 ? O6 Co2 2.102(4) 3_657 ? O7 Co1 2.106(4) 3_557 ? O13 H13A 0.8527 . ? O13 H13B 0.8200 . ? O14 H14A 0.8200 . ? O14 H14B 0.8559 . ? O15 Co1 2.150(4) 3_557 ? O15 H15A 0.8500 . ? O15 H15B 0.8484 . ? O16 H16A 0.8200 . ? O16 H16B 0.8518 . ? O17 H17B 0.8200 . ? O17 H17A 0.8636 . ? O18 H18A 0.8200 . ? O18 H18B 0.8212 . ? O19 H19A 0.8200 . ? O19 H19B 0.8455 . ? O20 H20A 0.8544 . ? O20 H20B 0.8489 . ? O21 H21A 0.8614 . ? O21 H21B 0.8621 . ? O22 H22A 0.8590 . ? O22 H22B 0.8595 . ? O23 H23A 0.8555 . ? O23 H23B 0.8641 . ? O24 H24A 0.8532 . ? O24 H24B 0.8492 . ? O25 H25A 0.8489 . ? O25 H25B 0.8631 . ? 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 O13 Co1 O15 166.61(15) . . ? O13 Co1 O11 94.74(15) . . ? O15 Co1 O11 86.09(14) . . ? O13 Co1 O7 91.07(15) . 3_557 ? O15 Co1 O7 87.51(14) . 3_557 ? O11 Co1 O7 173.35(14) . 3_557 ? O13 Co1 O14 95.15(16) . . ? O15 Co1 O14 98.21(15) . . ? O11 Co1 O14 90.34(14) . . ? O7 Co1 O14 92.34(15) 3_557 . ? O13 Co1 O15 85.91(15) . 3_557 ? O15 Co1 O15 80.74(14) . 3_557 ? O11 Co1 O15 89.34(14) . 3_557 ? O7 Co1 O15 87.86(14) 3_557 3_557 ? O14 Co1 O15 178.92(15) . 3_557 ? O9 Co2 O8 89.74(15) . . ? O9 Co2 O17 87.91(19) . . ? O8 Co2 O17 171.74(17) . . ? O9 Co2 O6 95.88(17) . 3_657 ? O8 Co2 O6 90.19(15) . 3_657 ? O17 Co2 O6 97.92(17) . 3_657 ? O9 Co2 O16 178.0(2) . . ? O8 Co2 O16 91.34(17) . . ? O17 Co2 O16 90.8(2) . . ? O6 Co2 O16 85.76(18) 3_657 . ? O9 Co2 O18 92.6(2) . . ? O8 Co2 O18 86.98(17) . . ? O17 Co2 O18 85.22(18) . . ? O6 Co2 O18 171.1(2) 3_657 . ? O16 Co2 O18 85.8(2) . . ? O4 Co3 O1 175.73(15) 4_565 . ? O4 Co3 O5 90.32(14) 4_565 4_565 ? O1 Co3 O5 91.54(15) . 4_565 ? O4 Co3 O12 94.69(15) 4_565 . ? O1 Co3 O12 88.80(14) . . ? O5 Co3 O12 99.38(15) 4_565 . ? O4 Co3 O20 89.99(16) 4_565 . ? O1 Co3 O20 86.29(16) . . ? O5 Co3 O20 86.48(16) 4_565 . ? O12 Co3 O20 172.46(16) . . ? O4 Co3 O19 85.85(16) 4_565 . ? O1 Co3 O19 91.88(17) . . ? O5 Co3 O19 172.83(17) 4_565 . ? O12 Co3 O19 86.99(17) . . ? O20 Co3 O19 87.46(18) . . ? O11 C1 O12 122.4(5) . . ? O11 C1 C8 119.6(5) . . ? O12 C1 C8 117.8(5) . . ? O2 C2 O1 121.8(5) . . ? O2 C2 C9 117.5(5) . . ? O1 C2 C9 120.2(5) . . ? O3 C3 O4 122.9(5) . . ? O3 C3 C10 116.9(4) . . ? O4 C3 C10 120.0(4) . . ? O5 C4 O6 122.4(5) . . ? O5 C4 C11 121.5(5) . . ? O6 C4 C11 115.5(5) . . ? O7 C5 O8 122.4(5) . . ? O7 C5 C12 119.2(5) . . ? O8 C5 C12 118.3(4) . . ? O10 C6 O9 122.4(5) . . ? O10 C6 C7 117.1(5) . . ? O9 C6 C7 120.1(5) . . ? C6 C7 C8 111.8(4) . . ? C6 C7 C12 117.7(4) . . ? C8 C7 C12 115.2(4) . . ? C6 C7 H7 103.3 . . ? C8 C7 H7 103.3 . . ? C12 C7 H7 103.3 . . ? C1 C8 C7 112.9(4) . . ? C1 C8 C9 117.4(4) . . ? C7 C8 C9 109.6(4) . . ? C1 C8 H8 105.3 . . ? C7 C8 H8 105.3 . . ? C9 C8 H8 105.3 . . ? C2 C9 C10 112.5(4) . . ? C2 C9 C8 116.5(4) . . ? C10 C9 C8 116.2(4) . . ? C2 C9 H9 103.0 . . ? C10 C9 H9 103.0 . . ? C8 C9 H9 103.0 . . ? C9 C10 C3 111.3(4) . . ? C9 C10 C11 107.8(4) . . ? C3 C10 C11 118.3(4) . . ? C9 C10 H10 106.2 . . ? C3 C10 H10 106.2 . . ? C11 C10 H10 106.2 . . ? C4 C11 C12 115.0(4) . . ? C4 C11 C10 116.9(4) . . ? C12 C11 C10 116.1(4) . . ? C4 C11 H11 101.7 . . ? C12 C11 H11 101.7 . . ? C10 C11 H11 101.7 . . ? C5 C12 C11 114.1(4) . . ? C5 C12 C7 116.9(4) . . ? C11 C12 C7 107.0(4) . . ? C5 C12 H12 106.0 . . ? C11 C12 H12 106.0 . . ? C7 C12 H12 106.0 . . ? C2 O1 Co3 135.6(4) . . ? C3 O4 Co3 134.1(3) . 4_666 ? C4 O5 Co3 143.9(3) . 4_666 ? C4 O6 Co2 123.5(3) . 3_657 ? C5 O7 Co1 127.5(3) . 3_557 ? C5 O8 Co2 138.1(3) . . ? C6 O9 Co2 138.1(4) . . ? C1 O11 Co1 129.7(3) . . ? C1 O12 Co3 134.0(3) . . ? Co1 O13 H13A 121.2 . . ? Co1 O13 H13B 109.5 . . ? H13A O13 H13B 107.3 . . ? Co1 O14 H14A 109.5 . . ? Co1 O14 H14B 91.5 . . ? H14A O14 H14B 90.5 . . ? Co1 O15 Co1 99.26(14) . 3_557 ? Co1 O15 H15A 115.3 . . ? Co1 O15 H15A 113.1 3_557 . ? Co1 O15 H15B 117.3 . . ? Co1 O15 H15B 104.3 3_557 . ? H15A O15 H15B 106.9 . . ? Co2 O16 H16A 109.5 . . ? Co2 O16 H16B 129.1 . . ? H16A O16 H16B 121.2 . . ? Co2 O17 H17B 109.5 . . ? Co2 O17 H17A 131.4 . . ? H17B O17 H17A 118.8 . . ? Co2 O18 H18A 109.5 . . ? Co2 O18 H18B 109.6 . . ? H18A O18 H18B 138.9 . . ? Co3 O19 H19A 109.5 . . ? Co3 O19 H19B 112.2 . . ? H19A O19 H19B 120.6 . . ? Co3 O20 H20A 112.3 . . ? Co3 O20 H20B 140.0 . . ? H20A O20 H20B 88.0 . . ? H21A O21 H21B 117.7 . . ? H22A O22 H22B 93.8 . . ? H23A O23 H23B 113.8 . . ? H24A O24 H24B 91.6 . . ? H25A O25 H25B 113.5 . . ? 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 O13 H13A O4 0.85 1.96 2.756(5) 155.0 3_557 O13 H13B O2 0.82 1.88 2.671(6) 161.0 4_565 O13 H13B O20 0.82 2.61 2.994(6) 110.2 2_446 O14 H14A O12 0.82 1.84 2.593(5) 151.6 . O14 H14B O2 0.86 1.86 2.716(6) 175.1 4_565 O14 H14B O13 0.86 2.64 3.093(5) 114.5 . O15 H15A O3 0.85 1.71 2.538(5) 165.2 . O15 H15B O8 0.85 1.86 2.572(5) 140.1 3_557 O15 H15B O18 0.85 2.56 3.255(6) 139.5 3_557 O16 H16A O25 0.82 1.96 2.711(7) 152.6 3_656 O16 H16B O10 0.85 2.03 2.862(6) 165.1 2_546 O17 H17B O23 0.82 2.10 2.875(8) 157.4 3_556 O17 H17A O1 0.86 2.20 3.034(6) 162.2 2_546 O17 H17A O5 0.86 2.29 2.765(6) 114.7 3_657 O18 H18A O13 0.82 2.17 2.809(6) 135.0 . O18 H18B O21 0.82 2.02 2.776(9) 152.3 1_445 O19 H19A O25 0.82 2.01 2.806(7) 165.5 1_456 O19 H19B O21 0.85 2.10 2.872(9) 151.9 2_546 O20 H20A O24 0.85 1.97 2.807(7) 165.9 3_666 O20 H20B O2 0.85 2.19 3.021(6) 166.9 3_567 O20 H20B O1 0.85 2.39 2.869(5) 116.2 3_567 O21 H21A O23 0.86 2.30 2.819(12) 119.1 3_666 O22 H22A O6 0.86 2.44 3.200(7) 147.7 . O22 H22A O8 0.86 2.45 3.103(7) 133.3 3_657 O22 H22A O16 0.86 2.57 3.168(8) 127.9 3_657 O22 H22B O14 0.86 1.97 2.782(7) 157.7 1_655 O23 H23A O10 0.86 1.94 2.775(8) 163.4 . O23 H23B O23 0.86 2.60 3.290(14) 138.1 3_556 O24 H24A O22 0.85 2.00 2.818(8) 160.7 4_665 O24 H24B O9 0.85 2.00 2.841(7) 173.5 4_665 O25 H25A O24 0.85 1.87 2.692(7) 162.5 . O25 H25B O3 0.86 1.90 2.727(6) 158.7 1_654 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.843 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.115 # Attachment 'web_deposit_cif_file_2_xingfeifei_1318817696.3.cif' data_11b _database_code_depnum_ccdc_archive 'CCDC 848875' #TrackingRef 'web_deposit_cif_file_2_xingfeifei_1318817696.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 Cu5 O38' _chemical_formula_weight 1256.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 17.0978(17) _cell_length_b 8.3863(8) _cell_length_c 27.613(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.6500(10) _cell_angle_gamma 90.00 _cell_volume 3830.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6586 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4803 _exptl_absorpt_correction_T_max 0.5980 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9700 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3391 _reflns_number_gt 3118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+9.4265P] 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 3391 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Cu1 Cu 0.5000 0.26199(5) 0.7500 0.01472(12) Uani 1 2 d S . . Cu2 Cu 0.435561(19) 0.01720(4) 0.581783(12) 0.01842(11) Uani 1 1 d . . . Cu3 Cu 0.679971(19) -0.21416(4) 0.724432(12) 0.01490(10) Uani 1 1 d . . . C1 C 0.61400(15) 0.2516(3) 0.62991(9) 0.0112(5) Uani 1 1 d . . . H1 H 0.6066 0.3618 0.6178 0.013 Uiso 1 1 calc R . . C2 C 0.60814(15) 0.1520(3) 0.58167(9) 0.0118(5) Uani 1 1 d . . . H2 H 0.5581 0.1851 0.5577 0.014 Uiso 1 1 calc R . . C3 C 0.67790(15) 0.2004(3) 0.55863(9) 0.0124(5) Uani 1 1 d . . . H3 H 0.6671 0.3124 0.5492 0.015 Uiso 1 1 calc R . . C4 C 0.76320(15) 0.2018(3) 0.59508(9) 0.0124(5) Uani 1 1 d . . . H4 H 0.7978 0.2593 0.5776 0.015 Uiso 1 1 calc R . . C5 C 0.76202(15) 0.3039(3) 0.64117(9) 0.0120(5) Uani 1 1 d . . . H5 H 0.7438 0.4088 0.6271 0.014 Uiso 1 1 calc R . . C6 C 0.69710(15) 0.2540(3) 0.66852(9) 0.0111(5) Uani 1 1 d . . . H6 H 0.6944 0.3418 0.6915 0.013 Uiso 1 1 calc R . . C7 C 0.54671(16) 0.2274(3) 0.65588(10) 0.0139(5) Uani 1 1 d . . . C8 C 0.60319(16) -0.0293(3) 0.58645(9) 0.0135(5) Uani 1 1 d . . . C9 C 0.67238(16) 0.1146(3) 0.50921(10) 0.0156(5) Uani 1 1 d . . . C10 C 0.80617(16) 0.0460(3) 0.61196(10) 0.0159(6) Uani 1 1 d . . . C11 C 0.84796(15) 0.3339(3) 0.67281(10) 0.0132(5) Uani 1 1 d . . . C12 C 0.71153(15) 0.1032(3) 0.70093(9) 0.0124(5) Uani 1 1 d . . . O1 O 0.56071(11) 0.2789(2) 0.69940(7) 0.0200(4) Uani 1 1 d . . . O2 O 0.47865(11) 0.1715(3) 0.63303(7) 0.0219(4) Uani 1 1 d . . . O3 O 0.53630(11) -0.0913(2) 0.58939(7) 0.0179(4) Uani 1 1 d . . . O4 O 0.66249(11) -0.1116(2) 0.58411(7) 0.0190(4) Uani 1 1 d . . . O5 O 0.60326(11) 0.1110(3) 0.47911(7) 0.0228(4) Uani 1 1 d . . . O6 O 0.73484(11) 0.0586(2) 0.49916(7) 0.0216(4) Uani 1 1 d . . . O7 O 0.82965(12) -0.0412(2) 0.57808(7) 0.0230(4) Uani 1 1 d . . . H7 H 0.8076 -0.0084 0.5500 0.035 Uiso 1 1 calc R . . O8 O 0.82706(13) 0.0098(2) 0.65569(7) 0.0254(5) Uani 1 1 d . . . O9 O 0.90191(11) 0.3492(2) 0.65017(7) 0.0208(4) Uani 1 1 d . . . O10 O 0.86154(11) 0.3569(2) 0.71991(7) 0.0186(4) Uani 1 1 d . . . O11 O 0.76685(11) 0.0997(2) 0.74099(7) 0.0166(4) Uani 1 1 d . . . O12 O 0.66362(11) -0.0110(2) 0.68754(7) 0.0149(4) Uani 1 1 d . . . O1W O 0.5000 0.0287(3) 0.7500 0.0277(7) Uani 1 2 d S . . H1WA H 0.5460 -0.0039 0.7622 0.042 Uiso 1 1 calc R . . O2W O 0.5000 0.4930(4) 0.7500 0.0439(10) Uani 1 2 d S . . H2WA H 0.4896 0.5255 0.7757 0.066 Uiso 1 1 calc R . . O3W O 0.37160(12) 0.2209(2) 0.69110(8) 0.0255(5) Uani 1 1 d . . . H3WB H 0.3552 0.3057 0.6775 0.038 Uiso 1 1 calc R . . O4W O 0.33109(12) 0.1218(3) 0.57727(8) 0.0260(5) Uani 1 1 d . . . H4WB H 0.2988 0.0953 0.5512 0.039 Uiso 1 1 calc R . . O5W O 0.54968(12) -0.3061(3) 0.68607(8) 0.0267(5) Uani 1 1 d . . . H5WB H 0.5498 -0.3498 0.6595 0.040 Uiso 1 1 calc R . . O6W O 0.70895(13) -0.3110(2) 0.66551(7) 0.0226(4) Uani 1 1 d . . . H6WB H 0.6915 -0.2549 0.6408 0.034 Uiso 1 1 calc R . . O7W O 0.5060(2) 0.5713(4) 0.57831(14) 0.0711(10) Uani 1 1 d . . . O8W O 0.6099(4) 0.6547(8) 0.5080(2) 0.182(3) Uani 1 1 d . . . H8WA H 0.5824 0.7328 0.4930 0.218 Uiso 1 1 d R . . H6WA H 0.7599 -0.3187 0.6705 0.218 Uiso 1 1 d R . . H3WA H 0.3979 0.1778 0.6722 0.218 Uiso 1 1 d R . . H7WA H 0.4810 0.5709 0.5473 0.218 Uiso 1 1 d R . . H5WA H 0.5094 -0.2428 0.6796 0.218 Uiso 1 1 d R . . H4WA H 0.3246 0.2213 0.5716 0.218 Uiso 1 1 d R . . H8WB H 0.6604 0.6451 0.5107 0.218 Uiso 1 1 d R . . H7WB H 0.4983 0.6706 0.5725 0.218 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0150(2) 0.0179(2) 0.0132(2) 0.000 0.00723(18) 0.000 Cu2 0.01312(18) 0.0240(2) 0.01710(19) -0.00639(13) 0.00186(13) -0.00127(13) Cu3 0.01648(18) 0.01599(18) 0.01212(18) 0.00203(12) 0.00343(13) 0.00278(13) C1 0.0122(13) 0.0115(12) 0.0100(12) 0.0003(9) 0.0027(10) 0.0010(10) C2 0.0078(12) 0.0176(13) 0.0099(12) 0.0003(10) 0.0017(9) 0.0006(10) C3 0.0119(13) 0.0149(13) 0.0103(13) -0.0004(10) 0.0028(10) -0.0006(10) C4 0.0110(12) 0.0174(13) 0.0093(12) -0.0003(10) 0.0034(10) -0.0013(10) C5 0.0119(13) 0.0130(12) 0.0119(13) -0.0008(10) 0.0046(10) -0.0006(10) C6 0.0102(12) 0.0141(12) 0.0091(12) -0.0009(10) 0.0027(10) -0.0010(10) C7 0.0142(13) 0.0127(13) 0.0153(14) -0.0004(10) 0.0047(11) 0.0014(10) C8 0.0139(13) 0.0185(13) 0.0068(12) -0.0016(10) 0.0003(10) -0.0014(11) C9 0.0173(14) 0.0172(13) 0.0126(13) 0.0003(10) 0.0042(11) -0.0052(11) C10 0.0136(13) 0.0176(14) 0.0169(14) -0.0037(11) 0.0044(11) -0.0018(11) C11 0.0135(13) 0.0110(12) 0.0151(13) -0.0009(10) 0.0036(11) -0.0013(10) C12 0.0139(13) 0.0145(13) 0.0110(12) -0.0024(10) 0.0070(10) 0.0005(10) O1 0.0158(10) 0.0315(11) 0.0149(10) -0.0083(8) 0.0079(8) -0.0064(8) O2 0.0118(10) 0.0342(11) 0.0203(10) -0.0125(9) 0.0052(8) -0.0056(8) O3 0.0134(9) 0.0180(10) 0.0220(10) -0.0009(8) 0.0037(8) -0.0032(8) O4 0.0174(10) 0.0200(10) 0.0214(10) 0.0007(8) 0.0081(8) 0.0038(8) O5 0.0168(10) 0.0355(12) 0.0139(10) -0.0093(8) -0.0002(8) 0.0010(9) O6 0.0163(10) 0.0343(12) 0.0153(10) -0.0073(8) 0.0062(8) -0.0015(9) O7 0.0223(11) 0.0279(11) 0.0178(10) -0.0042(8) 0.0033(9) 0.0092(9) O8 0.0336(12) 0.0256(11) 0.0163(11) 0.0032(8) 0.0049(9) 0.0102(9) O9 0.0136(10) 0.0313(11) 0.0185(10) -0.0016(8) 0.0057(8) -0.0043(8) O10 0.0194(10) 0.0247(10) 0.0113(9) -0.0033(8) 0.0029(8) -0.0082(8) O11 0.0190(10) 0.0161(9) 0.0114(9) 0.0008(7) -0.0020(7) -0.0024(8) O12 0.0179(10) 0.0148(9) 0.0110(9) 0.0003(7) 0.0016(7) -0.0034(7) O1W 0.0117(14) 0.0208(15) 0.0445(19) 0.000 -0.0039(14) 0.000 O2W 0.083(3) 0.0190(16) 0.049(2) 0.000 0.051(2) 0.000 O3W 0.0249(11) 0.0279(11) 0.0237(11) 0.0037(9) 0.0063(9) 0.0077(9) O4W 0.0192(10) 0.0309(12) 0.0238(11) -0.0078(9) -0.0020(8) 0.0054(9) O5W 0.0239(11) 0.0307(12) 0.0253(12) 0.0012(9) 0.0060(9) -0.0018(9) O6W 0.0285(11) 0.0225(10) 0.0179(10) 0.0023(8) 0.0080(9) 0.0056(9) O7W 0.064(2) 0.0391(16) 0.110(3) 0.0117(17) 0.0204(19) 0.0093(15) O8W 0.160(5) 0.237(7) 0.186(6) -0.158(6) 0.115(4) -0.067(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2W 1.937(3) . ? Cu1 O1 1.9449(18) 2_656 ? Cu1 O1 1.9450(18) . ? Cu1 O1W 1.956(3) . ? Cu1 O3W 2.404(2) 2_656 ? Cu1 O3W 2.404(2) . ? Cu2 O3 1.9120(19) . ? Cu2 O2 1.9213(19) . ? Cu2 O5 1.9645(19) 5_656 ? Cu2 O4W 1.965(2) . ? Cu3 O11 1.9329(18) 4_646 ? Cu3 O10 1.9425(18) 4_646 ? Cu3 O12 1.9684(18) . ? Cu3 O6W 1.9900(19) . ? Cu3 O5W 2.342(2) . ? C1 C7 1.516(3) . ? C1 C6 1.546(3) . ? C1 C2 1.554(3) . ? C1 H1 0.9800 . ? C2 C8 1.530(4) . ? C2 C3 1.541(3) . ? C2 H2 0.9800 . ? C3 C9 1.524(4) . ? C3 C4 1.549(3) . ? C3 H3 0.9800 . ? C4 C10 1.514(4) . ? C4 C5 1.538(3) . ? C4 H4 0.9800 . ? C5 C11 1.529(4) . ? C5 C6 1.550(3) . ? C5 H5 0.9800 . ? C6 C12 1.533(3) . ? C6 H6 0.9800 . ? C7 O1 1.242(3) . ? C7 O2 1.265(3) . ? C8 O4 1.242(3) . ? C8 O3 1.277(3) . ? C9 O6 1.260(3) . ? C9 O5 1.262(3) . ? C10 O8 1.208(3) . ? C10 O7 1.327(3) . ? C11 O9 1.245(3) . ? C11 O10 1.277(3) . ? C12 O12 1.254(3) . ? C12 O11 1.261(3) . ? O5 Cu2 1.9643(19) 5_656 ? O7 H7 0.8200 . ? O10 Cu3 1.9424(18) 4_656 ? O11 Cu3 1.9328(18) 4_656 ? O1W H1WA 0.8200 . ? O2W H2WA 0.8200 . ? O3W H3WB 0.8200 . ? O3W H3WA 0.8504 . ? O4W H4WB 0.8200 . ? O4W H4WA 0.8513 . ? O5W H5WB 0.8200 . ? O5W H5WA 0.8518 . ? O6W H6WB 0.8200 . ? O6W H6WA 0.8490 . ? O7W H7WA 0.8534 . ? O7W H7WB 0.8519 . ? O8W H8WA 0.8500 . ? O8W H8WB 0.8501 . ? 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 O2W Cu1 O1 85.81(6) . 2_656 ? O2W Cu1 O1 85.81(6) . . ? O1 Cu1 O1 171.62(12) 2_656 . ? O2W Cu1 O1W 180.000(2) . . ? O1 Cu1 O1W 94.19(6) 2_656 . ? O1 Cu1 O1W 94.19(6) . . ? O2W Cu1 O3W 98.24(5) . 2_656 ? O1 Cu1 O3W 94.96(8) 2_656 2_656 ? O1 Cu1 O3W 86.24(8) . 2_656 ? O1W Cu1 O3W 81.76(5) . 2_656 ? O2W Cu1 O3W 98.24(5) . . ? O1 Cu1 O3W 86.24(8) 2_656 . ? O1 Cu1 O3W 94.96(8) . . ? O1W Cu1 O3W 81.76(5) . . ? O3W Cu1 O3W 163.52(10) 2_656 . ? O3 Cu2 O2 94.16(8) . . ? O3 Cu2 O5 86.19(8) . 5_656 ? O2 Cu2 O5 169.25(9) . 5_656 ? O3 Cu2 O4W 176.72(9) . . ? O2 Cu2 O4W 85.37(8) . . ? O5 Cu2 O4W 94.87(8) 5_656 . ? O11 Cu3 O10 94.44(8) 4_646 4_646 ? O11 Cu3 O12 160.42(8) 4_646 . ? O10 Cu3 O12 96.40(8) 4_646 . ? O11 Cu3 O6W 83.74(8) 4_646 . ? O10 Cu3 O6W 171.32(9) 4_646 . ? O12 Cu3 O6W 87.83(8) . . ? O11 Cu3 O5W 103.42(8) 4_646 . ? O10 Cu3 O5W 87.87(8) 4_646 . ? O12 Cu3 O5W 93.25(8) . . ? O6W Cu3 O5W 84.31(8) . . ? C7 C1 C6 110.5(2) . . ? C7 C1 C2 116.2(2) . . ? C6 C1 C2 116.5(2) . . ? C7 C1 H1 103.9 . . ? C6 C1 H1 103.9 . . ? C2 C1 H1 103.9 . . ? C8 C2 C3 111.3(2) . . ? C8 C2 C1 117.0(2) . . ? C3 C2 C1 108.9(2) . . ? C8 C2 H2 106.4 . . ? C3 C2 H2 106.4 . . ? C1 C2 H2 106.4 . . ? C9 C3 C2 111.5(2) . . ? C9 C3 C4 114.9(2) . . ? C2 C3 C4 115.7(2) . . ? C9 C3 H3 104.4 . . ? C2 C3 H3 104.4 . . ? C4 C3 H3 104.4 . . ? C10 C4 C5 109.4(2) . . ? C10 C4 C3 119.8(2) . . ? C5 C4 C3 109.6(2) . . ? C10 C4 H4 105.7 . . ? C5 C4 H4 105.7 . . ? C3 C4 H4 105.7 . . ? C11 C5 C4 110.7(2) . . ? C11 C5 C6 118.0(2) . . ? C4 C5 C6 114.5(2) . . ? C11 C5 H5 103.9 . . ? C4 C5 H5 103.9 . . ? C6 C5 H5 103.9 . . ? C12 C6 C1 112.1(2) . . ? C12 C6 C5 118.5(2) . . ? C1 C6 C5 108.3(2) . . ? C12 C6 H6 105.6 . . ? C1 C6 H6 105.6 . . ? C5 C6 H6 105.6 . . ? O1 C7 O2 122.6(2) . . ? O1 C7 C1 115.3(2) . . ? O2 C7 C1 121.7(2) . . ? O4 C8 O3 122.2(2) . . ? O4 C8 C2 118.9(2) . . ? O3 C8 C2 118.7(2) . . ? O6 C9 O5 123.4(2) . . ? O6 C9 C3 120.6(2) . . ? O5 C9 C3 115.9(2) . . ? O8 C10 O7 120.1(2) . . ? O8 C10 C4 121.5(2) . . ? O7 C10 C4 117.9(2) . . ? O9 C11 O10 121.9(2) . . ? O9 C11 C5 117.2(2) . . ? O10 C11 C5 120.5(2) . . ? O12 C12 O11 122.0(2) . . ? O12 C12 C6 117.5(2) . . ? O11 C12 C6 120.4(2) . . ? C7 O1 Cu1 131.48(18) . . ? C7 O2 Cu2 138.60(17) . . ? C8 O3 Cu2 126.55(17) . . ? C9 O5 Cu2 129.40(18) . 5_656 ? C10 O7 H7 109.5 . . ? C11 O10 Cu3 138.68(17) . 4_656 ? C12 O11 Cu3 124.69(17) . 4_656 ? C12 O12 Cu3 120.79(17) . . ? Cu1 O1W H1WA 109.5 . . ? Cu1 O2W H2WA 109.5 . . ? Cu1 O3W H3WB 109.5 . . ? Cu1 O3W H3WA 86.7 . . ? H3WB O3W H3WA 105.0 . . ? Cu2 O4W H4WB 109.5 . . ? Cu2 O4W H4WA 121.6 . . ? H4WB O4W H4WA 94.4 . . ? Cu3 O5W H5WB 109.5 . . ? Cu3 O5W H5WA 121.0 . . ? H5WB O5W H5WA 106.0 . . ? Cu3 O6W H6WB 109.5 . . ? Cu3 O6W H6WA 110.8 . . ? H6WB O6W H6WA 108.7 . . ? H7WA O7W H7WB 78.6 . . ? H8WA O8W H8WB 122.7 . . ? 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 O10 0.82 1.93 2.716(2) 161.2 4_646 O1W H1WA O9 0.82 2.66 3.215(2) 126.5 4_646 O2W H2WA O5W 0.82 1.98 2.727(3) 151.2 2_666 O3W H3WB O8 0.82 1.84 2.652(3) 171.4 3_455 O4W H4WB O6 0.82 1.88 2.609(3) 148.2 5_656 O5W H5WB O7W 0.82 2.28 3.057(4) 159.4 1_545 O6W H6WB O4 0.82 1.94 2.752(3) 173.5 . O6W H6WA O3W 0.85 1.88 2.704(3) 163.4 3_545 O3W H3WA O2 0.85 1.96 2.753(3) 154.9 . O3W H3WA O4W 0.85 2.62 3.154(3) 121.7 . O5W H5WA O9 0.85 1.97 2.792(3) 162.1 3_445 O4W H4WA O7 0.85 2.00 2.827(3) 163.7 3_455 O8W H8WB O6 0.85 2.54 3.248(6) 141.5 7_656 O7W H7WB O3 0.85 2.11 2.879(4) 149.1 1_565 O7 H7 O6 0.82 1.72 2.508(3) 161.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.636 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.080 # Attachment 'web_deposit_cif_file_3_xingfeifei_1318817696.4.cif' data_090420b_0m _database_code_depnum_ccdc_archive 'CCDC 848876' #TrackingRef 'web_deposit_cif_file_3_xingfeifei_1318817696.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H14 Ni2 O13' _chemical_formula_weight 435.61 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.2531(12) _cell_length_b 14.2531(12) _cell_length_c 14.554(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2560.5(5) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1563 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.60 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1998 _exptl_absorpt_coefficient_mu 3.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4839 _exptl_absorpt_correction_T_max 0.5499 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4473 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1015 _reflns_number_gt 883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+15.8343P] 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 1015 _refine_ls_number_parameters 110 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.424 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.73286(5) 1.05310(5) 0.89221(5) 0.0139(3) Uani 1 1 d . . . C1 C 0.5012(4) 0.8948(4) 0.8973(3) 0.0118(11) Uani 1 1 d . . . C2 C 0.4155(4) 0.7815(4) 0.9301(4) 0.0108(11) Uani 1 1 d . . . H2 H 0.4154 0.7814 0.9975 0.013 Uiso 1 1 calc R . . C3 C 0.4492(4) 0.6992(4) 0.8969(4) 0.0125(11) Uani 1 1 d . . . H3 H 0.4516 0.6998 0.8296 0.015 Uiso 1 1 calc R . . C4 C 0.5595(4) 0.7243(4) 0.9345(4) 0.0132(11) Uani 1 1 d . . . O1 O 0.5848(3) 0.9440(3) 0.9456(3) 0.0169(9) Uani 1 1 d . . . O2 O 0.4867(3) 0.9308(3) 0.8231(3) 0.0174(8) Uani 1 1 d . . . O3 O 0.6261(3) 0.7177(3) 0.8821(3) 0.0189(9) Uani 1 1 d . . . O4 O 0.5759(3) 0.7455(3) 1.0184(3) 0.0184(9) Uani 1 1 d . . . O1W O 0.8033(3) 1.0060(4) 0.9927(3) 0.0238(10) Uani 1 1 d D . . H1WA H 0.7824 1.0129 1.0434 0.029 Uiso 1 1 calc RD . . H1WB H 0.7919 0.9400 0.9940 0.029 Uiso 1 1 d RD . . O2W O 0.6867(3) 1.1364(3) 0.8033(3) 0.0208(9) Uani 1 1 d . . . H2WA H 0.6801 1.1033 0.7530 0.025 Uiso 1 1 d R . . H2WB H 0.6245 1.1191 0.8244 0.025 Uiso 1 1 d R . . O3W O 0.6113(9) 1.0161(9) 0.7284(8) 0.061(4) Uani 0.50 1 d P . . H3WA H 0.5559 1.0081 0.6994 0.073 Uiso 0.50 1 d PR . . H3WB H 0.6786 1.0417 0.7193 0.073 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0130(4) 0.0127(4) 0.0147(5) 0.0006(3) 0.0010(3) 0.0056(3) C1 0.012(3) 0.010(3) 0.016(3) 0.001(2) 0.004(2) 0.007(2) C2 0.009(2) 0.008(3) 0.015(3) 0.000(2) 0.000(2) 0.004(2) C3 0.012(3) 0.010(3) 0.017(3) -0.001(2) 0.001(2) 0.006(2) C4 0.012(3) 0.007(2) 0.020(3) 0.001(2) -0.001(2) 0.004(2) O1 0.0095(19) 0.017(2) 0.015(2) 0.0023(16) -0.0019(15) -0.0002(16) O2 0.0132(19) 0.020(2) 0.018(2) 0.0053(16) -0.0003(16) 0.0078(17) O3 0.014(2) 0.022(2) 0.021(2) -0.0056(17) 0.0004(16) 0.0096(17) O4 0.020(2) 0.029(2) 0.014(2) -0.0028(17) -0.0027(16) 0.0186(19) O1W 0.027(2) 0.028(2) 0.022(2) 0.0097(18) 0.0079(18) 0.018(2) O2W 0.019(2) 0.024(2) 0.019(2) 0.0013(17) -0.0019(17) 0.0103(18) O3W 0.040(7) 0.064(9) 0.071(10) 0.000(6) -0.004(6) 0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 2.044(4) 11_567 ? Ni1 O1 2.047(4) . ? Ni1 O3 2.061(4) 16_666 ? Ni1 O1W 2.067(4) . ? Ni1 O2W 2.074(4) . ? Ni1 O2 2.081(4) 18_656 ? C1 O1 1.254(6) . ? C1 O2 1.255(6) . ? C1 C2 1.535(7) . ? C2 C3 1.540(7) 2_665 ? C2 C3 1.550(7) . ? C2 H2 0.9800 . ? C3 C4 1.529(7) . ? C3 C2 1.540(7) 3_565 ? C3 H3 0.9800 . ? C4 O4 1.252(6) . ? C4 O3 1.258(6) . ? O2 Ni1 2.080(4) 17_456 ? O3 Ni1 2.061(4) 16_666 ? O4 Ni1 2.045(4) 12_657 ? O1W H1WA 0.8200 . ? O1W H1WB 0.8707 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8501 . ? O3W H2WA 1.1896 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8500 . ? 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 Ni1 O1 90.82(16) 11_567 . ? O4 Ni1 O3 168.53(16) 11_567 16_666 ? O1 Ni1 O3 89.84(15) . 16_666 ? O4 Ni1 O1W 87.35(17) 11_567 . ? O1 Ni1 O1W 88.18(16) . . ? O3 Ni1 O1W 104.12(17) 16_666 . ? O4 Ni1 O2W 81.75(16) 11_567 . ? O1 Ni1 O2W 99.79(16) . . ? O3 Ni1 O2W 86.85(16) 16_666 . ? O1W Ni1 O2W 166.54(17) . . ? O4 Ni1 O2 91.69(15) 11_567 18_656 ? O1 Ni1 O2 173.88(16) . 18_656 ? O3 Ni1 O2 88.80(15) 16_666 18_656 ? O1W Ni1 O2 86.36(16) . 18_656 ? O2W Ni1 O2 86.10(16) . 18_656 ? O1 C1 O2 123.9(5) . . ? O1 C1 C2 116.6(4) . . ? O2 C1 C2 119.4(5) . . ? C1 C2 C3 112.2(4) . 2_665 ? C1 C2 C3 108.4(4) . . ? C3 C2 C3 111.5(5) 2_665 . ? C1 C2 H2 108.2 . . ? C3 C2 H2 108.2 2_665 . ? C3 C2 H2 108.2 . . ? C4 C3 C2 107.0(4) . 3_565 ? C4 C3 C2 112.5(4) . . ? C2 C3 C2 109.9(5) 3_565 . ? C4 C3 H3 109.1 . . ? C2 C3 H3 109.1 3_565 . ? C2 C3 H3 109.1 . . ? O4 C4 O3 123.6(5) . . ? O4 C4 C3 116.9(4) . . ? O3 C4 C3 119.5(5) . . ? C1 O1 Ni1 122.9(3) . . ? C1 O2 Ni1 137.2(4) . 17_456 ? C4 O3 Ni1 130.3(4) . 16_666 ? C4 O4 Ni1 130.9(3) . 12_657 ? Ni1 O1W H1WA 109.5 . . ? Ni1 O1W H1WB 120.5 . . ? H1WA O1W H1WB 103.2 . . ? Ni1 O2W H2WA 101.4 . . ? Ni1 O2W H2WB 101.1 . . ? H2WA O2W H2WB 109.9 . . ? H2WA O3W H3WA 121.0 . . ? H2WA O3W H3WB 55.6 . . ? H3WA O3W H3WB 138.9 . . ? 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 O3W 0.82 1.67 2.136(12) 113.7 5_665 O1W H1WA O3 0.82 2.08 2.790(6) 145.1 11_567 O1W H1WA O2 0.82 2.25 2.788(6) 123.0 5_665 O1W H1WB O1W 0.87 2.00 2.856(4) 168.0 12_657 O2W H2WA O3W 0.85 1.19 1.855(12) 130.1 . O2W H2WA O1 0.85 2.09 2.899(5) 158.4 9_564 O2W H2WB O2W 0.85 2.26 3.086(5) 164.5 17_456 O2W H2WB O2 0.85 2.41 2.906(6) 118.1 . O3W H3WA O4 0.85 1.70 2.357(13) 132.1 9_564 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.685 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.135 # Attachment 'web_deposit_cif_file_4_xingfeifei_1318817696.5.cif' data_090619a_0m _database_code_depnum_ccdc_archive 'CCDC 848877' #TrackingRef 'web_deposit_cif_file_4_xingfeifei_1318817696.5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N2 O15 Zn' _chemical_formula_weight 621.80 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2897(17) _cell_length_b 11.3848(19) _cell_length_c 20.042(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.712(2) _cell_angle_gamma 90.00 _cell_volume 2347.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2397 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 25.43 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8050 _exptl_absorpt_correction_T_max 0.8483 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9420 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4123 _reflns_number_gt 3127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.3976P] 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 4123 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 -0.27479(3) 0.56792(3) 0.110992(18) 0.02113(13) Uani 1 1 d . . . C1 C -0.0414(3) 0.5592(3) 0.16671(18) 0.0271(8) Uani 1 1 d . . . C2 C 0.0932(3) 0.5387(3) 0.19802(15) 0.0204(7) Uani 1 1 d . . . H2 H 0.0988 0.4530 0.2013 0.024 Uiso 1 1 calc R . . C3 C 0.1058(3) 0.5794(3) 0.27092(15) 0.0215(7) Uani 1 1 d . . . H3 H 0.0367 0.5395 0.2954 0.026 Uiso 1 1 calc R . . C4 C 0.2367(3) 0.5324(3) 0.29997(16) 0.0240(7) Uani 1 1 d . . . H4 H 0.2311 0.4469 0.2952 0.029 Uiso 1 1 calc R . . C5 C 0.3561(3) 0.5679(3) 0.25899(15) 0.0210(7) Uani 1 1 d . . . H5 H 0.4274 0.5191 0.2762 0.025 Uiso 1 1 calc R . . C6 C 0.3367(3) 0.5293(3) 0.18600(15) 0.0187(7) Uani 1 1 d . . . H6 H 0.3251 0.4441 0.1893 0.022 Uiso 1 1 calc R . . C7 C 0.2098(3) 0.5712(3) 0.15287(15) 0.0214(7) Uani 1 1 d . . . H7 H 0.1993 0.5226 0.1128 0.026 Uiso 1 1 calc R . . C8 C 0.0799(3) 0.7110(3) 0.27751(17) 0.0266(8) Uani 1 1 d . . . C9 C 0.2542(4) 0.5526(3) 0.37375(17) 0.0305(8) Uani 1 1 d . . . C10 C 0.3964(3) 0.6943(3) 0.27486(16) 0.0254(8) Uani 1 1 d . . . C11 C 0.4538(3) 0.5423(3) 0.14054(17) 0.0229(7) Uani 1 1 d . . . C12 C 0.2190(3) 0.6972(3) 0.12742(16) 0.0258(8) Uani 1 1 d . . . C13 C -0.3111(4) 0.3169(3) 0.05270(17) 0.0324(9) Uani 1 1 d . . . H13 H -0.3317 0.3571 0.0136 0.039 Uiso 1 1 calc R . . C14 C -0.3148(4) 0.1955(3) 0.05183(17) 0.0345(9) Uani 1 1 d . . . H14 H -0.3359 0.1557 0.0126 0.041 Uiso 1 1 calc R . . C15 C -0.2868(3) 0.1333(3) 0.10998(16) 0.0248(8) Uani 1 1 d . . . C16 C -0.2553(3) 0.1989(3) 0.16622(17) 0.0292(8) Uani 1 1 d . . . H16 H -0.2359 0.1614 0.2063 0.035 Uiso 1 1 calc R . . C17 C -0.2527(3) 0.3202(3) 0.16263(17) 0.0289(8) Uani 1 1 d . . . H17 H -0.2314 0.3623 0.2010 0.035 Uiso 1 1 calc R . . C18 C -0.2875(3) 0.0034(3) 0.11247(16) 0.0237(7) Uani 1 1 d . . . C19 C -0.3762(4) -0.0638(3) 0.07680(18) 0.0354(9) Uani 1 1 d . . . H19 H -0.4405 -0.0275 0.0511 0.042 Uiso 1 1 calc R . . C20 C -0.3692(4) -0.1843(3) 0.07943(19) 0.0373(9) Uani 1 1 d . . . H20 H -0.4298 -0.2274 0.0548 0.045 Uiso 1 1 calc R . . C21 C -0.1983(3) -0.1781(3) 0.15146(18) 0.0332(9) Uani 1 1 d . . . H21 H -0.1369 -0.2166 0.1780 0.040 Uiso 1 1 calc R . . C22 C -0.1995(4) -0.0578(3) 0.15157(19) 0.0374(9) Uani 1 1 d . . . H22 H -0.1404 -0.0170 0.1783 0.045 Uiso 1 1 calc R . . N1 N -0.2792(2) 0.3795(2) 0.10692(13) 0.0238(6) Uani 1 1 d . . . N2 N -0.2806(3) -0.2427(2) 0.11529(13) 0.0265(6) Uani 1 1 d . . . O1 O -0.1388(2) 0.5621(2) 0.20204(12) 0.0322(6) Uani 1 1 d . . . O2 O -0.0513(2) 0.5644(2) 0.10329(12) 0.0348(6) Uani 1 1 d . . . O3 O 0.0700(2) 0.7756(2) 0.23016(12) 0.0332(6) Uani 1 1 d . . . O4 O 0.0603(2) 0.7527(2) 0.33853(11) 0.0342(6) Uani 1 1 d . . . H4A H 0.0758 0.7012 0.3661 0.051 Uiso 1 1 calc R . . O5 O 0.1695(3) 0.5850(2) 0.41096(12) 0.0442(7) Uani 1 1 d . . . O6 O 0.3731(3) 0.5259(2) 0.39480(12) 0.0415(7) Uani 1 1 d . . . H6A H 0.3826 0.5471 0.4336 0.062 Uiso 1 1 calc R . . O7 O 0.3380(2) 0.7526(2) 0.31553(11) 0.0322(6) Uani 1 1 d . . . O8 O 0.5026(2) 0.7358(2) 0.24826(12) 0.0349(6) Uani 1 1 d . . . H8 H 0.5314 0.6879 0.2217 0.052 Uiso 1 1 calc R . . O9 O 0.5629(2) 0.56894(19) 0.16910(11) 0.0267(5) Uani 1 1 d . . . O10 O 0.4438(2) 0.5236(2) 0.08021(11) 0.0325(6) Uani 1 1 d . . . O11 O 0.3103(2) 0.7601(2) 0.13943(13) 0.0371(6) Uani 1 1 d . . . O12 O 0.1260(2) 0.7311(2) 0.08514(12) 0.0377(6) Uani 1 1 d . . . H12 H 0.0714 0.6790 0.0816 0.057 Uiso 1 1 calc R . . O1W O -0.2864(2) 0.5862(2) 0.00897(11) 0.0336(6) Uani 1 1 d . . . H1WB H -0.3458 0.5453 -0.0057 0.050 Uiso 1 1 calc R . . H1WA H -0.2239 0.6085 -0.0154 0.050 Uiso 1 1 d R . . O2W O 0.9339(3) 0.6580(2) 0.93970(13) 0.0458(7) Uani 1 1 d . . . O3W O 0.4468(3) 0.6268(3) 0.50488(14) 0.0703(10) Uani 1 1 d . . . H2WA H 0.9748 0.5939 0.9333 0.084 Uiso 1 1 d R . . H3WA H 0.4639 0.6984 0.4966 0.084 Uiso 1 1 d R . . H2WB H 0.9079 0.6578 0.8992 0.084 Uiso 1 1 d R . . H3WB H 0.4926 0.6171 0.5400 0.084 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0195(2) 0.0160(2) 0.0278(2) -0.00049(16) -0.00194(15) 0.00034(16) C1 0.0251(19) 0.0090(17) 0.047(2) -0.0035(15) -0.0084(16) -0.0008(14) C2 0.0168(16) 0.0158(17) 0.0285(18) -0.0020(13) -0.0025(13) 0.0014(13) C3 0.0174(16) 0.0212(18) 0.0260(17) -0.0012(14) 0.0001(13) -0.0037(14) C4 0.0247(18) 0.0179(18) 0.0294(18) -0.0001(14) -0.0026(15) -0.0005(14) C5 0.0176(16) 0.0186(17) 0.0267(17) -0.0012(14) -0.0044(13) 0.0037(14) C6 0.0155(16) 0.0137(16) 0.0267(17) -0.0017(13) -0.0046(13) 0.0000(13) C7 0.0199(17) 0.0180(17) 0.0263(17) -0.0043(14) -0.0033(13) -0.0009(14) C8 0.0177(17) 0.026(2) 0.036(2) -0.0061(16) 0.0011(15) -0.0044(14) C9 0.037(2) 0.025(2) 0.0289(19) 0.0041(15) -0.0011(17) -0.0047(16) C10 0.0195(18) 0.0252(19) 0.0312(19) 0.0009(15) -0.0062(15) -0.0005(14) C11 0.0219(18) 0.0136(17) 0.033(2) 0.0016(14) -0.0025(15) 0.0047(13) C12 0.0260(19) 0.0254(19) 0.0261(19) 0.0009(14) 0.0010(15) 0.0044(16) C13 0.048(2) 0.022(2) 0.0269(19) 0.0023(15) -0.0059(17) 0.0043(17) C14 0.051(2) 0.021(2) 0.031(2) -0.0031(15) -0.0047(17) 0.0006(17) C15 0.0236(18) 0.0174(18) 0.0336(19) 0.0001(15) 0.0016(15) 0.0001(14) C16 0.031(2) 0.027(2) 0.0299(19) 0.0049(15) -0.0073(15) -0.0036(16) C17 0.033(2) 0.024(2) 0.0294(19) -0.0036(15) -0.0026(16) -0.0035(16) C18 0.0252(18) 0.0185(18) 0.0274(18) 0.0006(14) 0.0005(15) 0.0002(14) C19 0.038(2) 0.023(2) 0.045(2) -0.0028(17) -0.0204(18) 0.0062(17) C20 0.040(2) 0.024(2) 0.048(2) -0.0072(17) -0.0192(18) -0.0001(17) C21 0.033(2) 0.0189(19) 0.047(2) -0.0003(16) -0.0154(17) 0.0032(16) C22 0.038(2) 0.021(2) 0.053(2) -0.0036(17) -0.0168(18) -0.0015(17) N1 0.0244(15) 0.0206(15) 0.0265(15) 0.0014(12) 0.0019(12) 0.0019(12) N2 0.0257(15) 0.0212(15) 0.0326(16) 0.0006(13) -0.0021(13) 0.0000(13) O1 0.0168(12) 0.0229(13) 0.0570(16) -0.0059(11) 0.0006(12) -0.0003(10) O2 0.0303(14) 0.0344(15) 0.0393(15) -0.0033(12) -0.0150(11) 0.0019(11) O3 0.0374(15) 0.0212(13) 0.0409(15) -0.0005(11) -0.0044(12) 0.0011(11) O4 0.0329(14) 0.0329(15) 0.0369(14) -0.0107(11) 0.0033(12) 0.0021(12) O5 0.0447(16) 0.061(2) 0.0266(14) 0.0009(13) 0.0068(12) 0.0015(14) O6 0.0430(16) 0.0501(18) 0.0311(14) -0.0016(13) -0.0138(12) 0.0091(13) O7 0.0301(13) 0.0258(14) 0.0408(14) -0.0127(11) 0.0036(11) -0.0023(11) O8 0.0263(13) 0.0342(15) 0.0442(15) -0.0150(12) 0.0045(11) -0.0103(11) O9 0.0151(12) 0.0295(13) 0.0354(13) -0.0067(11) -0.0024(10) -0.0024(10) O10 0.0295(14) 0.0424(15) 0.0257(14) -0.0034(11) -0.0014(11) 0.0009(11) O11 0.0300(14) 0.0211(14) 0.0601(17) 0.0057(12) -0.0047(12) -0.0049(11) O12 0.0374(15) 0.0323(15) 0.0432(15) 0.0124(12) -0.0129(12) 0.0001(12) O1W 0.0372(15) 0.0319(15) 0.0316(13) 0.0007(11) -0.0028(11) -0.0137(12) O2W 0.0576(18) 0.0355(16) 0.0443(16) -0.0028(12) 0.0007(14) 0.0006(13) O3W 0.101(3) 0.051(2) 0.058(2) -0.0020(16) -0.0369(19) -0.0130(18) _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 O9 2.048(2) 1_455 ? Zn1 O1W 2.057(2) . ? Zn1 N1 2.147(3) . ? Zn1 N2 2.159(3) 1_565 ? Zn1 O1 2.287(2) . ? Zn1 O2 2.308(2) . ? C1 O1 1.234(4) . ? C1 O2 1.275(4) . ? C1 C2 1.532(4) . ? C2 C3 1.537(4) . ? C2 C7 1.556(4) . ? C2 H2 0.9800 . ? C3 C8 1.529(5) . ? C3 C4 1.556(4) . ? C3 H3 0.9800 . ? C4 C9 1.505(5) . ? C4 C5 1.540(4) . ? C4 H4 0.9800 . ? C5 C10 1.529(4) . ? C5 C6 1.538(4) . ? C5 H5 0.9800 . ? C6 C11 1.527(4) . ? C6 C7 1.534(4) . ? C6 H6 0.9800 . ? C7 C12 1.525(4) . ? C7 H7 0.9800 . ? C8 O3 1.204(4) . ? C8 O4 1.329(4) . ? C9 O5 1.212(4) . ? C9 O6 1.324(4) . ? C10 O7 1.216(4) . ? C10 O8 1.310(4) . ? C11 O10 1.231(4) . ? C11 O9 1.290(4) . ? C12 O11 1.203(4) . ? C12 O12 1.328(4) . ? C13 N1 1.337(4) . ? C13 C14 1.383(5) . ? C13 H13 0.9300 . ? C14 C15 1.391(5) . ? C14 H14 0.9300 . ? C15 C16 1.388(4) . ? C15 C18 1.480(4) . ? C16 C17 1.382(5) . ? C16 H16 0.9300 . ? C17 N1 1.330(4) . ? C17 H17 0.9300 . ? C18 C22 1.379(5) . ? C18 C19 1.383(5) . ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 N2 1.332(4) . ? C20 H20 0.9300 . ? C21 N2 1.329(4) . ? C21 C22 1.370(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? N2 Zn1 2.159(3) 1_545 ? O4 H4A 0.8200 . ? O6 H6A 0.8200 . ? O8 H8 0.8200 . ? O9 Zn1 2.048(2) 1_655 ? O12 H12 0.8200 . ? O1W H1WB 0.8200 . ? O1W H1WA 0.8511 . ? O2W H2WA 0.8531 . ? O2W H2WB 0.8516 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Zn1 O1W 121.80(9) 1_455 . ? O9 Zn1 N1 90.58(9) 1_455 . ? O1W Zn1 N1 93.56(9) . . ? O9 Zn1 N2 87.04(9) 1_455 1_565 ? O1W Zn1 N2 86.42(10) . 1_565 ? N1 Zn1 N2 177.18(10) . 1_565 ? O9 Zn1 O1 92.39(9) 1_455 . ? O1W Zn1 O1 145.43(9) . . ? N1 Zn1 O1 90.79(9) . . ? N2 Zn1 O1 90.82(9) 1_565 . ? O9 Zn1 O2 149.18(9) 1_455 . ? O1W Zn1 O2 88.91(9) . . ? N1 Zn1 O2 90.06(9) . . ? N2 Zn1 O2 92.75(9) 1_565 . ? O1 Zn1 O2 56.78(8) . . ? O1 C1 O2 121.0(3) . . ? O1 C1 C2 120.3(3) . . ? O2 C1 C2 118.4(3) . . ? C1 C2 C3 114.1(3) . . ? C1 C2 C7 115.2(3) . . ? C3 C2 C7 115.2(2) . . ? C1 C2 H2 103.4 . . ? C3 C2 H2 103.4 . . ? C7 C2 H2 103.4 . . ? C8 C3 C2 111.4(3) . . ? C8 C3 C4 117.1(3) . . ? C2 C3 C4 108.3(2) . . ? C8 C3 H3 106.5 . . ? C2 C3 H3 106.5 . . ? C4 C3 H3 106.5 . . ? C9 C4 C5 113.4(3) . . ? C9 C4 C3 114.1(3) . . ? C5 C4 C3 113.8(3) . . ? C9 C4 H4 104.8 . . ? C5 C4 H4 104.8 . . ? C3 C4 H4 104.8 . . ? C10 C5 C6 119.9(3) . . ? C10 C5 C4 110.6(3) . . ? C6 C5 C4 109.7(2) . . ? C10 C5 H5 105.1 . . ? C6 C5 H5 105.1 . . ? C4 C5 H5 105.1 . . ? C11 C6 C7 112.7(2) . . ? C11 C6 C5 116.5(3) . . ? C7 C6 C5 115.0(2) . . ? C11 C6 H6 103.5 . . ? C7 C6 H6 103.5 . . ? C5 C6 H6 103.5 . . ? C12 C7 C6 112.4(3) . . ? C12 C7 C2 118.0(3) . . ? C6 C7 C2 109.4(2) . . ? C12 C7 H7 105.3 . . ? C6 C7 H7 105.3 . . ? C2 C7 H7 105.3 . . ? O3 C8 O4 119.7(3) . . ? O3 C8 C3 123.0(3) . . ? O4 C8 C3 117.3(3) . . ? O5 C9 O6 122.8(3) . . ? O5 C9 C4 125.0(3) . . ? O6 C9 C4 112.1(3) . . ? O7 C10 O8 119.8(3) . . ? O7 C10 C5 121.2(3) . . ? O8 C10 C5 118.7(3) . . ? O10 C11 O9 122.6(3) . . ? O10 C11 C6 120.8(3) . . ? O9 C11 C6 116.5(3) . . ? O11 C12 O12 120.6(3) . . ? O11 C12 C7 123.0(3) . . ? O12 C12 C7 116.1(3) . . ? N1 C13 C14 123.4(3) . . ? N1 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 116.7(3) . . ? C16 C15 C18 120.8(3) . . ? C14 C15 C18 122.4(3) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? N1 C17 C16 123.2(3) . . ? N1 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C22 C18 C19 116.0(3) . . ? C22 C18 C15 121.4(3) . . ? C19 C18 C15 122.6(3) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N2 C20 C19 123.6(3) . . ? N2 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? N2 C21 C22 123.2(3) . . ? N2 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C18 120.7(3) . . ? C21 C22 H22 119.7 . . ? C18 C22 H22 119.7 . . ? C17 N1 C13 117.2(3) . . ? C17 N1 Zn1 118.1(2) . . ? C13 N1 Zn1 124.6(2) . . ? C21 N2 C20 116.5(3) . . ? C21 N2 Zn1 123.8(2) . 1_545 ? C20 N2 Zn1 119.7(2) . 1_545 ? C1 O1 Zn1 92.1(2) . . ? C1 O2 Zn1 90.1(2) . . ? C8 O4 H4A 109.5 . . ? C9 O6 H6A 109.5 . . ? C10 O8 H8 109.5 . . ? C11 O9 Zn1 117.2(2) . 1_655 ? C12 O12 H12 109.5 . . ? Zn1 O1W H1WB 109.5 . . ? Zn1 O1W H1WA 124.5 . . ? H1WB O1W H1WA 121.9 . . ? H2WA O2W H2WB 90.2 . . ? H3WA O3W H3WB 100.0 . . ? 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 O10 0.82 1.95 2.703(3) 151.2 3_565 O12 H12 O2 0.82 1.87 2.660(3) 161.5 . O8 H8 O9 0.82 1.75 2.557(3) 167.8 . O6 H6A O3W 0.82 1.81 2.593(4) 159.2 . O4 H4A O5 0.82 1.86 2.641(4) 158.2 . O1W H1WA O2W 0.85 1.95 2.795(4) 172.2 1_454 O2W H2WA O2 0.85 2.10 2.939(3) 166.8 3_666 O3W H3WA O2W 0.85 2.02 2.779(4) 149.0 4_575 O3W H3WB O6 0.85 2.49 3.226(4) 144.8 3_666 O3W H3WB O12 0.85 2.38 2.921(4) 122.1 4_676 O2W H2WB O7 0.85 2.08 2.853(4) 150.1 4_676 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.538 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.073 # Attachment 'web_deposit_cif_file_5_xingfeifei_1318817696.6.cif' data_11c _database_code_depnum_ccdc_archive 'CCDC 848878' #TrackingRef 'web_deposit_cif_file_5_xingfeifei_1318817696.6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H35 N7 O16 Zn2' _chemical_formula_weight 1096.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c 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 38.326(3) _cell_length_b 11.3340(10) _cell_length_c 26.909(4) _cell_angle_alpha 90.00 _cell_angle_beta 131.0310(10) _cell_angle_gamma 90.00 _cell_volume 8817.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used 7250 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.93 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7989 _exptl_absorpt_correction_T_max 0.7989 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26940 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10078 _reflns_number_gt 7008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+7.2744P] 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 10078 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.156163(12) 0.40365(3) 0.289462(17) 0.03403(11) Uani 1 1 d . . . Zn2 Zn 0.083055(12) 0.02728(4) -0.034559(17) 0.04038(12) Uani 1 1 d . . . C1 C 0.17432(13) 0.5746(3) 0.3933(2) 0.0536(9) Uani 1 1 d . . . H1 H 0.1682 0.6347 0.3650 0.064 Uiso 1 1 calc R . . C2 C 0.18425(16) 0.6038(4) 0.4512(2) 0.0684(12) Uani 1 1 d . . . H2 H 0.1846 0.6826 0.4610 0.082 Uiso 1 1 calc R . . C3 C 0.19344(15) 0.5201(5) 0.4934(2) 0.0674(12) Uani 1 1 d . . . H3 H 0.2003 0.5406 0.5325 0.081 Uiso 1 1 calc R . . C4 C 0.19260(12) 0.4011(4) 0.47821(17) 0.0520(9) Uani 1 1 d . . . C5 C 0.20277(14) 0.3053(5) 0.5197(2) 0.0660(12) Uani 1 1 d . . . H5 H 0.2102 0.3203 0.5597 0.079 Uiso 1 1 calc R . . C6 C 0.20200(13) 0.1941(5) 0.5029(2) 0.0689(13) Uani 1 1 d . . . H6 H 0.2092 0.1337 0.5317 0.083 Uiso 1 1 calc R . . C7 C 0.19040(12) 0.1647(4) 0.4416(2) 0.0553(10) Uani 1 1 d . . . C8 C 0.19001(15) 0.0512(4) 0.4214(3) 0.0694(13) Uani 1 1 d . . . H8 H 0.1959 -0.0132 0.4474 0.083 Uiso 1 1 calc R . . C9 C 0.18099(16) 0.0341(3) 0.3639(3) 0.0719(13) Uani 1 1 d . . . H9 H 0.1814 -0.0415 0.3508 0.086 Uiso 1 1 calc R . . C10 C 0.17114(14) 0.1318(3) 0.3245(2) 0.0586(10) Uani 1 1 d . . . H10 H 0.1646 0.1195 0.2849 0.070 Uiso 1 1 calc R . . C11 C 0.18074(11) 0.2575(3) 0.39959(16) 0.0399(7) Uani 1 1 d . . . C12 C 0.18196(10) 0.3769(3) 0.41833(15) 0.0377(7) Uani 1 1 d . . . C13 C 0.22337(11) 0.3155(3) 0.28047(15) 0.0343(7) Uani 1 1 d . . . C14 C 0.23221(9) 0.2350(2) 0.24421(13) 0.0275(6) Uani 1 1 d . . . H14 H 0.2362 0.1569 0.2629 0.033 Uiso 1 1 calc R . . C15 C 0.19146(9) 0.2182(2) 0.17028(13) 0.0261(6) Uani 1 1 d . . . H15 H 0.1660 0.1879 0.1668 0.031 Uiso 1 1 calc R . . C16 C 0.20331(9) 0.1187(2) 0.14446(13) 0.0258(6) Uani 1 1 d . . . H16 H 0.2077 0.0495 0.1699 0.031 Uiso 1 1 calc R . . C17 C 0.24993(9) 0.1308(2) 0.16077(13) 0.0267(6) Uani 1 1 d . . . H17 H 0.2565 0.0521 0.1535 0.032 Uiso 1 1 calc R . . C18 C 0.28866(9) 0.1546(2) 0.23507(13) 0.0283(6) Uani 1 1 d . . . H18 H 0.2881 0.0847 0.2560 0.034 Uiso 1 1 calc R . . C19 C 0.27861(10) 0.2579(2) 0.26194(13) 0.0301(6) Uani 1 1 d . . . H19 H 0.3021 0.2519 0.3100 0.036 Uiso 1 1 calc R . . C20 C 0.28177(11) 0.3841(3) 0.24536(16) 0.0354(7) Uani 1 1 d . . . C21 C 0.33691(10) 0.1526(3) 0.25751(15) 0.0374(7) Uani 1 1 d . . . C22 C 0.25295(11) 0.2136(3) 0.11938(16) 0.0366(7) Uani 1 1 d . . . C23 C 0.16138(10) 0.0867(3) 0.07395(14) 0.0334(7) Uani 1 1 d . . . C24 C 0.17203(10) 0.3254(3) 0.12480(15) 0.0334(7) Uani 1 1 d . . . C25 C 0.07266(15) 0.3023(4) -0.0601(2) 0.0689(12) Uani 1 1 d . . . H25 H 0.0765 0.3087 -0.0224 0.083 Uiso 1 1 calc R . . C26 C 0.06660(19) 0.4058(5) -0.0930(3) 0.0908(16) Uani 1 1 d . . . H26 H 0.0652 0.4787 -0.0785 0.109 Uiso 1 1 calc R . . C27 C 0.0628(2) 0.3975(6) -0.1461(3) 0.105(2) Uani 1 1 d . . . H27 H 0.0592 0.4656 -0.1683 0.126 Uiso 1 1 calc R . . C28 C 0.06398(17) 0.2893(6) -0.1684(2) 0.0887(17) Uani 1 1 d . . . C29 C 0.06895(12) 0.1876(4) -0.13286(19) 0.0610(11) Uani 1 1 d . . . C30 C 0.0620(3) 0.2677(9) -0.2221(4) 0.139(3) Uani 1 1 d . . . H30 H 0.0618 0.3320 -0.2437 0.167 Uiso 1 1 calc R . . C31 C 0.0604(2) 0.1592(9) -0.2433(3) 0.129(3) Uani 1 1 d . . . H31 H 0.0575 0.1509 -0.2802 0.155 Uiso 1 1 calc R . . C32 C 0.06289(17) 0.0546(7) -0.2103(2) 0.0957(19) Uani 1 1 d . . . C33 C 0.0598(2) -0.0616(8) -0.2307(3) 0.108(2) Uani 1 1 d . . . H33 H 0.0555 -0.0755 -0.2685 0.129 Uiso 1 1 calc R . . C34 C 0.06317(19) -0.1542(7) -0.1956(3) 0.103(2) Uani 1 1 d . . . H34 H 0.0609 -0.2312 -0.2094 0.124 Uiso 1 1 calc R . . C35 C 0.07006(14) -0.1322(5) -0.1386(2) 0.0765(14) Uani 1 1 d . . . H35 H 0.0729 -0.1955 -0.1142 0.092 Uiso 1 1 calc R . . C36 C 0.06843(13) 0.0715(5) -0.15414(18) 0.0651(12) Uani 1 1 d . . . C37 C 0.12292(12) -0.2219(3) 0.03660(18) 0.0495(9) Uani 1 1 d . . . H37 H 0.1513 -0.1977 0.0504 0.059 Uiso 1 1 calc R . . C38 C 0.11966(13) -0.3330(4) 0.0547(2) 0.0591(10) Uani 1 1 d . . . H38 H 0.1453 -0.3825 0.0796 0.071 Uiso 1 1 calc R . . C39 C 0.07841(15) -0.3692(4) 0.0357(2) 0.0623(11) Uani 1 1 d . . . H39 H 0.0757 -0.4436 0.0474 0.075 Uiso 1 1 calc R . . C40 C 0.04035(12) -0.2929(3) -0.00141(18) 0.0489(8) Uani 1 1 d . . . C41 C -0.00445(15) -0.3199(4) -0.0233(2) 0.0743(13) Uani 1 1 d . . . H41 H -0.0094 -0.3936 -0.0137 0.089 Uiso 1 1 calc R . . C42 C -0.03951(14) -0.2416(4) -0.0573(2) 0.0680(12) Uani 1 1 d . . . H42 H -0.0680 -0.2623 -0.0705 0.082 Uiso 1 1 calc R . . C43 C -0.03374(11) -0.1288(3) -0.07324(17) 0.0459(8) Uani 1 1 d . . . C44 C -0.06818(12) -0.0413(4) -0.10515(18) 0.0564(10) Uani 1 1 d . . . H44 H -0.0974 -0.0580 -0.1200 0.068 Uiso 1 1 calc R . . C45 C -0.05853(12) 0.0674(4) -0.11413(18) 0.0568(10) Uani 1 1 d . . . H45 H -0.0809 0.1262 -0.1345 0.068 Uiso 1 1 calc R . . C46 C -0.01482(11) 0.0906(3) -0.09271(16) 0.0473(8) Uani 1 1 d . . . H46 H -0.0084 0.1659 -0.0986 0.057 Uiso 1 1 calc R . . C47 C 0.00896(10) -0.0988(3) -0.05357(15) 0.0385(7) Uani 1 1 d . . . C48 C 0.04644(10) -0.1828(3) -0.01805(15) 0.0380(7) Uani 1 1 d . . . N1 N 0.17089(9) 0.2411(2) 0.34181(14) 0.0414(6) Uani 1 1 d . . . N2 N 0.17318(9) 0.4630(2) 0.37662(13) 0.0383(6) Uani 1 1 d . . . N3 N 0.05843(16) 0.3657(5) 0.2057(2) 0.0906(14) Uani 1 1 d . . . N4 N 0.01787(8) 0.0093(2) -0.06437(12) 0.0392(6) Uani 1 1 d . . . N5 N 0.08698(9) -0.1483(2) 0.00008(13) 0.0409(6) Uani 1 1 d . . . N6 N 0.07271(10) -0.0227(3) -0.11833(15) 0.0582(9) Uani 1 1 d . . . N7 N 0.07334(10) 0.1956(3) -0.07938(14) 0.0539(8) Uani 1 1 d . . . O1 O 0.18039(8) 0.3442(2) 0.24779(11) 0.0438(5) Uani 1 1 d . . . O2 O 0.25492(8) 0.3426(2) 0.33775(11) 0.0468(6) Uani 1 1 d . . . O3 O 0.24935(8) 0.45064(18) 0.21596(12) 0.0434(5) Uani 1 1 d . . . O4 O 0.32283(8) 0.4215(2) 0.26963(15) 0.0586(7) Uani 1 1 d . . . H4 H 0.3406 0.3654 0.2845 0.070 Uiso 1 1 calc R . . O5 O 0.36627(8) 0.2268(2) 0.29929(13) 0.0620(8) Uani 1 1 d . . . O6 O 0.34668(8) 0.07345(19) 0.23624(12) 0.0454(6) Uani 1 1 d . . . O7 O 0.27986(9) 0.2943(2) 0.14233(13) 0.0531(6) Uani 1 1 d . . . O8 O 0.22735(8) 0.1857(2) 0.05629(11) 0.0486(6) Uani 1 1 d . . . H8A H 0.2073 0.1384 0.0459 0.058 Uiso 1 1 calc R . . O9 O 0.16555(7) 0.0445(2) 0.03501(10) 0.0441(5) Uani 1 1 d . . . O10 O 0.12241(7) 0.0979(2) 0.05754(10) 0.0420(5) Uani 1 1 d . . . O11 O 0.17313(8) 0.33664(19) 0.08167(10) 0.0425(5) Uani 1 1 d . . . O12 O 0.14857(8) 0.4023(2) 0.13082(12) 0.0447(6) Uani 1 1 d . . . H12 H 0.1529 0.3875 0.1644 0.054 Uiso 1 1 calc R . . O13 O 0.09034(13) 0.3511(5) 0.20899(19) 0.1320(18) Uani 1 1 d . . . O14 O 0.01895(12) 0.3358(5) 0.16483(18) 0.1290(17) Uani 1 1 d . . . O15 O 0.0701(2) 0.4265(6) 0.2526(3) 0.186(3) Uani 1 1 d . . . O1W O 0.45695(12) 0.1289(4) 0.3663(2) 0.1210(16) Uani 1 1 d . . . H1A H 0.4286 0.1440 0.3455 0.145 Uiso 1 1 d R . . H1B H 0.4547 0.0679 0.3460 0.145 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0405(2) 0.0314(2) 0.0377(2) 0.00049(15) 0.02893(17) 0.00197(15) Zn2 0.03461(19) 0.0451(2) 0.0325(2) -0.00530(16) 0.01821(16) -0.00630(17) C1 0.068(2) 0.037(2) 0.071(3) -0.0121(18) 0.052(2) -0.0073(18) C2 0.082(3) 0.062(3) 0.082(3) -0.034(2) 0.063(3) -0.016(2) C3 0.069(3) 0.093(4) 0.057(3) -0.030(2) 0.049(2) -0.020(2) C4 0.0428(19) 0.082(3) 0.0397(19) -0.0053(19) 0.0308(16) -0.0097(19) C5 0.061(2) 0.098(4) 0.047(2) 0.005(2) 0.039(2) -0.010(2) C6 0.053(2) 0.103(4) 0.056(2) 0.037(3) 0.038(2) 0.008(2) C7 0.0441(19) 0.055(2) 0.070(3) 0.025(2) 0.0388(19) 0.0088(18) C8 0.067(3) 0.050(3) 0.101(4) 0.034(2) 0.060(3) 0.018(2) C9 0.081(3) 0.028(2) 0.125(4) 0.009(2) 0.076(3) 0.011(2) C10 0.073(3) 0.034(2) 0.087(3) -0.0029(19) 0.061(2) 0.0052(18) C11 0.0372(16) 0.0409(19) 0.0450(18) 0.0098(15) 0.0286(15) 0.0039(14) C12 0.0331(15) 0.048(2) 0.0352(16) 0.0010(14) 0.0239(14) -0.0014(14) C13 0.0535(19) 0.0216(15) 0.0370(17) 0.0023(12) 0.0337(16) 0.0017(14) C14 0.0353(14) 0.0210(14) 0.0260(14) 0.0022(11) 0.0201(12) 0.0023(12) C15 0.0309(14) 0.0218(14) 0.0269(14) 0.0001(11) 0.0195(12) -0.0010(11) C16 0.0315(14) 0.0182(13) 0.0238(13) -0.0005(10) 0.0165(12) -0.0034(11) C17 0.0310(14) 0.0191(13) 0.0281(14) -0.0020(11) 0.0186(12) -0.0006(11) C18 0.0319(14) 0.0218(14) 0.0299(14) -0.0034(11) 0.0197(12) -0.0023(11) C19 0.0328(14) 0.0254(15) 0.0267(14) -0.0065(11) 0.0171(12) -0.0021(12) C20 0.0424(17) 0.0240(16) 0.0431(17) -0.0152(13) 0.0295(15) -0.0117(14) C21 0.0345(16) 0.0308(17) 0.0401(17) -0.0043(14) 0.0215(14) -0.0022(13) C22 0.0439(17) 0.0297(16) 0.0440(18) 0.0039(14) 0.0323(15) 0.0026(14) C23 0.0372(16) 0.0238(15) 0.0293(15) -0.0009(12) 0.0175(13) -0.0038(12) C24 0.0345(15) 0.0279(16) 0.0350(16) 0.0017(13) 0.0216(13) -0.0002(13) C25 0.066(3) 0.063(3) 0.065(3) 0.007(2) 0.037(2) -0.006(2) C26 0.096(4) 0.072(3) 0.090(4) 0.013(3) 0.055(3) -0.006(3) C27 0.112(5) 0.084(4) 0.101(5) 0.023(4) 0.062(4) -0.014(4) C28 0.075(3) 0.129(5) 0.055(3) 0.022(3) 0.040(3) -0.013(3) C29 0.0416(19) 0.086(3) 0.041(2) 0.005(2) 0.0213(17) -0.009(2) C30 0.130(6) 0.190(9) 0.088(5) 0.039(5) 0.068(5) -0.012(6) C31 0.121(5) 0.214(9) 0.059(4) 0.015(5) 0.062(4) -0.014(6) C32 0.069(3) 0.172(6) 0.048(3) -0.007(3) 0.039(2) -0.007(3) C33 0.087(4) 0.179(7) 0.061(3) -0.035(4) 0.050(3) -0.008(4) C34 0.083(4) 0.143(6) 0.077(4) -0.044(4) 0.050(3) -0.006(4) C35 0.059(3) 0.102(4) 0.055(3) -0.027(3) 0.032(2) -0.007(3) C36 0.0394(19) 0.112(4) 0.036(2) -0.001(2) 0.0208(16) -0.007(2) C37 0.0373(17) 0.048(2) 0.055(2) -0.0007(17) 0.0263(16) 0.0067(16) C38 0.052(2) 0.049(2) 0.062(2) 0.0075(19) 0.0312(19) 0.0160(19) C39 0.070(3) 0.040(2) 0.066(3) 0.0082(19) 0.040(2) 0.0028(19) C40 0.0474(19) 0.040(2) 0.053(2) 0.0002(16) 0.0301(17) -0.0039(16) C41 0.070(3) 0.052(3) 0.087(3) 0.006(2) 0.046(3) -0.013(2) C42 0.050(2) 0.073(3) 0.076(3) 0.007(2) 0.039(2) -0.006(2) C43 0.0354(17) 0.056(2) 0.0426(19) 0.0037(16) 0.0238(15) -0.0010(16) C44 0.0336(17) 0.078(3) 0.051(2) 0.011(2) 0.0245(16) 0.0042(19) C45 0.0378(18) 0.064(3) 0.054(2) 0.0169(19) 0.0243(17) 0.0186(18) C46 0.0406(18) 0.045(2) 0.0446(19) 0.0100(16) 0.0230(16) 0.0094(16) C47 0.0357(16) 0.0418(19) 0.0310(16) -0.0009(14) 0.0189(13) -0.0013(14) C48 0.0357(16) 0.0389(18) 0.0334(16) -0.0047(13) 0.0201(14) -0.0011(14) N1 0.0503(16) 0.0309(14) 0.0544(17) -0.0006(13) 0.0392(14) 0.0030(12) N2 0.0460(15) 0.0349(15) 0.0431(15) -0.0028(12) 0.0332(13) -0.0001(12) N3 0.073(3) 0.118(4) 0.072(3) 0.025(3) 0.044(3) 0.003(3) N4 0.0310(13) 0.0451(16) 0.0317(14) 0.0016(12) 0.0163(11) 0.0006(12) N5 0.0348(14) 0.0394(16) 0.0422(15) -0.0045(12) 0.0226(12) 0.0002(12) N6 0.0413(16) 0.085(3) 0.0409(17) -0.0185(17) 0.0238(14) -0.0094(16) N7 0.0459(17) 0.060(2) 0.0419(17) 0.0016(15) 0.0229(14) -0.0073(15) O1 0.0516(14) 0.0481(14) 0.0450(13) 0.0036(11) 0.0375(12) 0.0119(11) O2 0.0644(15) 0.0386(13) 0.0368(13) -0.0103(10) 0.0330(12) -0.0022(11) O3 0.0542(14) 0.0215(11) 0.0586(14) -0.0052(10) 0.0388(12) -0.0032(10) O4 0.0478(14) 0.0327(13) 0.088(2) -0.0209(13) 0.0413(15) -0.0183(11) O5 0.0347(12) 0.0539(16) 0.0755(18) -0.0342(14) 0.0267(12) -0.0123(12) O6 0.0452(13) 0.0358(13) 0.0662(16) -0.0125(11) 0.0412(12) -0.0042(10) O7 0.0649(16) 0.0393(14) 0.0685(16) 0.0001(12) 0.0495(14) -0.0142(12) O8 0.0582(15) 0.0569(17) 0.0400(13) 0.0040(11) 0.0362(12) -0.0023(12) O9 0.0420(12) 0.0468(14) 0.0304(11) -0.0126(10) 0.0181(10) -0.0013(11) O10 0.0315(11) 0.0514(14) 0.0335(11) -0.0064(10) 0.0171(9) -0.0084(10) O11 0.0565(14) 0.0377(13) 0.0383(12) 0.0096(10) 0.0333(11) 0.0056(11) O12 0.0532(14) 0.0378(13) 0.0493(14) 0.0130(11) 0.0363(12) 0.0189(11) O13 0.057(2) 0.233(6) 0.085(3) 0.014(3) 0.038(2) -0.001(3) O14 0.050(2) 0.220(5) 0.078(2) -0.020(3) 0.0245(18) -0.031(3) O15 0.173(5) 0.163(5) 0.170(6) -0.087(5) 0.089(5) -0.050(4) O1W 0.069(2) 0.128(3) 0.121(3) -0.052(3) 0.043(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.985(2) . ? Zn1 O6 2.024(2) 4 ? Zn1 O13 2.058(4) . ? Zn1 N2 2.091(3) . ? Zn1 N1 2.157(3) . ? Zn2 O10 2.037(2) . ? Zn2 N4 2.072(3) . ? Zn2 N6 2.094(3) . ? Zn2 N7 2.155(3) . ? Zn2 N5 2.160(3) . ? Zn2 O9 2.402(2) . ? C1 N2 1.332(4) . ? C1 C2 1.381(5) . ? C1 H1 0.9300 . ? C2 C3 1.336(6) . ? C2 H2 0.9300 . ? C3 C4 1.403(6) . ? C3 H3 0.9300 . ? C4 C12 1.405(4) . ? C4 C5 1.418(6) . ? C5 C6 1.333(6) . ? C5 H5 0.9300 . ? C6 C7 1.439(6) . ? C6 H6 0.9300 . ? C7 C8 1.392(6) . ? C7 C11 1.403(5) . ? C8 C9 1.362(7) . ? C8 H8 0.9300 . ? C9 C10 1.403(6) . ? C9 H9 0.9300 . ? C10 N1 1.326(4) . ? C10 H10 0.9300 . ? C11 N1 1.350(4) . ? C11 C12 1.434(5) . ? C12 N2 1.353(4) . ? C13 O2 1.219(4) . ? C13 O1 1.300(4) . ? C13 C14 1.527(4) . ? C14 C19 1.531(4) . ? C14 C15 1.534(4) . ? C14 H14 0.9800 . ? C15 C24 1.527(4) . ? C15 C16 1.541(4) . ? C15 H15 0.9800 . ? C16 C23 1.520(4) . ? C16 C17 1.541(4) . ? C16 H16 0.9800 . ? C17 C22 1.518(4) . ? C17 C18 1.542(4) . ? C17 H17 0.9800 . ? C18 C21 1.523(4) . ? C18 C19 1.551(4) . ? C18 H18 0.9800 . ? C19 C20 1.527(4) . ? C19 H19 0.9800 . ? C20 O3 1.203(4) . ? C20 O4 1.317(4) . ? C21 O6 1.246(4) . ? C21 O5 1.256(4) . ? C22 O7 1.202(4) . ? C22 O8 1.326(4) . ? C23 O9 1.254(4) . ? C23 O10 1.255(4) . ? C24 O11 1.195(4) . ? C24 O12 1.336(4) . ? C25 N7 1.323(5) . ? C25 C26 1.393(6) . ? C25 H25 0.9300 . ? C26 C27 1.341(8) . ? C26 H26 0.9300 . ? C27 C28 1.379(8) . ? C27 H27 0.9300 . ? C28 C30 1.417(9) . ? C28 C29 1.428(7) . ? C29 N7 1.338(5) . ? C29 C36 1.429(6) . ? C30 C31 1.340(10) . ? C30 H30 0.9300 . ? C31 C32 1.446(10) . ? C31 H31 0.9300 . ? C32 C36 1.393(6) . ? C32 C33 1.402(9) . ? C33 C34 1.359(9) . ? C33 H33 0.9300 . ? C34 C35 1.399(7) . ? C34 H34 0.9300 . ? C35 N6 1.331(6) . ? C35 H35 0.9300 . ? C36 N6 1.374(6) . ? C37 N5 1.335(4) . ? C37 C38 1.385(5) . ? C37 H37 0.9300 . ? C38 C39 1.366(6) . ? C38 H38 0.9300 . ? C39 C40 1.399(5) . ? C39 H39 0.9300 . ? C40 C48 1.396(5) . ? C40 C41 1.436(5) . ? C41 C42 1.347(6) . ? C41 H41 0.9300 . ? C42 C43 1.412(6) . ? C42 H42 0.9300 . ? C43 C47 1.391(4) . ? C43 C44 1.405(5) . ? C44 C45 1.353(6) . ? C44 H44 0.9300 . ? C45 C46 1.393(5) . ? C45 H45 0.9300 . ? C46 N4 1.321(4) . ? C46 H46 0.9300 . ? C47 N4 1.355(4) . ? C47 C48 1.442(4) . ? C48 N5 1.346(4) . ? N3 O13 1.178(5) . ? N3 O14 1.195(5) . ? N3 O15 1.235(7) . ? O4 H4 0.8200 . ? O6 Zn1 2.024(2) 4_545 ? O8 H8A 0.8200 . ? O12 H12 0.8200 . ? O1W H1A 0.8502 . ? O1W H1B 0.8501 . ? 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 Zn1 O6 94.01(10) . 4 ? O1 Zn1 O13 90.70(15) . . ? O6 Zn1 O13 99.32(16) 4 . ? O1 Zn1 N2 145.67(10) . . ? O6 Zn1 N2 89.11(10) 4 . ? O13 Zn1 N2 122.53(15) . . ? O1 Zn1 N1 93.44(10) . . ? O6 Zn1 N1 165.41(10) 4 . ? O13 Zn1 N1 93.11(16) . . ? N2 Zn1 N1 77.72(10) . . ? O10 Zn2 N4 104.55(10) . . ? O10 Zn2 N6 151.83(11) . . ? N4 Zn2 N6 103.21(11) . . ? O10 Zn2 N7 92.91(11) . . ? N4 Zn2 N7 98.55(11) . . ? N6 Zn2 N7 78.24(14) . . ? O10 Zn2 N5 92.92(10) . . ? N4 Zn2 N5 78.55(10) . . ? N6 Zn2 N5 97.20(13) . . ? N7 Zn2 N5 173.99(11) . . ? O10 Zn2 O9 58.35(8) . . ? N4 Zn2 O9 160.97(9) . . ? N6 Zn2 O9 94.77(10) . . ? N7 Zn2 O9 91.12(10) . . ? N5 Zn2 O9 93.18(9) . . ? N2 C1 C2 122.0(4) . . ? N2 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.8(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.5(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C12 117.1(4) . . ? C3 C4 C5 124.4(4) . . ? C12 C4 C5 118.5(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.0(4) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C11 116.7(4) . . ? C8 C7 C6 125.2(4) . . ? C11 C7 C6 118.0(4) . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N1 C10 C9 122.1(4) . . ? N1 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N1 C11 C7 123.3(3) . . ? N1 C11 C12 117.1(3) . . ? C7 C11 C12 119.6(3) . . ? N2 C12 C4 122.5(3) . . ? N2 C12 C11 117.1(3) . . ? C4 C12 C11 120.4(3) . . ? O2 C13 O1 123.8(3) . . ? O2 C13 C14 120.4(3) . . ? O1 C13 C14 115.5(3) . . ? C13 C14 C19 113.5(2) . . ? C13 C14 C15 116.0(2) . . ? C19 C14 C15 114.2(2) . . ? C13 C14 H14 103.7 . . ? C19 C14 H14 103.7 . . ? C15 C14 H14 103.7 . . ? C24 C15 C14 119.1(2) . . ? C24 C15 C16 110.7(2) . . ? C14 C15 C16 109.0(2) . . ? C24 C15 H15 105.7 . . ? C14 C15 H15 105.7 . . ? C16 C15 H15 105.7 . . ? C23 C16 C17 117.1(2) . . ? C23 C16 C15 110.7(2) . . ? C17 C16 C15 115.9(2) . . ? C23 C16 H16 103.7 . . ? C17 C16 H16 103.7 . . ? C15 C16 H16 103.7 . . ? C22 C17 C16 118.6(2) . . ? C22 C17 C18 111.8(2) . . ? C16 C17 C18 109.5(2) . . ? C22 C17 H17 105.3 . . ? C16 C17 H17 105.3 . . ? C18 C17 H17 105.3 . . ? C21 C18 C17 113.3(2) . . ? C21 C18 C19 115.8(2) . . ? C17 C18 C19 114.5(2) . . ? C21 C18 H18 103.7 . . ? C17 C18 H18 103.7 . . ? C19 C18 H18 103.7 . . ? C20 C19 C14 111.5(2) . . ? C20 C19 C18 118.6(2) . . ? C14 C19 C18 108.7(2) . . ? C20 C19 H19 105.7 . . ? C14 C19 H19 105.7 . . ? C18 C19 H19 105.7 . . ? O3 C20 O4 120.4(3) . . ? O3 C20 C19 122.2(3) . . ? O4 C20 C19 117.1(3) . . ? O6 C21 O5 122.0(3) . . ? O6 C21 C18 118.8(3) . . ? O5 C21 C18 119.1(3) . . ? O7 C22 O8 120.3(3) . . ? O7 C22 C17 123.1(3) . . ? O8 C22 C17 116.3(3) . . ? O9 C23 O10 121.3(3) . . ? O9 C23 C16 121.6(3) . . ? O10 C23 C16 117.0(3) . . ? O11 C24 O12 120.2(3) . . ? O11 C24 C15 123.6(3) . . ? O12 C24 C15 115.8(3) . . ? N7 C25 C26 124.0(5) . . ? N7 C25 H25 118.0 . . ? C26 C25 H25 118.0 . . ? C27 C26 C25 118.2(6) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C26 C27 C28 121.0(5) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C30 127.0(6) . . ? C27 C28 C29 117.1(5) . . ? C30 C28 C29 115.9(6) . . ? N7 C29 C28 122.2(5) . . ? N7 C29 C36 116.9(4) . . ? C28 C29 C36 120.9(4) . . ? C31 C30 C28 123.3(7) . . ? C31 C30 H30 118.4 . . ? C28 C30 H30 118.4 . . ? C30 C31 C32 121.7(6) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C36 C32 C33 118.0(6) . . ? C36 C32 C31 117.0(6) . . ? C33 C32 C31 125.1(6) . . ? C34 C33 C32 120.5(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.2(6) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N6 C35 C34 121.6(6) . . ? N6 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? N6 C36 C32 121.0(5) . . ? N6 C36 C29 118.1(4) . . ? C32 C36 C29 120.9(5) . . ? N5 C37 C38 122.6(3) . . ? N5 C37 H37 118.7 . . ? C38 C37 H37 118.7 . . ? C39 C38 C37 119.4(3) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 119.3(4) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C48 C40 C39 117.8(3) . . ? C48 C40 C41 117.7(3) . . ? C39 C40 C41 124.5(4) . . ? C42 C41 C40 122.0(4) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C41 C42 C43 121.2(4) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C47 C43 C44 117.3(3) . . ? C47 C43 C42 119.0(3) . . ? C44 C43 C42 123.6(3) . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 119.6(3) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? N4 C46 C45 122.3(3) . . ? N4 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? N4 C47 C43 122.6(3) . . ? N4 C47 C48 117.2(3) . . ? C43 C47 C48 120.1(3) . . ? N5 C48 C40 122.7(3) . . ? N5 C48 C47 117.3(3) . . ? C40 C48 C47 119.9(3) . . ? C10 N1 C11 118.2(3) . . ? C10 N1 Zn1 128.8(3) . . ? C11 N1 Zn1 112.9(2) . . ? C1 N2 C12 118.1(3) . . ? C1 N2 Zn1 126.9(2) . . ? C12 N2 Zn1 115.0(2) . . ? O13 N3 O14 130.8(6) . . ? O13 N3 O15 109.8(6) . . ? O14 N3 O15 119.3(6) . . ? C46 N4 C47 118.5(3) . . ? C46 N4 Zn2 126.9(2) . . ? C47 N4 Zn2 114.6(2) . . ? C37 N5 C48 118.2(3) . . ? C37 N5 Zn2 129.8(2) . . ? C48 N5 Zn2 112.0(2) . . ? C35 N6 C36 119.7(4) . . ? C35 N6 Zn2 127.0(3) . . ? C36 N6 Zn2 113.3(3) . . ? C25 N7 C29 117.5(4) . . ? C25 N7 Zn2 129.1(3) . . ? C29 N7 Zn2 113.3(3) . . ? C13 O1 Zn1 123.88(19) . . ? C20 O4 H4 109.5 . . ? C21 O6 Zn1 151.2(2) . 4_545 ? C22 O8 H8A 109.5 . . ? C23 O9 Zn2 81.81(17) . . ? C23 O10 Zn2 98.51(18) . . ? C24 O12 H12 109.5 . . ? N3 O13 Zn1 122.2(4) . . ? H1A O1W H1B 101.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.007 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.076 # Attachment 'web_deposit_cif_file_6_xingfeifei_1318817696.7.cif' data_090319c _database_code_depnum_ccdc_archive 'CCDC 848879' #TrackingRef 'web_deposit_cif_file_6_xingfeifei_1318817696.7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H54 Cd2 N6 O29' _chemical_formula_weight 1475.83 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.700(5) _cell_length_b 11.623(3) _cell_length_c 29.216(6) _cell_angle_alpha 90.00 _cell_angle_beta 118.682(13) _cell_angle_gamma 90.00 _cell_volume 6167(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5322 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.32 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8591 _exptl_absorpt_correction_T_max 0.9258 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30543 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.05 _reflns_number_total 10875 _reflns_number_gt 6266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+57.3644P] 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 10875 _refine_ls_number_parameters 828 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2763 _refine_ls_wR_factor_gt 0.2369 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 Cd1 Cd 0.80066(3) 0.54964(6) 0.84057(3) 0.0403(2) Uani 1 1 d . . . Cd2 Cd 0.30489(4) 0.55553(7) 0.83910(3) 0.0424(2) Uani 1 1 d . . . C1 C 0.6476(5) 0.5517(7) 0.7986(4) 0.034(2) Uani 1 1 d . . . C2 C 0.5642(4) 0.5721(8) 0.7677(3) 0.0302(19) Uani 1 1 d . . . H2 H 0.5594 0.6560 0.7654 0.036 Uiso 1 1 calc R . . C3 C 0.5268(5) 0.5321(7) 0.7098(3) 0.0304(19) Uani 1 1 d . . . H3 H 0.5514 0.5755 0.6937 0.036 Uiso 1 1 calc R . . C4 C 0.4467(5) 0.5739(7) 0.6823(3) 0.032(2) Uani 1 1 d . . . H4 H 0.4508 0.6578 0.6855 0.038 Uiso 1 1 calc R . . C5 C 0.4007(4) 0.5404(7) 0.7099(3) 0.0274(18) Uani 1 1 d . . . H5 H 0.3563 0.5881 0.6936 0.033 Uiso 1 1 calc R . . C6 C 0.4427(4) 0.5788(8) 0.7670(3) 0.0311(19) Uani 1 1 d . . . H6 H 0.4468 0.6625 0.7652 0.037 Uiso 1 1 calc R . . C7 C 0.5235(4) 0.5365(7) 0.7977(3) 0.0273(18) Uani 1 1 d . . . H7 H 0.5460 0.5817 0.8300 0.033 Uiso 1 1 calc R . . C8 C 0.5317(5) 0.4067(8) 0.6970(4) 0.036(2) Uani 1 1 d . . . C9 C 0.4073(5) 0.5524(8) 0.6229(4) 0.040(2) Uani 1 1 d . . . C10 C 0.3736(5) 0.4161(8) 0.7054(4) 0.037(2) Uani 1 1 d . . . C11 C 0.3970(5) 0.5620(7) 0.7946(4) 0.036(2) Uani 1 1 d . . . C12 C 0.5384(5) 0.4114(8) 0.8149(4) 0.037(2) Uani 1 1 d . . . C13 C 0.1478(5) 0.5443(8) 0.8013(4) 0.036(2) Uani 1 1 d . . . C14 C 0.0641(4) 0.5410(7) 0.7697(3) 0.0295(19) Uani 1 1 d . . . H14 H 0.0534 0.4586 0.7638 0.035 Uiso 1 1 calc R . . C15 C 0.0289(5) 0.5913(7) 0.7132(4) 0.033(2) Uani 1 1 d . . . H15 H 0.0530 0.5519 0.6957 0.040 Uiso 1 1 calc R . . C16 C -0.0520(5) 0.5540(8) 0.6846(4) 0.038(2) Uani 1 1 d . . . H16 H -0.0490 0.4702 0.6888 0.046 Uiso 1 1 calc R . . C17 C -0.0975(5) 0.5912(8) 0.7120(4) 0.036(2) Uani 1 1 d . . . H17 H -0.1441 0.5490 0.6943 0.043 Uiso 1 1 calc R . . C18 C -0.0577(5) 0.5450(7) 0.7692(4) 0.036(2) Uani 1 1 d . . . H18 H -0.0569 0.4617 0.7645 0.043 Uiso 1 1 calc R . . C19 C 0.0252(4) 0.5764(7) 0.8007(3) 0.0305(19) Uani 1 1 d . . . H19 H 0.0452 0.5250 0.8310 0.037 Uiso 1 1 calc R . . C20 C 0.0376(5) 0.7204(8) 0.7069(4) 0.040(2) Uani 1 1 d . . . C21 C -0.0890(7) 0.5689(9) 0.6266(4) 0.055(3) Uani 1 1 d . . . C22 C -0.1183(5) 0.7168(7) 0.7092(4) 0.033(2) Uani 1 1 d . . . C23 C -0.1042(5) 0.5576(8) 0.7961(4) 0.041(2) Uani 1 1 d . . . C24 C 0.0476(5) 0.6978(8) 0.8236(4) 0.040(2) Uani 1 1 d . . . C25 C 0.8855(6) 0.6319(11) 0.9625(5) 0.060(3) Uani 1 1 d . . . H25 H 0.8719 0.7047 0.9477 0.072 Uiso 1 1 calc R . . C26 C 0.9242(6) 0.6217(13) 1.0164(5) 0.067(3) Uani 1 1 d . . . H26 H 0.9357 0.6867 1.0374 0.080 Uiso 1 1 calc R . . C27 C 0.9454(6) 0.5144(13) 1.0383(4) 0.066(3) Uani 1 1 d . . . H27 H 0.9716 0.5062 1.0744 0.080 Uiso 1 1 calc R . . C28 C 0.9276(6) 0.4200(12) 1.0067(4) 0.061(3) Uani 1 1 d . . . H28 H 0.9417 0.3471 1.0212 0.073 Uiso 1 1 calc R . . C29 C 0.8874(5) 0.4334(10) 0.9516(4) 0.049(3) Uani 1 1 d . . . C30 C 0.8637(5) 0.3330(9) 0.9151(4) 0.046(2) Uani 1 1 d . . . C31 C 0.8845(7) 0.2209(11) 0.9299(5) 0.075(4) Uani 1 1 d . . . H31 H 0.9167 0.2043 0.9647 0.090 Uiso 1 1 calc R . . C32 C 0.8589(8) 0.1348(12) 0.8948(5) 0.079(4) Uani 1 1 d . . . H32 H 0.8749 0.0598 0.9051 0.095 Uiso 1 1 calc R . . C33 C 0.8091(7) 0.1583(10) 0.8436(5) 0.066(3) Uani 1 1 d . . . H33 H 0.7889 0.1001 0.8189 0.079 Uiso 1 1 calc R . . C34 C 0.7906(6) 0.2702(10) 0.8310(5) 0.057(3) Uani 1 1 d . . . H34 H 0.7577 0.2878 0.7964 0.068 Uiso 1 1 calc R . . C35 C 0.3815(6) 0.6019(12) 0.9651(4) 0.062(3) Uani 1 1 d . . . H35 H 0.3668 0.6774 0.9547 0.074 Uiso 1 1 calc R . . C36 C 0.4211(7) 0.5774(16) 1.0176(5) 0.078(4) Uani 1 1 d . . . H36 H 0.4317 0.6354 1.0422 0.093 Uiso 1 1 calc R . . C37 C 0.4442(8) 0.4688(17) 1.0332(5) 0.085(5) Uani 1 1 d . . . H37 H 0.4711 0.4512 1.0685 0.102 Uiso 1 1 calc R . . C38 C 0.4275(6) 0.3838(13) 0.9958(4) 0.066(4) Uani 1 1 d . . . H38 H 0.4440 0.3090 1.0061 0.079 Uiso 1 1 calc R . . C39 C 0.3865(5) 0.4092(11) 0.9433(4) 0.049(3) Uani 1 1 d . . . C40 C 0.3641(5) 0.3223(10) 0.9014(4) 0.052(3) Uani 1 1 d . . . C41 C 0.3855(8) 0.2110(12) 0.9119(6) 0.087(5) Uani 1 1 d . . . H41 H 0.4139 0.1865 0.9462 0.104 Uiso 1 1 calc R . . C42 C 0.3646(9) 0.1329(12) 0.8707(7) 0.092(5) Uani 1 1 d . . . H42 H 0.3812 0.0573 0.8772 0.111 Uiso 1 1 calc R . . C43 C 0.3208(6) 0.1677(11) 0.8222(5) 0.061(3) Uani 1 1 d . . . H43 H 0.3018 0.1151 0.7948 0.074 Uiso 1 1 calc R . . C44 C 0.3038(6) 0.2828(11) 0.8129(5) 0.059(3) Uani 1 1 d . . . H44 H 0.2766 0.3085 0.7787 0.070 Uiso 1 1 calc R . . C45 C 0.6882(7) 0.7721(12) 0.4392(5) 0.069(4) Uani 1 1 d . . . H45 H 0.6637 0.7421 0.4056 0.082 Uiso 1 1 calc R . . C46 C 0.7068(8) 0.7015(12) 0.4804(5) 0.076(4) Uani 1 1 d . . . H46 H 0.6949 0.6237 0.4758 0.091 Uiso 1 1 calc R . . C47 C 0.7450(7) 0.7505(11) 0.5310(5) 0.065(3) Uani 1 1 d . . . H47 H 0.7604 0.7039 0.5603 0.078 Uiso 1 1 calc R . . C48 C 0.7593(6) 0.8663(10) 0.5368(4) 0.055(3) Uani 1 1 d . . . H48 H 0.7831 0.8979 0.5701 0.066 Uiso 1 1 calc R . . C49 C 0.7391(5) 0.9364(10) 0.4942(4) 0.049(3) Uani 1 1 d . . . C50 C 0.7509(5) 1.0607(9) 0.4945(4) 0.047(3) Uani 1 1 d . . . C51 C 0.7874(6) 1.1229(11) 0.5398(5) 0.064(3) Uani 1 1 d . . . H51 H 0.8076 1.0866 0.5721 0.077 Uiso 1 1 calc R . . C52 C 0.7933(7) 1.2383(12) 0.5364(6) 0.079(4) Uani 1 1 d . . . H52 H 0.8178 1.2825 0.5665 0.095 Uiso 1 1 calc R . . C53 C 0.7619(8) 1.2911(12) 0.4866(6) 0.083(4) Uani 1 1 d . . . H53 H 0.7656 1.3701 0.4835 0.100 Uiso 1 1 calc R . . C54 C 0.7262(8) 1.2236(12) 0.4432(6) 0.076(4) Uani 1 1 d . . . H54 H 0.7048 1.2579 0.4105 0.092 Uiso 1 1 calc R . . N1 N 0.8672(4) 0.5395(8) 0.9311(3) 0.048(2) Uani 1 1 d . . . N2 N 0.8172(4) 0.3580(7) 0.8657(3) 0.0417(19) Uani 1 1 d . . . N3 N 0.3636(4) 0.5202(9) 0.9284(3) 0.050(2) Uani 1 1 d . . . N4 N 0.3257(4) 0.3586(7) 0.8521(3) 0.044(2) Uani 1 1 d . . . N5 N 0.7046(5) 0.8853(8) 0.4460(3) 0.051(2) Uani 1 1 d . . . N6 N 0.7211(5) 1.1095(9) 0.4467(4) 0.058(2) Uani 1 1 d . . . O1 O 0.6814(3) 0.5165(6) 0.7750(2) 0.0406(16) Uani 1 1 d . . . O2 O 0.6802(3) 0.5800(6) 0.8453(2) 0.0416(16) Uani 1 1 d . . . O3 O 0.5975(4) 0.3661(6) 0.7088(3) 0.0477(17) Uani 1 1 d . . . H3A H 0.6293 0.4078 0.7307 0.071 Uiso 1 1 calc R . . O4 O 0.4767(4) 0.3465(6) 0.6723(3) 0.0513(18) Uani 1 1 d . . . O5 O 0.4507(4) 0.5754(8) 0.6038(3) 0.058(2) Uani 1 1 d . . . H5A H 0.4270 0.5756 0.5719 0.087 Uiso 1 1 calc R . . O6 O 0.3435(4) 0.5252(7) 0.5978(3) 0.0528(19) Uani 1 1 d . . . O7 O 0.3195(4) 0.3853(6) 0.6582(3) 0.0543(19) Uani 1 1 d . . . H7A H 0.3153 0.4340 0.6366 0.082 Uiso 1 1 calc R . . O8 O 0.3936(4) 0.3524(6) 0.7416(3) 0.0518(18) Uani 1 1 d . . . O9 O 0.3296(4) 0.5749(6) 0.7698(3) 0.0524(19) Uani 1 1 d . . . O10 O 0.4307(4) 0.5405(6) 0.8437(3) 0.0489(18) Uani 1 1 d . . . O11 O 0.5191(4) 0.3747(6) 0.8492(3) 0.0504(18) Uani 1 1 d . . . H11 H 0.4893 0.4195 0.8503 0.076 Uiso 1 1 calc R . . O12 O 0.5729(4) 0.3492(6) 0.8011(3) 0.0489(17) Uani 1 1 d . . . O13 O 0.1849(3) 0.5911(6) 0.7816(3) 0.0545(19) Uani 1 1 d . . . O14 O 0.1785(3) 0.4942(6) 0.8435(3) 0.0460(17) Uani 1 1 d . . . O15 O 0.1048(4) 0.7564(6) 0.7192(3) 0.0558(19) Uani 1 1 d . . . H15A H 0.1336 0.7021 0.7301 0.084 Uiso 1 1 calc R . . O16 O -0.0129(4) 0.7867(6) 0.6888(3) 0.056(2) Uani 1 1 d . . . O17 O -0.0475(7) 0.5950(12) 0.6071(4) 0.112(4) Uani 1 1 d . . . O18 O -0.1556(6) 0.5435(8) 0.5987(4) 0.092(3) Uani 1 1 d . . . H18A H -0.1763 0.5951 0.5775 0.138 Uiso 1 1 calc R . . O19 O -0.1623(3) 0.7534(5) 0.6618(2) 0.0436(16) Uani 1 1 d . . . H19A H -0.1664 0.8235 0.6621 0.065 Uiso 1 1 calc R . . O20 O -0.0997(4) 0.7751(5) 0.7484(3) 0.0441(16) Uani 1 1 d . . . O21 O -0.1701(4) 0.5326(7) 0.7725(3) 0.060(2) Uani 1 1 d . . . O22 O -0.0736(4) 0.5871(7) 0.8438(3) 0.058(2) Uani 1 1 d . . . O23 O 0.0256(4) 0.7322(7) 0.8568(3) 0.0545(19) Uani 1 1 d . . . H23 H -0.0047 0.6865 0.8567 0.082 Uiso 1 1 calc R . . O24 O 0.0882(4) 0.7574(6) 0.8147(3) 0.0540(19) Uani 1 1 d . . . O1W O 0.7915(4) 0.7444(7) 0.8383(4) 0.078(3) Uani 1 1 d . . . O2W O 0.3351(5) 0.7461(8) 0.8592(4) 0.086(3) Uani 1 1 d . . . O3W O 0.8926(6) 0.8871(8) 0.8374(5) 0.105(4) Uani 1 1 d . . . O5W O 0.2189(7) 0.8781(10) 0.8167(7) 0.186(8) Uani 1 1 d . . . O4W O 0.4080(11) 0.5694(19) 0.5011(5) 0.246(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0266(4) 0.0516(5) 0.0398(4) 0.0114(3) 0.0137(3) 0.0035(3) Cd2 0.0320(4) 0.0588(5) 0.0400(4) -0.0012(4) 0.0201(3) 0.0037(3) C1 0.026(4) 0.036(5) 0.037(6) 0.011(4) 0.012(4) 0.000(4) C2 0.022(4) 0.039(5) 0.031(5) 0.006(4) 0.014(4) 0.001(3) C3 0.031(5) 0.032(5) 0.033(5) -0.004(4) 0.020(4) -0.003(4) C4 0.032(5) 0.028(4) 0.033(5) -0.005(4) 0.013(4) -0.004(3) C5 0.021(4) 0.032(4) 0.025(4) -0.005(4) 0.009(4) -0.002(3) C6 0.024(4) 0.036(5) 0.033(5) 0.002(4) 0.013(4) -0.002(4) C7 0.029(4) 0.031(4) 0.022(4) -0.002(4) 0.012(4) -0.002(3) C8 0.040(5) 0.034(5) 0.042(6) 0.010(4) 0.027(5) 0.008(4) C9 0.039(6) 0.042(5) 0.035(5) 0.006(4) 0.014(5) 0.007(4) C10 0.032(5) 0.043(5) 0.035(5) -0.011(5) 0.016(4) -0.010(4) C11 0.032(5) 0.036(5) 0.046(6) -0.006(4) 0.023(5) -0.008(4) C12 0.033(5) 0.038(5) 0.041(6) 0.000(4) 0.017(5) -0.005(4) C13 0.029(5) 0.037(5) 0.046(6) -0.006(5) 0.021(5) 0.003(4) C14 0.025(4) 0.026(4) 0.037(5) 0.004(4) 0.015(4) 0.006(3) C15 0.032(5) 0.030(4) 0.038(5) -0.001(4) 0.017(4) -0.002(4) C16 0.036(5) 0.034(5) 0.035(5) -0.006(4) 0.010(4) 0.001(4) C17 0.028(4) 0.032(5) 0.043(6) -0.001(4) 0.014(4) -0.001(4) C18 0.029(5) 0.030(5) 0.048(6) 0.008(4) 0.019(4) 0.005(4) C19 0.028(4) 0.036(5) 0.030(5) 0.007(4) 0.016(4) 0.004(4) C20 0.049(6) 0.038(5) 0.043(6) 0.005(5) 0.030(5) 0.000(5) C21 0.055(7) 0.048(6) 0.044(7) -0.014(5) 0.010(6) 0.012(5) C22 0.028(5) 0.033(5) 0.037(5) 0.000(4) 0.016(4) -0.002(4) C23 0.037(6) 0.038(5) 0.053(7) 0.021(5) 0.024(5) 0.012(4) C24 0.033(5) 0.046(6) 0.036(5) -0.006(4) 0.013(4) 0.006(4) C25 0.037(6) 0.069(8) 0.064(8) -0.006(7) 0.017(6) 0.000(5) C26 0.054(7) 0.100(10) 0.042(7) -0.005(7) 0.019(6) -0.004(7) C27 0.048(7) 0.109(11) 0.031(6) -0.001(7) 0.010(5) -0.003(7) C28 0.044(6) 0.092(9) 0.036(6) 0.021(6) 0.012(5) 0.006(6) C29 0.030(5) 0.068(7) 0.044(6) 0.018(5) 0.014(5) 0.011(5) C30 0.041(5) 0.059(7) 0.046(6) 0.011(5) 0.028(5) 0.002(5) C31 0.081(9) 0.071(8) 0.047(7) 0.021(7) 0.010(7) 0.024(7) C32 0.096(10) 0.064(8) 0.070(9) 0.016(8) 0.033(8) 0.012(7) C33 0.074(8) 0.044(6) 0.079(9) 0.004(6) 0.037(8) 0.003(6) C34 0.057(7) 0.060(7) 0.051(7) 0.004(6) 0.024(6) -0.003(6) C35 0.049(6) 0.100(9) 0.050(7) -0.032(7) 0.034(6) -0.018(6) C36 0.054(8) 0.139(14) 0.047(8) -0.044(9) 0.031(7) -0.033(9) C37 0.058(8) 0.148(15) 0.031(7) -0.008(9) 0.008(6) -0.029(9) C38 0.045(6) 0.106(10) 0.043(7) 0.015(7) 0.017(6) 0.002(6) C39 0.027(5) 0.082(8) 0.040(6) -0.002(6) 0.017(5) -0.008(5) C40 0.035(5) 0.069(7) 0.046(7) 0.004(6) 0.015(5) 0.007(5) C41 0.108(12) 0.072(9) 0.059(8) 0.010(7) 0.023(8) 0.028(8) C42 0.129(14) 0.062(9) 0.107(13) 0.026(9) 0.074(12) 0.037(9) C43 0.059(7) 0.064(8) 0.071(9) -0.019(7) 0.039(7) -0.013(6) C44 0.052(7) 0.079(9) 0.054(7) -0.018(6) 0.032(6) -0.009(6) C45 0.076(8) 0.089(10) 0.044(7) 0.009(7) 0.031(6) 0.023(7) C46 0.089(10) 0.070(9) 0.064(9) -0.006(7) 0.032(8) 0.011(7) C47 0.071(8) 0.064(8) 0.046(7) 0.007(6) 0.018(6) 0.010(6) C48 0.058(7) 0.069(8) 0.029(6) -0.002(5) 0.014(5) 0.006(6) C49 0.026(5) 0.081(8) 0.034(6) -0.004(6) 0.009(5) 0.011(5) C50 0.037(5) 0.064(7) 0.037(6) 0.010(5) 0.017(5) 0.017(5) C51 0.042(6) 0.063(8) 0.066(8) 0.014(7) 0.010(6) 0.007(5) C52 0.079(9) 0.076(9) 0.065(9) -0.003(8) 0.021(8) 0.010(7) C53 0.084(10) 0.065(9) 0.102(12) 0.004(9) 0.045(9) 0.016(7) C54 0.080(9) 0.078(10) 0.084(10) 0.026(8) 0.049(8) 0.030(8) N1 0.037(5) 0.062(6) 0.044(5) 0.014(5) 0.017(4) 0.010(4) N2 0.041(4) 0.056(5) 0.031(4) 0.006(4) 0.019(4) 0.005(4) N3 0.037(5) 0.082(7) 0.030(4) -0.023(5) 0.016(4) -0.017(4) N4 0.035(4) 0.057(5) 0.035(5) -0.005(4) 0.012(4) -0.003(4) N5 0.053(5) 0.061(6) 0.044(5) -0.001(5) 0.027(5) 0.010(4) N6 0.060(6) 0.066(6) 0.053(6) 0.010(5) 0.031(5) 0.020(5) O1 0.023(3) 0.064(4) 0.037(4) 0.005(3) 0.016(3) 0.002(3) O2 0.031(3) 0.058(4) 0.029(4) 0.005(3) 0.009(3) -0.003(3) O3 0.042(4) 0.052(4) 0.049(4) -0.011(3) 0.021(3) 0.014(3) O4 0.050(4) 0.047(4) 0.054(4) -0.012(4) 0.023(4) -0.001(3) O5 0.053(4) 0.095(6) 0.029(4) 0.002(4) 0.022(4) 0.000(4) O6 0.038(4) 0.073(5) 0.034(4) -0.007(4) 0.006(3) -0.004(3) O7 0.048(4) 0.064(5) 0.049(4) -0.016(4) 0.022(4) -0.025(4) O8 0.064(5) 0.039(4) 0.054(5) -0.003(4) 0.030(4) -0.010(3) O9 0.029(4) 0.075(5) 0.055(5) -0.004(4) 0.022(3) 0.001(3) O10 0.039(4) 0.079(5) 0.036(4) -0.007(4) 0.023(3) -0.001(3) O11 0.056(5) 0.056(4) 0.044(4) 0.009(4) 0.028(4) 0.004(3) O12 0.059(4) 0.039(4) 0.063(5) 0.008(3) 0.040(4) 0.007(3) O13 0.033(4) 0.062(4) 0.073(5) 0.016(4) 0.029(4) 0.008(3) O14 0.033(3) 0.052(4) 0.041(4) 0.002(3) 0.007(3) 0.005(3) O15 0.048(4) 0.045(4) 0.084(6) 0.009(4) 0.040(4) -0.004(3) O16 0.043(4) 0.043(4) 0.082(6) 0.017(4) 0.030(4) 0.007(3) O17 0.121(9) 0.173(11) 0.056(6) -0.005(7) 0.053(6) -0.031(8) O18 0.096(8) 0.087(7) 0.055(6) -0.006(5) 0.005(5) 0.026(6) O19 0.041(4) 0.038(4) 0.037(4) 0.011(3) 0.007(3) 0.010(3) O20 0.055(4) 0.033(3) 0.046(4) 0.001(3) 0.025(3) 0.001(3) O21 0.035(4) 0.070(5) 0.082(6) 0.024(4) 0.035(4) 0.007(3) O22 0.047(4) 0.083(5) 0.057(5) 0.015(4) 0.034(4) 0.014(4) O23 0.041(4) 0.072(5) 0.048(4) -0.024(4) 0.020(4) -0.001(3) O24 0.054(4) 0.051(4) 0.064(5) -0.017(4) 0.034(4) -0.018(4) O1W 0.070(5) 0.046(4) 0.148(9) 0.019(5) 0.074(6) 0.018(4) O2W 0.085(6) 0.070(6) 0.121(8) -0.032(6) 0.063(6) -0.012(5) O3W 0.127(9) 0.057(5) 0.184(11) -0.004(6) 0.117(9) -0.006(5) O5W 0.093(8) 0.070(7) 0.30(2) 0.008(10) 0.020(11) 0.014(6) O4W 0.25(2) 0.31(2) 0.050(8) 0.012(11) -0.036(10) -0.078(17) _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 Cd1 O1W 2.269(8) . ? Cd1 O1 2.317(6) . ? Cd1 N2 2.319(8) . ? Cd1 O21 2.348(8) 1_655 ? Cd1 N1 2.325(8) . ? Cd1 O2 2.587(6) . ? Cd1 O22 2.596(7) 1_655 ? Cd2 O13 2.271(7) . ? Cd2 O2W 2.300(9) . ? Cd2 N3 2.325(8) . ? Cd2 O9 2.324(7) . ? Cd2 N4 2.326(9) . ? Cd2 O10 2.547(6) . ? C1 O2 1.240(11) . ? C1 O1 1.264(11) . ? C1 C2 1.535(11) . ? C2 C7 1.534(11) . ? C2 C3 1.556(12) . ? C2 H2 0.9800 . ? C3 C8 1.521(12) . ? C3 C4 1.533(12) . ? C3 H3 0.9800 . ? C4 C9 1.542(13) . ? C4 C5 1.563(12) . ? C4 H4 0.9800 . ? C5 C10 1.533(12) . ? C5 C6 1.532(12) . ? C5 H5 0.9800 . ? C6 C11 1.523(12) . ? C6 C7 1.550(11) . ? C6 H6 0.9800 . ? C7 C12 1.521(12) . ? C7 H7 0.9800 . ? C8 O4 1.232(11) . ? C8 O3 1.322(10) . ? C9 O6 1.205(11) . ? C9 O5 1.293(12) . ? C10 O8 1.193(11) . ? C10 O7 1.341(11) . ? C11 O9 1.233(11) . ? C11 O10 1.283(12) . ? C12 O12 1.214(11) . ? C12 O11 1.316(11) . ? C13 O13 1.280(11) . ? C13 O14 1.228(11) . ? C13 C14 1.523(12) . ? C14 C19 1.529(12) . ? C14 C15 1.564(12) . ? C14 H14 0.9800 . ? C15 C16 1.532(12) . ? C15 C20 1.532(13) . ? C15 H15 0.9800 . ? C16 C17 1.564(13) . ? C16 C21 1.496(15) . ? C16 H16 0.9800 . ? C17 C22 1.512(12) . ? C17 C18 1.562(13) . ? C17 H17 0.9800 . ? C18 C23 1.513(13) . ? C18 C19 1.553(12) . ? C18 H18 0.9800 . ? C19 C24 1.535(13) . ? C19 H19 0.9800 . ? C20 O16 1.197(11) . ? C20 O15 1.328(11) . ? C21 O17 1.276(15) . ? C21 O18 1.253(14) . ? C22 O20 1.222(11) . ? C22 O19 1.312(10) . ? C23 O21 1.232(12) . ? C23 O22 1.271(13) . ? C24 O24 1.207(12) . ? C24 O23 1.319(11) . ? C25 C26 1.388(16) . ? C25 N1 1.343(14) . ? C25 H25 0.9300 . ? C26 C27 1.374(19) . ? C26 H26 0.9300 . ? C27 C28 1.365(18) . ? C27 H27 0.9300 . ? C28 C29 1.422(15) . ? C28 H28 0.9300 . ? C29 N1 1.347(13) . ? C29 C30 1.496(15) . ? C30 N2 1.327(12) . ? C30 C31 1.375(15) . ? C31 C32 1.345(18) . ? C31 H31 0.9300 . ? C32 C33 1.376(17) . ? C32 H32 0.9300 . ? C33 C34 1.357(16) . ? C33 H33 0.9300 . ? C34 N2 1.355(14) . ? C34 H34 0.9300 . ? C35 N3 1.345(13) . ? C35 C36 1.379(18) . ? C35 H35 0.9300 . ? C36 C37 1.35(2) . ? C36 H36 0.9300 . ? C37 C38 1.39(2) . ? C37 H37 0.9300 . ? C38 C39 1.381(15) . ? C38 H38 0.9300 . ? C39 N3 1.371(15) . ? C39 C40 1.479(15) . ? C40 C41 1.354(17) . ? C40 N4 1.337(13) . ? C41 C42 1.40(2) . ? C41 H41 0.9300 . ? C42 C43 1.326(18) . ? C42 H42 0.9300 . ? C43 C44 1.376(17) . ? C43 H43 0.9300 . ? C44 N4 1.340(13) . ? C44 H44 0.9300 . ? C45 C46 1.352(17) . ? C45 N5 1.349(16) . ? C45 H45 0.9300 . ? C46 C47 1.418(17) . ? C46 H46 0.9300 . ? C47 C48 1.372(16) . ? C47 H47 0.9300 . ? C48 C49 1.373(15) . ? C48 H48 0.9300 . ? C49 N5 1.372(13) . ? C49 C50 1.465(15) . ? C50 C51 1.375(16) . ? C50 N6 1.351(13) . ? C51 C52 1.355(18) . ? C51 H51 0.9300 . ? C52 C53 1.416(19) . ? C52 H52 0.9300 . ? C53 C54 1.367(19) . ? C53 H53 0.9300 . ? C54 N6 1.339(16) . ? C54 H54 0.9300 . ? O3 H3A 0.8200 . ? O5 H5A 0.8200 . ? O7 H7A 0.8200 . ? O11 H11 0.8200 . ? O15 H15A 0.8200 . ? O18 H18A 0.8200 . ? O19 H19A 0.8200 . ? O21 Cd1 2.348(8) 1_455 ? O22 Cd1 2.596(7) 1_455 ? O23 H23 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cd1 O1 95.8(3) . . ? O1W Cd1 N2 164.8(3) . . ? O1 Cd1 N2 92.2(3) . . ? O1W Cd1 O21 96.4(3) . 1_655 ? O1 Cd1 O21 83.8(2) . 1_655 ? N2 Cd1 O21 97.4(3) . 1_655 ? O1W Cd1 N1 94.5(3) . . ? O1 Cd1 N1 138.2(3) . . ? N2 Cd1 N1 71.0(3) . . ? O21 Cd1 N1 134.9(3) 1_655 . ? O1W Cd1 O2 78.3(2) . . ? O1 Cd1 O2 52.8(2) . . ? N2 Cd1 O2 96.6(2) . . ? O21 Cd1 O2 134.7(2) 1_655 . ? N1 Cd1 O2 90.4(2) . . ? O1W Cd1 O22 84.4(3) . 1_655 ? O1 Cd1 O22 135.2(2) . 1_655 ? N2 Cd1 O22 99.0(3) . 1_655 ? O21 Cd1 O22 51.9(3) 1_655 1_655 ? N1 Cd1 O22 86.0(3) . 1_655 ? O2 Cd1 O22 161.9(2) . 1_655 ? O13 Cd2 O2W 94.6(3) . . ? O13 Cd2 N3 131.2(3) . . ? O2W Cd2 N3 87.3(4) . . ? O13 Cd2 O9 87.6(3) . . ? O2W Cd2 O9 89.0(3) . . ? N3 Cd2 O9 141.1(3) . . ? O13 Cd2 N4 110.5(3) . . ? O2W Cd2 N4 154.1(3) . . ? N3 Cd2 N4 71.8(3) . . ? O9 Cd2 N4 97.9(3) . . ? O13 Cd2 O10 141.2(2) . . ? O2W Cd2 O10 84.6(3) . . ? N3 Cd2 O10 87.6(3) . . ? O9 Cd2 O10 53.6(2) . . ? N4 Cd2 O10 79.6(3) . . ? O2 C1 O1 122.3(8) . . ? O2 C1 C2 118.1(8) . . ? O1 C1 C2 119.3(8) . . ? C7 C2 C3 114.7(7) . . ? C7 C2 C1 113.1(7) . . ? C3 C2 C1 115.2(7) . . ? C7 C2 H2 104.0 . . ? C3 C2 H2 104.0 . . ? C1 C2 H2 104.0 . . ? C8 C3 C2 119.8(7) . . ? C8 C3 C4 110.9(7) . . ? C2 C3 C4 108.8(7) . . ? C8 C3 H3 105.4 . . ? C2 C3 H3 105.4 . . ? C4 C3 H3 105.4 . . ? C9 C4 C5 114.5(7) . . ? C9 C4 C3 113.2(7) . . ? C5 C4 C3 115.1(7) . . ? C9 C4 H4 104.1 . . ? C5 C4 H4 104.1 . . ? C3 C4 H4 104.1 . . ? C10 C5 C4 118.6(7) . . ? C10 C5 C6 111.2(7) . . ? C4 C5 C6 108.7(6) . . ? C10 C5 H5 105.8 . . ? C4 C5 H5 105.8 . . ? C6 C5 H5 105.8 . . ? C11 C6 C7 115.2(7) . . ? C11 C6 C5 111.5(7) . . ? C7 C6 C5 115.3(7) . . ? C11 C6 H6 104.4 . . ? C7 C6 H6 104.4 . . ? C5 C6 H6 104.4 . . ? C12 C7 C2 111.5(7) . . ? C12 C7 C6 119.0(7) . . ? C2 C7 C6 108.6(7) . . ? C12 C7 H7 105.5 . . ? C2 C7 H7 105.5 . . ? C6 C7 H7 105.6 . . ? O4 C8 O3 119.9(8) . . ? O4 C8 C3 122.5(8) . . ? O3 C8 C3 117.4(8) . . ? O6 C9 O5 125.2(9) . . ? O6 C9 C4 124.1(9) . . ? O5 C9 C4 110.5(8) . . ? O8 C10 O7 120.6(9) . . ? O8 C10 C5 123.5(8) . . ? O7 C10 C5 115.5(9) . . ? O9 C11 O10 122.3(9) . . ? O9 C11 C6 119.3(9) . . ? O10 C11 C6 118.3(8) . . ? O12 C12 O11 120.1(9) . . ? O12 C12 C7 121.2(8) . . ? O11 C12 C7 118.4(8) . . ? O13 C13 O14 121.2(8) . . ? O13 C13 C14 119.4(8) . . ? O14 C13 C14 119.2(8) . . ? C13 C14 C19 113.7(7) . . ? C13 C14 C15 116.7(7) . . ? C19 C14 C15 114.5(7) . . ? C13 C14 H14 103.2 . . ? C19 C14 H14 103.2 . . ? C15 C14 H14 103.2 . . ? C16 C15 C20 111.8(7) . . ? C16 C15 C14 107.7(7) . . ? C20 C15 C14 118.0(8) . . ? C16 C15 H15 106.2 . . ? C20 C15 H15 106.2 . . ? C14 C15 H15 106.2 . . ? C15 C16 C17 114.4(7) . . ? C15 C16 C21 114.7(9) . . ? C17 C16 C21 116.1(8) . . ? C15 C16 H16 103.1 . . ? C17 C16 H16 103.1 . . ? C21 C16 H16 103.1 . . ? C22 C17 C16 117.7(8) . . ? C22 C17 C18 112.3(8) . . ? C16 C17 C18 108.4(7) . . ? C22 C17 H17 105.9 . . ? C16 C17 H17 105.9 . . ? C18 C17 H17 105.9 . . ? C23 C18 C19 117.9(8) . . ? C23 C18 C17 112.5(7) . . ? C19 C18 C17 114.7(7) . . ? C23 C18 H18 103.1 . . ? C19 C18 H18 103.1 . . ? C17 C18 H18 103.1 . . ? C14 C19 C18 109.4(7) . . ? C14 C19 C24 111.7(7) . . ? C18 C19 C24 119.4(7) . . ? C14 C19 H19 105.0 . . ? C18 C19 H19 105.0 . . ? C24 C19 H19 105.0 . . ? O16 C20 O15 119.7(9) . . ? O16 C20 C15 123.8(9) . . ? O15 C20 C15 116.3(8) . . ? O17 C21 O18 122.1(12) . . ? O17 C21 C16 116.3(10) . . ? O18 C21 C16 121.1(12) . . ? O20 C22 O19 123.8(8) . . ? O20 C22 C17 122.1(8) . . ? O19 C22 C17 113.9(8) . . ? O21 C23 O22 120.8(10) . . ? O21 C23 C18 119.8(10) . . ? O22 C23 C18 119.3(9) . . ? O24 C24 O23 120.4(9) . . ? O24 C24 C19 122.0(8) . . ? O23 C24 C19 117.4(9) . . ? C26 C25 N1 121.8(12) . . ? C26 C25 H25 119.1 . . ? N1 C25 H25 119.1 . . ? C25 C26 C27 119.2(13) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 119.5(11) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.9(12) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? N1 C29 C28 119.5(11) . . ? N1 C29 C30 118.1(9) . . ? C28 C29 C30 122.3(10) . . ? N2 C30 C31 120.2(11) . . ? N2 C30 C29 115.0(9) . . ? C31 C30 C29 124.7(10) . . ? C32 C31 C30 121.1(11) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 119.7(12) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 116.9(12) . . ? C34 C33 H33 121.5 . . ? C32 C33 H33 121.5 . . ? C33 C34 N2 123.9(11) . . ? C33 C34 H34 118.1 . . ? N2 C34 H34 118.1 . . ? N3 C35 C36 122.1(14) . . ? N3 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C37 C36 C35 119.6(13) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 119.1(13) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 C37 120.6(14) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? N3 C39 C38 119.2(11) . . ? N3 C39 C40 117.1(9) . . ? C38 C39 C40 123.6(12) . . ? C41 C40 N4 120.4(11) . . ? C41 C40 C39 121.8(11) . . ? N4 C40 C39 117.7(10) . . ? C40 C41 C42 119.5(13) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 119.5(12) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 119.1(12) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? N4 C44 C43 121.4(12) . . ? N4 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 N5 121.1(12) . . ? C46 C45 H45 119.4 . . ? N5 C45 H45 119.4 . . ? C45 C46 C47 117.6(13) . . ? C45 C46 H46 121.2 . . ? C47 C46 H46 121.2 . . ? C48 C47 C46 120.1(12) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C49 C48 C47 121.1(11) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 N5 117.1(10) . . ? C48 C49 C50 127.1(10) . . ? N5 C49 C50 115.8(10) . . ? C51 C50 N6 122.9(10) . . ? C51 C50 C49 122.5(10) . . ? N6 C50 C49 114.6(10) . . ? C50 C51 C52 118.5(12) . . ? C50 C51 H51 120.8 . . ? C52 C51 H51 120.8 . . ? C51 C52 C53 119.4(14) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 118.8(13) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? N6 C54 C53 121.7(13) . . ? N6 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C25 N1 C29 120.1(9) . . ? C25 N1 Cd1 123.7(7) . . ? C29 N1 Cd1 116.2(7) . . ? C30 N2 C34 118.1(9) . . ? C30 N2 Cd1 118.3(7) . . ? C34 N2 Cd1 122.8(7) . . ? C39 N3 C35 119.4(10) . . ? C39 N3 Cd2 116.0(6) . . ? C35 N3 Cd2 124.4(9) . . ? C44 N4 C40 119.7(10) . . ? C44 N4 Cd2 123.2(8) . . ? C40 N4 Cd2 117.0(7) . . ? C45 N5 C49 122.9(10) . . ? C50 N6 C54 118.7(11) . . ? C1 O1 Cd1 98.3(5) . . ? C1 O2 Cd1 86.3(5) . . ? C8 O3 H3A 109.5 . . ? C9 O5 H5A 109.5 . . ? C10 O7 H7A 109.5 . . ? C11 O9 Cd2 97.9(6) . . ? C11 O10 Cd2 86.2(5) . . ? C12 O11 H11 109.5 . . ? C13 O13 Cd2 105.6(6) . . ? C20 O15 H15A 109.5 . . ? C21 O18 H18A 109.5 . . ? C22 O19 H19A 109.5 . . ? C23 O21 Cd1 100.0(7) . 1_455 ? C23 O22 Cd1 87.2(6) . 1_455 ? C24 O23 H23 109.5 . . ? 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 O2 C1 C2 C7 -44.1(11) . . . . ? O1 C1 C2 C7 141.9(8) . . . . ? O2 C1 C2 C3 -178.8(8) . . . . ? O1 C1 C2 C3 7.2(12) . . . . ? C7 C2 C3 C8 -74.8(10) . . . . ? C1 C2 C3 C8 59.1(10) . . . . ? C7 C2 C3 C4 54.2(9) . . . . ? C1 C2 C3 C4 -171.8(7) . . . . ? C8 C3 C4 C9 -53.5(10) . . . . ? C2 C3 C4 C9 172.7(7) . . . . ? C8 C3 C4 C5 80.8(9) . . . . ? C2 C3 C4 C5 -53.0(9) . . . . ? C9 C4 C5 C10 58.1(10) . . . . ? C3 C4 C5 C10 -75.6(10) . . . . ? C9 C4 C5 C6 -173.6(7) . . . . ? C3 C4 C5 C6 52.7(9) . . . . ? C10 C5 C6 C11 -54.5(9) . . . . ? C4 C5 C6 C11 173.1(7) . . . . ? C10 C5 C6 C7 79.4(9) . . . . ? C4 C5 C6 C7 -53.0(9) . . . . ? C3 C2 C7 C12 78.8(9) . . . . ? C1 C2 C7 C12 -56.1(10) . . . . ? C3 C2 C7 C6 -54.3(9) . . . . ? C1 C2 C7 C6 170.8(7) . . . . ? C11 C6 C7 C12 57.4(11) . . . . ? C5 C6 C7 C12 -74.8(10) . . . . ? C11 C6 C7 C2 -173.5(7) . . . . ? C5 C6 C7 C2 54.3(9) . . . . ? C2 C3 C8 O4 120.9(10) . . . . ? C4 C3 C8 O4 -7.2(12) . . . . ? C2 C3 C8 O3 -65.6(11) . . . . ? C4 C3 C8 O3 166.3(8) . . . . ? C5 C4 C9 O6 8.4(13) . . . . ? C3 C4 C9 O6 143.1(9) . . . . ? C5 C4 C9 O5 -175.9(8) . . . . ? C3 C4 C9 O5 -41.3(11) . . . . ? C4 C5 C10 O8 115.2(10) . . . . ? C6 C5 C10 O8 -11.9(12) . . . . ? C4 C5 C10 O7 -71.4(10) . . . . ? C6 C5 C10 O7 161.5(8) . . . . ? C7 C6 C11 O9 -167.9(8) . . . . ? C5 C6 C11 O9 -33.9(11) . . . . ? C7 C6 C11 O10 15.7(12) . . . . ? C5 C6 C11 O10 149.7(8) . . . . ? C2 C7 C12 O12 -6.2(12) . . . . ? C6 C7 C12 O12 121.4(9) . . . . ? C2 C7 C12 O11 167.2(8) . . . . ? C6 C7 C12 O11 -65.1(11) . . . . ? O13 C13 C14 C19 -134.0(9) . . . . ? O14 C13 C14 C19 51.6(11) . . . . ? O13 C13 C14 C15 2.7(12) . . . . ? O14 C13 C14 C15 -171.7(8) . . . . ? C13 C14 C15 C16 166.8(7) . . . . ? C19 C14 C15 C16 -56.8(9) . . . . ? C13 C14 C15 C20 -65.5(10) . . . . ? C19 C14 C15 C20 70.9(10) . . . . ? C20 C15 C16 C17 -74.2(10) . . . . ? C14 C15 C16 C17 57.0(10) . . . . ? C20 C15 C16 C21 63.5(10) . . . . ? C14 C15 C16 C21 -165.4(7) . . . . ? C15 C16 C17 C22 73.6(10) . . . . ? C21 C16 C17 C22 -63.5(11) . . . . ? C15 C16 C17 C18 -55.2(10) . . . . ? C21 C16 C17 C18 167.7(8) . . . . ? C22 C17 C18 C23 58.6(10) . . . . ? C16 C17 C18 C23 -169.6(7) . . . . ? C22 C17 C18 C19 -79.8(9) . . . . ? C16 C17 C18 C19 52.0(10) . . . . ? C13 C14 C19 C18 -167.8(7) . . . . ? C15 C14 C19 C18 54.5(9) . . . . ? C13 C14 C19 C24 57.7(9) . . . . ? C15 C14 C19 C24 -80.0(9) . . . . ? C23 C18 C19 C14 171.6(7) . . . . ? C17 C18 C19 C14 -52.3(9) . . . . ? C23 C18 C19 C24 -57.8(11) . . . . ? C17 C18 C19 C24 78.2(10) . . . . ? C16 C15 C20 O16 10.5(14) . . . . ? C14 C15 C20 O16 -115.1(11) . . . . ? C16 C15 C20 O15 -164.4(8) . . . . ? C14 C15 C20 O15 69.9(11) . . . . ? C15 C16 C21 O17 9.4(14) . . . . ? C17 C16 C21 O17 146.4(11) . . . . ? C15 C16 C21 O18 -178.8(9) . . . . ? C17 C16 C21 O18 -41.8(13) . . . . ? C16 C17 C22 O20 -121.4(10) . . . . ? C18 C17 C22 O20 5.5(12) . . . . ? C16 C17 C22 O19 63.9(10) . . . . ? C18 C17 C22 O19 -169.2(7) . . . . ? C19 C18 C23 O21 -179.4(8) . . . . ? C17 C18 C23 O21 43.6(11) . . . . ? C19 C18 C23 O22 -3.7(12) . . . . ? C17 C18 C23 O22 -140.7(9) . . . . ? C14 C19 C24 O24 3.7(12) . . . . ? C18 C19 C24 O24 -125.8(10) . . . . ? C14 C19 C24 O23 -171.1(8) . . . . ? C18 C19 C24 O23 59.3(11) . . . . ? N1 C25 C26 C27 1.0(18) . . . . ? C25 C26 C27 C28 -0.4(18) . . . . ? C26 C27 C28 C29 0.0(18) . . . . ? C27 C28 C29 N1 -0.1(16) . . . . ? C27 C28 C29 C30 -177.5(10) . . . . ? N1 C29 C30 N2 -7.4(13) . . . . ? C28 C29 C30 N2 170.0(9) . . . . ? N1 C29 C30 C31 175.1(11) . . . . ? C28 C29 C30 C31 -7.5(17) . . . . ? N2 C30 C31 C32 1(2) . . . . ? C29 C30 C31 C32 178.0(12) . . . . ? C30 C31 C32 C33 -3(2) . . . . ? C31 C32 C33 C34 3(2) . . . . ? C32 C33 C34 N2 -1.3(19) . . . . ? N3 C35 C36 C37 1.5(19) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C37 C38 C39 N3 1.3(17) . . . . ? C37 C38 C39 C40 -177.6(11) . . . . ? N3 C39 C40 C41 178.1(12) . . . . ? C38 C39 C40 C41 -3.0(18) . . . . ? N3 C39 C40 N4 2.5(14) . . . . ? C38 C39 C40 N4 -178.7(10) . . . . ? N4 C40 C41 C42 -3(2) . . . . ? C39 C40 C41 C42 -178.1(13) . . . . ? C40 C41 C42 C43 -4(2) . . . . ? C41 C42 C43 C44 7(2) . . . . ? C42 C43 C44 N4 -5.4(18) . . . . ? N5 C45 C46 C47 -0.9(19) . . . . ? C45 C46 C47 C48 3(2) . . . . ? C46 C47 C48 C49 -1.9(19) . . . . ? C47 C48 C49 N5 -0.3(16) . . . . ? C47 C48 C49 C50 -179.9(11) . . . . ? C48 C49 C50 C51 2.2(18) . . . . ? N5 C49 C50 C51 -177.3(9) . . . . ? C48 C49 C50 N6 -175.8(10) . . . . ? N5 C49 C50 N6 4.6(14) . . . . ? N6 C50 C51 C52 0.4(18) . . . . ? C49 C50 C51 C52 -177.5(12) . . . . ? C50 C51 C52 C53 0(2) . . . . ? C51 C52 C53 C54 0(2) . . . . ? C52 C53 C54 N6 -1(2) . . . . ? C26 C25 N1 C29 -1.2(16) . . . . ? C26 C25 N1 Cd1 178.9(8) . . . . ? C28 C29 N1 C25 0.7(15) . . . . ? C30 C29 N1 C25 178.2(9) . . . . ? C28 C29 N1 Cd1 -179.3(7) . . . . ? C30 C29 N1 Cd1 -1.9(11) . . . . ? O1W Cd1 N1 C25 1.1(8) . . . . ? O1 Cd1 N1 C25 -102.8(9) . . . . ? N2 Cd1 N1 C25 -174.0(9) . . . . ? O21 Cd1 N1 C25 104.8(8) 1_655 . . . ? O2 Cd1 N1 C25 -77.1(8) . . . . ? O22 Cd1 N1 C25 85.1(8) 1_655 . . . ? O1W Cd1 N1 C29 -178.8(7) . . . . ? O1 Cd1 N1 C29 77.2(8) . . . . ? N2 Cd1 N1 C29 6.1(7) . . . . ? O21 Cd1 N1 C29 -75.2(8) 1_655 . . . ? O2 Cd1 N1 C29 102.9(7) . . . . ? O22 Cd1 N1 C29 -94.8(7) 1_655 . . . ? C31 C30 N2 C34 0.9(15) . . . . ? C29 C30 N2 C34 -176.7(9) . . . . ? C31 C30 N2 Cd1 -169.3(9) . . . . ? C29 C30 N2 Cd1 13.1(11) . . . . ? C33 C34 N2 C30 -0.5(16) . . . . ? C33 C34 N2 Cd1 169.2(9) . . . . ? O1W Cd1 N2 C30 -29.6(14) . . . . ? O1 Cd1 N2 C30 -151.4(7) . . . . ? O21 Cd1 N2 C30 124.6(7) 1_655 . . . ? N1 Cd1 N2 C30 -10.5(7) . . . . ? O2 Cd1 N2 C30 -98.7(7) . . . . ? O22 Cd1 N2 C30 72.1(7) 1_655 . . . ? O1W Cd1 N2 C34 160.8(10) . . . . ? O1 Cd1 N2 C34 38.9(8) . . . . ? O21 Cd1 N2 C34 -45.1(8) 1_655 . . . ? N1 Cd1 N2 C34 179.8(8) . . . . ? O2 Cd1 N2 C34 91.7(8) . . . . ? O22 Cd1 N2 C34 -97.6(8) 1_655 . . . ? C38 C39 N3 C35 0.0(14) . . . . ? C40 C39 N3 C35 178.9(9) . . . . ? C38 C39 N3 Cd2 174.3(7) . . . . ? C40 C39 N3 Cd2 -6.7(11) . . . . ? C36 C35 N3 C39 -1.4(15) . . . . ? C36 C35 N3 Cd2 -175.2(8) . . . . ? O13 Cd2 N3 C39 107.7(7) . . . . ? O2W Cd2 N3 C39 -158.6(7) . . . . ? O9 Cd2 N3 C39 -73.6(8) . . . . ? N4 Cd2 N3 C39 6.0(6) . . . . ? O10 Cd2 N3 C39 -73.8(7) . . . . ? O13 Cd2 N3 C35 -78.2(9) . . . . ? O2W Cd2 N3 C35 15.5(8) . . . . ? O9 Cd2 N3 C35 100.4(9) . . . . ? N4 Cd2 N3 C35 -179.9(8) . . . . ? O10 Cd2 N3 C35 100.2(8) . . . . ? C43 C44 N4 C40 -0.8(16) . . . . ? C43 C44 N4 Cd2 176.3(8) . . . . ? C41 C40 N4 C44 4.7(17) . . . . ? C39 C40 N4 C44 -179.6(9) . . . . ? C41 C40 N4 Cd2 -172.6(10) . . . . ? C39 C40 N4 Cd2 3.1(12) . . . . ? O13 Cd2 N4 C44 49.8(8) . . . . ? O2W Cd2 N4 C44 -144.6(8) . . . . ? N3 Cd2 N4 C44 178.0(8) . . . . ? O9 Cd2 N4 C44 -40.5(8) . . . . ? O10 Cd2 N4 C44 -91.1(8) . . . . ? O13 Cd2 N4 C40 -132.9(7) . . . . ? O2W Cd2 N4 C40 32.6(12) . . . . ? N3 Cd2 N4 C40 -4.8(7) . . . . ? O9 Cd2 N4 C40 136.7(7) . . . . ? O10 Cd2 N4 C40 86.1(7) . . . . ? C46 C45 N5 C49 -1.5(18) . . . . ? C48 C49 N5 C45 2.1(15) . . . . ? C50 C49 N5 C45 -178.3(10) . . . . ? C51 C50 N6 C54 -1.1(16) . . . . ? C49 C50 N6 C54 176.9(10) . . . . ? C53 C54 N6 C50 1.4(19) . . . . ? O2 C1 O1 Cd1 -6.6(9) . . . . ? C2 C1 O1 Cd1 167.2(6) . . . . ? O1W Cd1 O1 C1 -67.1(6) . . . . ? N2 Cd1 O1 C1 99.9(5) . . . . ? O21 Cd1 O1 C1 -163.0(6) 1_655 . . . ? N1 Cd1 O1 C1 36.3(7) . . . . ? O2 Cd1 O1 C1 3.3(5) . . . . ? O22 Cd1 O1 C1 -155.0(5) 1_655 . . . ? O1 C1 O2 Cd1 5.8(8) . . . . ? C2 C1 O2 Cd1 -168.0(7) . . . . ? O1W Cd1 O2 C1 103.4(6) . . . . ? O1 Cd1 O2 C1 -3.4(5) . . . . ? N2 Cd1 O2 C1 -91.2(5) . . . . ? O21 Cd1 O2 C1 16.0(7) 1_655 . . . ? N1 Cd1 O2 C1 -162.1(5) . . . . ? O22 Cd1 O2 C1 119.7(8) 1_655 . . . ? O10 C11 O9 Cd2 2.2(10) . . . . ? C6 C11 O9 Cd2 -174.1(7) . . . . ? O13 Cd2 O9 C11 177.6(6) . . . . ? O2W Cd2 O9 C11 82.9(6) . . . . ? N3 Cd2 O9 C11 -1.4(8) . . . . ? N4 Cd2 O9 C11 -72.0(6) . . . . ? O10 Cd2 O9 C11 -1.2(5) . . . . ? O9 C11 O10 Cd2 -2.0(9) . . . . ? C6 C11 O10 Cd2 174.3(7) . . . . ? O13 Cd2 O10 C11 -0.9(7) . . . . ? O2W Cd2 O10 C11 -91.6(6) . . . . ? N3 Cd2 O10 C11 -179.0(6) . . . . ? O9 Cd2 O10 C11 1.1(5) . . . . ? N4 Cd2 O10 C11 109.1(6) . . . . ? O14 C13 O13 Cd2 0.7(11) . . . . ? C14 C13 O13 Cd2 -173.5(6) . . . . ? O2W Cd2 O13 C13 -116.0(6) . . . . ? N3 Cd2 O13 C13 -25.6(8) . . . . ? O9 Cd2 O13 C13 155.2(6) . . . . ? N4 Cd2 O13 C13 57.7(7) . . . . ? O10 Cd2 O13 C13 156.8(5) . . . . ? O22 C23 O21 Cd1 -2.8(10) . . . 1_455 ? C18 C23 O21 Cd1 172.8(7) . . . 1_455 ? O21 C23 O22 Cd1 2.5(9) . . . 1_455 ? C18 C23 O22 Cd1 -173.1(7) . . . 1_455 ? 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 O23 H23 O22 0.82 1.73 2.541(11) 169.0 . O19 H19A O14 0.82 2.00 2.815(9) 175.2 2_556 O15 H15A O13 0.82 1.88 2.620(10) 150.1 . O11 H11 O10 0.82 1.81 2.610(10) 165.9 . O7 H7A O6 0.82 1.84 2.616(11) 157.5 . O5 H5A O4W 0.82 1.91 2.692(16) 158.7 . O3 H3A O1 0.82 1.76 2.567(9) 167.8 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.574 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.171 # Attachment 'web_deposit_cif_file_7_xingfeifei_1318817696.8.cif' data_090518b _database_code_depnum_ccdc_archive 'CCDC 848880' #TrackingRef 'web_deposit_cif_file_7_xingfeifei_1318817696.8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 Co1.50 N6 O21' _chemical_formula_weight 1064.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8575(16) _cell_length_b 14.2518(17) _cell_length_c 16.053(3) _cell_angle_alpha 101.572(2) _cell_angle_beta 107.553(2) _cell_angle_gamma 112.3380(10) _cell_volume 2422.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5993 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1107 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8393 _exptl_absorpt_correction_T_max 0.8886 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12243 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8416 _reflns_number_gt 6920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+3.5672P] 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 SHELXL _refine_ls_extinction_coef 0.0081(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8416 _refine_ls_number_parameters 644 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.63645(4) -0.16921(3) 0.32132(3) 0.02461(15) Uani 1 1 d . . . Co2 Co 1.0000 0.5000 1.0000 0.02586(18) Uani 1 2 d S . . C1 C 0.8158(3) 0.0995(2) 0.5927(2) 0.0232(6) Uani 1 1 d . . . H1 H 0.8281 0.1563 0.5654 0.028 Uiso 1 1 calc R . . C2 C 0.7826(3) 0.1389(2) 0.6740(2) 0.0238(6) Uani 1 1 d . . . H2 H 0.7157 0.1556 0.6462 0.029 Uiso 1 1 calc R . . C3 C 0.8927(3) 0.2481(2) 0.7454(2) 0.0227(6) Uani 1 1 d . . . H3 H 0.9027 0.2956 0.7087 0.027 Uiso 1 1 calc R . . C4 C 1.0186(3) 0.2478(2) 0.7806(2) 0.0241(7) Uani 1 1 d . . . H4 H 1.0809 0.3243 0.8138 0.029 Uiso 1 1 calc R . . C5 C 1.0442(3) 0.2088(2) 0.6957(2) 0.0247(7) Uani 1 1 d . . . H5 H 1.0420 0.2602 0.6637 0.030 Uiso 1 1 calc R . . C6 C 0.9403(3) 0.0976(2) 0.6224(2) 0.0235(6) Uani 1 1 d . . . H6 H 0.9579 0.0900 0.5668 0.028 Uiso 1 1 calc R . . C7 C 0.7129(3) -0.0036(3) 0.5111(2) 0.0280(7) Uani 1 1 d . . . C8 C 0.7351(3) 0.0622(3) 0.7226(3) 0.0347(8) Uani 1 1 d . . . C9 C 0.8636(3) 0.3034(2) 0.8205(2) 0.0249(7) Uani 1 1 d . . . C10 C 1.0442(3) 0.1907(3) 0.8491(2) 0.0327(8) Uani 1 1 d . . . C11 C 1.1764(3) 0.2259(3) 0.7259(2) 0.0308(7) Uani 1 1 d . . . C12 C 0.9288(3) -0.0030(3) 0.6458(2) 0.0302(7) Uani 1 1 d . . . C13 C 0.5428(5) -0.3909(4) 0.3465(4) 0.0775(17) Uani 1 1 d . . . H13 H 0.4734 -0.4087 0.2937 0.093 Uiso 1 1 calc R . . C14 C 0.5457(5) -0.4717(4) 0.3804(4) 0.0836(19) Uani 1 1 d . . . H14 H 0.4805 -0.5420 0.3491 0.100 Uiso 1 1 calc R . . C15 C 0.6430(4) -0.4500(3) 0.4595(3) 0.0416(9) Uani 1 1 d . . . C16 C 0.7348(6) -0.3443(4) 0.4989(3) 0.084(2) Uani 1 1 d . . . H16 H 0.8038 -0.3235 0.5532 0.100 Uiso 1 1 calc R . . C17 C 0.7270(6) -0.2684(4) 0.4600(3) 0.0763(17) Uani 1 1 d . . . H17 H 0.7920 -0.1978 0.4883 0.092 Uiso 1 1 calc R . . C18 C 0.6516(4) -0.5341(3) 0.4990(3) 0.0481(10) Uani 1 1 d . . . C19 C 0.5898(5) -0.6430(4) 0.4450(4) 0.0778(17) Uani 1 1 d . . . H19 H 0.5392 -0.6667 0.3817 0.093 Uiso 1 1 calc R . . C20 C 0.6038(6) -0.7170(4) 0.4860(5) 0.092(2) Uani 1 1 d . . . H20 H 0.5620 -0.7899 0.4477 0.111 Uiso 1 1 calc R . . C21 C 0.7308(5) -0.5880(4) 0.6251(4) 0.0660(13) Uani 1 1 d . . . H21 H 0.7804 -0.5672 0.6882 0.079 Uiso 1 1 calc R . . C22 C 0.7251(5) -0.5071(4) 0.5919(3) 0.0590(12) Uani 1 1 d . . . H22 H 0.7704 -0.4349 0.6319 0.071 Uiso 1 1 calc R . . C23 C 0.5977(4) 0.0118(3) 0.2629(3) 0.0438(9) Uani 1 1 d . . . H23 H 0.5665 0.0128 0.3081 0.053 Uiso 1 1 calc R . . C24 C 0.5883(4) 0.0764(3) 0.2118(3) 0.0460(9) Uani 1 1 d . . . H24 H 0.5512 0.1194 0.2227 0.055 Uiso 1 1 calc R . . C25 C 0.6337(3) 0.0782(3) 0.1437(2) 0.0355(8) Uani 1 1 d . . . C26 C 0.6897(4) 0.0134(3) 0.1338(3) 0.0445(9) Uani 1 1 d . . . H26 H 0.7236 0.0125 0.0903 0.053 Uiso 1 1 calc R . . C27 C 0.6956(4) -0.0496(3) 0.1879(3) 0.0397(8) Uani 1 1 d . . . H27 H 0.7340 -0.0922 0.1794 0.048 Uiso 1 1 calc R . . C28 C 0.6197(3) 0.1426(3) 0.0825(3) 0.0382(8) Uani 1 1 d . . . C29 C 0.5571(4) 0.2018(4) 0.0882(3) 0.0565(11) Uani 1 1 d . . . H29 H 0.5255 0.2052 0.1331 0.068 Uiso 1 1 calc R . . C30 C 0.5414(5) 0.2560(4) 0.0272(4) 0.0647(13) Uani 1 1 d . . . H30 H 0.4981 0.2948 0.0321 0.078 Uiso 1 1 calc R . . C31 C 0.6466(4) 0.2012(4) -0.0423(3) 0.0551(11) Uani 1 1 d . . . H31 H 0.6793 0.2008 -0.0867 0.066 Uiso 1 1 calc R . . C32 C 0.6659(4) 0.1444(3) 0.0156(3) 0.0512(10) Uani 1 1 d . . . H32 H 0.7105 0.1072 0.0095 0.061 Uiso 1 1 calc R . . C33 C 0.9954(4) 0.6346(3) 0.8705(3) 0.0438(9) Uani 1 1 d . . . H33 H 0.9489 0.6539 0.8981 0.053 Uiso 1 1 calc R . . C34 C 1.0102(4) 0.6699(3) 0.7992(3) 0.0440(9) Uani 1 1 d . . . H34 H 0.9755 0.7128 0.7806 0.053 Uiso 1 1 calc R . . C35 C 1.0766(3) 0.6416(3) 0.7553(3) 0.0380(8) Uani 1 1 d . . . C36 C 1.1306(4) 0.5815(3) 0.7899(3) 0.0439(9) Uani 1 1 d . . . H36 H 1.1783 0.5620 0.7640 0.053 Uiso 1 1 calc R . . C37 C 1.1132(4) 0.5513(3) 0.8623(3) 0.0400(9) Uani 1 1 d . . . H37 H 1.1517 0.5125 0.8851 0.048 Uiso 1 1 calc R . . C38 C 1.0872(4) 0.6715(3) 0.6736(3) 0.0442(9) Uani 1 1 d . . . C39 C 1.0714(5) 0.7553(4) 0.6559(3) 0.0588(12) Uani 1 1 d . . . H39 H 1.0554 0.7983 0.6967 0.071 Uiso 1 1 calc R . . C40 C 1.0793(6) 0.7767(4) 0.5774(4) 0.0749(16) Uani 1 1 d . . . H40 H 1.0710 0.8365 0.5686 0.090 Uiso 1 1 calc R . . C41 C 1.1165(7) 0.6406(5) 0.5332(4) 0.088(2) Uani 1 1 d . . . H41 H 1.1328 0.5995 0.4910 0.106 Uiso 1 1 calc R . . C42 C 1.1146(6) 0.6136(5) 0.6105(4) 0.0772(17) Uani 1 1 d . . . H42 H 1.1313 0.5577 0.6204 0.093 Uiso 1 1 calc R . . N1 N 0.6307(3) -0.2919(2) 0.3837(2) 0.0347(7) Uani 1 1 d . . . N2 N 0.6716(4) -0.6919(3) 0.5747(3) 0.0735(13) Uani 1 1 d . . . N3 N 0.6492(3) -0.0527(2) 0.25190(19) 0.0318(6) Uani 1 1 d . . . N4 N 0.5849(3) 0.2559(3) -0.0385(2) 0.0543(9) Uani 1 1 d . . . N5 N 1.0440(3) 0.5742(2) 0.9024(2) 0.0355(7) Uani 1 1 d . . . N6 N 1.0976(5) 0.7186(4) 0.5140(3) 0.0807(15) Uani 1 1 d . . . O1 O 0.7429(2) -0.04076(18) 0.44965(14) 0.0288(5) Uani 1 1 d . . . O2 O 0.6050(2) -0.0432(2) 0.50685(18) 0.0534(8) Uani 1 1 d . . . O3 O 0.6295(3) -0.0267(2) 0.67215(19) 0.0484(7) Uani 1 1 d . . . H3A H 0.6068 -0.0320 0.6171 0.073 Uiso 1 1 calc R . . O4 O 0.7858(3) 0.0858(2) 0.80617(18) 0.0492(7) Uani 1 1 d . . . O5 O 0.7648(2) 0.3059(2) 0.79809(16) 0.0372(6) Uani 1 1 d . . . O6 O 0.9502(2) 0.35265(18) 0.90383(15) 0.0305(5) Uani 1 1 d . . . O7 O 1.0486(3) 0.2302(2) 0.93231(16) 0.0458(7) Uani 1 1 d . . . H7 H 1.0162 0.2698 0.9309 0.069 Uiso 1 1 calc R . . O8 O 1.0698(3) 0.1181(2) 0.83179(17) 0.0446(7) Uani 1 1 d . . . O9 O 1.2598(2) 0.3094(2) 0.7928(2) 0.0544(8) Uani 1 1 d . . . O10 O 1.1951(2) 0.15696(18) 0.67810(16) 0.0318(5) Uani 1 1 d . . . O11 O 1.0162(2) -0.0308(2) 0.6463(2) 0.0423(6) Uani 1 1 d . . . H11 H 1.0751 0.0202 0.6472 0.064 Uiso 1 1 calc R . . O12 O 0.8399(2) -0.0609(2) 0.65536(19) 0.0405(6) Uani 1 1 d . . . O1W O 0.4766(2) -0.1739(2) 0.32841(16) 0.0357(6) Uani 1 1 d . . . H1WB H 0.4914 -0.1428 0.3827 0.054 Uiso 1 1 calc R . . O2W O 0.5281(2) -0.30044(19) 0.18991(16) 0.0356(6) Uani 1 1 d . . . H2WB H 0.4972 -0.2794 0.1501 0.053 Uiso 1 1 calc R . . O3W O 1.1826(2) 0.5201(2) 1.06077(17) 0.0392(6) Uani 1 1 d . . . H3WB H 1.2261 0.5774 1.1056 0.059 Uiso 1 1 calc R . . O4W O 0.8499(7) 0.8015(5) 0.7564(4) 0.140(2) Uani 1 1 d . . . O5W O 0.6444(8) 0.7339(8) 0.7977(6) 0.235(5) Uani 1 1 d . . . O6W O 0.7322(6) 0.9488(5) 0.9071(5) 0.139(2) Uani 1 1 d . . . O7W O 0.3488(12) 0.4589(6) 0.9749(5) 0.283(6) Uani 1 1 d . . . O8W O 0.0461(6) 0.9749(5) 0.9304(4) 0.140(2) Uani 1 1 d . . . O9W O 0.3112(13) 0.3763(16) 0.0959(9) 0.406(11) Uani 1 1 d . . . H7WA H 0.4010 0.4331 0.9729 0.487 Uiso 1 1 d R . . H1WA H 0.3979 -0.2234 0.2990 0.487 Uiso 1 1 d R . . H5WA H 0.6280 0.7822 0.7798 0.487 Uiso 1 1 d R . . H2WA H 0.5873 -0.3054 0.1810 0.487 Uiso 1 1 d R . . H3WA H 1.2172 0.4802 1.0545 0.487 Uiso 1 1 d R . . H4WA H 0.8304 0.8239 0.7130 0.487 Uiso 1 1 d R . . H8WA H 0.0072 0.9221 0.8764 0.487 Uiso 1 1 d R . . H6WA H 0.7366 0.9831 0.8704 0.487 Uiso 1 1 d R . . H8WB H 0.0603 1.0268 0.9131 0.487 Uiso 1 1 d R . . H4WB H 0.7711 0.7690 0.7222 0.487 Uiso 1 1 d R . . H6WB H 0.7833 0.9344 0.8908 0.487 Uiso 1 1 d R . . H7WB H 0.3339 0.4061 0.9264 0.487 Uiso 1 1 d R . . H9WA H 0.3525 0.4451 0.1150 0.487 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0198(2) 0.0286(2) 0.0201(2) 0.00389(18) 0.00652(18) 0.01013(18) Co2 0.0262(3) 0.0271(3) 0.0179(3) -0.0002(2) 0.0063(3) 0.0127(3) C1 0.0228(16) 0.0249(15) 0.0196(15) 0.0039(12) 0.0090(13) 0.0108(13) C2 0.0210(15) 0.0249(15) 0.0193(15) 0.0002(12) 0.0066(13) 0.0101(13) C3 0.0243(16) 0.0228(15) 0.0188(14) 0.0036(12) 0.0086(13) 0.0112(13) C4 0.0209(15) 0.0231(15) 0.0196(15) -0.0002(12) 0.0043(12) 0.0091(13) C5 0.0246(16) 0.0243(15) 0.0220(15) 0.0049(12) 0.0086(13) 0.0109(13) C6 0.0238(16) 0.0245(15) 0.0192(15) 0.0036(12) 0.0087(13) 0.0107(13) C7 0.0246(17) 0.0297(17) 0.0211(16) 0.0013(13) 0.0063(13) 0.0110(14) C8 0.0347(19) 0.0295(17) 0.036(2) 0.0031(15) 0.0209(17) 0.0116(15) C9 0.0235(16) 0.0206(15) 0.0231(16) 0.0018(12) 0.0076(13) 0.0078(13) C10 0.0341(19) 0.0379(19) 0.0233(17) 0.0053(14) 0.0081(14) 0.0201(16) C11 0.0249(17) 0.0310(17) 0.0290(17) 0.0033(14) 0.0088(14) 0.0117(15) C12 0.0286(18) 0.0270(16) 0.0256(17) 0.0015(13) 0.0052(14) 0.0128(15) C13 0.061(3) 0.061(3) 0.069(3) 0.035(3) -0.004(3) 0.007(3) C14 0.074(4) 0.044(3) 0.075(4) 0.029(3) -0.007(3) -0.001(2) C15 0.037(2) 0.040(2) 0.040(2) 0.0156(17) 0.0108(17) 0.0141(17) C16 0.106(5) 0.043(3) 0.047(3) 0.013(2) -0.016(3) 0.022(3) C17 0.096(4) 0.039(2) 0.047(3) 0.006(2) -0.012(3) 0.024(3) C18 0.044(2) 0.044(2) 0.053(2) 0.0234(19) 0.017(2) 0.0159(19) C19 0.080(4) 0.042(3) 0.060(3) 0.016(2) 0.000(3) 0.002(2) C20 0.100(5) 0.041(3) 0.089(4) 0.031(3) 0.013(4) 0.006(3) C21 0.080(4) 0.068(3) 0.061(3) 0.040(3) 0.030(3) 0.037(3) C22 0.072(3) 0.047(2) 0.051(3) 0.024(2) 0.017(2) 0.026(2) C23 0.059(3) 0.048(2) 0.042(2) 0.0208(18) 0.033(2) 0.031(2) C24 0.059(3) 0.048(2) 0.052(2) 0.0254(19) 0.033(2) 0.035(2) C25 0.0333(19) 0.0341(18) 0.0291(18) 0.0084(15) 0.0091(15) 0.0108(16) C26 0.048(2) 0.059(2) 0.040(2) 0.0246(19) 0.0259(19) 0.029(2) C27 0.042(2) 0.051(2) 0.040(2) 0.0198(18) 0.0228(18) 0.0285(19) C28 0.0331(19) 0.0365(19) 0.0323(19) 0.0117(15) 0.0076(16) 0.0092(16) C29 0.062(3) 0.073(3) 0.053(3) 0.034(2) 0.029(2) 0.041(3) C30 0.069(3) 0.078(3) 0.064(3) 0.039(3) 0.025(3) 0.047(3) C31 0.060(3) 0.057(3) 0.048(2) 0.028(2) 0.025(2) 0.021(2) C32 0.062(3) 0.051(2) 0.049(2) 0.025(2) 0.028(2) 0.027(2) C33 0.055(2) 0.054(2) 0.039(2) 0.0189(18) 0.0260(19) 0.035(2) C34 0.054(2) 0.051(2) 0.041(2) 0.0206(18) 0.0244(19) 0.032(2) C35 0.037(2) 0.0321(18) 0.038(2) 0.0089(15) 0.0177(17) 0.0103(16) C36 0.049(2) 0.044(2) 0.050(2) 0.0178(18) 0.032(2) 0.0244(19) C37 0.043(2) 0.0374(19) 0.046(2) 0.0150(17) 0.0221(18) 0.0218(17) C38 0.052(2) 0.039(2) 0.043(2) 0.0152(17) 0.0276(19) 0.0163(18) C39 0.086(4) 0.060(3) 0.055(3) 0.029(2) 0.042(3) 0.044(3) C40 0.122(5) 0.076(3) 0.078(4) 0.050(3) 0.064(4) 0.067(4) C41 0.151(6) 0.099(4) 0.088(4) 0.055(4) 0.093(5) 0.085(5) C42 0.129(5) 0.084(4) 0.081(4) 0.055(3) 0.078(4) 0.072(4) N1 0.0321(16) 0.0357(16) 0.0313(15) 0.0104(13) 0.0100(13) 0.0146(13) N2 0.086(3) 0.052(2) 0.077(3) 0.040(2) 0.031(3) 0.022(2) N3 0.0298(15) 0.0357(15) 0.0270(14) 0.0092(12) 0.0108(12) 0.0143(13) N4 0.051(2) 0.054(2) 0.044(2) 0.0244(17) 0.0091(17) 0.0152(18) N5 0.0387(17) 0.0359(16) 0.0291(15) 0.0064(13) 0.0140(13) 0.0176(14) N6 0.142(5) 0.071(3) 0.080(3) 0.050(3) 0.080(3) 0.062(3) O1 0.0256(12) 0.0326(12) 0.0214(11) 0.0004(9) 0.0089(9) 0.0124(10) O2 0.0218(13) 0.0676(19) 0.0353(14) -0.0165(13) 0.0088(11) 0.0070(13) O3 0.0403(15) 0.0378(14) 0.0459(15) -0.0011(12) 0.0266(13) -0.0004(12) O4 0.0573(18) 0.0460(15) 0.0332(15) 0.0156(12) 0.0207(14) 0.0116(14) O5 0.0236(12) 0.0458(14) 0.0270(12) -0.0062(11) 0.0039(10) 0.0164(11) O6 0.0316(12) 0.0310(12) 0.0193(11) -0.0026(9) 0.0043(10) 0.0164(10) O7 0.0650(18) 0.0629(18) 0.0208(12) 0.0109(12) 0.0141(12) 0.0461(16) O8 0.0664(18) 0.0524(16) 0.0327(14) 0.0168(12) 0.0202(13) 0.0444(15) O9 0.0232(13) 0.0488(16) 0.0528(17) -0.0213(13) 0.0026(12) 0.0099(12) O10 0.0238(12) 0.0343(12) 0.0305(12) 0.0007(10) 0.0102(10) 0.0134(10) O11 0.0354(14) 0.0321(13) 0.0594(17) 0.0099(12) 0.0175(13) 0.0207(12) O12 0.0393(15) 0.0331(13) 0.0494(16) 0.0174(12) 0.0206(13) 0.0144(12) O1W 0.0219(12) 0.0469(14) 0.0267(12) 0.0026(11) 0.0085(10) 0.0116(11) O2W 0.0332(13) 0.0393(13) 0.0253(12) 0.0079(10) 0.0062(11) 0.0149(11) O3W 0.0306(13) 0.0387(14) 0.0324(13) -0.0018(11) 0.0048(11) 0.0147(11) O4W 0.244(7) 0.158(5) 0.165(5) 0.125(4) 0.139(5) 0.162(5) O5W 0.164(7) 0.229(9) 0.178(8) 0.001(7) 0.052(6) 0.016(7) O6W 0.188(6) 0.188(6) 0.182(6) 0.144(5) 0.143(5) 0.134(5) O7W 0.451(15) 0.115(5) 0.092(5) -0.025(4) 0.033(7) 0.044(7) O8W 0.188(6) 0.182(6) 0.167(5) 0.135(5) 0.116(5) 0.130(5) O9W 0.328(17) 0.69(3) 0.272(15) 0.248(19) 0.147(14) 0.25(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.069(2) . ? Co1 O1 2.086(2) . ? Co1 O10 2.103(2) 2_756 ? Co1 O2W 2.134(2) . ? Co1 N3 2.161(3) . ? Co1 N1 2.171(3) . ? Co2 O6 2.070(2) 2_767 ? Co2 O6 2.070(2) . ? Co2 O3W 2.132(2) . ? Co2 O3W 2.132(2) 2_767 ? Co2 N5 2.153(3) . ? Co2 N5 2.153(3) 2_767 ? C1 C7 1.526(4) . ? C1 C6 1.538(4) . ? C1 C2 1.558(4) . ? C1 H1 0.9800 . ? C2 C8 1.517(5) . ? C2 C3 1.540(4) . ? C2 H2 0.9800 . ? C3 C9 1.526(4) . ? C3 C4 1.548(4) . ? C3 H3 0.9800 . ? C4 C10 1.524(5) . ? C4 C5 1.542(4) . ? C4 H4 0.9800 . ? C5 C11 1.525(4) . ? C5 C6 1.541(4) . ? C5 H5 0.9800 . ? C6 C12 1.519(4) . ? C6 H6 0.9800 . ? C7 O2 1.256(4) . ? C7 O1 1.256(4) . ? C8 O4 1.210(4) . ? C8 O3 1.311(4) . ? C9 O5 1.229(4) . ? C9 O6 1.285(4) . ? C10 O8 1.207(4) . ? C10 O7 1.316(4) . ? C11 O9 1.241(4) . ? C11 O10 1.266(4) . ? C12 O12 1.204(4) . ? C12 O11 1.325(4) . ? C13 N1 1.292(6) . ? C13 C14 1.376(7) . ? C13 H13 0.9300 . ? C14 C15 1.364(6) . ? C14 H14 0.9300 . ? C15 C16 1.371(6) . ? C15 C18 1.489(5) . ? C16 C17 1.374(7) . ? C16 H16 0.9300 . ? C17 N1 1.323(6) . ? C17 H17 0.9300 . ? C18 C19 1.378(6) . ? C18 C22 1.382(6) . ? C19 C20 1.389(7) . ? C19 H19 0.9300 . ? C20 N2 1.313(7) . ? C20 H20 0.9300 . ? C21 N2 1.311(6) . ? C21 C22 1.380(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N3 1.335(5) . ? C23 C24 1.366(5) . ? C23 H23 0.9300 . ? C24 C25 1.386(5) . ? C24 H24 0.9300 . ? C25 C26 1.381(5) . ? C25 C28 1.491(5) . ? C26 C27 1.376(5) . ? C26 H26 0.9300 . ? C27 N3 1.335(4) . ? C27 H27 0.9300 . ? C28 C32 1.374(6) . ? C28 C29 1.378(6) . ? C29 C30 1.378(6) . ? C29 H29 0.9300 . ? C30 N4 1.334(6) . ? C30 H30 0.9300 . ? C31 N4 1.311(6) . ? C31 C32 1.377(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 N5 1.338(5) . ? C33 C34 1.374(5) . ? C33 H33 0.9300 . ? C34 C35 1.379(5) . ? C34 H34 0.9300 . ? C35 C36 1.390(6) . ? C35 C38 1.485(5) . ? C36 C37 1.368(5) . ? C36 H36 0.9300 . ? C37 N5 1.339(5) . ? C37 H37 0.9300 . ? C38 C39 1.353(6) . ? C38 C42 1.391(6) . ? C39 C40 1.379(6) . ? C39 H39 0.9300 . ? C40 N6 1.315(6) . ? C40 H40 0.9300 . ? C41 N6 1.300(7) . ? C41 C42 1.376(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? O3 H3A 0.8200 . ? O7 H7 0.8200 . ? O10 Co1 2.103(2) 2_756 ? O11 H11 0.8200 . ? O1W H1WB 0.8200 . ? O1W H1WA 0.8837 . ? O2W H2WB 0.8200 . ? O2W H2WA 0.8402 . ? O3W H3WB 0.8200 . ? O3W H3WA 0.8523 . ? O4W H4WA 0.8337 . ? O4W H4WB 0.8649 . ? O5W H5WA 0.8690 . ? O6W H6WA 0.8392 . ? O6W H6WB 0.8527 . ? O7W H7WA 0.8837 . ? O7W H7WB 0.8797 . ? O8W H8WA 0.8720 . ? O8W H8WB 0.8171 . ? O9W H9WA 0.8500 . ? 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 O1W Co1 O1 90.28(9) . . ? O1W Co1 O10 176.60(9) . 2_756 ? O1 Co1 O10 86.32(8) . 2_756 ? O1W Co1 O2W 89.93(9) . . ? O1 Co1 O2W 179.77(9) . . ? O10 Co1 O2W 93.47(9) 2_756 . ? O1W Co1 N3 90.28(11) . . ? O1 Co1 N3 89.10(10) . . ? O10 Co1 N3 89.75(10) 2_756 . ? O2W Co1 N3 90.83(10) . . ? O1W Co1 N1 93.94(11) . . ? O1 Co1 N1 93.67(10) . . ? O10 Co1 N1 86.20(10) 2_756 . ? O2W Co1 N1 86.39(10) . . ? N3 Co1 N1 174.93(11) . . ? O6 Co2 O6 179.999(1) 2_767 . ? O6 Co2 O3W 91.48(9) 2_767 . ? O6 Co2 O3W 88.52(9) . . ? O6 Co2 O3W 88.52(9) 2_767 2_767 ? O6 Co2 O3W 91.48(9) . 2_767 ? O3W Co2 O3W 180.000(1) . 2_767 ? O6 Co2 N5 92.23(10) 2_767 . ? O6 Co2 N5 87.77(10) . . ? O3W Co2 N5 90.93(11) . . ? O3W Co2 N5 89.07(11) 2_767 . ? O6 Co2 N5 87.77(10) 2_767 2_767 ? O6 Co2 N5 92.23(10) . 2_767 ? O3W Co2 N5 89.07(11) . 2_767 ? O3W Co2 N5 90.93(11) 2_767 2_767 ? N5 Co2 N5 180.000(1) . 2_767 ? C7 C1 C6 111.7(2) . . ? C7 C1 C2 116.0(2) . . ? C6 C1 C2 115.7(2) . . ? C7 C1 H1 103.8 . . ? C6 C1 H1 103.8 . . ? C2 C1 H1 103.8 . . ? C8 C2 C3 111.0(3) . . ? C8 C2 C1 119.3(3) . . ? C3 C2 C1 108.7(2) . . ? C8 C2 H2 105.6 . . ? C3 C2 H2 105.6 . . ? C1 C2 H2 105.6 . . ? C9 C3 C2 113.4(2) . . ? C9 C3 C4 115.8(2) . . ? C2 C3 C4 114.9(2) . . ? C9 C3 H3 103.6 . . ? C2 C3 H3 103.6 . . ? C4 C3 H3 103.6 . . ? C10 C4 C5 111.0(3) . . ? C10 C4 C3 119.4(3) . . ? C5 C4 C3 109.0(2) . . ? C10 C4 H4 105.4 . . ? C5 C4 H4 105.4 . . ? C3 C4 H4 105.4 . . ? C11 C5 C6 117.1(3) . . ? C11 C5 C4 111.5(3) . . ? C6 C5 C4 114.0(2) . . ? C11 C5 H5 104.2 . . ? C6 C5 H5 104.2 . . ? C4 C5 H5 104.2 . . ? C12 C6 C1 110.8(3) . . ? C12 C6 C5 117.8(3) . . ? C1 C6 C5 109.8(2) . . ? C12 C6 H6 105.9 . . ? C1 C6 H6 105.9 . . ? C5 C6 H6 105.9 . . ? O2 C7 O1 124.3(3) . . ? O2 C7 C1 119.8(3) . . ? O1 C7 C1 115.9(3) . . ? O4 C8 O3 120.5(3) . . ? O4 C8 C2 121.8(3) . . ? O3 C8 C2 117.4(3) . . ? O5 C9 O6 123.5(3) . . ? O5 C9 C3 119.6(3) . . ? O6 C9 C3 116.7(3) . . ? O8 C10 O7 120.3(3) . . ? O8 C10 C4 122.1(3) . . ? O7 C10 C4 117.3(3) . . ? O9 C11 O10 123.9(3) . . ? O9 C11 C5 118.1(3) . . ? O10 C11 C5 117.9(3) . . ? O12 C12 O11 120.6(3) . . ? O12 C12 C6 122.6(3) . . ? O11 C12 C6 116.6(3) . . ? N1 C13 C14 123.9(5) . . ? N1 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 114.6(4) . . ? C14 C15 C18 123.3(4) . . ? C16 C15 C18 122.1(4) . . ? C15 C16 C17 121.4(5) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? N1 C17 C16 122.5(5) . . ? N1 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C19 C18 C22 115.9(4) . . ? C19 C18 C15 122.2(4) . . ? C22 C18 C15 121.8(4) . . ? C18 C19 C20 119.3(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N2 C20 C19 124.9(5) . . ? N2 C20 H20 117.5 . . ? C19 C20 H20 117.5 . . ? N2 C21 C22 125.0(5) . . ? N2 C21 H21 117.5 . . ? C22 C21 H21 117.5 . . ? C21 C22 C18 119.7(4) . . ? C21 C22 H22 120.2 . . ? C18 C22 H22 120.2 . . ? N3 C23 C24 123.9(3) . . ? N3 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 115.7(3) . . ? C26 C25 C28 121.7(3) . . ? C24 C25 C28 122.5(3) . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N3 C27 C26 123.3(3) . . ? N3 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? C32 C28 C29 116.1(4) . . ? C32 C28 C25 122.0(4) . . ? C29 C28 C25 121.9(4) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N4 C30 C29 123.6(5) . . ? N4 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? N4 C31 C32 123.9(4) . . ? N4 C31 H31 118.1 . . ? C32 C31 H31 118.1 . . ? C28 C32 C31 120.3(4) . . ? C28 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? N5 C33 C34 123.7(4) . . ? N5 C33 H33 118.1 . . ? C34 C33 H33 118.1 . . ? C33 C34 C35 120.0(4) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 116.6(3) . . ? C34 C35 C38 121.5(4) . . ? C36 C35 C38 121.9(3) . . ? C37 C36 C35 119.7(4) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? N5 C37 C36 124.0(4) . . ? N5 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? C39 C38 C42 116.2(4) . . ? C39 C38 C35 123.0(4) . . ? C42 C38 C35 120.8(4) . . ? C38 C39 C40 119.9(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? N6 C40 C39 124.7(5) . . ? N6 C40 H40 117.7 . . ? C39 C40 H40 117.7 . . ? N6 C41 C42 125.6(5) . . ? N6 C41 H41 117.2 . . ? C42 C41 H41 117.2 . . ? C41 C42 C38 118.6(5) . . ? C41 C42 H42 120.7 . . ? C38 C42 H42 120.7 . . ? C13 N1 C17 116.7(4) . . ? C13 N1 Co1 123.9(3) . . ? C17 N1 Co1 119.1(3) . . ? C21 N2 C20 115.2(4) . . ? C23 N3 C27 116.0(3) . . ? C23 N3 Co1 121.2(2) . . ? C27 N3 Co1 122.3(2) . . ? C31 N4 C30 116.2(4) . . ? C37 N5 C33 115.8(3) . . ? C37 N5 Co2 120.1(2) . . ? C33 N5 Co2 123.7(2) . . ? C41 N6 C40 114.8(4) . . ? C7 O1 Co1 130.9(2) . . ? C8 O3 H3A 109.5 . . ? C9 O6 Co2 127.9(2) . . ? C10 O7 H7 109.5 . . ? C11 O10 Co1 128.7(2) . 2_756 ? C12 O11 H11 109.5 . . ? Co1 O1W H1WB 109.5 . . ? Co1 O1W H1WA 133.1 . . ? H1WB O1W H1WA 109.0 . . ? Co1 O2W H2WB 109.5 . . ? Co1 O2W H2WA 96.9 . . ? H2WB O2W H2WA 107.0 . . ? Co2 O3W H3WB 109.5 . . ? Co2 O3W H3WA 135.6 . . ? H3WB O3W H3WA 114.3 . . ? H4WA O4W H4WB 66.9 . . ? H6WA O6W H6WB 82.4 . . ? H7WA O7W H7WB 56.3 . . ? H8WA O8W H8WB 99.9 . . ? 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 O7W H7WB O9 0.88 2.00 2.833(7) 157.9 1_455 O4W H4WB O5W 0.86 2.28 2.778(11) 117.0 . O8W H8WB O8 0.82 2.02 2.807(5) 162.3 1_465 O6W H6WA O4 0.84 1.98 2.799(5) 166.9 1_565 O8W H8WA O4W 0.87 2.10 2.918(10) 154.9 1_455 O4W H4WA O12 0.83 2.02 2.799(5) 154.6 1_565 O3W H3WA O7W 0.85 2.48 3.152(13) 136.9 1_655 O3W H3WA O9W 0.85 2.32 3.118(17) 156.8 1_656 O2W H2WA O10 0.84 2.68 3.085(3) 111.2 2_756 O2W H2WA O9 0.84 1.91 2.711(4) 159.4 2_756 O5W H5WA O6W 0.87 2.36 2.785(12) 110.0 . O1W H1WA O5 0.88 1.90 2.743(3) 158.5 2_656 O3W H3WB O5 0.82 1.97 2.699(3) 147.9 2_767 O2W H2WB N4 0.82 1.95 2.759(4) 169.0 2_655 O1W H1WB O2 0.82 1.91 2.659(3) 151.0 . O11 H11 O10 0.82 1.81 2.603(3) 160.9 . O7 H7 O6 0.82 1.75 2.551(3) 167.0 . O3 H3A O2 0.82 1.74 2.527(4) 161.0 . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.204 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.075 # Attachment 'web_deposit_cif_file_8_xingfeifei_1318817696.9.cif' data_11d _database_code_depnum_ccdc_archive 'CCDC 848881' #TrackingRef 'web_deposit_cif_file_8_xingfeifei_1318817696.9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Mn N4 O19' _chemical_formula_weight 887.66 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.138(3) _cell_length_b 11.446(2) _cell_length_c 26.722(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.23 _cell_angle_gamma 90.00 _cell_volume 3895.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2416 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 20.45 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 0.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9195 _exptl_absorpt_correction_T_max 0.9195 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15958 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.1705 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5822 _reflns_number_gt 2697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5822 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.20482(6) 0.19860(6) 0.96570(3) 0.0392(2) Uani 1 1 d . . . C1 C 0.0473(4) 0.3533(5) 0.8792(2) 0.0522(15) Uani 1 1 d . . . H1 H 0.0434 0.2860 0.8593 0.063 Uiso 1 1 calc R . . C2 C -0.0099(4) 0.4516(6) 0.8569(3) 0.0661(18) Uani 1 1 d . . . H2 H -0.0518 0.4493 0.8234 0.079 Uiso 1 1 calc R . . C3 C -0.0020(5) 0.5512(6) 0.8862(3) 0.0638(17) Uani 1 1 d . . . H3 H -0.0370 0.6186 0.8719 0.077 Uiso 1 1 calc R . . C4 C 0.0575(4) 0.5522(5) 0.9366(2) 0.0511(15) Uani 1 1 d . . . C5 C 0.0660(5) 0.6534(5) 0.9701(3) 0.0662(18) Uani 1 1 d . . . H5 H 0.0307 0.7219 0.9576 0.079 Uiso 1 1 calc R . . C6 C 0.1240(5) 0.6493(5) 1.0189(3) 0.0613(17) Uani 1 1 d . . . H6 H 0.1290 0.7156 1.0395 0.074 Uiso 1 1 calc R . . C7 C 0.1777(4) 0.5473(4) 1.0398(2) 0.0470(14) Uani 1 1 d . . . C8 C 0.2394(5) 0.5381(5) 1.0909(2) 0.0626(17) Uani 1 1 d . . . H8 H 0.2492 0.6035 1.1122 0.075 Uiso 1 1 calc R . . C9 C 0.2848(5) 0.4346(5) 1.1095(2) 0.0618(16) Uani 1 1 d . . . H9 H 0.3238 0.4280 1.1435 0.074 Uiso 1 1 calc R . . C10 C 0.2712(5) 0.3394(5) 1.0762(2) 0.0569(16) Uani 1 1 d . . . H10 H 0.3018 0.2688 1.0891 0.068 Uiso 1 1 calc R . . C11 C 0.1717(4) 0.4457(4) 1.0089(2) 0.0412(12) Uani 1 1 d . . . C12 C 0.1113(4) 0.4505(4) 0.9562(2) 0.0407(12) Uani 1 1 d . . . C13 C 0.3123(5) -0.0062(5) 1.0427(2) 0.0595(16) Uani 1 1 d . . . H13 H 0.2450 -0.0373 1.0369 0.071 Uiso 1 1 calc R . . C14 C 0.3952(6) -0.0613(5) 1.0788(2) 0.0671(18) Uani 1 1 d . . . H14 H 0.3821 -0.1289 1.0955 0.080 Uiso 1 1 calc R . . C15 C 0.4916(5) -0.0171(5) 1.0892(2) 0.0626(17) Uani 1 1 d . . . H15 H 0.5457 -0.0521 1.1137 0.075 Uiso 1 1 calc R . . C16 C 0.5107(4) 0.0834(5) 1.0624(2) 0.0541(15) Uani 1 1 d . . . C17 C 0.6110(5) 0.1365(7) 1.0712(3) 0.077(2) Uani 1 1 d . . . H17 H 0.6670 0.1046 1.0957 0.092 Uiso 1 1 calc R . . C18 C 0.6269(5) 0.2332(6) 1.0445(3) 0.073(2) Uani 1 1 d . . . H18 H 0.6925 0.2690 1.0524 0.088 Uiso 1 1 calc R . . C19 C 0.5451(4) 0.2800(5) 1.0050(2) 0.0544(15) Uani 1 1 d . . . C20 C 0.5585(5) 0.3755(6) 0.9735(3) 0.072(2) Uani 1 1 d . . . H20 H 0.6234 0.4122 0.9789 0.087 Uiso 1 1 calc R . . C21 C 0.4775(5) 0.4132(6) 0.9359(3) 0.0678(19) Uani 1 1 d . . . H21 H 0.4863 0.4734 0.9140 0.081 Uiso 1 1 calc R . . C22 C 0.3802(4) 0.3602(5) 0.9304(2) 0.0571(16) Uani 1 1 d . . . H22 H 0.3242 0.3884 0.9049 0.068 Uiso 1 1 calc R . . C23 C 0.4448(4) 0.2311(5) 0.9961(2) 0.0453(13) Uani 1 1 d . . . C24 C 0.4265(4) 0.1318(5) 1.0265(2) 0.0432(13) Uani 1 1 d . . . C25 C 0.1024(4) 0.0091(4) 0.16963(17) 0.0339(11) Uani 1 1 d . . . H25 H 0.0300 0.0215 0.1722 0.041 Uiso 1 1 calc R . . C26 C 0.1603(4) 0.1192(4) 0.19521(18) 0.0332(11) Uani 1 1 d . . . H26 H 0.1210 0.1860 0.1773 0.040 Uiso 1 1 calc R . . C27 C 0.1513(4) 0.1265(4) 0.25156(18) 0.0332(11) Uani 1 1 d . . . H27 H 0.0753 0.1265 0.2484 0.040 Uiso 1 1 calc R . . C28 C 0.1899(3) 0.0173(4) 0.28430(17) 0.0325(11) Uani 1 1 d . . . H28 H 0.1666 0.0271 0.3162 0.039 Uiso 1 1 calc R . . C29 C 0.1285(4) -0.0892(4) 0.25632(18) 0.0337(11) Uani 1 1 d . . . H29 H 0.0549 -0.0676 0.2529 0.040 Uiso 1 1 calc R . . C30 C 0.1401(4) -0.2035(4) 0.2872(2) 0.0458(13) Uani 1 1 d . . . C31 C 0.2382(4) -0.1649(4) 0.1979(2) 0.0436(13) Uani 1 1 d . . . C32 C 0.0922(3) 0.0051(4) 0.11118(18) 0.0369(11) Uani 1 1 d . . . C33 C 0.2669(4) 0.1274(4) 0.18612(18) 0.0401(12) Uani 1 1 d . . . C34 C 0.1873(4) 0.2400(4) 0.2784(2) 0.0448(13) Uani 1 1 d . . . C35 C 0.3080(4) 0.0052(4) 0.30097(17) 0.0366(12) Uani 1 1 d . . . C88 C 0.1354(4) -0.1044(4) 0.20091(18) 0.0353(11) Uani 1 1 d . . . H88 H 0.0801 -0.1609 0.1861 0.042 Uiso 1 1 calc R . . N1 N 0.3618(3) 0.2722(4) 0.95915(16) 0.0472(11) Uani 1 1 d . . . N2 N 0.3276(3) 0.0889(4) 1.01684(17) 0.0447(11) Uani 1 1 d . . . N3 N 0.2171(3) 0.3428(3) 1.02699(17) 0.0443(11) Uani 1 1 d . . . N4 N 0.1068(3) 0.3515(4) 0.92721(16) 0.0405(10) Uani 1 1 d . . . O2W O 0.0820(3) 0.1082(3) 0.98852(13) 0.0495(9) Uani 1 1 d . . . O1 O 0.2351(3) 0.2465(3) 0.32348(14) 0.0601(12) Uani 1 1 d . . . O2 O 0.1550(3) 0.3317(3) 0.24935(14) 0.0555(10) Uani 1 1 d . . . H2A H 0.1848 0.3902 0.2635 0.083 Uiso 1 1 calc R . . O3 O 0.3125(3) 0.2317(3) 0.19876(15) 0.0521(10) Uani 1 1 d . . . H3A H 0.3721 0.2305 0.1944 0.078 Uiso 1 1 calc R . . O4 O 0.3078(3) 0.0500(3) 0.16613(16) 0.0594(11) Uani 1 1 d . . . O5 O 0.0709(3) 0.1006(3) 0.08748(13) 0.0467(9) Uani 1 1 d . . . O6 O 0.0975(3) -0.0914(3) 0.08968(13) 0.0496(9) Uani 1 1 d . . . O7 O 0.2428(3) -0.2029(3) 0.15121(14) 0.0553(10) Uani 1 1 d . . . H7 H 0.2004 -0.1667 0.1290 0.083 Uiso 1 1 calc R . . O8 O 0.3082(3) -0.1854(3) 0.23476(14) 0.0520(10) Uani 1 1 d . . . O9 O 0.1012(3) -0.2924(3) 0.26241(15) 0.0578(11) Uani 1 1 d . . . O10 O 0.1859(3) -0.2021(3) 0.33450(14) 0.0552(10) Uani 1 1 d . . . O11 O 0.3418(3) -0.0745(3) 0.33794(14) 0.0519(10) Uani 1 1 d . . . H11 H 0.4032 -0.0611 0.3526 0.078 Uiso 1 1 calc R . . O12 O 0.3692(3) 0.0654(3) 0.28528(14) 0.0504(10) Uani 1 1 d . . . O3W O 0.4302(6) 0.5173(8) 0.2682(5) 0.249(6) Uani 1 1 d . . . O5W O 0.5035(4) 0.2318(5) 0.1780(2) 0.1076(18) Uani 1 1 d . . . O4W O 0.4917(4) 0.2899(6) 0.3106(3) 0.137(2) Uani 1 1 d . . . O6W O 0.2381(4) 0.5223(4) 0.2910(2) 0.1022(18) Uani 1 1 d . . . O7W O 0.1372(3) 0.8749(3) 0.89491(16) 0.0604(11) Uani 1 1 d . . . O1W O 0.1761(3) 0.1064(3) 0.89399(13) 0.0593(11) Uani 1 1 d . . . H1WA H 0.1789 0.0323 0.8960 0.071 Uiso 1 1 d R . . H1WB H 0.2097 0.1158 0.8709 0.071 Uiso 1 1 d R . . H2WB H 0.0638 0.1133 1.0167 0.071 Uiso 1 1 d R . . H2WA H 0.0277 0.1517 0.9843 0.071 Uiso 1 1 d R . . H3WB H 0.4084 0.4841 0.2388 0.071 Uiso 1 1 d R . . H5WA H 0.4742 0.2573 0.1482 0.071 Uiso 1 1 d R . . H4WA H 0.5577 0.3020 0.3125 0.071 Uiso 1 1 d R . . H5WB H 0.5145 0.3004 0.1918 0.071 Uiso 1 1 d R . . H6WB H 0.1823 0.5819 0.2882 0.071 Uiso 1 1 d R . . H7WA H 0.0841 0.8665 0.9075 0.071 Uiso 1 1 d R . . H7WB H 0.1188 0.9208 0.8694 0.071 Uiso 1 1 d R . . H6WA H 0.1999 0.5143 0.3115 0.071 Uiso 1 1 d R . . H3WA H 0.4865 0.5083 0.2582 0.071 Uiso 1 1 d R . . H4WB H 0.4949 0.3583 0.2960 0.071 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0484(4) 0.0310(4) 0.0369(4) -0.0010(4) 0.0082(3) -0.0012(3) C1 0.044(3) 0.057(4) 0.053(4) 0.003(3) 0.007(3) -0.003(3) C2 0.050(3) 0.089(5) 0.060(4) 0.031(4) 0.014(3) 0.009(3) C3 0.065(4) 0.058(4) 0.074(5) 0.029(4) 0.029(4) 0.017(3) C4 0.049(3) 0.039(3) 0.074(4) 0.023(3) 0.030(3) 0.008(2) C5 0.075(4) 0.037(3) 0.098(6) 0.016(3) 0.043(4) 0.011(3) C6 0.081(4) 0.031(3) 0.084(5) -0.003(3) 0.042(4) 0.002(3) C7 0.065(3) 0.031(3) 0.057(4) -0.011(3) 0.040(3) -0.009(2) C8 0.087(4) 0.053(4) 0.053(4) -0.017(3) 0.028(3) -0.017(3) C9 0.087(4) 0.053(4) 0.045(4) -0.013(3) 0.016(3) -0.001(3) C10 0.080(4) 0.044(3) 0.044(4) -0.006(3) 0.011(3) 0.005(3) C11 0.046(3) 0.032(3) 0.051(3) 0.001(2) 0.021(3) -0.004(2) C12 0.040(3) 0.035(3) 0.053(4) 0.001(3) 0.022(3) -0.003(2) C13 0.068(4) 0.054(4) 0.057(4) 0.007(3) 0.017(3) 0.005(3) C14 0.105(6) 0.042(4) 0.059(4) 0.009(3) 0.029(4) 0.020(4) C15 0.073(4) 0.064(4) 0.051(4) 0.007(3) 0.015(3) 0.027(3) C16 0.048(3) 0.070(4) 0.043(3) -0.001(3) 0.008(3) 0.019(3) C17 0.054(4) 0.116(6) 0.058(4) 0.002(4) 0.010(3) 0.026(4) C18 0.047(4) 0.099(5) 0.070(5) 0.008(4) 0.006(3) 0.003(3) C19 0.047(3) 0.068(4) 0.050(4) -0.005(3) 0.014(3) -0.004(3) C20 0.056(4) 0.101(6) 0.061(4) -0.003(4) 0.017(3) -0.029(4) C21 0.060(4) 0.077(4) 0.064(4) 0.019(4) 0.010(3) -0.021(3) C22 0.060(4) 0.063(4) 0.048(4) 0.012(3) 0.013(3) -0.009(3) C23 0.050(3) 0.048(3) 0.038(3) -0.008(3) 0.011(3) 0.009(3) C24 0.047(3) 0.047(3) 0.036(3) -0.007(3) 0.011(2) 0.010(3) C25 0.039(3) 0.032(3) 0.029(3) 0.000(2) 0.006(2) 0.001(2) C26 0.043(3) 0.022(2) 0.031(3) 0.001(2) 0.002(2) -0.0011(19) C27 0.041(3) 0.027(3) 0.033(3) -0.001(2) 0.013(2) 0.004(2) C28 0.049(3) 0.023(2) 0.028(3) 0.001(2) 0.013(2) -0.001(2) C29 0.041(3) 0.026(2) 0.034(3) 0.005(2) 0.007(2) 0.0011(19) C30 0.048(3) 0.029(3) 0.064(4) -0.002(3) 0.019(3) -0.002(2) C31 0.056(3) 0.028(3) 0.047(4) -0.007(2) 0.012(3) -0.002(2) C32 0.031(3) 0.045(3) 0.033(3) -0.005(3) 0.005(2) -0.004(2) C33 0.054(3) 0.037(3) 0.026(3) -0.002(2) 0.005(2) -0.004(2) C34 0.063(4) 0.036(3) 0.038(3) 0.002(2) 0.018(3) 0.009(2) C35 0.057(3) 0.028(3) 0.024(3) -0.005(2) 0.006(2) 0.004(2) C88 0.041(3) 0.025(2) 0.038(3) -0.004(2) 0.006(2) -0.006(2) N1 0.053(3) 0.050(3) 0.037(3) 0.007(2) 0.008(2) -0.004(2) N2 0.056(3) 0.039(3) 0.043(3) 0.005(2) 0.018(2) 0.002(2) N3 0.054(3) 0.037(2) 0.042(3) -0.004(2) 0.012(2) -0.0034(19) N4 0.043(2) 0.041(2) 0.036(3) 0.000(2) 0.008(2) -0.0013(19) O2W 0.053(2) 0.058(2) 0.036(2) 0.0037(17) 0.0086(18) -0.0066(17) O1 0.111(3) 0.031(2) 0.031(2) -0.0084(16) 0.005(2) 0.004(2) O2 0.093(3) 0.0231(19) 0.045(2) 0.0026(17) 0.007(2) 0.0058(18) O3 0.063(2) 0.039(2) 0.056(2) -0.0036(18) 0.018(2) -0.0174(17) O4 0.055(2) 0.061(3) 0.068(3) -0.023(2) 0.028(2) -0.0083(19) O5 0.063(2) 0.044(2) 0.033(2) 0.0045(17) 0.0120(18) 0.0028(17) O6 0.063(2) 0.045(2) 0.036(2) -0.0112(17) 0.0046(18) -0.0010(17) O7 0.073(3) 0.045(2) 0.045(2) -0.0158(19) 0.008(2) 0.0097(19) O8 0.052(2) 0.053(2) 0.044(2) -0.0061(18) -0.0014(19) 0.0134(18) O9 0.071(2) 0.034(2) 0.064(3) 0.006(2) 0.009(2) -0.0137(18) O10 0.087(3) 0.039(2) 0.035(2) 0.0095(17) 0.006(2) -0.0014(19) O11 0.062(2) 0.043(2) 0.040(2) 0.0051(18) -0.0076(19) 0.0098(17) O12 0.053(2) 0.046(2) 0.048(2) 0.0091(18) 0.0045(19) -0.0051(18) O3W 0.139(6) 0.228(10) 0.337(14) 0.050(10) -0.025(8) -0.102(6) O5W 0.093(3) 0.131(5) 0.107(4) -0.036(4) 0.038(3) -0.043(3) O4W 0.112(4) 0.153(6) 0.150(6) -0.031(5) 0.039(4) -0.047(4) O6W 0.157(5) 0.037(2) 0.105(4) -0.005(3) 0.017(4) 0.018(3) O7W 0.066(2) 0.047(2) 0.069(3) 0.000(2) 0.019(2) 0.0031(18) O1W 0.108(3) 0.036(2) 0.040(2) -0.0052(17) 0.030(2) -0.0060(19) _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 O2W 2.128(4) . ? Mn1 O1W 2.138(3) . ? Mn1 N2 2.228(4) . ? Mn1 N4 2.265(4) . ? Mn1 N1 2.275(4) . ? Mn1 N3 2.303(4) . ? C1 N4 1.329(6) . ? C1 C2 1.401(8) . ? C1 H1 0.9300 . ? C2 C3 1.372(9) . ? C2 H2 0.9300 . ? C3 C4 1.381(8) . ? C3 H3 0.9300 . ? C4 C12 1.396(7) . ? C4 C5 1.453(9) . ? C5 C6 1.338(8) . ? C5 H5 0.9300 . ? C6 C7 1.407(8) . ? C6 H6 0.9300 . ? C7 C8 1.410(8) . ? C7 C11 1.418(7) . ? C8 C9 1.364(8) . ? C8 H8 0.9300 . ? C9 C10 1.391(8) . ? C9 H9 0.9300 . ? C10 N3 1.334(6) . ? C10 H10 0.9300 . ? C11 N3 1.355(6) . ? C11 C12 1.436(7) . ? C12 N4 1.366(6) . ? C13 N2 1.331(7) . ? C13 C14 1.414(8) . ? C13 H13 0.9300 . ? C14 C15 1.329(8) . ? C14 H14 0.9300 . ? C15 C16 1.408(8) . ? C15 H15 0.9300 . ? C16 C24 1.390(7) . ? C16 C17 1.417(9) . ? C17 C18 1.361(9) . ? C17 H17 0.9300 . ? C18 C19 1.415(8) . ? C18 H18 0.9300 . ? C19 C23 1.397(7) . ? C19 C20 1.415(9) . ? C20 C21 1.343(8) . ? C20 H20 0.9300 . ? C21 C22 1.389(8) . ? C21 H21 0.9300 . ? C22 N1 1.324(7) . ? C22 H22 0.9300 . ? C23 N1 1.362(6) . ? C23 C24 1.450(8) . ? C24 N2 1.354(6) . ? C25 C32 1.535(7) . ? C25 C26 1.543(6) . ? C25 C88 1.548(6) . ? C25 H25 0.9800 . ? C26 C33 1.481(7) . ? C26 C27 1.542(7) . ? C26 H26 0.9800 . ? C27 C34 1.502(7) . ? C27 C28 1.539(6) . ? C27 H27 0.9800 . ? C28 C35 1.512(7) . ? C28 C29 1.550(6) . ? C28 H28 0.9800 . ? C29 C88 1.516(7) . ? C29 C30 1.534(7) . ? C29 H29 0.9800 . ? C30 O9 1.252(6) . ? C30 O10 1.260(6) . ? C31 O8 1.194(6) . ? C31 O7 1.336(6) . ? C31 C88 1.538(7) . ? C32 O6 1.255(6) . ? C32 O5 1.260(6) . ? C33 O4 1.225(6) . ? C33 O3 1.341(6) . ? C34 O1 1.217(6) . ? C34 O2 1.312(6) . ? C35 O12 1.209(6) . ? C35 O11 1.338(5) . ? C88 H88 0.9800 . ? O2W H2WB 0.8467 . ? O2W H2WA 0.8549 . ? O2 H2A 0.8200 . ? O3 H3A 0.8200 . ? O7 H7 0.8200 . ? O11 H11 0.8200 . ? O3W H3WB 0.8576 . ? O3W H3WA 0.8537 . ? O5W H5WA 0.8471 . ? O5W H5WB 0.8643 . ? O4W H4WA 0.8668 . ? O4W H4WB 0.8801 . ? O6W H6WB 0.9904 . ? O6W H6WA 0.8334 . ? O7W H7WA 0.8505 . ? O7W H7WB 0.8467 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8501 . ? 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 O2W Mn1 O1W 92.15(14) . . ? O2W Mn1 N2 92.04(15) . . ? O1W Mn1 N2 102.31(15) . . ? O2W Mn1 N4 96.85(14) . . ? O1W Mn1 N4 91.09(14) . . ? N2 Mn1 N4 163.63(15) . . ? O2W Mn1 N1 165.45(14) . . ? O1W Mn1 N1 94.45(16) . . ? N2 Mn1 N1 73.89(16) . . ? N4 Mn1 N1 95.97(15) . . ? O2W Mn1 N3 94.03(15) . . ? O1W Mn1 N3 163.16(15) . . ? N2 Mn1 N3 93.12(15) . . ? N4 Mn1 N3 72.63(15) . . ? N1 Mn1 N3 83.28(16) . . ? N4 C1 C2 123.3(6) . . ? N4 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 117.9(6) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 118.2(6) . . ? C3 C4 C5 123.2(5) . . ? C12 C4 C5 118.5(6) . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.8(6) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C8 124.0(5) . . ? C6 C7 C11 119.9(6) . . ? C8 C7 C11 116.1(5) . . ? C9 C8 C7 120.9(5) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 118.1(6) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? N3 C10 C9 124.2(5) . . ? N3 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N3 C11 C7 123.2(5) . . ? N3 C11 C12 118.2(5) . . ? C7 C11 C12 118.6(5) . . ? N4 C12 C4 122.0(5) . . ? N4 C12 C11 117.4(4) . . ? C4 C12 C11 120.5(5) . . ? N2 C13 C14 122.0(6) . . ? N2 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 120.5(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.0(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C24 C16 C15 117.8(6) . . ? C24 C16 C17 119.5(6) . . ? C15 C16 C17 122.7(5) . . ? C18 C17 C16 121.2(6) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.9(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C23 C19 C18 119.1(6) . . ? C23 C19 C20 117.3(5) . . ? C18 C19 C20 123.6(6) . . ? C21 C20 C19 120.1(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 118.6(6) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? N1 C22 C21 124.3(5) . . ? N1 C22 H22 117.8 . . ? C21 C22 H22 117.8 . . ? N1 C23 C19 122.5(5) . . ? N1 C23 C24 117.6(5) . . ? C19 C23 C24 119.9(5) . . ? N2 C24 C16 123.4(5) . . ? N2 C24 C23 117.5(4) . . ? C16 C24 C23 119.1(5) . . ? C32 C25 C26 112.6(4) . . ? C32 C25 C88 117.9(4) . . ? C26 C25 C88 113.8(3) . . ? C32 C25 H25 103.4 . . ? C26 C25 H25 103.4 . . ? C88 C25 H25 103.4 . . ? C33 C26 C27 117.4(4) . . ? C33 C26 C25 111.2(4) . . ? C27 C26 C25 109.2(4) . . ? C33 C26 H26 106.1 . . ? C27 C26 H26 106.1 . . ? C25 C26 H26 106.1 . . ? C34 C27 C28 114.2(4) . . ? C34 C27 C26 114.9(4) . . ? C28 C27 C26 114.7(4) . . ? C34 C27 H27 103.7 . . ? C28 C27 H27 103.7 . . ? C26 C27 H27 103.7 . . ? C35 C28 C27 114.5(4) . . ? C35 C28 C29 116.4(4) . . ? C27 C28 C29 107.7(3) . . ? C35 C28 H28 105.8 . . ? C27 C28 H28 105.8 . . ? C29 C28 H28 105.8 . . ? C88 C29 C30 113.9(4) . . ? C88 C29 C28 114.4(4) . . ? C30 C29 C28 116.2(4) . . ? C88 C29 H29 103.4 . . ? C30 C29 H29 103.4 . . ? C28 C29 H29 103.4 . . ? O9 C30 O10 124.9(5) . . ? O9 C30 C29 115.8(5) . . ? O10 C30 C29 119.2(4) . . ? O8 C31 O7 120.3(5) . . ? O8 C31 C88 123.6(5) . . ? O7 C31 C88 115.9(4) . . ? O6 C32 O5 124.3(5) . . ? O6 C32 C25 119.4(4) . . ? O5 C32 C25 116.0(4) . . ? O4 C33 O3 122.4(5) . . ? O4 C33 C26 124.1(4) . . ? O3 C33 C26 113.4(4) . . ? O1 C34 O2 123.3(5) . . ? O1 C34 C27 123.4(4) . . ? O2 C34 C27 113.1(4) . . ? O12 C35 O11 121.1(4) . . ? O12 C35 C28 124.5(4) . . ? O11 C35 C28 114.2(4) . . ? C29 C88 C31 111.5(4) . . ? C29 C88 C25 110.8(4) . . ? C31 C88 C25 118.9(4) . . ? C29 C88 H88 104.7 . . ? C31 C88 H88 104.7 . . ? C25 C88 H88 104.7 . . ? C22 N1 C23 117.1(5) . . ? C22 N1 Mn1 128.6(4) . . ? C23 N1 Mn1 113.3(3) . . ? C13 N2 C24 117.3(5) . . ? C13 N2 Mn1 126.9(4) . . ? C24 N2 Mn1 115.4(3) . . ? C10 N3 C11 117.3(5) . . ? C10 N3 Mn1 127.4(3) . . ? C11 N3 Mn1 114.9(3) . . ? C1 N4 C12 118.0(4) . . ? C1 N4 Mn1 125.7(4) . . ? C12 N4 Mn1 116.3(3) . . ? Mn1 O2W H2WB 128.4 . . ? Mn1 O2W H2WA 110.3 . . ? H2WB O2W H2WA 70.6 . . ? C34 O2 H2A 109.5 . . ? C33 O3 H3A 109.5 . . ? C31 O7 H7 109.5 . . ? C35 O11 H11 109.5 . . ? H3WB O3W H3WA 77.1 . . ? H5WA O5W H5WB 94.5 . . ? H4WA O4W H4WB 74.2 . . ? H6WB O6W H6WA 64.7 . . ? H7WA O7W H7WB 106.8 . . ? Mn1 O1W H1WA 116.1 . . ? Mn1 O1W H1WB 125.5 . . ? H1WA O1W H1WB 98.6 . . ? 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 O2 H2A O6W 0.82 1.75 2.568(6) 174.8 . O3 H3A O5W 0.82 1.88 2.701(6) 174.6 . O7 H7 O6 0.82 1.72 2.536(5) 170.1 . O1W H1WA O7W 0.85 1.88 2.700(5) 161.2 1_545 O1W H1WB O1 0.85 2.10 2.776(5) 136.2 4_566 O2W H2WB O5 0.85 1.88 2.685(5) 159.5 1_556 O4W H4WA O8 0.87 2.41 3.167(8) 145.9 2_655 O4W H4WA O7 0.87 2.56 3.386(7) 159.0 2_655 O5W H5WB O8 0.86 2.66 3.101(6) 113.3 2_655 O5W H5WB O11 0.86 2.64 3.107(6) 114.8 2_655 O6W H6WB O9 0.99 1.82 2.764(6) 157.8 1_565 O7W H7WA O5 0.85 2.11 2.900(5) 154.7 3_566 O3W H3WA O12 0.85 2.54 3.339(12) 156.3 2_655 O4W H4WB O3W 0.88 2.07 2.874(12) 151.9 . _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 0.467 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.051