# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yaming Zhou' _publ_contact_author_email YMZHOU@FUDAN.EDU.CN _publ_section_title ; A rutile-type open porous zinc(II)-phosphonocarboxylate framework: local proton transfer and size-selected catalysis ; loop_ _publ_author_name 'Yaming Zhou.' 'Zhen-Xia Chen.' 'Teng-Biao Liao.' 'Yun Ling.' ; Lin-Hong Weng ; # Attachment '1a.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 746203' #TrackingRef '1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 O16 P2 Zn3' _chemical_formula_weight 718.31 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x, -y+1/2, -z+1/4' '-y+1/2, -x, z+3/4' '-x, y+1/2, -z+1/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1, -z+3/4' '-y+1, -x+1/2, z+5/4' '-x+1/2, y+1, -z+3/4' 'y+1, x+1/2, z+5/4' _cell_length_a 18.310(6) _cell_length_b 18.310(6) _cell_length_c 23.222(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7785(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6221 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.25 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6093 _exptl_absorpt_correction_T_max 0.7188 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18703 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.19 _reflns_number_total 3484 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.28(3) _refine_ls_number_reflns 3484 _refine_ls_number_parameters 169 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.193 _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 0.21949(4) 0.22488(4) 0.52767(3) 0.0231(2) Uani 1 1 d . . . Zn2 Zn 0.36793(6) 0.2500 0.6250 0.0262(3) Uani 1 2 d S . . C1 C 0.2273(4) 0.4539(3) 0.5991(3) 0.0295(14) Uani 1 1 d . . . C2 C 0.2213(4) 0.4944(4) 0.6500(3) 0.0372(16) Uani 1 1 d . . . H2 H 0.2220 0.4704 0.6852 0.045 Uiso 1 1 calc R . . C3 C 0.2142(4) 0.5715(4) 0.6486(3) 0.0369(17) Uani 1 1 d . . . C4 C 0.2133(4) 0.6072(3) 0.5967(3) 0.0312(15) Uani 1 1 d . . . H4 H 0.2080 0.6576 0.5956 0.037 Uiso 1 1 calc R . . C5 C 0.2202(4) 0.5680(3) 0.5461(3) 0.0306(15) Uani 1 1 d . . . C6 C 0.2267(4) 0.4909(4) 0.5474(3) 0.0314(15) Uani 1 1 d . . . H6 H 0.2306 0.4651 0.5130 0.038 Uiso 1 1 calc R . . C7 C 0.2116(5) 0.6121(4) 0.7050(3) 0.044(2) Uani 1 1 d . . . C8 C 0.2239(4) 0.6088(4) 0.4896(3) 0.0335(16) Uani 1 1 d . . . O1 O 0.2057(3) 0.3269(3) 0.5490(2) 0.0385(12) Uani 1 1 d . . . O2 O 0.3181(3) 0.3420(3) 0.6103(2) 0.0375(12) Uani 1 1 d . . . O3 O 0.1948(3) 0.3336(3) 0.6568(2) 0.0347(11) Uani 1 1 d . . . O4 O 0.2061(3) 0.6796(3) 0.7019(2) 0.0443(14) Uani 1 1 d . . . O5 O 0.2190(5) 0.5784(3) 0.7503(2) 0.073(2) Uani 1 1 d . . . O6 O 0.2117(4) 0.6752(3) 0.4910(2) 0.0454(14) Uani 1 1 d . . . O7 O 0.2354(3) 0.5715(2) 0.44423(17) 0.0375(12) Uani 1 1 d . . . O8 O 0.0451(10) 0.2500 0.6250 0.291(19) Uani 1 2 d SU . . H8A H 0.0587 0.2576 0.5745 0.437 Uiso 1 1 d R . . H8C H 0.0319 0.2912 0.6483 0.437 Uiso 1 1 d R . . H8B H 0.0236 0.2051 0.6390 0.437 Uiso 1 1 d R . . O8' O -0.011(2) 0.2500 0.6250 0.49(3) Uani 1 2 d SU . . P1 P 0.23739(10) 0.35775(9) 0.60399(7) 0.0272(4) 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 Zn1 0.0243(4) 0.0293(4) 0.0156(3) 0.0004(3) -0.0007(3) -0.0006(3) Zn2 0.0240(6) 0.0390(6) 0.0155(5) -0.0012(4) 0.000 0.000 C1 0.043(4) 0.021(3) 0.025(3) 0.005(3) 0.003(3) 0.004(3) C2 0.058(5) 0.037(4) 0.017(3) 0.002(3) -0.004(3) 0.000(4) C3 0.056(5) 0.031(4) 0.023(3) -0.006(3) 0.002(3) -0.004(3) C4 0.046(4) 0.020(3) 0.028(3) 0.000(3) 0.001(3) 0.000(3) C5 0.049(4) 0.025(3) 0.018(3) 0.003(2) -0.002(3) 0.001(3) C6 0.048(4) 0.030(4) 0.016(3) -0.002(2) 0.001(3) 0.000(3) C7 0.057(5) 0.046(5) 0.027(4) -0.014(3) 0.003(3) -0.001(4) C8 0.046(4) 0.031(4) 0.024(3) 0.004(3) 0.003(3) -0.006(3) O1 0.062(4) 0.023(2) 0.030(3) 0.002(2) -0.010(2) 0.003(2) O2 0.047(3) 0.034(3) 0.032(3) 0.004(2) -0.002(2) 0.000(2) O3 0.048(3) 0.031(3) 0.025(2) 0.011(2) 0.001(2) 0.002(2) O4 0.070(4) 0.033(3) 0.030(3) -0.014(2) -0.006(2) 0.003(3) O5 0.144(7) 0.057(4) 0.019(3) -0.003(2) 0.001(3) 0.001(4) O6 0.082(4) 0.018(3) 0.037(3) 0.003(2) 0.004(3) -0.002(2) O7 0.068(4) 0.026(3) 0.018(2) 0.0071(19) 0.009(2) 0.001(2) O8 0.089(13) 0.65(6) 0.136(15) -0.18(2) 0.000 0.000 O8' 0.25(4) 0.89(9) 0.32(4) -0.12(5) 0.000 0.000 P1 0.0402(11) 0.0210(8) 0.0205(8) 0.0033(6) -0.0004(7) 0.0016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.915(5) 5_556 ? Zn1 O4 1.935(5) 8_454 ? Zn1 O1 1.948(5) . ? Zn1 O6 1.991(5) 4_656 ? Zn2 O2 1.947(5) 5_556 ? Zn2 O2 1.947(5) . ? Zn2 O7 1.971(4) 14_554 ? Zn2 O7 1.971(4) 4_656 ? C1 C6 1.380(9) . ? C1 C2 1.399(9) . ? C1 P1 1.774(6) . ? C2 C3 1.416(10) . ? C3 C4 1.370(9) . ? C3 C7 1.509(9) . ? C4 C5 1.383(9) . ? C5 C6 1.417(9) . ? C5 C8 1.511(8) . ? C7 O5 1.226(9) . ? C7 O4 1.243(10) . ? C8 O6 1.237(8) . ? C8 O7 1.273(8) . ? O1 P1 1.512(5) . ? O2 P1 1.512(5) . ? O3 P1 1.519(5) . ? O3 Zn1 1.915(5) 5_556 ? O4 Zn1 1.935(5) 16_454 ? O6 Zn1 1.991(5) 2_566 ? O7 Zn2 1.971(4) 2_566 ? O8 O8' 1.02(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O4 122.3(2) 5_556 8_454 ? O3 Zn1 O1 107.7(2) 5_556 . ? O4 Zn1 O1 110.6(2) 8_454 . ? O3 Zn1 O6 109.5(2) 5_556 4_656 ? O4 Zn1 O6 98.4(2) 8_454 4_656 ? O1 Zn1 O6 107.3(2) . 4_656 ? O2 Zn2 O2 124.1(3) 5_556 . ? O2 Zn2 O7 103.8(2) 5_556 14_554 ? O2 Zn2 O7 106.8(2) . 14_554 ? O2 Zn2 O7 106.8(2) 5_556 4_656 ? O2 Zn2 O7 103.8(2) . 4_656 ? O7 Zn2 O7 111.5(3) 14_554 4_656 ? C6 C1 C2 118.3(6) . . ? C6 C1 P1 123.0(5) . . ? C2 C1 P1 118.8(5) . . ? C1 C2 C3 121.1(6) . . ? C4 C3 C2 119.7(6) . . ? C4 C3 C7 121.9(6) . . ? C2 C3 C7 118.3(6) . . ? C3 C4 C5 120.0(6) . . ? C4 C5 C6 120.4(6) . . ? C4 C5 C8 119.1(6) . . ? C6 C5 C8 120.4(5) . . ? C1 C6 C5 120.6(6) . . ? O5 C7 O4 124.0(7) . . ? O5 C7 C3 119.6(7) . . ? O4 C7 C3 116.3(7) . . ? O6 C8 O7 125.4(6) . . ? O6 C8 C5 117.0(6) . . ? O7 C8 C5 117.4(6) . . ? P1 O1 Zn1 121.6(3) . . ? P1 O2 Zn2 129.8(3) . . ? P1 O3 Zn1 133.1(3) . 5_556 ? C7 O4 Zn1 108.0(5) . 16_454 ? C8 O6 Zn1 157.6(6) . 2_566 ? C8 O7 Zn2 113.3(4) . 2_566 ? O1 P1 O2 112.6(3) . . ? O1 P1 O3 112.1(3) . . ? O2 P1 O3 111.6(3) . . ? O1 P1 C1 106.1(3) . . ? O2 P1 C1 107.3(3) . . ? O3 P1 C1 106.6(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.700 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.140 # Attachment '1b.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 746472' #TrackingRef '1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 O16 P2 Zn3' _chemical_formula_weight 718.31 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 18.218(4) _cell_length_b 18.218(4) _cell_length_c 23.552(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7817(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1902 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.53 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 1.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6303 _exptl_absorpt_correction_T_max 0.7197 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15733 _diffrn_reflns_av_R_equivalents 0.1222 _diffrn_reflns_av_sigmaI/netI 0.1459 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3433 _reflns_number_gt 2140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(5) _refine_ls_number_reflns 3433 _refine_ls_number_parameters 168 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.2031 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.088 _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 0.28309(7) 0.27122(8) 0.02850(5) 0.0254(4) Uani 1 1 d . . . Zn2 Zn 0.13068(11) 0.2500 0.1250 0.0279(6) Uani 1 2 d S . . P1 P 0.2620(2) 0.14023(19) 0.10779(12) 0.0322(9) Uani 1 1 d . . . O1 O 0.2983(5) 0.1719(5) 0.0554(4) 0.042(3) Uani 1 1 d . . . O2 O 0.1807(5) 0.1578(5) 0.1113(3) 0.039(3) Uani 1 1 d . . . O3 O 0.3017(5) 0.1596(5) 0.1623(4) 0.044(3) Uani 1 1 d . . . O4 O 0.2795(7) -0.1890(6) 0.1970(4) 0.058(3) Uani 1 1 d . . . O5 O 0.2809(8) -0.0893(6) 0.2457(4) 0.077(4) Uani 1 1 d . . . O6 O 0.2811(6) -0.1751(5) -0.0130(4) 0.052(3) Uani 1 1 d . . . O7 O 0.2603(6) -0.0682(5) -0.0564(3) 0.045(3) Uani 1 1 d . . . C1 C 0.2708(8) 0.0428(7) 0.0998(5) 0.036(4) Uani 1 1 d . . . C2 C 0.2723(9) -0.0012(7) 0.1481(5) 0.039(4) Uani 1 1 d . . . H2 H 0.2705 0.0210 0.1837 0.046 Uiso 1 1 calc R . . C3 C 0.2763(9) -0.0776(7) 0.1448(5) 0.041(4) Uani 1 1 d . . . C4 C 0.2779(8) -0.1114(7) 0.0932(5) 0.039(4) Uani 1 1 d . . . H4 H 0.2829 -0.1621 0.0908 0.047 Uiso 1 1 calc R . . C5 C 0.2720(8) -0.0696(7) 0.0446(4) 0.031(3) Uani 1 1 d . . . C6 C 0.2689(8) 0.0068(7) 0.0483(4) 0.035(3) Uani 1 1 d . . . H6 H 0.2654 0.0342 0.0151 0.042 Uiso 1 1 calc R . . C7 C 0.2810(9) -0.1228(10) 0.1995(6) 0.046(4) Uani 1 1 d . . . C8 C 0.2693(9) -0.1085(7) -0.0124(5) 0.038(4) Uani 1 1 d . . . O8 O 0.193(2) 0.012(2) 0.3403(17) 0.45(3) Uani 1 1 d U . . H8B H 0.1757 0.0041 0.3803 0.674 Uiso 1 1 d R . . H8C H 0.2166 0.0621 0.3392 0.674 Uiso 1 1 d R . . H8A H 0.1989 -0.0367 0.3023 0.674 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0272(9) 0.0345(9) 0.0146(6) -0.0014(6) 0.0005(6) 0.0007(8) Zn2 0.0278(13) 0.0428(15) 0.0132(9) 0.0005(9) 0.000 0.000 P1 0.049(3) 0.026(2) 0.0218(16) -0.0044(14) 0.0010(15) -0.0011(19) O1 0.063(8) 0.029(5) 0.033(5) -0.003(4) 0.015(5) 0.000(5) O2 0.050(7) 0.035(6) 0.032(6) 0.004(4) -0.006(4) -0.003(5) O3 0.057(7) 0.050(6) 0.026(5) -0.017(4) -0.002(4) 0.007(5) O4 0.109(10) 0.031(6) 0.035(5) 0.017(4) 0.007(6) 0.000(7) O5 0.145(13) 0.064(8) 0.022(5) 0.011(5) -0.004(7) -0.007(8) O6 0.101(9) 0.018(5) 0.038(5) -0.007(4) 0.000(6) -0.005(6) O7 0.083(8) 0.038(6) 0.015(4) -0.003(4) -0.010(5) -0.010(6) C1 0.040(10) 0.047(9) 0.020(6) -0.002(6) 0.003(7) 0.000(8) C2 0.065(11) 0.034(8) 0.017(6) 0.004(6) 0.005(7) -0.016(8) C3 0.072(11) 0.026(8) 0.024(7) -0.002(6) 0.008(7) -0.006(8) C4 0.068(11) 0.033(8) 0.016(6) 0.007(6) 0.003(7) -0.005(8) C5 0.046(9) 0.036(8) 0.012(6) -0.003(5) 0.010(6) 0.015(8) C6 0.056(10) 0.036(8) 0.014(6) 0.003(5) 0.003(6) 0.001(8) C7 0.059(11) 0.054(11) 0.026(7) 0.015(7) 0.003(7) 0.009(10) C8 0.068(12) 0.026(8) 0.021(6) 0.000(5) -0.009(7) -0.011(8) O8 0.56(5) 0.40(4) 0.39(4) -0.27(3) -0.01(3) 0.10(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 O3 1.910(8) 14_454 ? Zn1 O1 1.937(9) . ? Zn1 O4 1.990(9) 8_554 ? Zn1 O6 2.009(9) 4 ? Zn1 O5 2.456(10) 8_554 ? Zn1 C7 2.537(14) 8_554 ? Zn2 O2 1.939(9) 14_454 ? Zn2 O2 1.939(9) . ? Zn2 O7 1.985(8) 15_454 ? Zn2 O7 1.985(8) 4 ? P1 O1 1.514(9) . ? P1 O3 1.515(9) . ? P1 O2 1.516(10) . ? P1 C1 1.793(13) . ? O3 Zn1 1.910(8) 14_454 ? O4 C7 1.209(17) . ? O4 Zn1 1.990(9) 16_444 ? O5 C7 1.247(16) . ? O5 Zn1 2.456(10) 16_444 ? O6 C8 1.233(14) . ? O6 Zn1 2.009(9) 3 ? O7 C8 1.280(13) . ? O7 Zn2 1.985(8) 3 ? C1 C6 1.379(16) . ? C1 C2 1.393(15) . ? C2 C3 1.396(17) . ? C3 C4 1.363(15) . ? C3 C7 1.530(17) . ? C4 C5 1.380(15) . ? C5 C6 1.396(17) . ? C5 C8 1.519(15) . ? C7 Zn1 2.537(14) 16_444 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 110.6(4) 14_454 . ? O3 Zn1 O4 127.5(5) 14_454 8_554 ? O1 Zn1 O4 110.5(4) . 8_554 ? O3 Zn1 O6 104.3(4) 14_454 4 ? O1 Zn1 O6 106.4(4) . 4 ? O4 Zn1 O6 93.9(4) 8_554 4 ? O3 Zn1 O5 90.8(4) 14_454 8_554 ? O1 Zn1 O5 92.0(4) . 8_554 ? O4 Zn1 O5 56.6(4) 8_554 8_554 ? O6 Zn1 O5 149.7(4) 4 8_554 ? O3 Zn1 C7 111.7(5) 14_454 8_554 ? O1 Zn1 C7 102.0(5) . 8_554 ? O4 Zn1 C7 27.8(4) 8_554 8_554 ? O6 Zn1 C7 121.5(5) 4 8_554 ? O5 Zn1 C7 28.9(4) 8_554 8_554 ? O2 Zn2 O2 123.9(5) 14_454 . ? O2 Zn2 O7 102.5(4) 14_454 15_454 ? O2 Zn2 O7 108.8(4) . 15_454 ? O2 Zn2 O7 108.8(4) 14_454 4 ? O2 Zn2 O7 102.5(4) . 4 ? O7 Zn2 O7 110.1(5) 15_454 4 ? O1 P1 O3 113.1(6) . . ? O1 P1 O2 113.0(6) . . ? O3 P1 O2 111.8(5) . . ? O1 P1 C1 104.6(5) . . ? O3 P1 C1 106.1(6) . . ? O2 P1 C1 107.6(6) . . ? P1 O1 Zn1 124.0(6) . . ? P1 O2 Zn2 130.6(6) . . ? P1 O3 Zn1 133.5(6) . 14_454 ? C7 O4 Zn1 102.2(9) . 16_444 ? C7 O5 Zn1 79.2(9) . 16_444 ? C8 O6 Zn1 162.0(11) . 3 ? C8 O7 Zn2 110.0(8) . 3 ? C6 C1 C2 116.5(12) . . ? C6 C1 P1 124.1(10) . . ? C2 C1 P1 119.1(9) . . ? C1 C2 C3 122.0(11) . . ? C4 C3 C2 120.1(11) . . ? C4 C3 C7 120.4(12) . . ? C2 C3 C7 119.5(11) . . ? C3 C4 C5 119.4(12) . . ? C4 C5 C6 120.1(10) . . ? C4 C5 C8 118.6(11) . . ? C6 C5 C8 121.3(10) . . ? C1 C6 C5 121.9(11) . . ? O4 C7 O5 122.0(12) . . ? O4 C7 C3 119.7(13) . . ? O5 C7 C3 118.1(14) . . ? O4 C7 Zn1 50.1(7) . 16_444 ? O5 C7 Zn1 72.0(7) . 16_444 ? C3 C7 Zn1 167.6(12) . 16_444 ? O6 C8 O7 125.2(11) . . ? O6 C8 C5 117.6(11) . . ? O7 C8 C5 116.9(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.918 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.199