data_1100149 _journal_name_full 'Z. Anorg. Allg. Chem.' _journal_volume 629 _journal_page_first 244 _journal_page_last 248 _journal_year 2003 _publ_section_title ; 'Unexpected formation and crystal structures of the mixed ligand complexes [Cu(OAc)(bipy)2]Cl.4H2O.1/2MeOH and [Co(OH2)2(phen)2](AcO)2. 6H2O' ; loop_ _publ_author_name 'Carballo, Rosa' 'Covelo, Berta' 'Vazquez-Lopez, Ezequiel M.' 'Garcia-Martinez, Emilia' _chemical_name_systematic ; 'Diaqua-bis(1,10-phenanthroline-N,N')cobalt(II) acetate hexahydrate' ; _chemical_formula_sum 'C28 H38 Co N4 O12' _chemical_formula_weight 681.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 9.5560(17) _cell_length_b 13.408(3) _cell_length_c 14.480(3) _cell_angle_alpha 108.097(4) _cell_angle_beta 94.267(5) _cell_angle_gamma 110.194(4) _cell_volume 1620.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.8607 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 9185 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.2258 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.98 _reflns_number_total 6450 _reflns_number_gt 2446 _reflns_threshold_expression >2sigma(I) _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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6450 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1578 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 0.724 _refine_ls_restrained_S_all 0.724 _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 Co Co 0.77190(7) -0.03302(6) 0.24906(5) 0.03610(18) Uani 1 1 d . . . N4 N 0.6526(4) -0.0751(3) 0.1011(2) 0.0380(9) Uani 1 1 d . . . N1 N 0.6917(4) 0.1022(3) 0.3145(2) 0.0395(10) Uani 1 1 d . . . N2 N 0.5756(4) -0.1186(3) 0.3001(2) 0.0366(9) Uani 1 1 d . . . N3 N 0.9360(4) 0.0768(3) 0.1966(3) 0.0393(10) Uani 1 1 d . . . C5 C 0.5606(5) 0.0659(4) 0.3481(3) 0.0356(11) Uani 1 1 d . . . C20 C 0.5397(7) -0.1138(5) -0.0956(4) 0.0672(17) Uani 1 1 d . . . H20 H 0.5005 -0.1269 -0.1610 0.081 Uiso 1 1 calc R . . C6 C 0.4987(5) -0.0518(4) 0.3417(3) 0.0375(12) Uani 1 1 d . . . C18 C 0.7384(5) -0.0137(4) 0.0509(3) 0.0396(12) Uani 1 1 d . . . C17 C 0.8896(5) 0.0684(4) 0.1026(4) 0.0408(12) Uani 1 1 d . . . C23 C 0.9240(7) 0.1199(5) -0.0447(4) 0.0720(18) Uani 1 1 d . . . H23 H 0.9842 0.1644 -0.0761 0.086 Uiso 1 1 calc R . . C10 C 0.5218(5) -0.2252(4) 0.2986(3) 0.0493(13) Uani 1 1 d . . . H10 H 0.5729 -0.2715 0.2714 0.059 Uiso 1 1 calc R . . C14 C 1.1729(6) 0.2210(4) 0.2035(5) 0.0674(17) Uani 1 1 d . . . H14 H 1.2698 0.2716 0.2396 0.081 Uiso 1 1 calc R . . C4 C 0.4861(6) 0.1372(5) 0.3886(3) 0.0490(13) Uani 1 1 d . . . C16 C 0.9805(6) 0.1352(4) 0.0552(4) 0.0529(14) Uani 1 1 d . . . C13 C 1.0752(5) 0.1518(4) 0.2453(4) 0.0536(14) Uani 1 1 d . . . H13 H 1.1083 0.1581 0.3096 0.064 Uiso 1 1 calc R . . C24 C 0.7849(7) 0.0417(5) -0.0935(4) 0.0720(18) Uani 1 1 d . . . H24 H 0.7519 0.0330 -0.1586 0.086 Uiso 1 1 calc R . . C1 C 0.7496(5) 0.2100(4) 0.3205(3) 0.0517(14) Uani 1 1 d . . . H1 H 0.8391 0.2358 0.2979 0.062 Uiso 1 1 calc R . . C3 C 0.5492(6) 0.2510(5) 0.3930(4) 0.0649(16) Uani 1 1 d . . . H3 H 0.5020 0.3008 0.4181 0.078 Uiso 1 1 calc R . . C9 C 0.3939(5) -0.2713(4) 0.3352(3) 0.0578(15) Uani 1 1 d . . . H9 H 0.3623 -0.3460 0.3330 0.069 Uiso 1 1 calc R . . C22 C 0.5170(5) -0.1539(4) 0.0534(3) 0.0520(14) Uani 1 1 d . . . H22 H 0.4589 -0.1963 0.0871 0.062 Uiso 1 1 calc R . . C2 C 0.6803(6) 0.2862(4) 0.3599(4) 0.0630(15) Uani 1 1 d . . . H2 H 0.7244 0.3612 0.3633 0.076 Uiso 1 1 calc R . . C19 C 0.6841(7) -0.0298(5) -0.0491(4) 0.0554(15) Uani 1 1 d . . . C7 C 0.3668(5) -0.0933(5) 0.3786(3) 0.0472(13) Uani 1 1 d . . . C15 C 1.1263(6) 0.2148(5) 0.1089(5) 0.0681(18) Uani 1 1 d . . . H15 H 1.1899 0.2622 0.0810 0.082 Uiso 1 1 calc R . . C21 C 0.4553(6) -0.1770(5) -0.0469(4) 0.0622(15) Uani 1 1 d . . . H21 H 0.3597 -0.2338 -0.0784 0.075 Uiso 1 1 calc R . . C8 C 0.3154(5) -0.2063(5) 0.3744(4) 0.0618(16) Uani 1 1 d . . . H8 H 0.2288 -0.2364 0.3981 0.074 Uiso 1 1 calc R . . C11 C 0.3480(6) 0.0922(5) 0.4234(4) 0.0628(16) Uani 1 1 d . . . H11 H 0.2967 0.1387 0.4494 0.075 Uiso 1 1 calc R . . C12 C 0.2938(6) -0.0167(5) 0.4182(4) 0.0672(17) Uani 1 1 d . . . H12 H 0.2052 -0.0435 0.4413 0.081 Uiso 1 1 calc R . . O6 O 0.2053(4) 0.4867(3) 0.1311(3) 0.0735(11) Uani 1 1 d . . . O5 O 0.3179(4) 0.5635(3) 0.0275(2) 0.0740(11) Uani 1 1 d . . . O2 O 0.8217(3) -0.1763(3) 0.1921(2) 0.0449(8) Uani 1 1 d . . . O1 O 0.9217(3) 0.0038(3) 0.3781(2) 0.0530(9) Uani 1 1 d . . . C28 C 0.1331(5) 0.6273(4) 0.0989(4) 0.0709(16) Uani 1 1 d . . . H28A H 0.1979 0.7045 0.1388 0.106 Uiso 1 1 calc R . . H28B H 0.0518 0.5998 0.1312 0.106 Uiso 1 1 calc R . . H28C H 0.0914 0.6243 0.0352 0.106 Uiso 1 1 calc R . . O4 O 0.8705(4) 0.7069(3) 0.2989(2) 0.0719(11) Uani 1 1 d . . . O3 O 0.9167(4) 0.8385(3) 0.4441(2) 0.0666(10) Uani 1 1 d . . . C25 C 0.8827(5) 0.7382(5) 0.3913(4) 0.0467(13) Uani 1 1 d . . . C27 C 0.2260(5) 0.5526(4) 0.0851(4) 0.0507(14) Uani 1 1 d . . . C26 C 0.8579(6) 0.6507(4) 0.4366(4) 0.101(2) Uani 1 1 d . . . H26A H 0.7510 0.6048 0.4231 0.151 Uiso 1 1 calc R . . H26B H 0.8950 0.6869 0.5070 0.151 Uiso 1 1 calc R . . H26C H 0.9114 0.6033 0.4091 0.151 Uiso 1 1 calc R . . O1W O 0.7346(4) 0.4791(3) 0.1765(3) 0.0637(10) Uani 1 1 d . . . O2W O 0.3672(4) 0.3546(3) 0.9685(3) 0.0656(10) Uani 1 1 d . . . O3W O 0.4551(4) 0.4764(3) 0.2398(2) 0.0798(12) Uani 1 1 d . . . O4W O 0.9616(4) 0.4021(3) 0.2231(3) 0.0813(12) Uani 1 1 d . . . O5W O 0.3886(4) 0.4740(3) 0.4233(3) 0.0903(13) Uani 1 1 d . . . O6W O 0.0997(4) 0.4950(4) 0.4248(3) 0.1195(18) Uani 1 1 d . . . H2B H 0.7496 -0.2397 0.1394 0.020(11) Uiso 1 1 d . . . H1A H 0.9723 0.0642 0.4248 0.07(2) Uiso 1 1 d . . . H2A H 0.8478 -0.2046 0.2455 0.15(3) Uiso 1 1 d . . . H1B H 0.9249 -0.0439 0.4064 0.14(3) Uiso 1 1 d . . . H310 H 0.5330 0.4763 0.2056 0.13(2) Uiso 1 1 d . . . H320 H 0.3629 0.4455 0.1860 0.13(2) Uiso 1 1 d . . . H410 H 0.9033 0.4569 0.2177 0.12(2) Uiso 1 1 d . . . H510 H 0.4083 0.4733 0.3643 0.09(2) Uiso 1 1 d . . . H420 H 1.0076 0.4066 0.1708 0.11(2) Uiso 1 1 d . . . H520 H 0.3080 0.4956 0.4187 0.13(3) Uiso 1 1 d . . . H120 H 0.7230 0.4734 0.1166 0.15(3) Uiso 1 1 d . . . H610 H 0.0588 0.5249 0.4551 0.49(10) Uiso 1 1 d . . . H620 H 0.0574 0.4656 0.3594 0.08(2) Uiso 1 1 d . . . H210 H 0.4657 0.3801 0.9697 0.14(3) Uiso 1 1 d . . . H220 H 0.3642 0.4159 1.0083 0.15(3) Uiso 1 1 d . . . H110 H 0.7774 0.5515 0.2155 0.12(3) Uiso 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 Co 0.0403(4) 0.0363(4) 0.0331(4) 0.0140(3) 0.0100(3) 0.0147(3) N4 0.042(2) 0.038(3) 0.037(2) 0.015(2) 0.006(2) 0.020(2) N1 0.044(2) 0.042(3) 0.035(2) 0.016(2) 0.0113(19) 0.017(2) N2 0.042(2) 0.031(2) 0.035(2) 0.010(2) 0.0072(19) 0.013(2) N3 0.046(2) 0.031(3) 0.038(3) 0.009(2) 0.012(2) 0.015(2) C5 0.041(3) 0.042(3) 0.026(3) 0.010(3) 0.006(2) 0.021(3) C20 0.086(5) 0.085(5) 0.038(3) 0.010(4) 0.005(3) 0.055(4) C6 0.035(3) 0.052(4) 0.024(3) 0.013(3) 0.004(2) 0.017(3) C18 0.058(3) 0.042(3) 0.037(3) 0.018(3) 0.021(3) 0.036(3) C17 0.049(3) 0.043(3) 0.050(3) 0.023(3) 0.031(3) 0.031(3) C23 0.106(5) 0.078(5) 0.078(5) 0.052(4) 0.060(4) 0.061(4) C10 0.054(3) 0.047(4) 0.048(3) 0.020(3) 0.015(3) 0.018(3) C14 0.051(3) 0.044(4) 0.105(5) 0.024(4) 0.039(4) 0.013(3) C4 0.059(4) 0.066(4) 0.035(3) 0.014(3) 0.012(3) 0.042(3) C16 0.066(4) 0.049(4) 0.072(4) 0.036(4) 0.043(3) 0.036(3) C13 0.046(3) 0.041(3) 0.062(4) 0.012(3) 0.016(3) 0.008(3) C24 0.121(5) 0.099(6) 0.045(4) 0.046(4) 0.043(4) 0.077(5) C1 0.056(3) 0.044(4) 0.057(4) 0.018(3) 0.015(3) 0.021(3) C3 0.081(4) 0.065(4) 0.061(4) 0.013(4) 0.014(3) 0.051(4) C9 0.060(4) 0.047(4) 0.055(4) 0.022(3) 0.016(3) 0.004(3) C22 0.053(3) 0.046(4) 0.048(4) 0.008(3) 0.001(3) 0.018(3) C2 0.075(4) 0.044(4) 0.067(4) 0.010(3) 0.009(3) 0.030(4) C19 0.087(4) 0.071(4) 0.043(3) 0.030(3) 0.027(3) 0.060(4) C7 0.038(3) 0.063(4) 0.042(3) 0.019(3) 0.016(2) 0.020(3) C15 0.075(4) 0.050(4) 0.110(5) 0.047(4) 0.065(4) 0.035(4) C21 0.065(4) 0.057(4) 0.051(4) -0.001(3) -0.007(3) 0.029(3) C8 0.049(3) 0.075(5) 0.059(4) 0.032(4) 0.020(3) 0.012(4) C11 0.062(4) 0.089(5) 0.052(4) 0.019(4) 0.020(3) 0.051(4) C12 0.052(4) 0.096(5) 0.069(4) 0.034(4) 0.027(3) 0.040(4) O6 0.075(3) 0.075(3) 0.094(3) 0.046(3) 0.024(2) 0.041(2) O5 0.066(2) 0.101(3) 0.059(2) 0.030(2) 0.024(2) 0.034(2) O2 0.055(2) 0.038(2) 0.040(2) 0.009(2) 0.0059(18) 0.021(2) O1 0.068(2) 0.044(2) 0.037(2) 0.011(2) -0.0045(19) 0.016(2) C28 0.067(4) 0.066(4) 0.083(4) 0.024(4) 0.010(3) 0.033(4) O4 0.118(3) 0.058(3) 0.050(2) 0.022(2) 0.016(2) 0.044(2) O3 0.093(3) 0.040(2) 0.052(2) 0.009(2) -0.002(2) 0.020(2) C25 0.054(3) 0.046(4) 0.044(4) 0.019(3) 0.014(3) 0.020(3) C27 0.043(3) 0.045(4) 0.046(3) 0.002(3) -0.004(3) 0.012(3) C26 0.169(6) 0.076(5) 0.088(5) 0.050(4) 0.045(4) 0.062(5) O1W 0.070(2) 0.063(3) 0.060(3) 0.020(2) 0.0144(19) 0.029(2) O2W 0.063(3) 0.045(2) 0.067(3) 0.001(2) 0.0045(19) 0.014(2) O3W 0.060(2) 0.119(4) 0.057(2) 0.035(3) 0.016(2) 0.026(2) O4W 0.101(3) 0.102(3) 0.078(3) 0.052(3) 0.037(2) 0.063(3) O5W 0.091(3) 0.145(4) 0.057(3) 0.040(3) 0.026(2) 0.066(3) O6W 0.109(3) 0.205(6) 0.071(3) 0.056(3) 0.025(3) 0.085(4) _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 Co O2 2.074(3) . ? Co O1 2.080(3) . ? Co N3 2.118(3) . ? Co N2 2.151(3) . ? Co N4 2.157(3) . ? Co N1 2.184(4) . ? N4 C22 1.319(5) . ? N4 C18 1.369(5) . ? N1 C1 1.328(5) . ? N1 C5 1.364(4) . ? N2 C10 1.334(5) . ? N2 C6 1.374(5) . ? N3 C13 1.332(5) . ? N3 C17 1.357(5) . ? C5 C4 1.397(5) . ? C5 C6 1.450(5) . ? C20 C21 1.360(6) . ? C20 C19 1.394(6) . ? C6 C7 1.410(5) . ? C18 C19 1.425(5) . ? C18 C17 1.445(5) . ? C17 C16 1.401(5) . ? C23 C24 1.343(6) . ? C23 C16 1.431(6) . ? C10 C9 1.391(5) . ? C14 C15 1.376(6) . ? C14 C13 1.390(6) . ? C4 C3 1.412(6) . ? C4 C11 1.448(6) . ? C16 C15 1.408(6) . ? C24 C19 1.447(6) . ? C1 C2 1.403(6) . ? C3 C2 1.358(6) . ? C9 C8 1.361(6) . ? C22 C21 1.421(6) . ? C7 C8 1.401(6) . ? C7 C12 1.434(6) . ? C11 C12 1.345(6) . ? O6 C27 1.236(5) . ? O5 C27 1.259(5) . ? C28 C27 1.532(6) . ? O4 C25 1.254(5) . ? O3 C25 1.233(5) . ? C25 C26 1.475(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co O1 85.72(13) . . ? O2 Co N3 97.98(12) . . ? O1 Co N3 94.15(14) . . ? O2 Co N2 94.49(13) . . ? O1 Co N2 93.20(12) . . ? N3 Co N2 165.95(13) . . ? O2 Co N4 87.04(13) . . ? O1 Co N4 168.69(12) . . ? N3 Co N4 78.27(14) . . ? N2 Co N4 96.02(13) . . ? O2 Co N1 171.91(13) . . ? O1 Co N1 94.91(13) . . ? N3 Co N1 90.02(13) . . ? N2 Co N1 77.42(14) . . ? N4 Co N1 93.48(12) . . ? C22 N4 C18 118.2(4) . . ? C22 N4 Co 129.1(3) . . ? C18 N4 Co 112.5(3) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Co 128.5(3) . . ? C5 N1 Co 113.3(3) . . ? C10 N2 C6 116.7(4) . . ? C10 N2 Co 129.0(3) . . ? C6 N2 Co 114.3(3) . . ? C13 N3 C17 118.0(4) . . ? C13 N3 Co 127.5(3) . . ? C17 N3 Co 114.4(3) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C6 117.7(4) . . ? C4 C5 C6 119.5(4) . . ? C21 C20 C19 121.0(5) . . ? N2 C6 C7 122.5(4) . . ? N2 C6 C5 117.1(4) . . ? C7 C6 C5 120.4(4) . . ? N4 C18 C19 122.2(5) . . ? N4 C18 C17 117.5(4) . . ? C19 C18 C17 120.2(5) . . ? N3 C17 C16 123.1(5) . . ? N3 C17 C18 117.2(4) . . ? C16 C17 C18 119.7(5) . . ? C24 C23 C16 120.5(5) . . ? N2 C10 C9 124.0(5) . . ? C15 C14 C13 120.1(5) . . ? C5 C4 C3 117.9(5) . . ? C5 C4 C11 119.3(5) . . ? C3 C4 C11 122.8(5) . . ? C17 C16 C15 117.6(5) . . ? C17 C16 C23 119.7(5) . . ? C15 C16 C23 122.7(5) . . ? N3 C13 C14 122.5(5) . . ? C23 C24 C19 122.9(5) . . ? N1 C1 C2 122.2(4) . . ? C2 C3 C4 118.7(5) . . ? C8 C9 C10 119.5(5) . . ? N4 C22 C21 123.2(5) . . ? C3 C2 C1 120.4(5) . . ? C20 C19 C18 117.0(5) . . ? C20 C19 C24 126.1(5) . . ? C18 C19 C24 116.9(5) . . ? C8 C7 C6 118.1(5) . . ? C8 C7 C12 124.3(5) . . ? C6 C7 C12 117.6(5) . . ? C14 C15 C16 118.6(5) . . ? C20 C21 C22 118.3(5) . . ? C9 C8 C7 119.2(5) . . ? C12 C11 C4 120.2(5) . . ? C11 C12 C7 122.9(5) . . ? O3 C25 O4 122.4(5) . . ? O3 C25 C26 120.0(5) . . ? O4 C25 C26 117.6(5) . . ? O6 C27 O5 125.2(5) . . ? O6 C27 C28 117.8(5) . . ? O5 C27 C28 117.0(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 O2 H2B O2W 0.945(3) 1.766(4) 2.706(5) 172.5(2) 2_656 O1 H1A O3 0.829(4) 1.907(3) 2.694(5) 157.9(2) 2_766 O2 H2A O4 1.012(3) 1.666(3) 2.639(4) 159.9(2) 1_545 O1 H1B O3 0.868(3) 1.802(3) 2.661(4) 170.1(3) 1_545 O3W H310 O1W 0.924(3) 1.992(3) 2.879(4) 160.2(2) . O3W H320 O6 1.001(3) 1.969(3) 2.829(4) 142.5(2) . O4W H410 O1W 1.080(3) 1.829(3) 2.826(4) 151.7(2) . O5W H510 O3W 0.886(3) 1.898(3) 2.784(5) 178.3(3) . O4W H420 O6 0.911(4) 2.048(3) 2.839(5) 144.4(2) 1_655 O5W H520 O6W 0.917(4) 1.996(4) 2.872(5) 159.1(3) . O1W H120 O5 0.842(4) 1.963(3) 2.800(5) 171.8(3) 2_665 O6W H610 O6W 0.728(5) 2.407(4) 3.001(9) 140.0(2) 2_566 O6W H620 O4W 0.904(4) 1.900(3) 2.803(5) 178.0(3) 1_455 O2W H210 O5 0.880(4) 1.933(3) 2.813(5) 179.8(2) 2_666 O2W H220 O5 0.856(4) 2.114(3) 2.878(5) 148.2(2) 1_556 O2W H220 O6 0.856(4) 2.592(3) 3.305(5) 141.4(3) 1_556 C23 H23 O2 0.93 2.59 3.395(6) 145.2 2_755 O1W H110 O4 0.882(4) 1.894(3) 2.776(5) 179.6(2) . _diffrn_measured_fraction_theta_max 0.825 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.825 _refine_diff_density_max 0.274 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.052