# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Qi-Bing Bo' _publ_contact_author_email chm_boqb@ujn.edu.cn loop_ _publ_author_name 'Qi-Bing Bo' 'Hong-Yan Wang' 'Daqi Wang' #===END data_ZnMg-mip _database_code_depnum_ccdc_archive 'CCDC 865282' #TrackingRef 'revised_cif[1].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Mg O13 Zn' _chemical_formula_weight 536.04 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' Mg Mg 0.0486 0.0363 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 22.0170(17) _cell_length_b 16.2879(16) _cell_length_c 13.7909(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4945.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8637 _exptl_absorpt_correction_T_max 0.8906 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16243 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5216 _reflns_number_gt 3231 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+5.3459P] 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 5216 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.33117(2) -0.00209(3) 1.02021(4) 0.03956(19) Uani 1 1 d . . . Mg1 Mg 0.25915(6) -0.05091(9) 1.27790(10) 0.0366(4) Uani 1 1 d . . . O1 O 0.38959(18) 0.0145(3) 0.9177(3) 0.0804(13) Uani 1 1 d . . . O2 O 0.32988(16) 0.0573(3) 0.7994(3) 0.0828(14) Uani 1 1 d . . . O3 O 0.60774(16) 0.0258(3) 0.8831(3) 0.0740(12) Uani 1 1 d . . . O4 O 0.65054(17) 0.0525(3) 0.7420(3) 0.1002(17) Uani 1 1 d . . . O5 O 0.28827(15) 0.09998(18) 1.0500(2) 0.0465(8) Uani 1 1 d . . . O6 O 0.24563(14) 0.0337(2) 1.1720(3) 0.0520(9) Uani 1 1 d . . . O7 O 0.28322(15) -0.0999(2) 0.9959(2) 0.0471(8) Uani 1 1 d . . . O8 O 0.23056(16) -0.0334(2) 0.8853(3) 0.0617(10) Uani 1 1 d . . . O1W O 0.2524(3) -0.1461(2) 1.1802(3) 0.1006(18) Uani 1 1 d . . . H1WB H 0.2135 -0.1569 1.1619 0.151 Uiso 1 1 d R . . H1WA H 0.2728 -0.1358 1.1243 0.151 Uiso 1 1 d R . . O2W O 0.2675(3) -0.1459(2) 1.3782(3) 0.106(2) Uani 1 1 d . . . H2WA H 0.3082 -0.1581 1.3954 0.160 Uiso 1 1 d R . . H2WB H 0.2484 -0.1373 1.4399 0.160 Uiso 1 1 d R . . C1 C 0.3806(2) 0.0398(3) 0.8321(4) 0.0474(12) Uani 1 1 d . . . C2 C 0.43585(19) 0.0509(3) 0.7693(3) 0.0411(11) Uani 1 1 d . . . C3 C 0.4297(2) 0.0744(3) 0.6735(3) 0.0558(14) Uani 1 1 d . . . H3 H 0.3911 0.0811 0.6473 0.067 Uiso 1 1 calc R . . C4 C 0.4796(3) 0.0882(4) 0.6164(4) 0.0648(16) Uani 1 1 d . . . C5 C 0.4709(4) 0.1138(6) 0.5096(4) 0.111(3) Uani 1 1 d . . . H5A H 0.4315 0.0965 0.4878 0.167 Uiso 1 1 calc R . . H5B H 0.5017 0.0884 0.4705 0.167 Uiso 1 1 calc R . . H5C H 0.4741 0.1724 0.5042 0.167 Uiso 1 1 calc R . . C6 C 0.5372(2) 0.0754(3) 0.6546(3) 0.0559(14) Uani 1 1 d . . . H6 H 0.5714 0.0828 0.6159 0.067 Uiso 1 1 calc R . . C7 C 0.5439(2) 0.0514(3) 0.7515(3) 0.0436(11) Uani 1 1 d . . . C8 C 0.6061(2) 0.0425(3) 0.7934(4) 0.0491(12) Uani 1 1 d . . . C9 C 0.49319(18) 0.0391(3) 0.8075(3) 0.0423(11) Uani 1 1 d . . . H9 H 0.4975 0.0227 0.8717 0.051 Uiso 1 1 calc R . . C10 C 0.25445(18) 0.0975(3) 1.1253(3) 0.0344(10) Uani 1 1 d . . . C11 C 0.22494(17) 0.1761(3) 1.1548(3) 0.0337(9) Uani 1 1 d . . . C12 C 0.2494(2) 0.2500 1.1219(4) 0.0320(13) Uani 1 2 d S . . H12 H 0.2817 0.2500 1.0785 0.038 Uiso 1 2 calc SR . . C13 C 0.1759(2) 0.1769(3) 1.2161(4) 0.0489(12) Uani 1 1 d . . . H13 H 0.1595 0.1273 1.2367 0.059 Uiso 1 1 calc R . . C14 C 0.1500(3) 0.2500 1.2485(5) 0.0522(19) Uani 1 2 d S . . C15 C 0.0971(4) 0.2500 1.3181(8) 0.099(3) Uani 1 2 d S . . H15A H 0.0828 0.3052 1.3269 0.148 Uiso 0.50 1 calc PR . . H15B H 0.1099 0.2281 1.3793 0.148 Uiso 0.50 1 calc PR . . H15C H 0.0650 0.2168 1.2922 0.148 Uiso 0.50 1 calc PR . . C16 C 0.2436(2) -0.0973(3) 0.9277(3) 0.0426(11) Uani 1 1 d . . . C17 C 0.21258(19) -0.1768(3) 0.9033(3) 0.0382(10) Uani 1 1 d . . . C18 C 0.1608(2) -0.1766(3) 0.8458(4) 0.0525(13) Uani 1 1 d . . . H18 H 0.1439 -0.1271 0.8260 0.063 Uiso 1 1 calc R . . C19 C 0.1343(3) -0.2500 0.8180(6) 0.061(2) Uani 1 2 d S . . C20 C 0.0761(4) -0.2500 0.7559(9) 0.123(5) Uani 1 2 d S . . H20A H 0.0637 -0.1944 0.7439 0.185 Uiso 0.50 1 calc PR . . H20B H 0.0444 -0.2785 0.7898 0.185 Uiso 0.50 1 calc PR . . H20C H 0.0840 -0.2770 0.6954 0.185 Uiso 0.50 1 calc PR . . C21 C 0.2374(3) -0.2500 0.9329(4) 0.0364(14) Uani 1 2 d S . . H21 H 0.2713 -0.2500 0.9732 0.044 Uiso 1 2 calc SR . . 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 0.0406(3) 0.0478(4) 0.0303(3) 0.0003(2) 0.0003(2) 0.0071(3) Mg1 0.0423(8) 0.0373(8) 0.0303(8) 0.0001(6) 0.0063(6) 0.0099(6) O1 0.068(2) 0.125(4) 0.048(2) 0.017(2) 0.0221(19) 0.024(2) O2 0.042(2) 0.129(4) 0.078(3) 0.005(3) -0.010(2) -0.032(2) O3 0.052(2) 0.132(4) 0.039(2) 0.002(2) -0.0151(17) 0.000(2) O4 0.046(2) 0.188(5) 0.067(3) 0.026(3) 0.020(2) 0.056(3) O5 0.061(2) 0.0424(18) 0.0366(17) 0.0021(15) 0.0052(16) 0.0081(15) O6 0.056(2) 0.0435(19) 0.057(2) 0.0155(17) 0.0021(17) 0.0024(15) O7 0.053(2) 0.0481(19) 0.0399(18) -0.0079(15) -0.0095(15) 0.0013(16) O8 0.062(2) 0.057(2) 0.066(2) 0.023(2) 0.0003(19) -0.0055(18) O1W 0.219(6) 0.045(2) 0.037(2) -0.0026(19) 0.020(3) -0.020(3) O2W 0.203(6) 0.078(3) 0.038(2) 0.014(2) 0.035(3) 0.079(3) C1 0.043(3) 0.049(3) 0.050(3) -0.013(3) 0.000(2) -0.001(2) C2 0.039(2) 0.050(3) 0.034(2) -0.001(2) -0.0021(18) 0.001(2) C3 0.047(3) 0.083(4) 0.037(3) 0.003(3) -0.015(2) 0.008(3) C4 0.060(3) 0.102(5) 0.033(3) 0.013(3) -0.007(2) 0.015(3) C5 0.108(6) 0.185(9) 0.041(3) 0.038(5) -0.010(4) 0.024(6) C6 0.055(3) 0.079(4) 0.034(3) 0.008(3) 0.011(2) 0.007(3) C7 0.044(3) 0.056(3) 0.031(2) -0.001(2) 0.0017(19) 0.010(2) C8 0.048(3) 0.056(3) 0.044(3) -0.011(2) -0.002(2) 0.015(2) C9 0.041(2) 0.062(3) 0.024(2) 0.004(2) -0.0006(18) 0.012(2) C10 0.035(2) 0.038(2) 0.030(2) 0.002(2) -0.0061(18) -0.0014(18) C11 0.029(2) 0.045(3) 0.027(2) -0.0017(19) -0.0025(17) 0.0016(18) C12 0.033(3) 0.039(3) 0.024(3) 0.000 0.004(2) 0.000 C13 0.036(3) 0.052(3) 0.058(3) 0.013(3) 0.003(2) -0.008(2) C14 0.029(3) 0.071(5) 0.056(5) 0.000 0.018(3) 0.000 C15 0.071(6) 0.114(8) 0.112(8) 0.000 0.052(6) 0.000 C16 0.041(3) 0.055(3) 0.032(2) 0.003(2) 0.005(2) 0.002(2) C17 0.035(2) 0.055(3) 0.025(2) 0.002(2) 0.0070(18) 0.004(2) C18 0.041(3) 0.073(4) 0.043(3) 0.015(3) -0.003(2) 0.008(2) C19 0.040(4) 0.092(6) 0.052(5) 0.000 -0.019(3) 0.000 C20 0.070(7) 0.164(11) 0.137(10) 0.000 -0.071(7) 0.000 C21 0.027(3) 0.054(4) 0.028(3) 0.000 -0.004(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.930(4) . ? Zn1 O3 1.933(3) 5_657 ? Zn1 O7 1.941(3) . ? Zn1 O5 1.956(3) . ? Mg1 O2 1.985(4) 2 ? Mg1 O4 2.007(4) 5_657 ? Mg1 O6 2.030(4) . ? Mg1 O8 2.032(4) 2 ? Mg1 O1W 2.060(4) . ? Mg1 O2W 2.084(4) . ? O1 C1 1.265(6) . ? O2 C1 1.238(6) . ? O2 Mg1 1.985(4) 2_554 ? O3 C8 1.266(6) . ? O3 Zn1 1.933(3) 5_657 ? O4 C8 1.219(6) . ? O4 Mg1 2.007(4) 5_657 ? O5 C10 1.278(5) . ? O6 C10 1.239(5) . ? O7 C16 1.285(5) . ? O8 C16 1.228(5) . ? O8 Mg1 2.032(4) 2_554 ? O1W H1WB 0.9109 . ? O1W H1WA 0.9081 . ? O2W H2WA 0.9488 . ? O2W H2WB 0.9591 . ? C1 C2 1.504(6) . ? C2 C9 1.382(6) . ? C2 C3 1.383(6) . ? C3 C4 1.371(7) . ? C3 H3 0.9300 . ? C4 C6 1.389(7) . ? C4 C5 1.541(7) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.400(6) . ? C6 H6 0.9300 . ? C7 C9 1.373(6) . ? C7 C8 1.494(6) . ? C9 H9 0.9300 . ? C10 C11 1.491(6) . ? C11 C13 1.371(6) . ? C11 C12 1.395(5) . ? C12 C11 1.395(5) 8_565 ? C12 H12 0.9300 . ? C13 C14 1.394(6) . ? C13 H13 0.9300 . ? C14 C13 1.394(6) 8_565 ? C14 C15 1.508(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.502(6) . ? C17 C21 1.373(5) . ? C17 C18 1.388(6) . ? C18 C19 1.384(6) . ? C18 H18 0.9300 . ? C19 C18 1.384(6) 8 ? C19 C20 1.540(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C17 1.373(5) 8 ? C21 H21 0.9300 . ? 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 O3 94.00(18) . 5_657 ? O1 Zn1 O7 110.55(17) . . ? O3 Zn1 O7 109.45(17) 5_657 . ? O1 Zn1 O5 110.89(16) . . ? O3 Zn1 O5 111.19(16) 5_657 . ? O7 Zn1 O5 118.14(15) . . ? O2 Mg1 O4 176.2(2) 2 5_657 ? O2 Mg1 O6 89.91(17) 2 . ? O4 Mg1 O6 93.20(17) 5_657 . ? O2 Mg1 O8 92.10(17) 2 2 ? O4 Mg1 O8 89.86(19) 5_657 2 ? O6 Mg1 O8 94.72(16) . 2 ? O2 Mg1 O1W 89.3(2) 2 . ? O4 Mg1 O1W 88.4(2) 5_657 . ? O6 Mg1 O1W 91.70(16) . . ? O8 Mg1 O1W 173.43(18) 2 . ? O2 Mg1 O2W 87.1(2) 2 . ? O4 Mg1 O2W 89.6(2) 5_657 . ? O6 Mg1 O2W 174.1(2) . . ? O8 Mg1 O2W 90.45(17) 2 . ? O1W Mg1 O2W 83.20(17) . . ? C1 O1 Zn1 128.7(4) . . ? C1 O2 Mg1 158.9(4) . 2_554 ? C8 O3 Zn1 137.4(4) . 5_657 ? C8 O4 Mg1 150.7(4) . 5_657 ? C10 O5 Zn1 115.2(3) . . ? C10 O6 Mg1 157.1(3) . . ? C16 O7 Zn1 118.0(3) . . ? C16 O8 Mg1 153.3(3) . 2_554 ? Mg1 O1W H1WB 113.2 . . ? Mg1 O1W H1WA 112.3 . . ? H1WB O1W H1WA 105.5 . . ? Mg1 O2W H2WA 113.8 . . ? Mg1 O2W H2WB 116.2 . . ? H2WA O2W H2WB 102.9 . . ? O2 C1 O1 123.7(5) . . ? O2 C1 C2 119.5(5) . . ? O1 C1 C2 116.8(4) . . ? C9 C2 C3 119.5(4) . . ? C9 C2 C1 120.2(4) . . ? C3 C2 C1 120.3(4) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C6 119.3(5) . . ? C3 C4 C5 119.5(5) . . ? C6 C4 C5 121.1(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 120.1(5) . . ? C4 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C9 C7 C6 119.5(4) . . ? C9 C7 C8 120.9(4) . . ? C6 C7 C8 119.5(4) . . ? O4 C8 O3 125.1(5) . . ? O4 C8 C7 119.8(5) . . ? O3 C8 C7 115.1(4) . . ? C7 C9 C2 120.6(4) . . ? C7 C9 H9 119.7 . . ? C2 C9 H9 119.7 . . ? O6 C10 O5 122.7(4) . . ? O6 C10 C11 120.7(4) . . ? O5 C10 C11 116.7(4) . . ? C13 C11 C12 119.7(4) . . ? C13 C11 C10 121.3(4) . . ? C12 C11 C10 118.9(4) . . ? C11 C12 C11 119.4(5) 8_565 . ? C11 C12 H12 120.3 8_565 . ? C11 C12 H12 120.3 . . ? C11 C13 C14 121.9(5) . . ? C11 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C13 117.3(6) . 8_565 ? C13 C14 C15 121.3(3) . . ? C13 C14 C15 121.3(3) 8_565 . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 122.3(5) . . ? O8 C16 C17 121.3(4) . . ? O7 C16 C17 116.4(4) . . ? C21 C17 C18 119.9(5) . . ? C21 C17 C16 120.1(4) . . ? C18 C17 C16 119.9(4) . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C18 119.3(6) . 8 ? C18 C19 C20 120.3(3) . . ? C18 C19 C20 120.3(3) 8 . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C17 120.4(6) 8 . ? C17 C21 H21 119.8 8 . ? C17 C21 H21 119.8 . . ? 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 O3 Zn1 O1 C1 -173.2(5) 5_657 . . . ? O7 Zn1 O1 C1 74.3(5) . . . . ? O5 Zn1 O1 C1 -58.7(5) . . . . ? O1 Zn1 O5 C10 -171.3(3) . . . . ? O3 Zn1 O5 C10 -68.1(3) 5_657 . . . ? O7 Zn1 O5 C10 59.7(3) . . . . ? O2 Mg1 O6 C10 135.6(8) 2 . . . ? O4 Mg1 O6 C10 -46.7(8) 5_657 . . . ? O8 Mg1 O6 C10 43.5(8) 2 . . . ? O1W Mg1 O6 C10 -135.2(8) . . . . ? O2W Mg1 O6 C10 -165.3(15) . . . . ? O1 Zn1 O7 C16 -72.2(3) . . . . ? O3 Zn1 O7 C16 -174.4(3) 5_657 . . . ? O5 Zn1 O7 C16 57.0(3) . . . . ? Mg1 O2 C1 O1 -36.0(15) 2_554 . . . ? Mg1 O2 C1 C2 146.0(10) 2_554 . . . ? Zn1 O1 C1 O2 -1.2(8) . . . . ? Zn1 O1 C1 C2 176.9(3) . . . . ? O2 C1 C2 C9 173.8(5) . . . . ? O1 C1 C2 C9 -4.4(7) . . . . ? O2 C1 C2 C3 -5.0(7) . . . . ? O1 C1 C2 C3 176.9(5) . . . . ? C9 C2 C3 C4 -1.6(8) . . . . ? C1 C2 C3 C4 177.2(5) . . . . ? C2 C3 C4 C6 2.3(9) . . . . ? C2 C3 C4 C5 179.5(6) . . . . ? C3 C4 C6 C7 -2.2(9) . . . . ? C5 C4 C6 C7 -179.3(6) . . . . ? C4 C6 C7 C9 1.3(8) . . . . ? C4 C6 C7 C8 -176.5(5) . . . . ? Mg1 O4 C8 O3 5.7(14) 5_657 . . . ? Mg1 O4 C8 C7 -175.5(7) 5_657 . . . ? Zn1 O3 C8 O4 -4.5(10) 5_657 . . . ? Zn1 O3 C8 C7 176.7(4) 5_657 . . . ? C9 C7 C8 O4 178.9(5) . . . . ? C6 C7 C8 O4 -3.4(8) . . . . ? C9 C7 C8 O3 -2.2(7) . . . . ? C6 C7 C8 O3 175.5(5) . . . . ? C6 C7 C9 C2 -0.6(7) . . . . ? C8 C7 C9 C2 177.2(5) . . . . ? C3 C2 C9 C7 0.7(8) . . . . ? C1 C2 C9 C7 -178.1(4) . . . . ? Mg1 O6 C10 O5 94.0(9) . . . . ? Mg1 O6 C10 C11 -86.6(9) . . . . ? Zn1 O5 C10 O6 -5.3(5) . . . . ? Zn1 O5 C10 C11 175.2(3) . . . . ? O6 C10 C11 C13 -17.5(6) . . . . ? O5 C10 C11 C13 162.0(4) . . . . ? O6 C10 C11 C12 160.1(4) . . . . ? O5 C10 C11 C12 -20.5(6) . . . . ? C13 C11 C12 C11 2.3(8) . . . 8_565 ? C10 C11 C12 C11 -175.3(3) . . . 8_565 ? C12 C11 C13 C14 -1.2(8) . . . . ? C10 C11 C13 C14 176.4(5) . . . . ? C11 C13 C14 C13 0.0(10) . . . 8_565 ? C11 C13 C14 C15 -178.4(7) . . . . ? Mg1 O8 C16 O7 90.4(9) 2_554 . . . ? Mg1 O8 C16 C17 -90.9(8) 2_554 . . . ? Zn1 O7 C16 O8 -8.2(6) . . . . ? Zn1 O7 C16 C17 173.1(3) . . . . ? O8 C16 C17 C21 163.7(5) . . . . ? O7 C16 C17 C21 -17.5(6) . . . . ? O8 C16 C17 C18 -12.3(6) . . . . ? O7 C16 C17 C18 166.4(4) . . . . ? C21 C17 C18 C19 -0.2(8) . . . . ? C16 C17 C18 C19 175.9(5) . . . . ? C17 C18 C19 C18 -1.8(11) . . . 8 ? C17 C18 C19 C20 178.8(7) . . . . ? C18 C17 C21 C17 2.2(8) . . . 8 ? C16 C17 C21 C17 -173.9(3) . . . 8 ? # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.017 0.250 -0.283 317 53 ' ' 2 0.517 0.250 -0.218 318 53 ' ' 3 0.983 0.750 0.282 317 53 ' ' 4 0.483 0.750 0.217 317 53 ' ' 5 0.045 0.118 0.190 8 1 ' ' 6 0.045 0.382 0.190 8 1 ' ' 7 0.545 0.118 0.309 7 1 ' ' 8 0.545 0.382 0.309 7 1 ' ' 9 0.455 0.618 0.690 8 1 ' ' 10 0.455 0.882 0.690 8 1 ' ' 11 0.955 0.618 0.809 8 1 ' ' 12 0.955 0.882 0.809 8 1 ' ' _platon_squeeze_details ; ; # The results of the SQUEEZE/PLATON show that the contributions of 220 electrons are removed from the asymmetric unit contents. # This would approximate to 22 water molecules per asymmetric unit. # Considering the asymmetric (formula) unit is 1/8 of the unit cell, # it implies that the asymmetric unit also contains three additional lattice water molecules, # which has been treated as a diffuse contribution to the overall scattering without specific atom positions. # Therefore,three additional lattice water molecules should be added to the overall formulation. _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.409 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.080 data_Zn-mip _database_code_depnum_ccdc_archive 'CCDC 865283' #TrackingRef 'revised_cif[1].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 O9 Zn2' _chemical_formula_weight 505.03 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 P21/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 12.0711(4) _cell_length_b 12.2504(4) _cell_length_c 13.3746(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.194(3) _cell_angle_gamma 90.00 _cell_volume 1940.16(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3967 _exptl_absorpt_correction_T_max 0.6070 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10282 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3956 _reflns_number_gt 3348 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.9327P] 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 0.0090(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3956 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.71323(3) -0.36109(2) 0.45709(2) 0.02119(11) Uani 1 1 d . . . Zn2 Zn 0.64498(2) -0.18127(2) 0.23110(2) 0.01878(11) Uani 1 1 d . . . O1 O 0.70656(17) -0.21418(15) 0.51474(14) 0.0312(5) Uani 1 1 d . . . O2 O 0.60862(17) -0.15944(17) 0.36591(14) 0.0325(5) Uani 1 1 d . . . O3 O 0.47012(18) 0.21531(18) 0.32498(15) 0.0380(5) Uani 1 1 d . . . O4 O 0.5360(2) 0.34303(17) 0.43881(18) 0.0476(6) Uani 1 1 d . . . O5 O 0.68788(16) -0.04019(15) 0.18505(16) 0.0314(5) Uani 1 1 d . . . O6 O 0.79501(18) -0.04803(18) 0.06661(15) 0.0386(5) Uani 1 1 d . . . O7 O 1.16606(18) 0.13312(18) 0.12158(16) 0.0381(5) Uani 1 1 d . . . O8 O 1.20413(17) 0.25516(18) 0.24687(15) 0.0397(5) Uani 1 1 d . . . O1W O 0.5654(2) -0.4214(2) 0.38548(19) 0.0570(7) Uani 1 1 d . . . H1WA H 0.5685 -0.4910 0.3860 0.085 Uiso 1 1 d R . . H1WB H 0.5134 -0.4005 0.4161 0.085 Uiso 1 1 d R . . C1 C 0.6581(2) -0.1408(2) 0.45635(19) 0.0227(6) Uani 1 1 d . . . C2 C 0.6565(2) -0.0275(2) 0.49668(18) 0.0212(5) Uani 1 1 d . . . C3 C 0.7080(2) -0.0037(2) 0.59661(19) 0.0277(6) Uani 1 1 d . . . H3 H 0.7439 -0.0591 0.6382 0.033 Uiso 1 1 calc R . . C4 C 0.7069(3) 0.1015(2) 0.6356(2) 0.0328(7) Uani 1 1 d . . . C5 C 0.7642(4) 0.1273(3) 0.7440(3) 0.0670(14) Uani 1 1 d . . . H5A H 0.7727 0.0614 0.7836 0.100 Uiso 1 1 calc R . . H5B H 0.7190 0.1783 0.7730 0.100 Uiso 1 1 calc R . . H5C H 0.8372 0.1585 0.7442 0.100 Uiso 1 1 calc R . . C6 C 0.6522(3) 0.1825(2) 0.5719(2) 0.0300(6) Uani 1 1 d . . . H6 H 0.6518 0.2536 0.5962 0.036 Uiso 1 1 calc R . . C7 C 0.5980(2) 0.1598(2) 0.4725(2) 0.0240(6) Uani 1 1 d . . . C8 C 0.5317(2) 0.2469(2) 0.4086(2) 0.0299(7) Uani 1 1 d . . . C9 C 0.6000(2) 0.0546(2) 0.43524(19) 0.0227(6) Uani 1 1 d . . . H9 H 0.5636 0.0388 0.3690 0.027 Uiso 1 1 calc R . . C10 C 0.7758(2) -0.0177(2) 0.1512(2) 0.0242(6) Uani 1 1 d . . . C11 C 0.8649(2) 0.0521(2) 0.21424(19) 0.0233(6) Uani 1 1 d . . . C12 C 0.8554(2) 0.0819(3) 0.3132(2) 0.0324(7) Uani 1 1 d . . . H12 H 0.7930 0.0588 0.3389 0.039 Uiso 1 1 calc R . . C13 C 0.9370(3) 0.1452(3) 0.3735(2) 0.0401(8) Uani 1 1 d . . . C14 C 0.9270(4) 0.1780(5) 0.4808(3) 0.0859(18) Uani 1 1 d . . . H14A H 0.8563 0.2144 0.4790 0.129 Uiso 1 1 calc R . . H14C H 0.9879 0.2263 0.5085 0.129 Uiso 1 1 calc R . . H14B H 0.9307 0.1140 0.5227 0.129 Uiso 1 1 calc R . . C15 C 1.0285(2) 0.1794(3) 0.3329(2) 0.0331(7) Uani 1 1 d . . . H15 H 1.0828 0.2240 0.3717 0.040 Uiso 1 1 calc R . . C16 C 1.0410(2) 0.1485(2) 0.23542(19) 0.0223(6) Uani 1 1 d . . . C17 C 1.1448(2) 0.1819(2) 0.1977(2) 0.0236(6) Uani 1 1 d . . . C18 C 0.9593(2) 0.0839(2) 0.17667(19) 0.0221(6) Uani 1 1 d . . . H18 H 0.9677 0.0619 0.1120 0.027 Uiso 1 1 calc 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 0.02244(18) 0.01803(18) 0.02403(17) 0.00234(12) 0.00686(12) 0.00502(12) Zn2 0.01728(16) 0.01722(17) 0.02126(17) 0.00008(12) 0.00228(11) -0.00045(12) O1 0.0391(12) 0.0190(10) 0.0335(10) -0.0018(9) 0.0022(9) 0.0075(9) O2 0.0330(12) 0.0412(12) 0.0243(10) -0.0087(9) 0.0081(8) 0.0001(10) O3 0.0378(12) 0.0413(12) 0.0340(11) 0.0112(10) 0.0044(9) 0.0192(10) O4 0.0575(16) 0.0239(12) 0.0612(15) 0.0108(11) 0.0110(12) 0.0153(11) O5 0.0207(10) 0.0210(10) 0.0536(12) 0.0070(9) 0.0099(9) -0.0057(8) O6 0.0404(13) 0.0404(13) 0.0352(11) -0.0174(10) 0.0084(9) -0.0193(10) O7 0.0352(13) 0.0427(13) 0.0437(12) -0.0116(10) 0.0255(10) -0.0116(10) O8 0.0284(11) 0.0503(14) 0.0424(12) -0.0114(11) 0.0114(9) -0.0220(11) O1W 0.0488(15) 0.0407(14) 0.0786(18) 0.0009(13) 0.0050(13) -0.0068(12) C1 0.0212(14) 0.0233(14) 0.0253(13) -0.0006(11) 0.0090(10) -0.0008(11) C2 0.0220(13) 0.0186(13) 0.0243(13) 0.0024(11) 0.0077(10) 0.0017(11) C3 0.0348(16) 0.0213(14) 0.0242(13) 0.0052(11) -0.0010(11) 0.0031(12) C4 0.0391(17) 0.0240(15) 0.0317(15) -0.0022(13) -0.0017(12) 0.0043(13) C5 0.106(4) 0.036(2) 0.043(2) -0.0101(16) -0.026(2) 0.011(2) C6 0.0326(16) 0.0192(14) 0.0380(16) -0.0004(12) 0.0060(12) 0.0024(12) C7 0.0213(14) 0.0208(14) 0.0314(14) 0.0062(12) 0.0091(11) 0.0051(11) C8 0.0248(15) 0.0323(17) 0.0358(15) 0.0138(13) 0.0140(12) 0.0086(12) C9 0.0205(13) 0.0270(15) 0.0211(12) 0.0043(11) 0.0056(10) 0.0018(11) C10 0.0222(14) 0.0167(13) 0.0330(14) 0.0017(12) 0.0037(11) -0.0040(11) C11 0.0212(14) 0.0251(14) 0.0239(13) -0.0023(11) 0.0050(10) -0.0049(11) C12 0.0240(15) 0.0470(19) 0.0299(14) -0.0052(14) 0.0143(11) -0.0117(14) C13 0.0334(17) 0.062(2) 0.0275(15) -0.0136(15) 0.0133(12) -0.0126(16) C14 0.066(3) 0.156(5) 0.044(2) -0.052(3) 0.032(2) -0.050(3) C15 0.0262(15) 0.0424(18) 0.0304(15) -0.0127(14) 0.0052(12) -0.0102(14) C16 0.0199(13) 0.0234(14) 0.0238(13) 0.0007(11) 0.0051(10) -0.0025(11) C17 0.0196(13) 0.0236(14) 0.0269(13) 0.0063(12) 0.0028(10) -0.0005(11) C18 0.0237(13) 0.0251(14) 0.0189(12) -0.0017(11) 0.0074(10) -0.0033(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.9489(19) 4_556 ? Zn1 O7 1.957(2) 2_745 ? Zn1 O1 1.9656(19) . ? Zn1 O1W 1.996(2) . ? Zn2 O3 1.9218(19) 2_645 ? Zn2 O5 1.9387(19) . ? Zn2 O8 1.9500(19) 2_745 ? Zn2 O2 1.9550(19) . ? O1 C1 1.258(3) . ? O2 C1 1.262(3) . ? O3 C8 1.276(3) . ? O3 Zn2 1.9218(19) 2_655 ? O4 C8 1.243(4) . ? O5 C10 1.263(3) . ? O6 C10 1.254(3) . ? O6 Zn1 1.9489(19) 4 ? O7 C17 1.249(3) . ? O7 Zn1 1.957(2) 2_755 ? O8 C17 1.252(3) . ? O8 Zn2 1.9500(19) 2_755 ? O1W H1WA 0.8537 . ? O1W H1WB 0.8531 . ? C1 C2 1.490(4) . ? C2 C9 1.391(4) . ? C2 C3 1.391(3) . ? C3 C4 1.391(4) . ? C3 H3 0.9300 . ? C4 C6 1.389(4) . ? C4 C5 1.514(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.391(4) . ? C6 H6 0.9300 . ? C7 C9 1.384(4) . ? C7 C8 1.498(4) . ? C9 H9 0.9300 . ? C10 C11 1.499(3) . ? C11 C18 1.388(4) . ? C11 C12 1.399(4) . ? C12 C13 1.383(4) . ? C12 H12 0.9300 . ? C13 C15 1.387(4) . ? C13 C14 1.518(4) . ? C14 H14A 0.9600 . ? C14 H14C 0.9600 . ? C14 H14B 0.9600 . ? C15 C16 1.394(4) . ? C15 H15 0.9300 . ? C16 C18 1.383(4) . ? C16 C17 1.496(4) . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O7 93.56(9) 4_556 2_745 ? O6 Zn1 O1 106.35(8) 4_556 . ? O7 Zn1 O1 109.61(9) 2_745 . ? O6 Zn1 O1W 115.11(10) 4_556 . ? O7 Zn1 O1W 114.71(11) 2_745 . ? O1 Zn1 O1W 115.24(10) . . ? O3 Zn2 O5 132.93(9) 2_645 . ? O3 Zn2 O8 112.27(10) 2_645 2_745 ? O5 Zn2 O8 96.01(9) . 2_745 ? O3 Zn2 O2 100.11(9) 2_645 . ? O5 Zn2 O2 107.01(9) . . ? O8 Zn2 O2 106.60(8) 2_745 . ? C1 O1 Zn1 117.41(17) . . ? C1 O2 Zn2 139.45(19) . . ? C8 O3 Zn2 113.34(19) . 2_655 ? C10 O5 Zn2 127.12(18) . . ? C10 O6 Zn1 133.80(19) . 4 ? C17 O7 Zn1 135.45(19) . 2_755 ? C17 O8 Zn2 142.0(2) . 2_755 ? Zn1 O1W H1WA 109.4 . . ? Zn1 O1W H1WB 109.4 . . ? H1WA O1W H1WB 109.3 . . ? O1 C1 O2 122.8(2) . . ? O1 C1 C2 118.5(2) . . ? O2 C1 C2 118.6(2) . . ? C9 C2 C3 119.5(2) . . ? C9 C2 C1 119.9(2) . . ? C3 C2 C1 120.6(2) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C6 C4 C3 118.0(2) . . ? C6 C4 C5 120.9(3) . . ? C3 C4 C5 121.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 121.5(3) . . ? C4 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C9 C7 C6 119.5(2) . . ? C9 C7 C8 120.2(2) . . ? C6 C7 C8 120.2(2) . . ? O4 C8 O3 123.5(3) . . ? O4 C8 C7 120.3(3) . . ? O3 C8 C7 116.1(3) . . ? C7 C9 C2 120.1(2) . . ? C7 C9 H9 119.9 . . ? C2 C9 H9 119.9 . . ? O6 C10 O5 125.0(2) . . ? O6 C10 C11 116.1(2) . . ? O5 C10 C11 118.9(2) . . ? C18 C11 C12 119.6(2) . . ? C18 C11 C10 120.4(2) . . ? C12 C11 C10 120.0(2) . . ? C13 C12 C11 121.2(3) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C15 118.2(3) . . ? C12 C13 C14 121.4(3) . . ? C15 C13 C14 120.3(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C13 C15 C16 121.5(3) . . ? C13 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C18 C16 C15 119.5(3) . . ? C18 C16 C17 121.1(2) . . ? C15 C16 C17 119.4(2) . . ? O7 C17 O8 125.8(3) . . ? O7 C17 C16 117.5(2) . . ? O8 C17 C16 116.7(3) . . ? C16 C18 C11 120.0(2) . . ? C16 C18 H18 120.0 . . ? C11 C18 H18 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O1 C1 179.1(2) 4_556 . . . ? O7 Zn1 O1 C1 79.2(2) 2_745 . . . ? O1W Zn1 O1 C1 -52.0(2) . . . . ? O3 Zn2 O2 C1 146.2(3) 2_645 . . . ? O5 Zn2 O2 C1 -72.7(3) . . . . ? O8 Zn2 O2 C1 29.2(3) 2_745 . . . ? O3 Zn2 O5 C10 -108.7(2) 2_645 . . . ? O8 Zn2 O5 C10 19.5(2) 2_745 . . . ? O2 Zn2 O5 C10 128.9(2) . . . . ? Zn1 O1 C1 O2 4.5(4) . . . . ? Zn1 O1 C1 C2 -177.16(18) . . . . ? Zn2 O2 C1 O1 -79.7(4) . . . . ? Zn2 O2 C1 C2 102.0(3) . . . . ? O1 C1 C2 C9 -177.6(3) . . . . ? O2 C1 C2 C9 0.8(4) . . . . ? O1 C1 C2 C3 0.3(4) . . . . ? O2 C1 C2 C3 178.7(3) . . . . ? C9 C2 C3 C4 -1.8(4) . . . . ? C1 C2 C3 C4 -179.7(3) . . . . ? C2 C3 C4 C6 0.3(5) . . . . ? C2 C3 C4 C5 -179.3(3) . . . . ? C3 C4 C6 C7 1.2(5) . . . . ? C5 C4 C6 C7 -179.2(3) . . . . ? C4 C6 C7 C9 -1.2(5) . . . . ? C4 C6 C7 C8 175.0(3) . . . . ? Zn2 O3 C8 O4 -16.2(4) 2_655 . . . ? Zn2 O3 C8 C7 161.85(19) 2_655 . . . ? C9 C7 C8 O4 -174.9(3) . . . . ? C6 C7 C8 O4 9.0(4) . . . . ? C9 C7 C8 O3 7.0(4) . . . . ? C6 C7 C8 O3 -169.2(3) . . . . ? C6 C7 C9 C2 -0.3(4) . . . . ? C8 C7 C9 C2 -176.5(2) . . . . ? C3 C2 C9 C7 1.8(4) . . . . ? C1 C2 C9 C7 179.7(2) . . . . ? Zn1 O6 C10 O5 -2.3(5) 4 . . . ? Zn1 O6 C10 C11 178.8(2) 4 . . . ? Zn2 O5 C10 O6 70.6(3) . . . . ? Zn2 O5 C10 C11 -110.5(3) . . . . ? O6 C10 C11 C18 2.9(4) . . . . ? O5 C10 C11 C18 -176.1(2) . . . . ? O6 C10 C11 C12 -174.5(3) . . . . ? O5 C10 C11 C12 6.6(4) . . . . ? C18 C11 C12 C13 1.8(5) . . . . ? C10 C11 C12 C13 179.2(3) . . . . ? C11 C12 C13 C15 0.6(5) . . . . ? C11 C12 C13 C14 179.8(4) . . . . ? C12 C13 C15 C16 -2.2(5) . . . . ? C14 C13 C15 C16 178.6(4) . . . . ? C13 C15 C16 C18 1.3(5) . . . . ? C13 C15 C16 C17 -176.3(3) . . . . ? Zn1 O7 C17 O8 0.1(5) 2_755 . . . ? Zn1 O7 C17 C16 -178.33(19) 2_755 . . . ? Zn2 O8 C17 O7 -16.5(5) 2_755 . . . ? Zn2 O8 C17 C16 161.9(2) 2_755 . . . ? C18 C16 C17 O7 -13.7(4) . . . . ? C15 C16 C17 O7 163.8(3) . . . . ? C18 C16 C17 O8 167.8(3) . . . . ? C15 C16 C17 O8 -14.7(4) . . . . ? C15 C16 C18 C11 1.1(4) . . . . ? C17 C16 C18 C11 178.7(2) . . . . ? C12 C11 C18 C16 -2.7(4) . . . . ? C10 C11 C18 C16 180.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.534 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.078 #===END data_Zn-tbip _database_code_depnum_ccdc_archive 'CCDC 884314' #TrackingRef 'revised_cif[1].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 O10 Zn3' _chemical_formula_weight 670.56 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0667(3) _cell_length_b 12.2547(8) _cell_length_c 12.5910(6) _cell_angle_alpha 95.846(5) _cell_angle_beta 93.184(4) _cell_angle_gamma 95.283(4) _cell_volume 1230.30(11) _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 sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 2.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3697 _exptl_absorpt_correction_T_max 0.6180 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11667 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.67 _reflns_number_total 4568 _reflns_number_gt 4060 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The restraints, such as ISOR C19 C20 C21, ISOR C30 C31 C29, EADP C19 C20 C21, EADP C30 C31 C29, EADP H5 H4, and FREE Zn1 H5, are performed in order to facilitate the refinement of pseudosymmetric structure of Zn-tbip. ; _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^)+(0.0451P)^2^+5.0052P] 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 4568 _refine_ls_number_parameters 335 _refine_ls_number_restraints 240 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.068 _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 0.56898(6) 0.29877(4) 1.10125(4) 0.01275(14) Uani 1 1 d U . . Zn2 Zn 1.04764(6) 0.60362(4) 0.78420(4) 0.01300(14) Uani 1 1 d U . . Zn3 Zn 0.80522(6) 0.50855(4) 0.96119(4) 0.01387(14) Uani 1 1 d U . . O1 O 0.6393(4) 0.7807(3) 0.9625(3) 0.0239(8) Uani 1 1 d U . . O2 O 0.8153(5) 0.6657(3) 1.0226(3) 0.0281(8) Uani 1 1 d U . . O3 O 0.7144(4) 1.1769(3) 1.0950(3) 0.0251(8) Uani 1 1 d U . . O4 O 0.9659(4) 1.2436(3) 1.1697(3) 0.0316(9) Uani 1 1 d U . . O5 O 0.6790(4) 0.4808(3) 0.8133(3) 0.0250(8) Uani 1 1 d U . . O6 O 0.8499(4) 0.5443(3) 0.6946(3) 0.0223(7) Uani 1 1 d U . . O7 O 0.5352(4) 0.3209(3) 0.2532(3) 0.0259(8) Uani 1 1 d U . . O8 O 0.7834(4) 0.4031(3) 0.3194(3) 0.0274(8) Uani 1 1 d U . . O9 O 0.6274(5) 0.4153(3) 1.0149(3) 0.0243(8) Uani 1 1 d U . . O10 O 1.0342(4) 0.5030(3) 0.8964(3) 0.0149(7) Uani 1 1 d U . . C1 C 0.7682(5) 0.7600(4) 1.0150(4) 0.0157(9) Uani 1 1 d U . . C2 C 0.8729(5) 0.8580(4) 1.0742(4) 0.0155(9) Uani 1 1 d U . . C3 C 0.8156(5) 0.9614(4) 1.0776(4) 0.0165(9) Uani 1 1 d U . . H3 H 0.7120 0.9702 1.0450 0.020 Uiso 1 1 calc R . . C4 C 0.9148(5) 1.0520(4) 1.1301(4) 0.0149(9) Uani 1 1 d U . . C5 C 0.8593(5) 1.1657(4) 1.1323(4) 0.0144(9) Uani 1 1 d U . . C6 C 1.0699(5) 1.0381(4) 1.1793(4) 0.0164(9) Uani 1 1 d U . . H6 H 1.1344 1.0992 1.2147 0.020 Uiso 1 1 calc R . . C7 C 1.1304(5) 0.9352(4) 1.1769(4) 0.0146(9) Uani 1 1 d U . . C8 C 1.0296(5) 0.8458(4) 1.1232(4) 0.0161(9) Uani 1 1 d U . . H8 H 1.0672 0.7761 1.1198 0.019 Uiso 1 1 calc R . . C9 C 1.3029(6) 0.9231(4) 1.2309(4) 0.0185(10) Uani 1 1 d U . . C10 C 1.4259(8) 1.0194(7) 1.2152(9) 0.081(3) Uani 1 1 d U . . H10A H 1.4203 1.0322 1.1412 0.122 Uiso 1 1 calc R . . H10B H 1.5366 1.0033 1.2361 0.122 Uiso 1 1 calc R . . H10C H 1.3994 1.0839 1.2582 0.122 Uiso 1 1 calc R . . C11 C 1.2900(8) 0.9209(9) 1.3492(5) 0.076(3) Uani 1 1 d U . . H11A H 1.2407 0.9850 1.3779 0.114 Uiso 1 1 calc R . . H11B H 1.3993 0.9203 1.3833 0.114 Uiso 1 1 calc R . . H11C H 1.2216 0.8558 1.3621 0.114 Uiso 1 1 calc R . . C12 C 1.3719(9) 0.8201(7) 1.1839(7) 0.078(3) Uani 1 1 d U . . H12A H 1.3129 0.7569 1.2086 0.117 Uiso 1 1 calc R . . H12B H 1.4882 0.8230 1.2059 0.117 Uiso 1 1 calc R . . H12C H 1.3587 0.8149 1.1073 0.117 Uiso 1 1 calc R . . C13 C 0.7218(5) 0.4884(4) 0.7193(4) 0.0160(9) Uani 1 1 d U . . C14 C 0.6166(5) 0.4240(4) 0.6276(4) 0.0153(9) Uani 1 1 d U . . C15 C 0.6760(5) 0.4196(4) 0.5252(4) 0.0165(9) Uani 1 1 d U . . H15 H 0.7800 0.4546 0.5145 0.020 Uiso 1 1 calc R . . C16 C 0.5781(5) 0.3623(4) 0.4398(3) 0.0145(9) Uani 1 1 d U . . C17 C 0.6370(5) 0.3618(4) 0.3288(4) 0.0158(9) Uani 1 1 d U . . C18 C 0.4214(6) 0.3103(4) 0.4562(4) 0.0176(9) Uani 1 1 d U . . H18 H 0.3565 0.2731 0.3980 0.021 Uiso 1 1 calc R . . C19 C 0.3600(6) 0.3129(4) 0.5577(4) 0.0187(6) Uani 1 1 d U . . C20 C 0.4606(5) 0.3702(4) 0.6428(4) 0.0187(6) Uani 1 1 d U . . H20 H 0.4230 0.3728 0.7114 0.022 Uiso 1 1 calc R . . C21 C 0.1883(6) 0.2547(4) 0.5754(4) 0.0187(6) Uani 1 1 d U . . C22 C 0.1032(8) 0.3220(6) 0.6618(6) 0.0491(18) Uani 1 1 d U . . H22A H 0.1629 0.3213 0.7298 0.074 Uiso 1 1 calc R . . H22B H -0.0095 0.2903 0.6651 0.074 Uiso 1 1 calc R . . H22C H 0.1028 0.3965 0.6448 0.074 Uiso 1 1 calc R . . C23 C 0.2103(8) 0.1407(5) 0.6110(6) 0.0465(17) Uani 1 1 d U . . H23A H 0.2627 0.0977 0.5567 0.070 Uiso 1 1 calc R . . H23B H 0.1031 0.1041 0.6218 0.070 Uiso 1 1 calc R . . H23C H 0.2790 0.1487 0.6766 0.070 Uiso 1 1 calc R . . C24 C 0.0717(7) 0.2408(7) 0.4740(5) 0.051(2) Uani 1 1 d U . . H24A H 0.0720 0.3100 0.4442 0.076 Uiso 1 1 calc R . . H24B H -0.0394 0.2172 0.4912 0.076 Uiso 1 1 calc R . . H24C H 0.1094 0.1866 0.4227 0.076 Uiso 1 1 calc R . . H4 H 1.034(7) 0.452(5) 0.875(4) 0.014(12) Uiso 1 1 d . . . H5 H 0.561(7) 0.411(5) 0.982(5) 0.014(12) 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 Zn1 0.0135(2) 0.0121(3) 0.0126(3) 0.0019(2) -0.00091(19) 0.00115(19) Zn2 0.0147(3) 0.0110(3) 0.0130(3) 0.0015(2) 0.0017(2) -0.00081(19) Zn3 0.0150(3) 0.0124(3) 0.0144(3) 0.0024(2) 0.0010(2) 0.00088(19) O1 0.0192(16) 0.0167(17) 0.033(2) 0.0015(15) -0.0129(15) -0.0017(14) O2 0.038(2) 0.0096(16) 0.034(2) -0.0020(15) -0.0122(17) 0.0032(15) O3 0.0240(17) 0.0152(17) 0.036(2) 0.0009(15) -0.0052(15) 0.0098(14) O4 0.0250(18) 0.0125(17) 0.055(3) -0.0049(17) -0.0041(17) 0.0021(14) O5 0.0201(16) 0.041(2) 0.0123(16) 0.0007(15) 0.0004(13) -0.0056(15) O6 0.0204(16) 0.0268(19) 0.0177(17) 0.0051(14) -0.0020(14) -0.0089(14) O7 0.0224(17) 0.041(2) 0.0127(16) -0.0002(15) 0.0028(14) -0.0026(16) O8 0.0233(18) 0.035(2) 0.0223(18) -0.0017(16) 0.0097(15) -0.0053(16) O9 0.0183(18) 0.029(2) 0.028(2) 0.0201(16) -0.0030(16) -0.0039(16) O10 0.0209(16) 0.0113(16) 0.0127(16) 0.0016(13) -0.0006(13) 0.0036(14) C1 0.016(2) 0.012(2) 0.018(2) 0.0017(18) 0.0029(18) -0.0024(17) C2 0.016(2) 0.011(2) 0.019(2) 0.0010(18) -0.0009(18) 0.0010(17) C3 0.0111(19) 0.017(2) 0.021(2) -0.0001(19) -0.0011(17) 0.0000(17) C4 0.016(2) 0.010(2) 0.020(2) 0.0028(18) 0.0022(18) 0.0050(17) C5 0.016(2) 0.011(2) 0.018(2) 0.0025(18) 0.0023(18) 0.0056(17) C6 0.017(2) 0.012(2) 0.020(2) -0.0006(18) -0.0010(18) 0.0015(17) C7 0.014(2) 0.015(2) 0.016(2) 0.0034(18) -0.0007(17) 0.0037(17) C8 0.017(2) 0.010(2) 0.022(2) 0.0018(18) -0.0005(18) 0.0054(17) C9 0.016(2) 0.018(2) 0.022(2) 0.0035(19) -0.0033(19) 0.0065(18) C10 0.020(3) 0.074(6) 0.155(9) 0.071(6) -0.023(4) -0.011(3) C11 0.026(3) 0.176(10) 0.027(3) 0.016(5) -0.002(3) 0.014(5) C12 0.053(4) 0.075(6) 0.096(6) -0.044(5) -0.052(5) 0.046(4) C13 0.016(2) 0.016(2) 0.017(2) 0.0040(18) -0.0011(18) 0.0037(18) C14 0.015(2) 0.017(2) 0.014(2) 0.0057(18) 0.0006(17) -0.0006(18) C15 0.014(2) 0.019(2) 0.018(2) 0.0052(19) 0.0004(18) 0.0004(18) C16 0.014(2) 0.018(2) 0.013(2) 0.0034(18) 0.0038(17) 0.0015(17) C17 0.017(2) 0.017(2) 0.014(2) 0.0017(18) 0.0060(18) 0.0031(18) C18 0.018(2) 0.021(2) 0.013(2) -0.0013(18) -0.0001(18) -0.0019(18) C19 0.0153(13) 0.0223(14) 0.0178(13) 0.0024(11) 0.0021(11) -0.0031(11) C20 0.0153(13) 0.0223(14) 0.0178(13) 0.0024(11) 0.0021(11) -0.0031(11) C21 0.0153(13) 0.0223(14) 0.0178(13) 0.0024(11) 0.0021(11) -0.0031(11) C22 0.036(3) 0.048(4) 0.059(4) -0.011(3) 0.027(3) -0.012(3) C23 0.030(3) 0.035(3) 0.077(5) 0.022(3) 0.002(3) -0.005(3) C24 0.023(3) 0.092(6) 0.037(3) 0.027(4) -0.005(3) -0.019(3) _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 1.921(4) . ? Zn1 O7 1.942(3) 1_556 ? Zn1 O1 1.951(3) 2_667 ? Zn1 O3 1.980(3) 1_545 ? Zn1 H5 2.14(6) . ? Zn2 O4 1.918(3) 2_777 ? Zn2 O8 1.940(3) 2_766 ? Zn2 O6 1.940(3) . ? Zn2 O10 1.968(3) . ? Zn3 O9 1.946(4) . ? Zn3 O2 1.993(3) . ? Zn3 O5 2.054(3) . ? Zn3 O10 2.064(3) . ? Zn3 O10 2.177(3) 2_767 ? O1 C1 1.260(6) . ? O1 Zn1 1.951(3) 2_667 ? O2 C1 1.260(6) . ? O3 C5 1.260(5) . ? O3 Zn1 1.980(3) 1_565 ? O4 C5 1.260(5) . ? O4 Zn2 1.918(3) 2_777 ? O5 C13 1.261(6) . ? O6 C13 1.258(6) . ? O7 C17 1.253(5) . ? O7 Zn1 1.942(3) 1_554 ? O8 C17 1.258(6) . ? O8 Zn2 1.940(3) 2_766 ? O9 H5 0.65(5) . ? O10 Zn3 2.177(3) 2_767 ? O10 H4 0.66(6) . ? C1 C2 1.508(6) . ? C2 C3 1.386(6) . ? C2 C8 1.402(6) . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C6 1.397(6) . ? C4 C5 1.500(6) . ? C6 C7 1.391(6) . ? C6 H6 0.9300 . ? C7 C8 1.394(6) . ? C7 C9 1.541(6) . ? C8 H8 0.9300 . ? C9 C11 1.503(8) . ? C9 C12 1.506(8) . ? C9 C10 1.506(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.502(6) . ? C14 C15 1.398(6) . ? C14 C20 1.398(6) . ? C15 C16 1.386(6) . ? C15 H15 0.9300 . ? C16 C18 1.397(6) . ? C16 C17 1.502(6) . ? C18 C19 1.394(6) . ? C18 H18 0.9300 . ? C19 C20 1.396(6) . ? C19 C21 1.537(6) . ? C20 H20 0.9300 . ? C21 C22 1.529(7) . ? C21 C24 1.529(7) . ? C21 C23 1.533(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 O7 124.42(17) . 1_556 ? O9 Zn1 O1 107.36(15) . 2_667 ? O7 Zn1 O1 104.48(15) 1_556 2_667 ? O9 Zn1 O3 115.96(16) . 1_545 ? O7 Zn1 O3 101.61(16) 1_556 1_545 ? O1 Zn1 O3 99.90(14) 2_667 1_545 ? O9 Zn1 H5 17.5(14) . . ? O7 Zn1 H5 130.4(15) 1_556 . ? O1 Zn1 H5 90.0(15) 2_667 . ? O3 Zn1 H5 122.6(15) 1_545 . ? O4 Zn2 O8 107.08(17) 2_777 2_766 ? O4 Zn2 O6 109.97(15) 2_777 . ? O8 Zn2 O6 100.72(14) 2_766 . ? O4 Zn2 O10 116.01(16) 2_777 . ? O8 Zn2 O10 121.65(16) 2_766 . ? O6 Zn2 O10 99.50(14) . . ? O9 Zn3 O2 113.01(17) . . ? O9 Zn3 O5 88.08(15) . . ? O2 Zn3 O5 112.26(15) . . ? O9 Zn3 O10 141.97(15) . . ? O2 Zn3 O10 101.90(15) . . ? O5 Zn3 O10 92.47(13) . . ? O9 Zn3 O10 90.72(15) . 2_767 ? O2 Zn3 O10 82.24(14) . 2_767 ? O5 Zn3 O10 164.66(14) . 2_767 ? O10 Zn3 O10 79.13(14) . 2_767 ? C1 O1 Zn1 137.8(3) . 2_667 ? C1 O2 Zn3 147.7(3) . . ? C5 O3 Zn1 134.9(3) . 1_565 ? C5 O4 Zn2 133.3(3) . 2_777 ? C13 O5 Zn3 133.6(3) . . ? C13 O6 Zn2 128.9(3) . . ? C17 O7 Zn1 128.9(3) . 1_554 ? C17 O8 Zn2 138.5(3) . 2_766 ? Zn1 O9 Zn3 147.0(2) . . ? Zn1 O9 H5 101(5) . . ? Zn3 O9 H5 109(5) . . ? Zn2 O10 Zn3 108.70(15) . . ? Zn2 O10 Zn3 131.98(17) . 2_767 ? Zn3 O10 Zn3 100.87(13) . 2_767 ? Zn2 O10 H4 110(5) . . ? Zn3 O10 H4 105(5) . . ? Zn3 O10 H4 98(5) 2_767 . ? O1 C1 O2 126.0(4) . . ? O1 C1 C2 116.1(4) . . ? O2 C1 C2 118.0(4) . . ? C3 C2 C8 119.9(4) . . ? C3 C2 C1 119.5(4) . . ? C8 C2 C1 120.5(4) . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C6 120.1(4) . . ? C3 C4 C5 120.7(4) . . ? C6 C4 C5 119.2(4) . . ? O4 C5 O3 125.0(4) . . ? O4 C5 C4 116.0(4) . . ? O3 C5 C4 118.9(4) . . ? C7 C6 C4 121.8(4) . . ? C7 C6 H6 119.1 . . ? C4 C6 H6 119.1 . . ? C6 C7 C8 117.2(4) . . ? C6 C7 C9 120.4(4) . . ? C8 C7 C9 122.4(4) . . ? C7 C8 C2 121.8(4) . . ? C7 C8 H8 119.1 . . ? C2 C8 H8 119.1 . . ? C11 C9 C12 110.0(6) . . ? C11 C9 C10 107.5(7) . . ? C12 C9 C10 107.4(7) . . ? C11 C9 C7 109.9(4) . . ? C12 C9 C7 111.0(4) . . ? C10 C9 C7 110.9(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 O5 125.3(4) . . ? O6 C13 C14 115.8(4) . . ? O5 C13 C14 118.9(4) . . ? C15 C14 C20 119.8(4) . . ? C15 C14 C13 118.9(4) . . ? C20 C14 C13 121.2(4) . . ? C16 C15 C14 119.2(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C18 120.2(4) . . ? C15 C16 C17 119.6(4) . . ? C18 C16 C17 120.1(4) . . ? O7 C17 O8 125.6(4) . . ? O7 C17 C16 117.0(4) . . ? O8 C17 C16 117.4(4) . . ? C19 C18 C16 121.7(4) . . ? C19 C18 H18 119.2 . . ? C16 C18 H18 119.2 . . ? C18 C19 C20 117.4(4) . . ? C18 C19 C21 121.5(4) . . ? C20 C19 C21 121.1(4) . . ? C19 C20 C14 121.7(4) . . ? C19 C20 H20 119.2 . . ? C14 C20 H20 119.2 . . ? C22 C21 C24 107.1(5) . . ? C22 C21 C23 109.1(5) . . ? C24 C21 C23 108.9(5) . . ? C22 C21 C19 110.4(4) . . ? C24 C21 C19 112.0(4) . . ? C23 C21 C19 109.3(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 O9 Zn3 O2 C1 -90.1(7) . . . . ? O5 Zn3 O2 C1 7.7(7) . . . . ? O10 Zn3 O2 C1 105.4(7) . . . . ? O10 Zn3 O2 C1 -177.5(7) 2_767 . . . ? O9 Zn3 O5 C13 -159.4(5) . . . . ? O2 Zn3 O5 C13 86.5(5) . . . . ? O10 Zn3 O5 C13 -17.4(5) . . . . ? O10 Zn3 O5 C13 -73.6(7) 2_767 . . . ? O4 Zn2 O6 C13 -99.3(4) 2_777 . . . ? O8 Zn2 O6 C13 148.0(4) 2_766 . . . ? O10 Zn2 O6 C13 23.0(4) . . . . ? O7 Zn1 O9 Zn3 88.6(4) 1_556 . . . ? O1 Zn1 O9 Zn3 -149.3(4) 2_667 . . . ? O3 Zn1 O9 Zn3 -38.7(5) 1_545 . . . ? O2 Zn3 O9 Zn1 -110.9(4) . . . . ? O5 Zn3 O9 Zn1 135.7(4) . . . . ? O10 Zn3 O9 Zn1 44.1(5) . . . . ? O10 Zn3 O9 Zn1 -29.0(4) 2_767 . . . ? O4 Zn2 O10 Zn3 62.0(2) 2_777 . . . ? O8 Zn2 O10 Zn3 -164.80(14) 2_766 . . . ? O6 Zn2 O10 Zn3 -55.86(18) . . . . ? O4 Zn2 O10 Zn3 -62.9(3) 2_777 . . 2_767 ? O8 Zn2 O10 Zn3 70.3(3) 2_766 . . 2_767 ? O6 Zn2 O10 Zn3 179.2(2) . . . 2_767 ? O9 Zn3 O10 Zn2 141.4(2) . . . . ? O2 Zn3 O10 Zn2 -62.06(18) . . . . ? O5 Zn3 O10 Zn2 51.30(18) . . . . ? O10 Zn3 O10 Zn2 -141.6(2) 2_767 . . . ? O9 Zn3 O10 Zn3 -77.0(3) . . . 2_767 ? O2 Zn3 O10 Zn3 79.58(16) . . . 2_767 ? O5 Zn3 O10 Zn3 -167.06(15) . . . 2_767 ? O10 Zn3 O10 Zn3 0.0 2_767 . . 2_767 ? Zn1 O1 C1 O2 17.1(8) 2_667 . . . ? Zn1 O1 C1 C2 -162.3(4) 2_667 . . . ? Zn3 O2 C1 O1 21.2(10) . . . . ? Zn3 O2 C1 C2 -159.4(5) . . . . ? O1 C1 C2 C3 6.6(6) . . . . ? O2 C1 C2 C3 -172.9(4) . . . . ? O1 C1 C2 C8 -171.6(4) . . . . ? O2 C1 C2 C8 9.0(7) . . . . ? C8 C2 C3 C4 -0.2(7) . . . . ? C1 C2 C3 C4 -178.4(4) . . . . ? C2 C3 C4 C6 -0.4(7) . . . . ? C2 C3 C4 C5 178.0(4) . . . . ? Zn2 O4 C5 O3 15.7(8) 2_777 . . . ? Zn2 O4 C5 C4 -166.2(4) 2_777 . . . ? Zn1 O3 C5 O4 -15.1(8) 1_565 . . . ? Zn1 O3 C5 C4 166.9(3) 1_565 . . . ? C3 C4 C5 O4 -171.3(4) . . . . ? C6 C4 C5 O4 7.1(6) . . . . ? C3 C4 C5 O3 6.9(7) . . . . ? C6 C4 C5 O3 -174.7(4) . . . . ? C3 C4 C6 C7 0.6(7) . . . . ? C5 C4 C6 C7 -177.9(4) . . . . ? C4 C6 C7 C8 -0.1(7) . . . . ? C4 C6 C7 C9 179.2(4) . . . . ? C6 C7 C8 C2 -0.5(7) . . . . ? C9 C7 C8 C2 -179.8(4) . . . . ? C3 C2 C8 C7 0.7(7) . . . . ? C1 C2 C8 C7 178.8(4) . . . . ? C6 C7 C9 C11 80.5(7) . . . . ? C8 C7 C9 C11 -100.2(7) . . . . ? C6 C7 C9 C12 -157.6(6) . . . . ? C8 C7 C9 C12 21.7(8) . . . . ? C6 C7 C9 C10 -38.2(7) . . . . ? C8 C7 C9 C10 141.1(6) . . . . ? Zn2 O6 C13 O5 17.5(7) . . . . ? Zn2 O6 C13 C14 -160.7(3) . . . . ? Zn3 O5 C13 O6 -20.4(8) . . . . ? Zn3 O5 C13 C14 157.8(3) . . . . ? O6 C13 C14 C15 7.4(6) . . . . ? O5 C13 C14 C15 -170.9(4) . . . . ? O6 C13 C14 C20 -171.6(4) . . . . ? O5 C13 C14 C20 10.0(7) . . . . ? C20 C14 C15 C16 0.5(7) . . . . ? C13 C14 C15 C16 -178.6(4) . . . . ? C14 C15 C16 C18 0.4(7) . . . . ? C14 C15 C16 C17 177.0(4) . . . . ? Zn1 O7 C17 O8 4.2(7) 1_554 . . . ? Zn1 O7 C17 C16 -176.4(3) 1_554 . . . ? Zn2 O8 C17 O7 -21.4(8) 2_766 . . . ? Zn2 O8 C17 C16 159.2(4) 2_766 . . . ? C15 C16 C17 O7 -171.1(4) . . . . ? C18 C16 C17 O7 5.4(7) . . . . ? C15 C16 C17 O8 8.3(7) . . . . ? C18 C16 C17 O8 -175.2(4) . . . . ? C15 C16 C18 C19 -0.9(7) . . . . ? C17 C16 C18 C19 -177.4(4) . . . . ? C16 C18 C19 C20 0.5(7) . . . . ? C16 C18 C19 C21 -179.4(4) . . . . ? C18 C19 C20 C14 0.5(7) . . . . ? C21 C19 C20 C14 -179.6(4) . . . . ? C15 C14 C20 C19 -0.9(7) . . . . ? C13 C14 C20 C19 178.1(4) . . . . ? C18 C19 C21 C22 -143.8(5) . . . . ? C20 C19 C21 C22 36.3(7) . . . . ? C18 C19 C21 C24 -24.5(7) . . . . ? C20 C19 C21 C24 155.6(5) . . . . ? C18 C19 C21 C23 96.2(6) . . . . ? C20 C19 C21 C23 -83.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.157 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.133 #===END data_ZnBa-tbip _database_code_depnum_ccdc_archive 'CCDC 884317' #TrackingRef 'revised_cif[1].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 Ba O14 Zn2' _chemical_formula_weight 888.71 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' Ba Ba -0.3244 2.2819 '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 Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 18.1400(10) _cell_length_b 31.2496(19) _cell_length_c 6.8627(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.350(6) _cell_angle_gamma 90.00 _cell_volume 3732.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4354 _exptl_absorpt_correction_T_max 0.6232 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11966 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6783 _reflns_number_gt 6385 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The restraints, such as ISOR 0.1 0.2 C32 C33 C31, ISOR 0.1 0.2 C20 C18 C19, ISOR 0.1 0.2 C9 C8 C7, EADP C32 C33 C31, EADP C20 C18 C19, EADP C9 C8 C7, FREE Ba1 O1, and FREE H8B H7A, are performed in order to facilitate the refinement of pseudosymmetric structure of ZnBa-tbip. ; _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^)+(0.0354P)^2^+2.7895P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(13) _refine_ls_number_reflns 6783 _refine_ls_number_parameters 405 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.038 _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 0.687041(17) 0.704224(9) 1.18308(3) 0.02442(8) Uani 1 1 d . . . Zn1 Zn 0.74191(3) 0.630829(19) 0.82235(9) 0.02515(14) Uani 1 1 d . . . Zn2 Zn 0.81381(3) 0.733936(19) 0.82009(8) 0.02280(13) Uani 1 1 d . . . O1 O 0.7026(2) 0.61448(11) 1.1915(7) 0.0349(10) Uani 1 1 d . . . O2 O 0.7520(2) 0.57810(13) 0.9808(6) 0.0393(10) Uani 1 1 d . . . O3 O 0.7859(3) 0.61119(17) 0.6032(7) 0.0582(13) Uani 1 1 d . . . H3B H 0.8101 0.5872 0.6363 0.087 Uiso 1 1 d R . . H3A H 0.7497 0.6074 0.4913 0.087 Uiso 1 1 d R . . O4 O 0.79513(19) 0.68099(11) 0.9577(5) 0.0241(8) Uani 1 1 d . . . O5 O 0.7268(2) 0.75640(13) 0.6015(6) 0.0316(9) Uani 1 1 d . . . O6 O 0.6589(2) 0.74140(14) 0.8166(6) 0.0369(10) Uani 1 1 d . . . O7 O 0.3326(2) 0.81736(14) 0.4199(7) 0.0375(10) Uani 1 1 d . . . O8 O 0.3953(2) 0.77789(13) 0.6867(6) 0.0345(9) Uani 1 1 d . . . O9 O 0.5308(3) 0.7231(3) 1.0122(9) 0.097(2) Uani 1 1 d . . . H9D H 0.5023 0.7004 1.0143 0.145 Uiso 1 1 d R . . H9E H 0.5159 0.7438 1.0805 0.145 Uiso 1 1 d R . . O10 O 0.6284(2) 0.67137(14) 0.4693(6) 0.0377(10) Uani 1 1 d . . . O11 O 0.6321(2) 0.64244(14) 0.7674(6) 0.0398(10) Uani 1 1 d . . . O12 O 0.3745(2) 0.72900(12) 0.0437(6) 0.0332(9) Uani 1 1 d . . . O13 O 0.2770(2) 0.72705(13) 0.1795(7) 0.0412(10) Uani 1 1 d . . . C1 C 0.7182(3) 0.58038(18) 1.1208(8) 0.0300(12) Uani 1 1 d . . . C2 C 0.6947(4) 0.53845(15) 1.1942(10) 0.0278(11) Uani 1 1 d . . . C3 C 0.7211(5) 0.5000 1.1371(11) 0.0289(17) Uani 1 2 d S . . H3 H 0.7562 0.5000 1.0611 0.035 Uiso 1 2 calc SR . . C4 C 0.6413(3) 0.53799(18) 1.3049(8) 0.0296(12) Uani 1 1 d . . . H4 H 0.6235 0.5638 1.3416 0.036 Uiso 1 1 calc R . . C5 C 0.6138(5) 0.5000 1.3621(12) 0.0320(18) Uani 1 2 d S . . C6 C 0.5532(5) 0.5000 1.4781(14) 0.039(2) Uani 1 2 d S . . C7 C 0.4780(8) 0.4839(5) 1.338(2) 0.075(4) Uani 0.50 1 d PU . 1 H7B H 0.4679 0.5000 1.2090 0.113 Uiso 1 2 d SR . 1 H7C H 0.4370 0.4896 1.3970 0.113 Uiso 0.50 1 d PR . 1 H7A H 0.4815 0.4536 1.3179 0.113 Uiso 0.50 1 d PR . 1 C8 C 0.5417(10) 0.5426(7) 1.562(3) 0.075(4) Uani 0.50 1 d PU . 1 H8C H 0.5904 0.5539 1.6392 0.113 Uiso 0.50 1 d PR . 1 H8A H 0.5084 0.5397 1.6480 0.113 Uiso 0.50 1 d PR . 1 H8B H 0.5187 0.5618 1.4522 0.113 Uiso 0.50 1 d PR . 1 C9 C 0.5807(10) 0.5305(7) 1.668(3) 0.075(4) Uani 0.50 1 d PU . 2 H9B H 0.6231 0.5176 1.7666 0.113 Uiso 0.50 1 d PR . 2 H9A H 0.5391 0.5351 1.7263 0.113 Uiso 0.50 1 d PR . 2 H9C H 0.5965 0.5575 1.6254 0.113 Uiso 0.50 1 d PR . 2 C10 C 0.6652(3) 0.75871(17) 0.6607(8) 0.0259(12) Uani 1 1 d . . . C11 C 0.5995(3) 0.78373(17) 0.5347(8) 0.0259(12) Uani 1 1 d . . . C12 C 0.5292(3) 0.77998(18) 0.5765(8) 0.0258(12) Uani 1 1 d . . . H12 H 0.5238 0.7605 0.6739 0.031 Uiso 1 1 calc R . . C13 C 0.4671(3) 0.80475(17) 0.4759(8) 0.0236(11) Uani 1 1 d . . . C14 C 0.3917(3) 0.79945(17) 0.5280(8) 0.0248(11) Uani 1 1 d . . . C15 C 0.4755(3) 0.83459(18) 0.3331(8) 0.0278(12) Uani 1 1 d . . . H15 H 0.4341 0.8519 0.2692 0.033 Uiso 1 1 calc R . . C16 C 0.5445(3) 0.83919(18) 0.2833(8) 0.0296(12) Uani 1 1 d . . . C17 C 0.5538(4) 0.8719(2) 0.1321(11) 0.0449(16) Uani 1 1 d . . . C18 C 0.4803(7) 0.8794(4) -0.0356(16) 0.123(3) Uani 1 1 d U . . H18A H 0.4559 0.8524 -0.0795 0.184 Uiso 1 1 calc R . . H18C H 0.4920 0.8933 -0.1480 0.184 Uiso 1 1 calc R . . H18B H 0.4463 0.8971 0.0143 0.184 Uiso 1 1 calc R . . C19 C 0.5754(7) 0.9135(4) 0.2407(17) 0.123(3) Uani 1 1 d U . . H19A H 0.5453 0.9178 0.3338 0.184 Uiso 1 1 calc R . . H19C H 0.5660 0.9365 0.1438 0.184 Uiso 1 1 calc R . . H19B H 0.6290 0.9130 0.3143 0.184 Uiso 1 1 calc R . . C20 C 0.6160(7) 0.8598(4) 0.0328(17) 0.123(3) Uani 1 1 d U . . H20B H 0.6644 0.8572 0.1351 0.184 Uiso 1 1 calc R . . H20C H 0.6198 0.8815 -0.0629 0.184 Uiso 1 1 calc R . . H20A H 0.6032 0.8329 -0.0365 0.184 Uiso 1 1 calc R . . C21 C 0.6061(3) 0.81291(18) 0.3841(8) 0.0287(12) Uani 1 1 d . . . H21 H 0.6523 0.8148 0.3508 0.034 Uiso 1 1 calc R . . C22 C 0.5958(3) 0.65850(18) 0.5936(9) 0.0286(12) Uani 1 1 d . . . C23 C 0.5098(3) 0.66085(18) 0.5475(8) 0.0272(12) Uani 1 1 d . . . C24 C 0.4689(3) 0.68560(17) 0.3896(8) 0.0263(12) Uani 1 1 d . . . H24 H 0.4944 0.7005 0.3109 0.032 Uiso 1 1 calc R . . C25 C 0.3890(3) 0.68860(18) 0.3458(8) 0.0272(11) Uani 1 1 d . . . C26 C 0.3429(3) 0.71696(19) 0.1801(8) 0.0289(12) Uani 1 1 d . . . C27 C 0.3524(3) 0.66518(17) 0.4657(8) 0.0284(12) Uani 1 1 d . . . H27 H 0.2994 0.6673 0.4384 0.034 Uiso 1 1 calc R . . C28 C 0.3920(3) 0.63916(18) 0.6226(9) 0.0315(13) Uani 1 1 d . . . C29 C 0.4729(3) 0.63760(18) 0.6646(8) 0.0300(13) Uani 1 1 d . . . H29 H 0.5015 0.6209 0.7714 0.036 Uiso 1 1 calc R . . C30 C 0.3504(3) 0.6111(2) 0.7390(11) 0.0405(15) Uani 1 1 d . . . C31 C 0.2798(5) 0.6326(3) 0.7722(15) 0.0799(16) Uani 1 1 d U . . H31C H 0.2928 0.6612 0.8216 0.120 Uiso 1 1 calc R . . H31A H 0.2622 0.6167 0.8699 0.120 Uiso 1 1 calc R . . H31B H 0.2399 0.6337 0.6460 0.120 Uiso 1 1 calc R . . C32 C 0.3239(5) 0.5709(3) 0.6127(14) 0.0799(16) Uani 1 1 d U . . H32C H 0.2825 0.5780 0.4954 0.120 Uiso 1 1 calc R . . H32A H 0.3066 0.5501 0.6929 0.120 Uiso 1 1 calc R . . H32B H 0.3659 0.5593 0.5703 0.120 Uiso 1 1 calc R . . C33 C 0.4005(5) 0.5977(3) 0.9477(14) 0.0799(16) Uani 1 1 d U . . H33B H 0.4420 0.5802 0.9326 0.120 Uiso 1 1 calc R . . H33A H 0.3702 0.5818 1.0169 0.120 Uiso 1 1 calc R . . H33C H 0.4209 0.6227 1.0253 0.120 Uiso 1 1 calc 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 Ba1 0.02103(13) 0.02929(16) 0.02606(14) 0.00355(15) 0.01172(11) -0.00167(15) Zn1 0.0247(3) 0.0262(3) 0.0257(3) 0.0016(3) 0.0089(3) -0.0022(3) Zn2 0.0172(3) 0.0282(3) 0.0247(3) -0.0024(3) 0.0088(2) -0.0025(3) O1 0.053(3) 0.0205(19) 0.033(2) -0.0013(19) 0.014(2) -0.0044(19) O2 0.055(3) 0.030(2) 0.042(2) 0.0092(18) 0.028(2) 0.0068(19) O3 0.056(3) 0.084(4) 0.036(3) -0.011(3) 0.017(2) 0.004(3) O4 0.0248(18) 0.0214(19) 0.0268(19) 0.0014(15) 0.0085(16) -0.0018(15) O5 0.0197(18) 0.040(2) 0.037(2) 0.0056(19) 0.0106(18) 0.0026(18) O6 0.035(2) 0.049(3) 0.028(2) 0.0133(19) 0.0114(19) 0.013(2) O7 0.0186(19) 0.046(3) 0.046(3) -0.003(2) 0.0060(19) 0.0020(19) O8 0.0222(18) 0.051(3) 0.035(2) 0.0039(19) 0.0153(18) 0.0000(18) O9 0.034(3) 0.200(7) 0.061(4) 0.061(5) 0.021(3) 0.023(4) O10 0.031(2) 0.051(3) 0.037(2) 0.009(2) 0.0182(19) 0.0007(19) O11 0.0231(19) 0.056(3) 0.040(2) 0.025(2) 0.0084(18) 0.0031(19) O12 0.030(2) 0.037(2) 0.034(2) 0.0130(18) 0.0124(18) 0.0121(18) O13 0.031(2) 0.045(3) 0.049(3) 0.013(2) 0.014(2) 0.017(2) C1 0.032(3) 0.031(3) 0.025(3) 0.004(2) 0.003(2) 0.001(3) C2 0.040(3) 0.021(2) 0.021(2) 0.002(3) 0.007(2) -0.002(3) C3 0.041(4) 0.027(4) 0.022(4) 0.000 0.014(4) 0.000 C4 0.034(3) 0.024(3) 0.032(3) 0.003(2) 0.012(3) 0.003(2) C5 0.037(4) 0.031(4) 0.030(4) 0.000 0.012(4) 0.000 C6 0.045(5) 0.030(5) 0.052(6) 0.000 0.030(5) 0.000 C7 0.062(6) 0.108(10) 0.069(8) -0.032(7) 0.040(5) -0.023(7) C8 0.062(6) 0.108(10) 0.069(8) -0.032(7) 0.040(5) -0.023(7) C9 0.062(6) 0.108(10) 0.069(8) -0.032(7) 0.040(5) -0.023(7) C10 0.020(3) 0.030(3) 0.029(3) -0.002(2) 0.010(3) 0.001(2) C11 0.024(3) 0.029(3) 0.027(3) -0.006(2) 0.011(2) -0.004(2) C12 0.024(3) 0.032(3) 0.026(3) 0.002(2) 0.013(2) -0.004(2) C13 0.019(2) 0.027(3) 0.023(3) -0.001(2) 0.004(2) 0.001(2) C14 0.019(2) 0.029(3) 0.026(3) -0.005(2) 0.007(2) 0.000(2) C15 0.018(2) 0.034(3) 0.027(3) 0.003(2) 0.000(2) -0.001(2) C16 0.026(3) 0.031(3) 0.031(3) 0.003(2) 0.006(2) -0.001(2) C17 0.033(3) 0.040(4) 0.057(4) 0.014(3) 0.007(3) -0.006(3) C18 0.124(6) 0.145(6) 0.099(5) 0.081(5) 0.033(4) -0.010(5) C19 0.124(6) 0.145(6) 0.099(5) 0.081(5) 0.033(4) -0.010(5) C20 0.124(6) 0.145(6) 0.099(5) 0.081(5) 0.033(4) -0.010(5) C21 0.022(3) 0.036(3) 0.030(3) -0.001(3) 0.012(2) -0.006(2) C22 0.025(3) 0.029(3) 0.034(3) 0.003(2) 0.013(3) 0.002(2) C23 0.019(2) 0.035(3) 0.028(3) 0.008(2) 0.008(2) 0.002(2) C24 0.027(3) 0.030(3) 0.025(3) 0.004(2) 0.012(2) 0.002(2) C25 0.027(3) 0.029(3) 0.026(3) 0.001(2) 0.008(2) 0.003(2) C26 0.028(3) 0.029(3) 0.030(3) -0.001(2) 0.010(2) 0.004(2) C27 0.021(3) 0.034(3) 0.032(3) 0.007(2) 0.009(2) 0.001(2) C28 0.028(3) 0.032(3) 0.038(3) 0.003(3) 0.015(3) 0.002(3) C29 0.031(3) 0.031(3) 0.030(3) 0.007(2) 0.013(3) 0.004(2) C30 0.036(3) 0.037(4) 0.057(4) 0.013(3) 0.026(3) 0.005(3) C31 0.078(3) 0.081(4) 0.099(4) 0.028(3) 0.054(3) -0.001(3) C32 0.078(3) 0.081(4) 0.099(4) 0.028(3) 0.054(3) -0.001(3) C33 0.078(3) 0.081(4) 0.099(4) 0.028(3) 0.054(3) -0.001(3) _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 O6 2.686(4) . ? Ba1 O10 2.688(4) 1_556 ? Ba1 O13 2.701(4) 4_566 ? Ba1 O7 2.766(4) 4_566 ? Ba1 O9 2.808(5) . ? Ba1 O4 2.910(3) . ? Ba1 O5 3.203(4) 1_556 ? Ba1 Zn1 3.7104(7) . ? Ba1 Zn2 3.9472(6) . ? Zn1 O4 1.936(4) . ? Zn1 O11 1.954(4) . ? Zn1 O2 1.954(4) . ? Zn1 O3 1.987(4) . ? Zn2 O5 1.975(4) . ? Zn2 O8 1.980(3) 4_565 ? Zn2 O4 1.981(3) . ? Zn2 O12 1.989(4) 4_566 ? O1 C1 1.237(6) . ? O2 C1 1.279(6) . ? O3 H3B 0.8655 . ? O3 H3A 0.8659 . ? O5 C10 1.294(6) . ? O5 Ba1 3.203(4) 1_554 ? O6 C10 1.232(6) . ? O7 C14 1.251(7) . ? O7 Ba1 2.766(4) 4_464 ? O8 C14 1.267(6) . ? O8 Zn2 1.980(3) 4_465 ? O9 H9D 0.8822 . ? O9 H9E 0.8842 . ? O10 C22 1.233(6) . ? O10 Ba1 2.688(4) 1_554 ? O11 C22 1.291(7) . ? O12 C26 1.284(6) . ? O12 Zn2 1.989(4) 4_464 ? O13 C26 1.235(6) . ? O13 Ba1 2.701(4) 4_464 ? C1 C2 1.508(7) . ? C2 C4 1.389(8) . ? C2 C3 1.390(6) . ? C3 C2 1.390(6) 2_565 ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 H4 0.9300 . ? C5 C4 1.387(6) 2_565 ? C5 C6 1.528(10) . ? C6 C8 1.49(2) . ? C6 C8 1.49(2) 2_565 ? C6 C7 1.518(16) 2_565 ? C6 C7 1.519(16) . ? C6 C9 1.577(19) . ? C6 C9 1.577(19) 2_565 ? C7 C7 1.01(3) 2_565 ? C7 C8 1.84(2) 2_565 ? C7 H7B 0.9875 . ? C7 H7C 0.9600 . ? C7 H7A 0.9601 . ? C8 C7 1.84(2) 2_565 ? C8 H8C 0.9601 . ? C8 H8A 0.9599 . ? C8 H8B 0.9599 . ? C8 H9A 1.1662 . ? C8 H9C 1.0733 . ? C9 C9 1.91(4) 2_565 ? C9 H8C 0.7871 . ? C9 H9B 0.9600 . ? C9 H9A 0.9601 . ? C9 H9C 0.9601 . ? C10 C11 1.483(8) . ? C11 C12 1.389(7) . ? C11 C21 1.409(7) . ? C12 C13 1.380(7) . ? C12 H12 0.9300 . ? C13 C15 1.392(7) . ? C13 C14 1.518(7) . ? C15 C16 1.394(7) . ? C15 H15 0.9300 . ? C16 C21 1.402(8) . ? C16 C17 1.500(8) . ? C17 C19 1.495(14) . ? C17 C18 1.515(12) . ? C17 C20 1.522(13) . ? C18 H18A 0.9600 . ? C18 H18C 0.9600 . ? C18 H18B 0.9600 . ? C19 H19A 0.9600 . ? C19 H19C 0.9600 . ? C19 H19B 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 H20A 0.9600 . ? C21 H21 0.9300 . ? C22 C23 1.504(7) . ? C23 C24 1.367(7) . ? C23 C29 1.387(7) . ? C24 C25 1.399(7) . ? C24 H24 0.9300 . ? C25 C27 1.399(7) . ? C25 C26 1.497(8) . ? C27 C28 1.379(8) . ? C27 H27 0.9300 . ? C28 C29 1.415(7) . ? C28 C30 1.523(8) . ? C29 H29 0.9300 . ? C30 C31 1.519(10) . ? C30 C32 1.523(11) . ? C30 C33 1.523(11) . ? C31 H31C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 H32C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 H33B 0.9600 . ? C33 H33A 0.9600 . ? C33 H33C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ba1 O10 147.10(13) . 1_556 ? O6 Ba1 O13 66.65(14) . 4_566 ? O10 Ba1 O13 132.44(13) 1_556 4_566 ? O6 Ba1 O7 123.64(12) . 4_566 ? O10 Ba1 O7 89.23(12) 1_556 4_566 ? O13 Ba1 O7 73.75(13) 4_566 4_566 ? O6 Ba1 O9 67.31(13) . . ? O10 Ba1 O9 79.91(14) 1_556 . ? O13 Ba1 O9 111.7(2) 4_566 . ? O7 Ba1 O9 168.79(13) 4_566 . ? O6 Ba1 O4 65.75(11) . . ? O10 Ba1 O4 139.27(11) 1_556 . ? O13 Ba1 O4 72.22(11) 4_566 . ? O7 Ba1 O4 64.97(11) 4_566 . ? O9 Ba1 O4 125.61(15) . . ? O6 Ba1 O5 123.70(11) . 1_556 ? O10 Ba1 O5 64.84(11) 1_556 1_556 ? O13 Ba1 O5 67.61(11) 4_566 1_556 ? O7 Ba1 O5 70.16(11) 4_566 1_556 ? O9 Ba1 O5 102.32(19) . 1_556 ? O4 Ba1 O5 126.01(9) . 1_556 ? O6 Ba1 Zn1 70.04(9) . . ? O10 Ba1 Zn1 119.17(9) 1_556 . ? O13 Ba1 Zn1 102.09(9) 4_566 . ? O7 Ba1 Zn1 81.39(9) 4_566 . ? O9 Ba1 Zn1 106.27(18) . . ? O4 Ba1 Zn1 31.12(7) . . ? O5 Ba1 Zn1 151.38(7) 1_556 . ? O6 Ba1 Zn2 45.43(8) . . ? O10 Ba1 Zn2 166.44(9) 1_556 . ? O13 Ba1 Zn2 49.21(9) 4_566 . ? O7 Ba1 Zn2 78.39(8) 4_566 . ? O9 Ba1 Zn2 112.68(10) . . ? O4 Ba1 Zn2 28.84(7) . . ? O5 Ba1 Zn2 114.95(7) 1_556 . ? Zn1 Ba1 Zn2 53.912(13) . . ? O4 Zn1 O11 106.61(18) . . ? O4 Zn1 O2 117.37(17) . . ? O11 Zn1 O2 101.22(16) . . ? O4 Zn1 O3 111.18(17) . . ? O11 Zn1 O3 121.0(2) . . ? O2 Zn1 O3 99.6(2) . . ? O4 Zn1 Ba1 50.98(10) . . ? O11 Zn1 Ba1 64.13(14) . . ? O2 Zn1 Ba1 98.66(11) . . ? O3 Zn1 Ba1 159.39(15) . . ? O5 Zn2 O8 104.83(16) . 4_565 ? O5 Zn2 O4 116.85(15) . . ? O8 Zn2 O4 108.34(16) 4_565 . ? O5 Zn2 O12 121.97(17) . 4_566 ? O8 Zn2 O12 98.17(16) 4_565 4_566 ? O4 Zn2 O12 104.49(15) . 4_566 ? O5 Zn2 Ba1 94.59(11) . . ? O8 Zn2 Ba1 153.02(12) 4_565 . ? O4 Zn2 Ba1 45.12(10) . . ? O12 Zn2 Ba1 86.81(11) 4_566 . ? C1 O2 Zn1 112.4(3) . . ? Zn1 O3 H3B 110.5 . . ? Zn1 O3 H3A 110.4 . . ? H3B O3 H3A 108.5 . . ? Zn1 O4 Zn2 125.21(18) . . ? Zn1 O4 Ba1 97.90(12) . . ? Zn2 O4 Ba1 106.04(13) . . ? C10 O5 Zn2 110.9(3) . . ? C10 O5 Ba1 108.3(3) . 1_554 ? Zn2 O5 Ba1 115.48(16) . 1_554 ? C10 O6 Ba1 164.4(4) . . ? C14 O7 Ba1 139.1(4) . 4_464 ? C14 O8 Zn2 129.3(3) . 4_465 ? Ba1 O9 H9D 110.6 . . ? Ba1 O9 H9E 110.8 . . ? H9D O9 H9E 108.2 . . ? C22 O10 Ba1 174.4(4) . 1_554 ? C22 O11 Zn1 118.5(3) . . ? C26 O12 Zn2 118.0(3) . 4_464 ? C26 O13 Ba1 142.1(4) . 4_464 ? O1 C1 O2 123.6(5) . . ? O1 C1 C2 120.0(5) . . ? O2 C1 C2 116.3(5) . . ? C4 C2 C3 119.6(5) . . ? C4 C2 C1 119.9(5) . . ? C3 C2 C1 120.3(6) . . ? C2 C3 C2 119.7(7) . 2_565 ? C2 C3 H3 120.2 . . ? C2 C3 H3 120.2 2_565 . ? C5 C4 C2 121.7(5) . . ? C5 C4 H4 119.2 . . ? C2 C4 H4 119.2 . . ? C4 C5 C4 117.8(7) . 2_565 ? C4 C5 C6 121.1(3) . . ? C4 C5 C6 121.1(4) 2_565 . ? C8 C6 C8 127.0(15) . 2_565 ? C8 C6 C7 75.5(10) . 2_565 ? C8 C6 C7 110.1(11) 2_565 2_565 ? C8 C6 C7 110.1(11) . . ? C8 C6 C7 75.5(10) 2_565 . ? C7 C6 C7 38.8(13) 2_565 . ? C8 C6 C5 113.6(7) . . ? C8 C6 C5 113.6(7) 2_565 . ? C7 C6 C5 108.6(8) 2_565 . ? C7 C6 C5 108.6(8) . . ? C8 C6 C9 35.5(10) . . ? C8 C6 C9 105.6(12) 2_565 . ? C7 C6 C9 110.0(10) 2_565 . ? C7 C6 C9 138.0(10) . . ? C5 C6 C9 108.8(8) . . ? C8 C6 C9 105.6(12) . 2_565 ? C8 C6 C9 35.5(10) 2_565 2_565 ? C7 C6 C9 138.0(10) 2_565 2_565 ? C7 C6 C9 110.0(10) . 2_565 ? C5 C6 C9 108.8(8) . 2_565 ? C9 C6 C9 74.5(16) . 2_565 ? C7 C7 C6 70.6(7) 2_565 . ? C7 C7 C8 116.7(8) 2_565 2_565 ? C6 C7 C8 51.5(8) . 2_565 ? C7 C7 H7B 59.3 2_565 . ? C6 C7 H7B 107.8 . . ? C8 C7 H7B 153.1 2_565 . ? C7 C7 H7C 79.2 2_565 . ? C6 C7 H7C 109.5 . . ? C8 C7 H7C 96.2 2_565 . ? H7B C7 H7C 108.3 . . ? C7 C7 H7A 170.1 2_565 . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 67.9 2_565 . ? H7B C7 H7A 112.3 . . ? H7C C7 H7A 109.5 . . ? C6 C8 C7 53.0(8) . 2_565 ? C6 C8 H8C 109.5 . . ? C7 C8 H8C 152.9 2_565 . ? C6 C8 H8A 109.5 . . ? C7 C8 H8A 96.7 2_565 . ? H8C C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C7 C8 H8B 66.1 2_565 . ? H8C C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H9A 104.0 . . ? C7 C8 H9A 122.2 2_565 . ? H8C C8 H9A 79.6 . . ? H8A C8 H9A 35.1 . . ? H8B C8 H9A 139.2 . . ? C6 C8 H9C 109.1 . . ? C7 C8 H9C 145.7 2_565 . ? H8C C8 H9C 9.4 . . ? H8A C8 H9C 117.5 . . ? H8B C8 H9C 101.3 . . ? H9A C8 H9C 88.8 . . ? C6 C9 C9 52.7(8) . 2_565 ? C6 C9 H8C 113.4 . . ? C9 C9 H8C 157.8 2_565 . ? C6 C9 H8A 88.4 . . ? C9 C9 H8A 102.6 2_565 . ? H8C C9 H8A 93.4 . . ? C6 C9 H9B 109.5 . . ? C9 C9 H9B 65.1 2_565 . ? H8C C9 H9B 112.0 . . ? H8A C9 H9B 138.0 . . ? C6 C9 H9A 109.5 . . ? C9 C9 H9A 98.6 2_565 . ? H8C C9 H9A 102.8 . . ? H8A C9 H9A 29.6 . . ? H9B C9 H9A 109.5 . . ? C6 C9 H9C 109.5 . . ? C9 C9 H9C 151.2 2_565 . ? H8C C9 H9C 6.7 . . ? H8A C9 H9C 98.8 . . ? H9B C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? O6 C10 O5 123.2(5) . . ? O6 C10 C11 118.8(4) . . ? O5 C10 C11 118.0(5) . . ? C12 C11 C21 118.6(5) . . ? C12 C11 C10 118.0(5) . . ? C21 C11 C10 123.3(5) . . ? C13 C12 C11 121.1(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C15 119.5(5) . . ? C12 C13 C14 118.9(5) . . ? C15 C13 C14 121.6(5) . . ? O7 C14 O8 125.2(5) . . ? O7 C14 C13 119.4(5) . . ? O8 C14 C13 115.4(5) . . ? C13 C15 C16 121.7(5) . . ? C13 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C21 117.7(5) . . ? C15 C16 C17 121.6(5) . . ? C21 C16 C17 120.7(5) . . ? C19 C17 C16 108.2(6) . . ? C19 C17 C18 107.3(8) . . ? C16 C17 C18 112.6(6) . . ? C19 C17 C20 108.5(8) . . ? C16 C17 C20 112.4(6) . . ? C18 C17 C20 107.7(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C16 C21 C11 121.4(5) . . ? C16 C21 H21 119.3 . . ? C11 C21 H21 119.3 . . ? O10 C22 O11 123.2(5) . . ? O10 C22 C23 120.6(5) . . ? O11 C22 C23 116.3(4) . . ? C24 C23 C29 120.9(5) . . ? C24 C23 C22 119.6(5) . . ? C29 C23 C22 119.6(5) . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C27 118.2(5) . . ? C24 C25 C26 121.8(5) . . ? C27 C25 C26 120.0(5) . . ? O13 C26 O12 123.6(5) . . ? O13 C26 C25 119.1(5) . . ? O12 C26 C25 117.3(4) . . ? C28 C27 C25 122.6(5) . . ? C28 C27 H27 118.7 . . ? C25 C27 H27 118.7 . . ? C27 C28 C29 117.5(5) . . ? C27 C28 C30 121.6(5) . . ? C29 C28 C30 120.8(5) . . ? C23 C29 C28 120.4(5) . . ? C23 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C28 112.7(5) . . ? C31 C30 C32 107.9(6) . . ? C28 C30 C32 107.5(5) . . ? C31 C30 C33 106.6(6) . . ? C28 C30 C33 113.5(5) . . ? C32 C30 C33 108.6(6) . . ? C30 C31 H31C 109.5 . . ? C30 C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C32 H32C 109.5 . . ? C30 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C33 H33B 109.5 . . ? C30 C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C30 C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? H33A C33 H33C 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 O6 Ba1 Zn1 O4 75.88(16) . . . . ? O10 Ba1 Zn1 O4 -139.00(16) 1_556 . . . ? O13 Ba1 Zn1 O4 16.48(17) 4_566 . . . ? O7 Ba1 Zn1 O4 -54.75(16) 4_566 . . . ? O9 Ba1 Zn1 O4 133.6(2) . . . . ? O5 Ba1 Zn1 O4 -48.64(19) 1_556 . . . ? Zn2 Ba1 Zn1 O4 27.12(13) . . . . ? O6 Ba1 Zn1 O11 -67.42(16) . . . . ? O10 Ba1 Zn1 O11 77.70(16) 1_556 . . . ? O13 Ba1 Zn1 O11 -126.83(16) 4_566 . . . ? O7 Ba1 Zn1 O11 161.95(15) 4_566 . . . ? O9 Ba1 Zn1 O11 -9.7(2) . . . . ? O4 Ba1 Zn1 O11 -143.30(18) . . . . ? O5 Ba1 Zn1 O11 168.06(19) 1_556 . . . ? Zn2 Ba1 Zn1 O11 -116.18(13) . . . . ? O6 Ba1 Zn1 O2 -165.75(16) . . . . ? O10 Ba1 Zn1 O2 -20.63(16) 1_556 . . . ? O13 Ba1 Zn1 O2 134.84(16) 4_566 . . . ? O7 Ba1 Zn1 O2 63.62(16) 4_566 . . . ? O9 Ba1 Zn1 O2 -108.0(2) . . . . ? O4 Ba1 Zn1 O2 118.37(19) . . . . ? O5 Ba1 Zn1 O2 69.7(2) 1_556 . . . ? Zn2 Ba1 Zn1 O2 145.49(13) . . . . ? O6 Ba1 Zn1 O3 42.4(4) . . . . ? O10 Ba1 Zn1 O3 -172.5(4) 1_556 . . . ? O13 Ba1 Zn1 O3 -17.1(4) 4_566 . . . ? O7 Ba1 Zn1 O3 -88.3(4) 4_566 . . . ? O9 Ba1 Zn1 O3 100.1(5) . . . . ? O4 Ba1 Zn1 O3 -33.5(5) . . . . ? O5 Ba1 Zn1 O3 -82.2(5) 1_556 . . . ? Zn2 Ba1 Zn1 O3 -6.4(4) . . . . ? O6 Ba1 Zn2 O5 -2.40(18) . . . . ? O10 Ba1 Zn2 O5 158.1(4) 1_556 . . . ? O13 Ba1 Zn2 O5 -99.02(17) 4_566 . . . ? O7 Ba1 Zn2 O5 -177.48(15) 4_566 . . . ? O9 Ba1 Zn2 O5 0.7(3) . . . . ? O4 Ba1 Zn2 O5 124.02(19) . . . . ? O5 Ba1 Zn2 O5 -116.02(17) 1_556 . . . ? Zn1 Ba1 Zn2 O5 94.78(12) . . . . ? O6 Ba1 Zn2 O8 -138.8(3) . . . 4_565 ? O10 Ba1 Zn2 O8 21.7(5) 1_556 . . 4_565 ? O13 Ba1 Zn2 O8 124.6(3) 4_566 . . 4_565 ? O7 Ba1 Zn2 O8 46.2(3) 4_566 . . 4_565 ? O9 Ba1 Zn2 O8 -135.7(3) . . . 4_565 ? O4 Ba1 Zn2 O8 -12.3(3) . . . 4_565 ? O5 Ba1 Zn2 O8 107.6(3) 1_556 . . 4_565 ? Zn1 Ba1 Zn2 O8 -41.6(3) . . . 4_565 ? O6 Ba1 Zn2 O4 -126.4(2) . . . . ? O10 Ba1 Zn2 O4 34.0(4) 1_556 . . . ? O13 Ba1 Zn2 O4 136.96(19) 4_566 . . . ? O7 Ba1 Zn2 O4 58.50(17) 4_566 . . . ? O9 Ba1 Zn2 O4 -123.3(3) . . . . ? O5 Ba1 Zn2 O4 119.96(16) 1_556 . . . ? Zn1 Ba1 Zn2 O4 -29.24(15) . . . . ? O6 Ba1 Zn2 O12 119.44(18) . . . 4_566 ? O10 Ba1 Zn2 O12 -80.1(4) 1_556 . . 4_566 ? O13 Ba1 Zn2 O12 22.82(18) 4_566 . . 4_566 ? O7 Ba1 Zn2 O12 -55.64(15) 4_566 . . 4_566 ? O9 Ba1 Zn2 O12 122.5(3) . . . 4_566 ? O4 Ba1 Zn2 O12 -114.14(19) . . . 4_566 ? O5 Ba1 Zn2 O12 5.82(14) 1_556 . . 4_566 ? Zn1 Ba1 Zn2 O12 -143.38(12) . . . 4_566 ? O4 Zn1 O2 C1 68.5(4) . . . . ? O11 Zn1 O2 C1 -47.1(4) . . . . ? O3 Zn1 O2 C1 -171.6(4) . . . . ? Ba1 Zn1 O2 C1 18.1(4) . . . . ? O11 Zn1 O4 Zn2 -81.9(2) . . . . ? O2 Zn1 O4 Zn2 165.55(18) . . . . ? O3 Zn1 O4 Zn2 51.9(3) . . . . ? Ba1 Zn1 O4 Zn2 -116.1(2) . . . . ? O11 Zn1 O4 Ba1 34.13(16) . . . . ? O2 Zn1 O4 Ba1 -78.39(16) . . . . ? O3 Zn1 O4 Ba1 167.96(17) . . . . ? O5 Zn2 O4 Zn1 44.4(3) . . . . ? O8 Zn2 O4 Zn1 -73.7(2) 4_565 . . . ? O12 Zn2 O4 Zn1 -177.6(2) 4_566 . . . ? Ba1 Zn2 O4 Zn1 112.2(2) . . . . ? O5 Zn2 O4 Ba1 -67.83(18) . . . . ? O8 Zn2 O4 Ba1 174.14(14) 4_565 . . . ? O12 Zn2 O4 Ba1 70.23(16) 4_566 . . . ? O6 Ba1 O4 Zn1 -91.24(16) . . . . ? O10 Ba1 O4 Zn1 61.4(2) 1_556 . . . ? O13 Ba1 O4 Zn1 -163.07(17) 4_566 . . . ? O7 Ba1 O4 Zn1 116.99(17) 4_566 . . . ? O9 Ba1 O4 Zn1 -58.7(3) . . . . ? O5 Ba1 O4 Zn1 153.61(11) 1_556 . . . ? Zn2 Ba1 O4 Zn1 -130.2(2) . . . . ? O6 Ba1 O4 Zn2 38.96(15) . . . . ? O10 Ba1 O4 Zn2 -168.39(15) 1_556 . . . ? O13 Ba1 O4 Zn2 -32.86(15) 4_566 . . . ? O7 Ba1 O4 Zn2 -112.81(17) 4_566 . . . ? O9 Ba1 O4 Zn2 71.5(3) . . . . ? O5 Ba1 O4 Zn2 -76.18(17) 1_556 . . . ? Zn1 Ba1 O4 Zn2 130.2(2) . . . . ? O8 Zn2 O5 C10 169.3(4) 4_565 . . . ? O4 Zn2 O5 C10 49.3(4) . . . . ? O12 Zn2 O5 C10 -81.0(4) 4_566 . . . ? Ba1 Zn2 O5 C10 8.2(4) . . . . ? O8 Zn2 O5 Ba1 45.6(2) 4_565 . . 1_554 ? O4 Zn2 O5 Ba1 -74.33(18) . . . 1_554 ? O12 Zn2 O5 Ba1 155.39(14) 4_566 . . 1_554 ? Ba1 Zn2 O5 Ba1 -115.50(12) . . . 1_554 ? O10 Ba1 O6 C10 176.9(14) 1_556 . . . ? O13 Ba1 O6 C10 43.6(15) 4_566 . . . ? O7 Ba1 O6 C10 -5.6(15) 4_566 . . . ? O9 Ba1 O6 C10 171.7(15) . . . . ? O4 Ba1 O6 C10 -36.6(14) . . . . ? O5 Ba1 O6 C10 81.8(15) 1_556 . . . ? Zn1 Ba1 O6 C10 -69.9(15) . . . . ? Zn2 Ba1 O6 C10 -11.4(14) . . . . ? O4 Zn1 O11 C22 93.3(4) . . . . ? O2 Zn1 O11 C22 -143.5(4) . . . . ? O3 Zn1 O11 C22 -35.0(5) . . . . ? Ba1 Zn1 O11 C22 122.2(5) . . . . ? Zn1 O2 C1 O1 -21.5(7) . . . . ? Zn1 O2 C1 C2 156.2(4) . . . . ? O1 C1 C2 C4 14.4(9) . . . . ? O2 C1 C2 C4 -163.4(6) . . . . ? O1 C1 C2 C3 -171.1(6) . . . . ? O2 C1 C2 C3 11.1(9) . . . . ? C4 C2 C3 C2 -1.0(12) . . . 2_565 ? C1 C2 C3 C2 -175.6(4) . . . 2_565 ? C3 C2 C4 C5 0.6(11) . . . . ? C1 C2 C4 C5 175.1(6) . . . . ? C2 C4 C5 C4 -0.1(12) . . . 2_565 ? C2 C4 C5 C6 -178.0(7) . . . . ? C4 C5 C6 C8 -13.4(15) . . . . ? C4 C5 C6 C8 168.7(11) 2_565 . . . ? C4 C5 C6 C8 -168.7(11) . . . 2_565 ? C4 C5 C6 C8 13.4(15) 2_565 . . 2_565 ? C4 C5 C6 C7 68.4(11) . . . 2_565 ? C4 C5 C6 C7 -109.4(9) 2_565 . . 2_565 ? C4 C5 C6 C7 109.4(9) . . . . ? C4 C5 C6 C7 -68.4(11) 2_565 . . . ? C4 C5 C6 C9 -51.3(13) . . . . ? C4 C5 C6 C9 130.8(10) 2_565 . . . ? C4 C5 C6 C9 -130.8(10) . . . 2_565 ? C4 C5 C6 C9 51.3(13) 2_565 . . 2_565 ? C8 C6 C7 C7 28.2(8) . . . 2_565 ? C8 C6 C7 C7 152.7(8) 2_565 . . 2_565 ? C5 C6 C7 C7 -96.8(4) . . . 2_565 ? C9 C6 C7 C7 55.4(14) . . . 2_565 ? C9 C6 C7 C7 144.2(9) 2_565 . . 2_565 ? C8 C6 C7 C8 -124.5(16) . . . 2_565 ? C7 C6 C7 C8 -152.7(8) 2_565 . . 2_565 ? C5 C6 C7 C8 110.5(8) . . . 2_565 ? C9 C6 C7 C8 -97.4(16) . . . 2_565 ? C9 C6 C7 C8 -8.5(11) 2_565 . . 2_565 ? C8 C6 C8 C7 -104.4(18) 2_565 . . 2_565 ? C7 C6 C8 C7 -17.8(8) . . . 2_565 ? C5 C6 C8 C7 104.3(9) . . . 2_565 ? C9 C6 C8 C7 -166.1(18) . . . 2_565 ? C9 C6 C8 C7 -136.5(11) 2_565 . . 2_565 ? C8 C6 C9 C9 150.4(14) . . . 2_565 ? C8 C6 C9 C9 17.3(8) 2_565 . . 2_565 ? C7 C6 C9 C9 136.1(10) 2_565 . . 2_565 ? C7 C6 C9 C9 102.8(15) . . . 2_565 ? C5 C6 C9 C9 -105.0(8) . . . 2_565 ? Ba1 O6 C10 O5 20.8(19) . . . . ? Ba1 O6 C10 C11 -158.7(12) . . . . ? Zn2 O5 C10 O6 -13.1(7) . . . . ? Ba1 O5 C10 O6 114.6(5) 1_554 . . . ? Zn2 O5 C10 C11 166.4(4) . . . . ? Ba1 O5 C10 C11 -65.9(5) 1_554 . . . ? O6 C10 C11 C12 -11.9(8) . . . . ? O5 C10 C11 C12 168.6(5) . . . . ? O6 C10 C11 C21 164.1(5) . . . . ? O5 C10 C11 C21 -15.5(8) . . . . ? C21 C11 C12 C13 -1.1(8) . . . . ? C10 C11 C12 C13 175.0(5) . . . . ? C11 C12 C13 C15 -1.3(8) . . . . ? C11 C12 C13 C14 -179.8(5) . . . . ? Ba1 O7 C14 O8 -62.0(8) 4_464 . . . ? Ba1 O7 C14 C13 120.8(5) 4_464 . . . ? Zn2 O8 C14 O7 -1.5(8) 4_465 . . . ? Zn2 O8 C14 C13 175.8(3) 4_465 . . . ? C12 C13 C14 O7 -170.5(5) . . . . ? C15 C13 C14 O7 11.0(8) . . . . ? C12 C13 C14 O8 12.1(7) . . . . ? C15 C13 C14 O8 -166.4(5) . . . . ? C12 C13 C15 C16 2.3(8) . . . . ? C14 C13 C15 C16 -179.3(5) . . . . ? C13 C15 C16 C21 -0.7(9) . . . . ? C13 C15 C16 C17 -178.9(5) . . . . ? C15 C16 C17 C19 85.1(8) . . . . ? C21 C16 C17 C19 -93.0(8) . . . . ? C15 C16 C17 C18 -33.3(10) . . . . ? C21 C16 C17 C18 148.6(8) . . . . ? C15 C16 C17 C20 -155.1(7) . . . . ? C21 C16 C17 C20 26.8(10) . . . . ? C15 C16 C21 C11 -1.8(8) . . . . ? C17 C16 C21 C11 176.4(5) . . . . ? C12 C11 C21 C16 2.7(8) . . . . ? C10 C11 C21 C16 -173.2(5) . . . . ? Ba1 O10 C22 O11 -157(4) 1_554 . . . ? Ba1 O10 C22 C23 23(5) 1_554 . . . ? Zn1 O11 C22 O10 -8.5(8) . . . . ? Zn1 O11 C22 C23 171.4(4) . . . . ? O10 C22 C23 C24 -14.5(8) . . . . ? O11 C22 C23 C24 165.6(5) . . . . ? O10 C22 C23 C29 165.0(6) . . . . ? O11 C22 C23 C29 -14.9(8) . . . . ? C29 C23 C24 C25 1.3(9) . . . . ? C22 C23 C24 C25 -179.2(5) . . . . ? C23 C24 C25 C27 -0.9(8) . . . . ? C23 C24 C25 C26 177.2(5) . . . . ? Ba1 O13 C26 O12 -58.4(9) 4_464 . . . ? Ba1 O13 C26 C25 122.6(6) 4_464 . . . ? Zn2 O12 C26 O13 0.2(8) 4_464 . . . ? Zn2 O12 C26 C25 179.2(4) 4_464 . . . ? C24 C25 C26 O13 -161.8(5) . . . . ? C27 C25 C26 O13 16.3(9) . . . . ? C24 C25 C26 O12 19.2(8) . . . . ? C27 C25 C26 O12 -162.8(5) . . . . ? C24 C25 C27 C28 -0.7(9) . . . . ? C26 C25 C27 C28 -178.8(5) . . . . ? C25 C27 C28 C29 1.8(9) . . . . ? C25 C27 C28 C30 -174.6(6) . . . . ? C24 C23 C29 C28 -0.1(9) . . . . ? C22 C23 C29 C28 -179.5(5) . . . . ? C27 C28 C29 C23 -1.5(9) . . . . ? C30 C28 C29 C23 175.0(5) . . . . ? C27 C28 C30 C31 -37.7(9) . . . . ? C29 C28 C30 C31 145.9(7) . . . . ? C27 C28 C30 C32 81.0(7) . . . . ? C29 C28 C30 C32 -95.4(7) . . . . ? C27 C28 C30 C33 -159.0(6) . . . . ? C29 C28 C30 C33 24.7(9) . . . . ? # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.547 0.000 0.029 302 19 ' ' 2 0.047 0.500 -0.238 302 19 ' ' 3 0.924 0.000 0.820 8 1 ' ' 4 0.424 0.500 0.820 8 1 ' ' _platon_squeeze_details ; ; # The results of the SQUEEZE/PLATON show that the contributions of some 38 to 40 electrons were removed from the unit cell contents. # This would approximate to 4 water molecules per unit cell. # Considering the asymmetric (formula) unit is 1/4 of the unit cell, # it implies that the unit cell also contains one additional lattice water molecule, # which has been treated as a diffuse contribution to the overall scattering without specific atom positions. _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.617 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.087 #===END