# Supplementary Material (ESI) for PCCP # This journal is (c) the Owner Societies 2010 data_global _journal_coden_Cambridge 1326 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Furman, Joshua' 'Melot, Brent' 'Teat, Simon' 'Mikhailovsky, Alexander' 'Cheetham, Tony' _publ_contact_author_name 'Furman, Joshua' _publ_contact_author_email akc30@cam.ac.uk _publ_section_title ; Towards enhanced ligand-centered photoluminescence in inorganic-organic frameworks for solid state lighting ; # Attachment '- bafdc.cif' data_bafdc _database_code_depnum_ccdc_archive 'CCDC 793002' #TrackingRef '- bafdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H8 Ba O6' _chemical_formula_weight 421.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Ba Ba -0.4622 2.6692 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.7676(6) _cell_length_b 7.2311(7) _cell_length_c 14.1591(13) _cell_angle_alpha 82.763(2) _cell_angle_beta 84.102(2) _cell_angle_gamma 66.047(2) _cell_volume 627.17(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 33.59 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 3.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'TWINABS v2008/2 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20394 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 33.59 _reflns_number_total 3737 _reflns_number_gt 3658 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.60a' _computing_data_reduction 'Bruker SAINT v7.60a' _computing_structure_solution 'SIR97 run through WinGX' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. A single crystal could not be found and therefore the data were collected on a twin. CELL_NOW was used to determined the orientation matrices and the domains were related by a 180 deg rotation around the recipocal axis 0 0 1. The integration was preformed with both matrice. TWINABS was you to produce a merged HKLF4 file, for structure solution and initial refinement, and HKLF5 file for for final structure refinement. The HKLF5 file contained the merged reflections first component and those that overlapped with the second component were split into 2 reflection. As the crystal was found to be non-centrosymmetry the second component was tried as determined and invrted to see what gave the better refinement. All non-hydrogen atoms were refined anisotropically. O11 has a large min:max dispalcement parameter ratio, I split site model was tried but this did not yield a chemically sensible result. The largest q-peak is near O11, on the Ba1 side. This is not in a cheimally sensible position and is probably results from the impurification in the processing of the twinned data. Hydrogen atoms were placed geometrically on the carbon atoms and refined using a riding model. The hydrogen atoms on the waters could neither be place nor found in the difference map and were therefore omitted from the refinement. ; _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^)+(0.0452P)^2^+0.7435P] 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 . _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.153(19) _refine_ls_number_reflns 3737 _refine_ls_number_parameters 398 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Ba1 Ba -0.44486(4) 0.07350(4) 0.48042(2) 0.01216(10) Uani 1 1 d . . . Ba2 Ba -0.10027(3) 0.43895(3) 0.39963(2) 0.01128(10) Uani 1 1 d . . . O1 O -0.5167(8) 0.1399(7) 0.9452(4) 0.0159(9) Uani 1 1 d . . . O2 O -0.6844(8) 0.3214(9) 1.3227(4) 0.0165(9) Uani 1 1 d . . . O3 O -0.5113(8) 0.5070(8) 1.3557(4) 0.0143(8) Uani 1 1 d . . . O4 O -0.3656(10) 0.3671(9) 0.5651(4) 0.0141(11) Uani 1 1 d . . . O5 O -0.3650(12) 0.6748(11) 0.5374(5) 0.0152(13) Uani 1 1 d . . . O6 O -0.0201(8) -0.3639(7) -0.0541(4) 0.0170(9) Uani 1 1 d . . . O7 O -0.1618(13) -0.1851(11) 0.3246(5) 0.0184(14) Uani 1 1 d . . . O8 O -0.1378(10) 0.1079(9) 0.3438(4) 0.0144(11) Uani 1 1 d . . . O9 O -0.0552(7) -0.0691(7) -0.4314(4) 0.0125(8) Uani 1 1 d . . . O10 O 0.1330(8) 0.1247(8) -0.4699(4) 0.0138(9) Uani 1 1 d . . . C1 C -0.5581(9) 0.3631(9) 1.1264(4) 0.0103(10) Uani 1 1 d . . . H1A H -0.5862 0.2452 1.1464 0.012 Uiso 1 1 calc R . . C2 C -0.5519(12) 0.4881(12) 1.1928(6) 0.0111(14) Uani 1 1 d . . . C3 C -0.5089(10) 0.6625(9) 1.1614(4) 0.0117(10) Uani 1 1 d . . . H3A H -0.4985 0.7428 1.2074 0.014 Uiso 1 1 calc R . . C4 C -0.4809(9) 0.7203(9) 1.0634(4) 0.0109(10) Uani 1 1 d . . . H4A H -0.4571 0.8402 1.0427 0.013 Uiso 1 1 calc R . . C5 C -0.4896(11) 0.5946(10) 0.9985(5) 0.0115(11) Uani 1 1 d . . . C6 C -0.4653(10) 0.6111(10) 0.8928(5) 0.0116(11) Uani 1 1 d . . . C7 C -0.4284(10) 0.7554(9) 0.8283(4) 0.0122(10) Uani 1 1 d . . . H7A H -0.4183 0.8709 0.8492 0.015 Uiso 1 1 calc R . . C8 C -0.4065(10) 0.7265(10) 0.7318(4) 0.0132(11) Uani 1 1 d . . . H8A H -0.3784 0.8233 0.6869 0.016 Uiso 1 1 calc R . . C9 C -0.4245(11) 0.5601(9) 0.6985(4) 0.0104(10) Uani 1 1 d . . . C10 C -0.4623(10) 0.4141(9) 0.7644(4) 0.0120(10) Uani 1 1 d . . . H10A H -0.4736 0.2991 0.7436 0.014 Uiso 1 1 calc R . . C11 C -0.4825(11) 0.4425(9) 0.8603(5) 0.0108(10) Uani 1 1 d . . . C12 C -0.5114(10) 0.3060(10) 0.9450(4) 0.0116(10) Uani 1 1 d . . . C13 C -0.5223(10) 0.4155(9) 1.0309(5) 0.0107(10) Uani 1 1 d . . . C14 C -0.5850(13) 0.4366(12) 1.2959(6) 0.0073(14) Uani 1 1 d . . . C15 C -0.3871(17) 0.5347(15) 0.5937(7) 0.0115(17) Uani 1 1 d . . . C16 C -0.0591(10) -0.1337(9) 0.1242(4) 0.0111(10) Uani 1 1 d . . . H16A H -0.0883 -0.2503 0.1461 0.013 Uiso 1 1 calc R . . C17 C -0.0561(11) -0.0012(10) 0.1884(5) 0.0122(11) Uani 1 1 d . . . C18 C -0.0086(10) 0.1687(9) 0.1541(4) 0.0126(10) Uani 1 1 d . . . H18A H -0.0037 0.2549 0.1984 0.015 Uiso 1 1 calc R . . C19 C 0.0314(10) 0.2142(9) 0.0576(4) 0.0123(10) Uani 1 1 d . . . H19A H 0.0646 0.3287 0.0360 0.015 Uiso 1 1 calc R . . C20 C 0.0216(10) 0.0875(9) -0.0066(5) 0.0106(10) Uani 1 1 d . . . C21 C 0.0443(11) 0.0979(9) -0.1123(5) 0.0115(10) Uani 1 1 d . . . C22 C 0.0796(9) 0.2397(9) -0.1800(4) 0.0108(10) Uani 1 1 d . . . H22A H 0.0972 0.3535 -0.1613 0.013 Uiso 1 1 calc R . . C23 C 0.0884(10) 0.2105(9) -0.2766(4) 0.0125(11) Uani 1 1 d . . . H23A H 0.1183 0.3030 -0.3236 0.015 Uiso 1 1 calc R . . C24 C 0.0545(13) 0.0486(12) -0.3050(6) 0.0112(14) Uani 1 1 d . . . C25 C 0.0198(10) -0.0950(10) -0.2369(4) 0.0123(10) Uani 1 1 d . . . H25A H -0.0022 -0.2067 -0.2554 0.015 Uiso 1 1 calc R . . C26 C 0.0188(12) -0.0685(10) -0.1420(5) 0.0111(11) Uani 1 1 d . . . C27 C -0.0111(10) -0.1994(10) -0.0557(4) 0.0122(10) Uani 1 1 d . . . C28 C -0.0177(10) -0.0882(9) 0.0278(5) 0.0099(10) Uani 1 1 d . . . C29 C -0.1225(17) -0.0266(16) 0.2923(7) 0.0129(18) Uani 1 1 d . . . C30 C 0.0461(17) 0.0281(13) -0.4104(7) 0.0141(18) Uani 1 1 d . . . O11 O -0.6430(14) -0.0849(14) 0.3730(8) 0.049(3) Uani 1 1 d . . . O12 O 0.1572(10) 0.5536(10) 0.5033(5) 0.0173(12) 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 Ba1 0.0116(2) 0.0125(2) 0.0122(2) 0.00143(17) -0.00001(17) -0.00551(18) Ba2 0.0129(2) 0.0135(2) 0.0098(2) -0.00139(16) 0.00023(17) -0.00775(19) O1 0.020(2) 0.011(2) 0.016(2) -0.0034(16) 0.0009(17) -0.0064(17) O2 0.018(2) 0.026(3) 0.011(2) -0.0010(19) 0.0008(18) -0.016(2) O3 0.016(2) 0.016(2) 0.013(2) -0.0025(18) -0.0017(17) -0.0083(18) O4 0.016(2) 0.013(3) 0.013(3) -0.0032(19) -0.0022(19) -0.004(2) O5 0.021(3) 0.012(2) 0.014(3) -0.003(2) 0.003(2) -0.008(2) O6 0.020(2) 0.012(2) 0.019(2) -0.0036(17) -0.0012(18) -0.0058(18) O7 0.032(3) 0.018(3) 0.012(3) -0.001(2) -0.001(2) -0.017(3) O8 0.016(2) 0.015(3) 0.015(3) -0.004(2) 0.004(2) -0.008(2) O9 0.014(2) 0.0095(19) 0.013(2) 0.0002(17) -0.0023(16) -0.0031(16) O10 0.0141(19) 0.019(2) 0.011(2) 0.0022(18) -0.0016(17) -0.0104(18) C1 0.010(2) 0.012(3) 0.009(2) -0.0021(19) 0.0011(19) -0.005(2) C2 0.010(3) 0.013(3) 0.010(3) -0.002(2) 0.001(2) -0.005(2) C3 0.012(2) 0.012(3) 0.012(3) -0.003(2) 0.001(2) -0.007(2) C4 0.012(2) 0.009(2) 0.013(3) -0.001(2) 0.001(2) -0.006(2) C5 0.011(3) 0.014(3) 0.010(3) -0.003(2) 0.001(2) -0.006(2) C6 0.007(2) 0.018(3) 0.010(3) 0.000(2) 0.001(2) -0.007(2) C7 0.012(2) 0.011(2) 0.012(2) -0.002(2) -0.005(2) -0.002(2) C8 0.015(3) 0.014(3) 0.010(2) 0.000(2) 0.000(2) -0.005(2) C9 0.012(3) 0.006(2) 0.011(3) 0.0042(19) -0.001(2) -0.002(2) C10 0.014(2) 0.011(3) 0.012(3) -0.004(2) 0.001(2) -0.006(2) C11 0.011(2) 0.010(3) 0.011(3) -0.0024(19) 0.000(2) -0.004(2) C12 0.012(2) 0.013(3) 0.011(3) 0.000(2) -0.0012(19) -0.006(2) C13 0.011(2) 0.013(3) 0.008(2) -0.0008(19) -0.001(2) -0.004(2) C14 0.007(3) 0.007(3) 0.009(3) -0.004(2) -0.003(2) -0.001(2) C15 0.014(4) 0.013(4) 0.010(3) -0.005(3) 0.002(3) -0.007(3) C16 0.014(2) 0.014(3) 0.006(2) -0.0010(19) -0.0001(19) -0.006(2) C17 0.011(3) 0.012(3) 0.014(3) -0.001(2) 0.002(2) -0.005(2) C18 0.015(3) 0.011(3) 0.011(3) -0.003(2) 0.001(2) -0.004(2) C19 0.016(3) 0.012(3) 0.011(3) -0.001(2) -0.002(2) -0.008(2) C20 0.008(3) 0.011(3) 0.013(3) -0.005(2) 0.003(2) -0.004(2) C21 0.012(3) 0.014(3) 0.008(3) -0.002(2) 0.003(2) -0.005(2) C22 0.011(2) 0.011(2) 0.010(2) -0.0033(19) 0.0003(19) -0.003(2) C23 0.012(2) 0.013(3) 0.011(3) 0.001(2) 0.001(2) -0.005(2) C24 0.012(3) 0.011(3) 0.012(3) 0.001(2) -0.001(2) -0.006(2) C25 0.013(2) 0.015(3) 0.011(3) 0.000(2) -0.001(2) -0.009(2) C26 0.015(3) 0.010(3) 0.008(3) -0.002(2) -0.002(2) -0.005(2) C27 0.015(3) 0.017(3) 0.008(2) -0.003(2) 0.001(2) -0.009(2) C28 0.007(2) 0.010(3) 0.011(3) -0.0005(19) 0.000(2) -0.001(2) C29 0.015(4) 0.012(4) 0.011(3) 0.004(3) -0.003(3) -0.006(3) C30 0.019(3) 0.008(3) 0.015(3) -0.003(3) 0.003(3) -0.005(3) O11 0.026(4) 0.036(5) 0.066(6) 0.017(4) 0.017(4) -0.004(3) O12 0.014(3) 0.020(3) 0.022(3) -0.006(2) 0.000(2) -0.009(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 Ba1 Ba2 4.1743(4) . ? Ba1 O2 2.864(5) 1_554 ? Ba1 O3 3.282(5) 1_554 ? Ba1 O4 2.816(6) . ? Ba1 O5 2.737(7) 1_545 ? Ba1 O7 3.049(7) . ? Ba1 O8 2.756(6) . ? Ba1 O9 2.779(5) 1_556 ? Ba1 O10 2.755(5) 1_456 ? Ba1 C14 3.373(9) 1_554 ? Ba1 C29 3.223(11) . ? Ba1 O11 2.744(12) . ? Ba2 Ba1 4.3278(5) 1_655 ? Ba2 Ba1 4.4595(5) 1_565 ? Ba2 O2 2.737(5) 1_654 ? Ba2 O3 2.745(5) 1_554 ? Ba2 O4 2.927(6) . ? Ba2 O5 2.750(7) . ? Ba2 O7 2.671(7) 1_565 ? Ba2 O8 2.725(6) . ? Ba2 O10 2.774(5) 1_556 ? Ba2 C15 3.177(10) . ? Ba2 O12 2.808(6) . ? O1 C12 1.216(8) . ? O2 Ba1 2.864(5) 1_556 ? O2 Ba2 2.737(5) 1_456 ? O2 C14 1.270(10) . ? O3 Ba1 3.282(5) 1_556 ? O3 Ba2 2.745(5) 1_556 ? O3 C14 1.276(9) . ? O4 C15 1.274(11) . ? O5 Ba1 2.737(7) 1_565 ? O5 C15 1.257(12) . ? O6 C27 1.212(8) . ? O7 Ba2 2.671(7) 1_545 ? O7 C29 1.298(12) . ? O8 C29 1.253(12) . ? O9 Ba1 2.779(5) 1_554 ? O9 C30 1.240(11) . ? O10 Ba1 2.755(5) 1_654 ? O10 Ba2 2.774(5) 1_554 ? O10 C30 1.276(11) . ? C1 H1A 0.9500 . ? C1 C2 1.399(10) . ? C1 C13 1.381(8) . ? C2 C3 1.415(10) . ? C2 C14 1.478(12) . ? C3 H3A 0.9500 . ? C3 C4 1.414(9) . ? C4 H4A 0.9500 . ? C4 C5 1.393(9) . ? C5 C6 1.484(10) . ? C5 C13 1.414(9) . ? C6 C7 1.382(9) . ? C6 C11 1.406(9) . ? C7 H7A 0.9500 . ? C7 C8 1.392(8) . ? C8 H8A 0.9500 . ? C8 C9 1.399(9) . ? C9 C10 1.404(9) . ? C9 C15 1.501(12) . ? C10 H10A 0.9500 . ? C10 C11 1.384(9) . ? C11 C12 1.504(9) . ? C12 C13 1.512(9) . ? C14 Ba1 3.373(9) 1_556 ? C16 H16A 0.9500 . ? C16 C17 1.408(9) . ? C16 C28 1.391(8) . ? C17 C18 1.409(9) . ? C17 C29 1.505(12) . ? C18 H18A 0.9500 . ? C18 C19 1.390(8) . ? C19 H19A 0.9500 . ? C19 C20 1.393(8) . ? C20 C21 1.484(9) . ? C20 C28 1.419(9) . ? C21 C22 1.390(8) . ? C21 C26 1.402(9) . ? C22 H22A 0.9500 . ? C22 C23 1.401(8) . ? C23 H23A 0.9500 . ? C23 C24 1.394(10) . ? C24 C25 1.400(10) . ? C24 C30 1.527(13) . ? C25 H25A 0.9500 . ? C25 C26 1.381(9) . ? C26 C27 1.498(10) . ? C27 C28 1.499(9) . ? 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 Ba2 Ba1 O2 79.77(10) . 1_554 ? Ba2 Ba1 O3 41.05(8) . 1_554 ? Ba2 Ba1 O4 44.44(12) . . ? Ba2 Ba1 O5 138.95(16) . 1_545 ? Ba2 Ba1 O7 84.97(14) . . ? Ba2 Ba1 O8 40.13(13) . . ? Ba2 Ba1 O9 67.69(11) . 1_556 ? Ba2 Ba1 O10 137.80(11) . 1_456 ? Ba2 Ba1 C14 58.20(14) . 1_554 ? Ba2 Ba1 C29 62.55(19) . . ? Ba2 Ba1 O11 130.81(19) . . ? O2 Ba1 O3 41.71(14) 1_554 1_554 ? O2 Ba1 O4 99.97(16) 1_554 . ? O2 Ba1 O5 127.9(2) 1_554 1_545 ? O2 Ba1 O7 83.10(19) 1_554 . ? O2 Ba1 O8 74.71(16) 1_554 . ? O2 Ba1 O9 145.46(14) 1_554 1_556 ? O2 Ba1 O10 75.35(14) 1_554 1_456 ? O2 Ba1 C14 21.58(16) 1_554 1_554 ? O2 Ba1 C29 72.9(2) 1_554 . ? O2 Ba1 O11 60.8(2) 1_554 . ? O3 Ba1 O4 61.27(14) 1_554 . ? O3 Ba1 O5 164.74(16) 1_554 1_545 ? O3 Ba1 O7 94.30(16) 1_554 . ? O3 Ba1 O8 58.30(16) 1_554 . ? O3 Ba1 O9 108.49(13) 1_554 1_556 ? O3 Ba1 O10 101.60(13) 1_554 1_456 ? O3 Ba1 C14 22.05(15) 1_554 1_554 ? O3 Ba1 C29 72.4(2) 1_554 . ? O3 Ba1 O11 101.7(2) 1_554 . ? O4 Ba1 O5 131.76(19) . 1_545 ? O4 Ba1 O7 126.45(19) . . ? O4 Ba1 O8 83.78(18) . . ? O4 Ba1 O9 64.71(15) . 1_556 ? O4 Ba1 O10 107.67(17) . 1_456 ? O4 Ba1 C14 83.19(18) . 1_554 ? O4 Ba1 C29 106.2(2) . . ? O4 Ba1 O11 158.9(2) . . ? O5 Ba1 O7 71.55(18) 1_545 . ? O5 Ba1 O8 111.3(2) 1_545 . ? O5 Ba1 O9 76.13(19) 1_545 1_556 ? O5 Ba1 O10 82.65(19) 1_545 1_456 ? O5 Ba1 C14 144.5(2) 1_545 1_554 ? O5 Ba1 C29 94.4(2) 1_545 . ? O5 Ba1 O11 67.2(2) 1_545 . ? O7 Ba1 O8 45.08(19) . . ? O7 Ba1 O9 82.81(18) . 1_556 ? O7 Ba1 O10 124.38(19) . 1_456 ? O7 Ba1 C14 82.3(2) . 1_554 ? O7 Ba1 C29 23.7(2) . . ? O7 Ba1 O11 63.5(2) . . ? O8 Ba1 O9 73.01(17) . 1_556 ? O8 Ba1 O10 149.38(17) . 1_456 ? O8 Ba1 C14 59.2(2) . 1_554 ? O8 Ba1 C29 22.5(2) . . ? O8 Ba1 O11 98.1(2) . . ? O9 Ba1 O10 137.62(15) 1_556 1_456 ? O9 Ba1 C14 124.74(18) 1_556 1_554 ? O9 Ba1 C29 81.8(2) 1_556 . ? O9 Ba1 O11 136.0(2) 1_556 . ? O10 Ba1 C14 93.29(17) 1_456 1_554 ? O10 Ba1 C29 136.7(2) 1_456 . ? O10 Ba1 O11 61.2(2) 1_456 . ? C14 Ba1 C29 64.8(2) 1_554 . ? C14 Ba1 O11 79.8(2) 1_554 . ? C29 Ba1 O11 77.7(3) . . ? Ba1 Ba2 Ba1 105.484(10) . 1_655 ? Ba1 Ba2 Ba1 113.721(10) . 1_565 ? Ba1 Ba2 Ba1 120.753(9) 1_655 1_565 ? Ba1 Ba2 O2 127.44(12) . 1_654 ? Ba1 Ba2 O2 40.48(11) 1_655 1_654 ? Ba1 Ba2 O2 118.49(12) 1_565 1_654 ? Ba1 Ba2 O3 51.74(11) . 1_554 ? Ba1 Ba2 O3 155.53(11) 1_655 1_554 ? Ba1 Ba2 O3 80.97(10) 1_565 1_554 ? Ba1 Ba2 O4 42.34(12) . . ? Ba1 Ba2 O4 103.33(11) 1_655 . ? Ba1 Ba2 O4 80.57(12) 1_565 . ? Ba1 Ba2 O5 84.36(15) . . ? Ba1 Ba2 O5 114.59(16) 1_655 . ? Ba1 Ba2 O5 35.55(15) 1_565 . ? Ba1 Ba2 O7 140.50(18) . 1_565 ? Ba1 Ba2 O7 113.94(18) 1_655 1_565 ? Ba1 Ba2 O7 41.92(15) 1_565 1_565 ? Ba1 Ba2 O8 40.67(12) . . ? Ba1 Ba2 O8 91.04(13) 1_655 . ? Ba1 Ba2 O8 146.57(13) 1_565 . ? Ba1 Ba2 O10 71.39(10) . 1_556 ? Ba1 Ba2 O10 38.33(10) 1_655 1_556 ? Ba1 Ba2 O10 121.26(12) 1_565 1_556 ? Ba1 Ba2 C15 65.19(18) . . ? Ba1 Ba2 C15 105.85(19) 1_655 . ? Ba1 Ba2 C15 58.61(18) 1_565 . ? Ba1 Ba2 O12 131.36(14) . . ? Ba1 Ba2 O12 52.81(13) 1_655 . ? Ba1 Ba2 O12 67.94(13) 1_565 . ? O2 Ba2 O3 141.99(16) 1_654 1_554 ? O2 Ba2 O4 143.48(16) 1_654 . ? O2 Ba2 O5 139.5(2) 1_654 . ? O2 Ba2 O7 86.8(2) 1_654 1_565 ? O2 Ba2 O8 91.95(18) 1_654 . ? O2 Ba2 O10 77.11(15) 1_654 1_556 ? O2 Ba2 C15 143.2(2) 1_654 . ? O2 Ba2 O12 67.78(18) 1_654 . ? O3 Ba2 O4 66.97(16) 1_554 . ? O3 Ba2 O5 75.66(19) 1_554 . ? O3 Ba2 O7 89.6(2) 1_554 1_565 ? O3 Ba2 O8 65.93(17) 1_554 . ? O3 Ba2 O10 122.68(15) 1_554 1_556 ? O3 Ba2 C15 74.6(2) 1_554 . ? O3 Ba2 O12 146.74(16) 1_554 . ? O4 Ba2 O5 45.7(2) . . ? O4 Ba2 O7 121.4(2) . 1_565 ? O4 Ba2 O8 82.24(17) . . ? O4 Ba2 O10 66.45(15) . 1_556 ? O4 Ba2 C15 23.6(2) . . ? O4 Ba2 O12 95.55(18) . . ? O5 Ba2 O7 77.4(2) . 1_565 ? O5 Ba2 O8 124.7(2) . . ? O5 Ba2 O10 94.1(2) . 1_556 ? O5 Ba2 C15 23.1(2) . . ? O5 Ba2 O12 72.2(2) . . ? O7 Ba2 O8 137.0(2) 1_565 . ? O7 Ba2 O10 143.9(2) 1_565 1_556 ? O7 Ba2 C15 100.5(2) 1_565 . ? O7 Ba2 O12 75.4(2) 1_565 . ? O8 Ba2 O10 76.44(17) . 1_556 ? O8 Ba2 C15 105.6(2) . . ? O8 Ba2 O12 142.48(19) . . ? O10 Ba2 C15 76.0(2) 1_556 . ? O10 Ba2 O12 68.59(18) 1_556 . ? C15 Ba2 O12 79.2(2) . . ? Ba1 O2 Ba2 101.18(16) 1_556 1_456 ? Ba1 O2 C14 102.4(5) 1_556 . ? Ba2 O2 C14 126.3(5) 1_456 . ? Ba1 O3 Ba2 87.20(14) 1_556 1_556 ? Ba1 O3 C14 83.0(5) 1_556 . ? Ba2 O3 C14 133.3(5) 1_556 . ? Ba1 O4 Ba2 93.22(17) . . ? Ba1 O4 C15 162.2(6) . . ? Ba2 O4 C15 89.2(6) . . ? Ba1 O5 Ba2 108.7(2) 1_565 . ? Ba1 O5 C15 153.4(6) 1_565 . ? Ba2 O5 C15 97.9(6) . . ? Ba1 O7 Ba2 102.2(2) . 1_545 ? Ba1 O7 C29 85.7(6) . . ? Ba2 O7 C29 160.7(7) 1_545 . ? Ba1 O8 Ba2 99.21(18) . . ? Ba1 O8 C29 100.2(6) . . ? Ba2 O8 C29 159.8(6) . . ? Ba1 O9 C30 128.8(5) 1_554 . ? Ba1 O10 Ba2 103.03(15) 1_654 1_554 ? Ba1 O10 C30 133.6(6) 1_654 . ? Ba2 O10 C30 123.1(6) 1_554 . ? H1A C1 C2 120.9 . . ? H1A C1 C13 120.9 . . ? C2 C1 C13 118.3(6) . . ? C1 C2 C3 119.9(7) . . ? C1 C2 C14 120.4(7) . . ? C3 C2 C14 119.7(7) . . ? C2 C3 H3A 119.2 . . ? C2 C3 C4 121.7(6) . . ? H3A C3 C4 119.2 . . ? C3 C4 H4A 121.3 . . ? C3 C4 C5 117.4(6) . . ? H4A C4 C5 121.3 . . ? C4 C5 C6 130.6(6) . . ? C4 C5 C13 120.4(6) . . ? C6 C5 C13 108.9(6) . . ? C5 C6 C7 131.1(6) . . ? C5 C6 C11 108.7(6) . . ? C7 C6 C11 120.2(6) . . ? C6 C7 H7A 121.0 . . ? C6 C7 C8 118.0(6) . . ? H7A C7 C8 121.0 . . ? C7 C8 H8A 118.8 . . ? C7 C8 C9 122.5(6) . . ? H8A C8 C9 118.8 . . ? C8 C9 C10 119.3(6) . . ? C8 C9 C15 119.0(6) . . ? C10 C9 C15 121.6(7) . . ? C9 C10 H10A 120.9 . . ? C9 C10 C11 118.2(6) . . ? H10A C10 C11 120.9 . . ? C6 C11 C10 121.9(6) . . ? C6 C11 C12 108.9(5) . . ? C10 C11 C12 129.0(6) . . ? O1 C12 C11 127.7(6) . . ? O1 C12 C13 127.1(6) . . ? C11 C12 C13 105.1(5) . . ? C1 C13 C5 122.2(6) . . ? C1 C13 C12 129.6(6) . . ? C5 C13 C12 108.2(5) . . ? Ba1 C14 O2 56.0(4) 1_556 . ? Ba1 C14 O3 74.9(5) 1_556 . ? Ba1 C14 C2 146.4(5) 1_556 . ? O2 C14 O3 121.6(8) . . ? O2 C14 C2 119.1(7) . . ? O3 C14 C2 119.3(7) . . ? Ba2 C15 O4 67.1(5) . . ? Ba2 C15 O5 59.0(5) . . ? Ba2 C15 C9 154.6(6) . . ? O4 C15 O5 121.8(9) . . ? O4 C15 C9 119.1(8) . . ? O5 C15 C9 119.0(8) . . ? H16A C16 C17 121.1 . . ? H16A C16 C28 121.1 . . ? C17 C16 C28 117.7(6) . . ? C16 C17 C18 119.9(6) . . ? C16 C17 C29 121.1(7) . . ? C18 C17 C29 118.8(7) . . ? C17 C18 H18A 118.9 . . ? C17 C18 C19 122.1(6) . . ? H18A C18 C19 118.9 . . ? C18 C19 H19A 120.9 . . ? C18 C19 C20 118.3(6) . . ? H19A C19 C20 120.9 . . ? C19 C20 C21 132.0(6) . . ? C19 C20 C28 119.8(6) . . ? C21 C20 C28 108.3(5) . . ? C20 C21 C22 131.5(6) . . ? C20 C21 C26 108.9(6) . . ? C22 C21 C26 119.6(6) . . ? C21 C22 H22A 120.9 . . ? C21 C22 C23 118.3(6) . . ? H22A C22 C23 120.9 . . ? C22 C23 H23A 119.3 . . ? C22 C23 C24 121.4(6) . . ? H23A C23 C24 119.3 . . ? C23 C24 C25 120.4(7) . . ? C23 C24 C30 120.9(7) . . ? C25 C24 C30 118.7(7) . . ? C24 C25 H25A 121.2 . . ? C24 C25 C26 117.7(6) . . ? H25A C25 C26 121.2 . . ? C21 C26 C25 122.6(6) . . ? C21 C26 C27 108.8(5) . . ? C25 C26 C27 128.6(6) . . ? O6 C27 C26 127.0(6) . . ? O6 C27 C28 127.6(6) . . ? C26 C27 C28 105.4(5) . . ? C16 C28 C20 122.1(6) . . ? C16 C28 C27 129.5(6) . . ? C20 C28 C27 108.4(5) . . ? Ba1 C29 O7 70.6(5) . . ? Ba1 C29 O8 57.3(5) . . ? Ba1 C29 C17 155.6(6) . . ? O7 C29 O8 123.0(9) . . ? O7 C29 C17 119.0(9) . . ? O8 C29 C17 118.0(8) . . ? O9 C30 O10 125.4(9) . . ? O9 C30 C24 118.0(8) . . ? O10 C30 C24 116.5(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.097 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.156 # Attachment '- cdfdc.cif' data_cdfdc _database_code_depnum_ccdc_archive 'CCDC 793003' #TrackingRef '- cdfdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H12 Cd O8' _chemical_formula_weight 432.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cd Cd -0.9197 1.4096 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _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 7.7123(2) _cell_length_b 28.5057(8) _cell_length_c 6.6459(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.050(2) _cell_angle_gamma 90.00 _cell_volume 1410.95(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 33.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20326 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 33.61 _reflns_number_total 4304 _reflns_number_gt 3946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.60a' _computing_data_reduction 'Bruker SAINT v7.60a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically on the carbon atoms and rided using a riding model. The hydrogen atoms on the waters were found in the difference map, and their distances to their oxygens restrained to being the similar within an su of 0.01. Their displacement parameters were riden on their oxygens. ; _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^)+(0.0267P)^2^+0.9406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _refine_ls_number_reflns 4304 _refine_ls_number_parameters 235 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.006 _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 0.783610(16) 0.523252(4) 0.330768(19) 0.01055(5) Uani 1 1 d . . . C1 C 0.4144(2) 0.18545(6) 0.3702(3) 0.0117(3) Uani 1 1 d . . . H1 H 0.2871 0.1837 0.3295 0.014 Uiso 1 1 calc R . . C2 C 0.5192(2) 0.14461(6) 0.3966(3) 0.0116(3) Uani 1 1 d . . . C3 C 0.7070(2) 0.14768(6) 0.4595(3) 0.0122(3) Uani 1 1 d . . . H3 H 0.7765 0.1197 0.4770 0.015 Uiso 1 1 calc R . . C4 C 0.7940(2) 0.19101(6) 0.4970(3) 0.0119(3) Uani 1 1 d . . . H4 H 0.9212 0.1928 0.5421 0.014 Uiso 1 1 calc R . . C5 C 0.6901(2) 0.23129(6) 0.4669(3) 0.0104(3) Uani 1 1 d . . . C6 C 0.7429(2) 0.28140(6) 0.4818(3) 0.0107(3) Uani 1 1 d . . . C7 C 0.9104(2) 0.30256(6) 0.5306(3) 0.0126(3) Uani 1 1 d . . . H7 H 1.0169 0.2843 0.5681 0.015 Uiso 1 1 calc R . . C8 C 0.9189(2) 0.35164(6) 0.5234(3) 0.0119(3) Uani 1 1 d . . . H8 H 1.0327 0.3667 0.5566 0.014 Uiso 1 1 calc R . . C9 C 0.7631(2) 0.37889(6) 0.4683(3) 0.0111(3) Uani 1 1 d . . . C10 C 0.5935(2) 0.35724(6) 0.4205(3) 0.0117(3) Uani 1 1 d . . . H10 H 0.4868 0.3755 0.3837 0.014 Uiso 1 1 calc R . . C11 C 0.5853(2) 0.30889(6) 0.4282(3) 0.0106(3) Uani 1 1 d . . . C12 C 0.4259(2) 0.27692(6) 0.3771(3) 0.0119(3) Uani 1 1 d . . . O1 O 0.26768(18) 0.28792(5) 0.3192(2) 0.0171(3) Uani 1 1 d . . . C13 C 0.5016(2) 0.22843(6) 0.4049(3) 0.0108(3) Uani 1 1 d . . . C14 C 0.4301(3) 0.09775(6) 0.3430(3) 0.0123(3) Uani 1 1 d . . . O2 O 0.51881(19) 0.06241(5) 0.3188(2) 0.0163(3) Uani 1 1 d . . . O3 O 0.25901(18) 0.09631(5) 0.3130(2) 0.0149(3) Uani 1 1 d . . . C15 C 0.7735(2) 0.43118(6) 0.4434(3) 0.0106(3) Uani 1 1 d . . . O4 O 0.92334(18) 0.45208(5) 0.4995(2) 0.0150(3) Uani 1 1 d . . . O5 O 0.63122(18) 0.45317(4) 0.3552(2) 0.0135(2) Uani 1 1 d . . . O6 O 0.72896(18) 0.54311(5) 0.6454(2) 0.0154(3) Uani 1 1 d D . . H6A H 0.6174(19) 0.5440(10) 0.633(4) 0.023 Uiso 1 1 d D . . H6B H 0.780(4) 0.5679(7) 0.700(4) 0.023 Uiso 1 1 d D . . O7 O 0.8136(2) 0.48861(5) 0.0282(2) 0.0171(3) Uani 1 1 d D . . H7A H 0.729(3) 0.4705(8) -0.029(4) 0.026 Uiso 1 1 d D . . H7B H 0.819(4) 0.5063(9) -0.071(4) 0.026 Uiso 1 1 d D . . O8 O 0.8619(2) 0.62203(5) 0.8435(2) 0.0195(3) Uani 1 1 d D . . H8A H 0.831(4) 0.6181(10) 0.956(3) 0.029 Uiso 1 1 d D . . H8B H 0.819(4) 0.6485(6) 0.798(4) 0.029 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01018(8) 0.00669(8) 0.01377(8) 0.00134(4) 0.00129(5) 0.00008(4) C1 0.0122(8) 0.0089(7) 0.0130(8) -0.0004(6) 0.0012(6) -0.0002(6) C2 0.0141(8) 0.0079(7) 0.0124(7) -0.0006(6) 0.0025(6) -0.0013(6) C3 0.0138(8) 0.0090(7) 0.0128(7) -0.0004(6) 0.0018(6) 0.0014(6) C4 0.0121(8) 0.0095(7) 0.0134(8) 0.0000(6) 0.0020(6) 0.0000(6) C5 0.0113(8) 0.0086(7) 0.0108(7) 0.0001(5) 0.0019(6) -0.0008(6) C6 0.0123(8) 0.0090(7) 0.0106(7) 0.0002(6) 0.0023(6) -0.0003(6) C7 0.0117(8) 0.0093(7) 0.0158(8) -0.0001(6) 0.0015(6) 0.0007(6) C8 0.0106(8) 0.0110(8) 0.0136(8) -0.0009(6) 0.0024(6) -0.0023(6) C9 0.0125(8) 0.0086(7) 0.0116(7) 0.0000(6) 0.0024(6) -0.0019(6) C10 0.0121(8) 0.0090(7) 0.0141(8) 0.0001(6) 0.0036(6) 0.0001(6) C11 0.0093(7) 0.0094(7) 0.0129(7) -0.0008(6) 0.0025(6) -0.0011(6) C12 0.0125(8) 0.0089(7) 0.0140(8) 0.0001(6) 0.0030(6) 0.0000(6) O1 0.0134(7) 0.0133(7) 0.0240(7) 0.0011(5) 0.0036(5) 0.0000(5) C13 0.0113(8) 0.0086(7) 0.0119(7) 0.0000(5) 0.0021(6) 0.0004(6) C14 0.0159(8) 0.0085(7) 0.0109(7) 0.0001(6) 0.0005(6) -0.0008(6) O2 0.0175(7) 0.0085(6) 0.0214(7) -0.0029(5) 0.0022(5) 0.0004(5) O3 0.0133(6) 0.0099(6) 0.0195(7) -0.0020(5) 0.0007(5) -0.0017(5) C15 0.0119(8) 0.0089(7) 0.0108(7) 0.0009(6) 0.0027(6) -0.0012(6) O4 0.0121(6) 0.0101(6) 0.0212(7) 0.0012(5) 0.0011(5) -0.0024(5) O5 0.0118(6) 0.0088(6) 0.0193(6) 0.0030(5) 0.0029(5) 0.0004(4) O6 0.0125(6) 0.0152(7) 0.0188(7) -0.0020(5) 0.0042(5) -0.0016(5) O7 0.0176(7) 0.0162(6) 0.0175(7) -0.0015(5) 0.0045(5) -0.0034(5) O8 0.0203(7) 0.0160(7) 0.0221(7) -0.0003(5) 0.0054(6) -0.0015(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 Cd1 O3 2.2793(14) 2_655 ? Cd1 O7 2.3050(15) . ? Cd1 O6 2.3080(14) . ? Cd1 O5 2.3447(13) . ? Cd1 O4 2.3561(14) 3_766 ? Cd1 O4 2.4305(13) . ? Cd1 O2 2.5437(14) 2_655 ? Cd1 C15 2.7357(17) . ? Cd1 C14 2.7516(18) 2_655 ? C1 C13 1.388(2) . ? C1 C2 1.402(2) . ? C1 H1 0.9500 . ? C2 C3 1.402(2) . ? C2 C14 1.502(2) . ? C3 C4 1.397(2) . ? C3 H3 0.9500 . ? C4 C5 1.385(2) . ? C4 H4 0.9500 . ? C5 C13 1.407(2) . ? C5 C6 1.481(2) . ? C6 C7 1.386(2) . ? C6 C11 1.412(2) . ? C7 C8 1.402(2) . ? C7 H7 0.9500 . ? C8 C9 1.397(2) . ? C8 H8 0.9500 . ? C9 C10 1.406(2) . ? C9 C15 1.504(2) . ? C10 C11 1.381(2) . ? C10 H10 0.9500 . ? C11 C12 1.496(2) . ? C12 O1 1.221(2) . ? C12 C13 1.493(2) . ? C14 O2 1.251(2) . ? C14 O3 1.283(2) . ? C14 Cd1 2.7515(18) 2_645 ? O2 Cd1 2.5436(14) 2_645 ? O3 Cd1 2.2792(14) 2_645 ? C15 O4 1.267(2) . ? C15 O5 1.267(2) . ? O4 Cd1 2.3561(13) 3_766 ? O6 H6A 0.844(13) . ? O6 H6B 0.845(13) . ? O7 H7A 0.843(13) . ? O7 H7B 0.839(13) . ? O8 H8A 0.845(13) . ? O8 H8B 0.848(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O7 93.56(5) 2_655 . ? O3 Cd1 O6 96.61(5) 2_655 . ? O7 Cd1 O6 168.12(5) . . ? O3 Cd1 O5 141.93(5) 2_655 . ? O7 Cd1 O5 82.02(5) . . ? O6 Cd1 O5 86.19(5) . . ? O3 Cd1 O4 86.79(5) 2_655 3_766 ? O7 Cd1 O4 104.15(5) . 3_766 ? O6 Cd1 O4 82.59(5) . 3_766 ? O5 Cd1 O4 131.06(5) . 3_766 ? O3 Cd1 O4 162.65(5) 2_655 . ? O7 Cd1 O4 84.94(5) . . ? O6 Cd1 O4 87.15(5) . . ? O5 Cd1 O4 55.04(4) . . ? O4 Cd1 O4 76.88(5) 3_766 . ? O3 Cd1 O2 54.37(5) 2_655 2_655 ? O7 Cd1 O2 97.87(5) . 2_655 ? O6 Cd1 O2 83.20(5) . 2_655 ? O5 Cd1 O2 88.61(4) . 2_655 ? O4 Cd1 O2 136.41(4) 3_766 2_655 ? O4 Cd1 O2 142.97(5) . 2_655 ? O3 Cd1 C15 168.51(5) 2_655 . ? O7 Cd1 C15 81.03(5) . . ? O6 Cd1 C15 87.86(5) . . ? O5 Cd1 C15 27.54(5) . . ? O4 Cd1 C15 104.32(5) 3_766 . ? O4 Cd1 C15 27.59(5) . . ? O2 Cd1 C15 116.07(5) 2_655 . ? O3 Cd1 C14 27.56(5) 2_655 2_655 ? O7 Cd1 C14 98.60(5) . 2_655 ? O6 Cd1 C14 87.74(5) . 2_655 ? O5 Cd1 C14 115.48(5) . 2_655 ? O4 Cd1 C14 111.48(5) 3_766 2_655 ? O4 Cd1 C14 169.53(5) . 2_655 ? O2 Cd1 C14 26.97(5) 2_655 2_655 ? C15 Cd1 C14 143.00(5) . 2_655 ? C13 C1 C2 118.30(16) . . ? C13 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? C1 C2 C3 120.17(16) . . ? C1 C2 C14 119.71(16) . . ? C3 C2 C14 119.99(16) . . ? C4 C3 C2 121.31(16) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 118.32(17) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C13 120.62(16) . . ? C4 C5 C6 130.65(16) . . ? C13 C5 C6 108.69(15) . . ? C7 C6 C11 120.45(16) . . ? C7 C6 C5 131.17(16) . . ? C11 C6 C5 108.34(15) . . ? C6 C7 C8 118.36(16) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 121.28(16) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 120.09(16) . . ? C8 C9 C15 120.85(15) . . ? C10 C9 C15 118.90(16) . . ? C11 C10 C9 118.58(16) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C6 121.22(16) . . ? C10 C11 C12 129.94(16) . . ? C6 C11 C12 108.78(15) . . ? O1 C12 C13 127.09(17) . . ? O1 C12 C11 127.57(16) . . ? C13 C12 C11 105.31(15) . . ? C1 C13 C5 121.26(16) . . ? C1 C13 C12 129.80(16) . . ? C5 C13 C12 108.87(15) . . ? O2 C14 O3 121.94(17) . . ? O2 C14 C2 120.97(17) . . ? O3 C14 C2 116.99(16) . . ? O2 C14 Cd1 67.22(10) . 2_645 ? O3 C14 Cd1 55.27(9) . 2_645 ? C2 C14 Cd1 166.68(12) . 2_645 ? C14 O2 Cd1 85.81(11) . 2_645 ? C14 O3 Cd1 97.17(11) . 2_645 ? O4 C15 O5 121.17(16) . . ? O4 C15 C9 120.28(16) . . ? O5 C15 C9 118.44(15) . . ? O4 C15 Cd1 62.67(9) . . ? O5 C15 Cd1 58.79(9) . . ? C9 C15 Cd1 170.71(12) . . ? C15 O4 Cd1 165.79(12) . 3_766 ? C15 O4 Cd1 89.74(10) . . ? Cd1 O4 Cd1 103.12(5) 3_766 . ? C15 O5 Cd1 93.67(11) . . ? Cd1 O6 H6A 110.1(19) . . ? Cd1 O6 H6B 114.8(19) . . ? H6A O6 H6B 112(3) . . ? Cd1 O7 H7A 114(2) . . ? Cd1 O7 H7B 118(2) . . ? H7A O7 H7B 102(3) . . ? H8A O8 H8B 105(3) . . ? 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 O6 H6A O5 0.844(13) 1.940(14) 2.7789(19) 173(3) 3_666 O6 H6B O8 0.845(13) 1.836(14) 2.673(2) 170(3) . O7 H7A O2 0.843(13) 1.917(14) 2.753(2) 171(3) 4_565 O7 H7B O6 0.839(13) 2.111(17) 2.907(2) 158(3) 1_554 O8 H8A O3 0.845(13) 1.947(14) 2.779(2) 168(3) 2_656 O8 H8B O1 0.848(13) 2.016(14) 2.863(2) 176(3) 3_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.594 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.112 # Attachment '- mnfdc.cif' data_mnfdc _database_code_depnum_ccdc_archive 'CCDC 793004' #TrackingRef '- mnfdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H10 Mn O7' _chemical_formula_weight 357.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Mn Mn 0.2237 0.8587 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _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 26.943(2) _cell_length_b 7.2476(6) _cell_length_c 6.9261(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.703(2) _cell_angle_gamma 90.00 _cell_volume 1340.27(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4730 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 33.57 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'TWINABS v2008/2 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14469 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 33.60 _reflns_number_total 2016 _reflns_number_gt 1811 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.60a' _computing_data_reduction 'Bruker SAINT v7.60a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. A single crystal could not be found and therefore the data were collected on a twin. CELL_NOW was used to determined the orientation matrices and the domains were related by a 180 deg rotation around the recipocal axis 0 0 1. The integration was preformed with both matrice. TWINABS was you to produce a merged HKLF4 file, for structure solution and initial refinement, and HKLF5 file for for final structure refinement. The HKLF5 file contained the merged reflections first component and those that overlapped with the second component were split into 2 reflection. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically on the carbon atoms and refined using a riding model. The hydrogen atoms on the water were found in the difference map, and refined freely. ; _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^)+(0.0356P)^2^+0.8982P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _refine_ls_number_reflns 2016 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Mn1 Mn 0.2500 0.7500 0.0000 0.01056(8) Uani 1 2 d S . . O1 O 0.0000 0.8255(2) 0.2500 0.0243(4) Uani 1 2 d S . . O2 O 0.21209(4) 0.33697(13) 0.21582(17) 0.01266(19) Uani 1 1 d . . . O3 O 0.19208(4) 0.63223(14) 0.14824(16) 0.0142(2) Uani 1 1 d . . . C1 C 0.09294(5) 0.57709(19) 0.2192(2) 0.0132(3) Uani 1 1 d . . . H1A H 0.1034 0.7017 0.2112 0.016 Uiso 1 1 calc R . . C2 C 0.12705(5) 0.43129(18) 0.2148(2) 0.0121(2) Uani 1 1 d . . . C3 C 0.11108(5) 0.24814(19) 0.2289(2) 0.0158(3) Uani 1 1 d . . . H3A H 0.1348 0.1512 0.2301 0.019 Uiso 1 1 calc R . . C4 C 0.06095(5) 0.2049(2) 0.2411(3) 0.0171(3) Uani 1 1 d . . . H4A H 0.0503 0.0804 0.2476 0.021 Uiso 1 1 calc R . . C5 C 0.02732(5) 0.34959(19) 0.2433(2) 0.0137(3) Uani 1 1 d . . . C6 C 0.04362(5) 0.53403(18) 0.2356(2) 0.0131(3) Uani 1 1 d . . . C7 C 0.0000 0.6581(3) 0.2500 0.0145(4) Uani 1 2 d S . . C8 C 0.18054(5) 0.47134(18) 0.1920(2) 0.0111(2) Uani 1 1 d . . . O4 O 0.28846(4) 0.48028(14) 0.03761(19) 0.0150(2) Uani 1 1 d . . . H1WA H 0.2971(8) 0.413(3) -0.048(4) 0.032(6) Uiso 1 1 d . . . H2WA H 0.2719(9) 0.408(4) 0.104(4) 0.044(7) 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 Mn1 0.01050(12) 0.00762(12) 0.01372(13) -0.00029(10) 0.00218(12) -0.00109(10) O1 0.0183(7) 0.0113(7) 0.0441(11) 0.000 0.0069(7) 0.000 O2 0.0116(4) 0.0101(4) 0.0162(5) 0.0012(4) 0.0020(4) 0.0017(3) O3 0.0132(4) 0.0102(4) 0.0197(5) 0.0012(4) 0.0046(4) -0.0009(4) C1 0.0117(6) 0.0111(5) 0.0169(7) 0.0011(5) 0.0022(5) -0.0008(5) C2 0.0096(5) 0.0120(5) 0.0149(7) 0.0010(5) 0.0017(5) -0.0002(5) C3 0.0123(6) 0.0113(6) 0.0241(8) 0.0012(5) 0.0036(5) 0.0008(5) C4 0.0121(6) 0.0112(5) 0.0284(8) 0.0018(5) 0.0039(5) -0.0001(5) C5 0.0116(6) 0.0114(6) 0.0185(7) -0.0001(5) 0.0032(5) 0.0003(5) C6 0.0121(6) 0.0101(6) 0.0172(7) 0.0006(5) 0.0022(5) 0.0005(5) C7 0.0115(8) 0.0122(8) 0.0195(10) 0.000 0.0013(7) 0.000 C8 0.0101(5) 0.0122(6) 0.0110(6) -0.0007(5) 0.0018(5) -0.0002(4) O4 0.0163(4) 0.0111(4) 0.0184(6) 0.0000(4) 0.0053(5) 0.0001(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 Mn1 O2 2.1853(11) 6_565 ? Mn1 O2 2.1853(11) 4 ? Mn1 O3 2.1557(10) . ? Mn1 O3 2.1557(10) 7_565 ? Mn1 O4 2.2114(10) . ? Mn1 O4 2.2114(10) 7_565 ? O1 C7 1.213(3) . ? O2 Mn1 2.1853(11) 4_545 ? O2 C8 1.2888(15) . ? O3 C8 1.2544(16) . ? C1 H1A 0.9500 . ? C1 C2 1.4034(18) . ? C1 C6 1.3845(18) . ? C2 C3 1.4028(18) . ? C2 C8 1.4990(18) . ? C3 H3A 0.9500 . ? C3 C4 1.3999(19) . ? C4 H4A 0.9500 . ? C4 C5 1.387(2) . ? C5 C5 1.487(3) 2 ? C5 C6 1.4103(19) . ? C6 C7 1.4938(18) . ? C7 C6 1.4937(18) 2 ? O4 H1WA 0.82(3) . ? O4 H2WA 0.86(3) . ? 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 Mn1 O2 180.0 6_565 4 ? O2 Mn1 O3 91.95(4) 6_565 . ? O2 Mn1 O3 88.05(4) 6_565 7_565 ? O2 Mn1 O3 88.05(4) 4 . ? O2 Mn1 O3 91.95(4) 4 7_565 ? O2 Mn1 O4 89.65(4) 6_565 7_565 ? O2 Mn1 O4 90.35(4) 4 7_565 ? O2 Mn1 O4 90.35(4) 6_565 . ? O2 Mn1 O4 89.65(4) 4 . ? O3 Mn1 O3 180.0 . 7_565 ? O3 Mn1 O4 87.22(4) . . ? O3 Mn1 O4 92.78(4) . 7_565 ? O3 Mn1 O4 87.22(4) 7_565 7_565 ? O3 Mn1 O4 92.78(4) 7_565 . ? O4 Mn1 O4 180.00(5) . 7_565 ? Mn1 O2 C8 123.64(9) 4_545 . ? Mn1 O3 C8 134.58(9) . . ? H1A C1 C2 121.0 . . ? H1A C1 C6 121.0 . . ? C2 C1 C6 118.07(12) . . ? C1 C2 C3 120.20(12) . . ? C1 C2 C8 119.87(12) . . ? C3 C2 C8 119.92(12) . . ? C2 C3 H3A 119.2 . . ? C2 C3 C4 121.56(13) . . ? H3A C3 C4 119.2 . . ? C3 C4 H4A 121.0 . . ? C3 C4 C5 117.93(13) . . ? H4A C4 C5 121.0 . . ? C4 C5 C5 130.85(8) . 2 ? C4 C5 C6 120.59(13) . . ? C5 C5 C6 108.55(8) 2 . ? C1 C6 C5 121.60(13) . . ? C1 C6 C7 129.95(12) . . ? C5 C6 C7 108.45(12) . . ? O1 C7 C6 127.02(8) . . ? O1 C7 C6 127.02(8) . 2 ? C6 C7 C6 105.96(16) . 2 ? O2 C8 O3 123.55(12) . . ? O2 C8 C2 117.85(12) . . ? O3 C8 C2 118.59(12) . . ? Mn1 O4 H1WA 127.6(17) . . ? Mn1 O4 H2WA 109.5(17) . . ? H1WA O4 H2WA 104(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1WA O2 0.82(3) 2.15(3) 2.8916(16) 150(2) 7 O4 H2WA O2 0.86(3) 1.95(3) 2.7416(15) 153(2) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.502 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.068