# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chen, Zhenxia' _publ_contact_author_email ymzhou@fudan.edu.cn _publ_section_title ; Two-step synthesis, structure and adsorption property of a dynamic zinc phosphonocarboxylate framework ; loop_ _publ_author_name 'Zhenxia Chen' 'Yaming Zhou' 'Yun Ling' 'Linhong Weng' # Attachment '- 1.cif' data_f61121b _database_code_depnum_ccdc_archive 'CCDC 776834' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H12 N2 O5 P Zn1.50' _chemical_formula_sum 'C17 H12 N2 O5 P Zn1.50' _chemical_formula_weight 453.31 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.330(5) _cell_length_b 13.962(5) _cell_length_c 17.424(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.347(4) _cell_angle_gamma 90.00 _cell_volume 3449(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1021 _cell_measurement_theta_min 2.873 _cell_measurement_theta_max 26.868 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 2.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8079 _exptl_absorpt_correction_T_max 0.8419 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 7689 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3399 _reflns_number_gt 2854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3399 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 0.926757(17) 0.392409(17) 0.429868(14) 0.02417(9) Uani 1 1 d . . . Zn2 Zn 1.0000 0.54034(2) 0.2500 0.02243(10) Uani 1 2 d S . . P1 P 0.94293(4) 0.62369(4) 0.40501(3) 0.02256(13) Uani 1 1 d . . . O1 O 1.00291(11) 0.66118(12) 0.47775(9) 0.0344(4) Uani 1 1 d . . . O2 O 0.89969(12) 0.52703(11) 0.41598(10) 0.0341(4) Uani 1 1 d . . . O3 O 0.99572(11) 0.62886(10) 0.33546(9) 0.0290(4) Uani 1 1 d . . . O4 O 0.61662(11) 0.96404(11) 0.27898(10) 0.0309(4) Uani 1 1 d . . . O5 O 0.53907(12) 0.88791(11) 0.36123(11) 0.0392(4) Uani 1 1 d . . . C1 C 0.84574(15) 0.70741(15) 0.38476(12) 0.0242(5) Uani 1 1 d . . . C2 C 0.85267(16) 0.78790(16) 0.33837(14) 0.0318(5) Uani 1 1 d . . . H2 H 0.9098 0.7999 0.3184 0.038 Uiso 1 1 calc R . . C3 C 0.77754(16) 0.85050(16) 0.32098(14) 0.0308(5) Uani 1 1 d . . . H3 H 0.7833 0.9041 0.2885 0.037 Uiso 1 1 calc R . . C4 C 0.69393(15) 0.83556(16) 0.35066(12) 0.0256(5) Uani 1 1 d . . . C5 C 0.68683(17) 0.75688(17) 0.39829(13) 0.0317(5) Uani 1 1 d . . . H5 H 0.6306 0.7464 0.4200 0.038 Uiso 1 1 calc R . . C6 C 0.76175(17) 0.69363(17) 0.41413(13) 0.0318(5) Uani 1 1 d . . . H6 H 0.7554 0.6394 0.4459 0.038 Uiso 1 1 calc R . . C7 C 0.61042(16) 0.90069(15) 0.32992(13) 0.0260(5) Uani 1 1 d . . . N1 N 0.86464(13) 0.27637(14) 0.36484(11) 0.0292(4) Uani 1 1 d . . . N2 N 0.78349(14) 0.38550(13) 0.46005(12) 0.0322(5) Uani 1 1 d . . . C8 C 0.91112(19) 0.21837(18) 0.32234(15) 0.0390(6) Uani 1 1 d . . . H8 H 0.9760 0.2304 0.3204 0.047 Uiso 1 1 calc R . . C9 C 0.8684(2) 0.14185(19) 0.28119(16) 0.0457(7) Uani 1 1 d . . . H9 H 0.9033 0.1026 0.2510 0.055 Uiso 1 1 calc R . . C10 C 0.7760(2) 0.12326(18) 0.28436(16) 0.0455(7) Uani 1 1 d . . . H10 H 0.7453 0.0712 0.2560 0.055 Uiso 1 1 calc R . . C11 C 0.72735(19) 0.18034(18) 0.32890(16) 0.0407(6) Uani 1 1 d . . . H11 H 0.6630 0.1675 0.3324 0.049 Uiso 1 1 calc R . . C12 C 0.77345(16) 0.25764(16) 0.36909(14) 0.0317(5) Uani 1 1 d . . . C13 C 0.72671(16) 0.32321(17) 0.41780(14) 0.0327(5) Uani 1 1 d . . . C14 C 0.63055(19) 0.3210(2) 0.42139(18) 0.0495(7) Uani 1 1 d . . . H14 H 0.5908 0.2764 0.3912 0.059 Uiso 1 1 calc R . . C15 C 0.5940(2) 0.3841(2) 0.4691(2) 0.0613(9) Uani 1 1 d . . . H15 H 0.5285 0.3832 0.4728 0.074 Uiso 1 1 calc R . . C16 C 0.6526(2) 0.4492(2) 0.51204(19) 0.0537(8) Uani 1 1 d . . . H16 H 0.6283 0.4941 0.5450 0.064 Uiso 1 1 calc R . . C17 C 0.7471(2) 0.44720(19) 0.50567(16) 0.0424(6) Uani 1 1 d . . . H17 H 0.7880 0.4916 0.5350 0.051 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 0.02074(15) 0.02188(14) 0.02788(15) 0.00127(10) -0.00326(10) -0.00089(10) Zn2 0.01800(19) 0.02010(18) 0.02775(19) 0.000 -0.00154(14) 0.000 P1 0.0196(3) 0.0201(3) 0.0265(3) 0.0009(2) -0.0018(2) 0.0028(2) O1 0.0349(10) 0.0346(9) 0.0292(9) 0.0007(7) -0.0099(7) 0.0018(8) O2 0.0295(9) 0.0201(7) 0.0534(11) 0.0034(7) 0.0084(8) 0.0029(7) O3 0.0297(9) 0.0249(8) 0.0327(9) -0.0039(6) 0.0051(7) -0.0002(7) O4 0.0212(8) 0.0274(8) 0.0426(10) 0.0079(7) -0.0002(7) 0.0066(7) O5 0.0284(10) 0.0398(10) 0.0520(11) 0.0057(8) 0.0139(8) 0.0086(8) C1 0.0237(11) 0.0235(11) 0.0235(11) -0.0017(8) -0.0028(8) 0.0043(9) C2 0.0219(12) 0.0293(12) 0.0445(14) 0.0081(10) 0.0056(10) 0.0027(10) C3 0.0263(12) 0.0246(11) 0.0416(14) 0.0096(10) 0.0052(10) 0.0046(10) C4 0.0225(11) 0.0255(11) 0.0274(11) -0.0016(9) -0.0017(9) 0.0022(9) C5 0.0280(12) 0.0363(13) 0.0317(12) 0.0070(10) 0.0076(10) 0.0056(10) C6 0.0315(13) 0.0323(12) 0.0314(12) 0.0106(10) 0.0042(10) 0.0083(10) C7 0.0206(12) 0.0247(11) 0.0311(12) -0.0048(9) -0.0009(9) 0.0005(9) N1 0.0254(10) 0.0302(10) 0.0304(10) 0.0016(8) -0.0016(8) -0.0061(8) N2 0.0280(11) 0.0291(10) 0.0386(11) 0.0058(9) 0.0017(9) -0.0024(8) C8 0.0353(14) 0.0396(14) 0.0422(14) -0.0044(12) 0.0053(11) -0.0061(12) C9 0.0536(18) 0.0369(14) 0.0462(16) -0.0062(12) 0.0065(13) -0.0060(14) C10 0.0560(19) 0.0313(13) 0.0444(16) 0.0004(11) -0.0087(13) -0.0124(13) C11 0.0334(14) 0.0354(13) 0.0498(15) 0.0059(12) -0.0063(11) -0.0123(12) C12 0.0285(12) 0.0303(12) 0.0336(13) 0.0098(10) -0.0046(10) -0.0056(10) C13 0.0240(12) 0.0306(12) 0.0417(13) 0.0112(11) -0.0008(10) -0.0039(10) C14 0.0274(14) 0.0507(16) 0.0695(19) 0.0022(15) 0.0043(13) -0.0093(13) C15 0.0322(16) 0.069(2) 0.086(3) 0.0069(18) 0.0178(16) 0.0013(15) C16 0.0494(18) 0.0552(18) 0.0606(19) 0.0068(15) 0.0213(15) 0.0113(15) C17 0.0455(16) 0.0381(14) 0.0449(15) 0.0032(12) 0.0104(12) 0.0005(12) _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 1.9225(16) 5_766 ? Zn1 O2 1.9273(16) . ? Zn1 N1 2.100(2) . ? Zn1 O5 2.1409(18) 3_545 ? Zn1 N2 2.194(2) . ? Zn2 O3 1.9430(16) . ? Zn2 O3 1.9430(16) 2_755 ? Zn2 O4 1.9844(16) 4_645 ? Zn2 O4 1.9844(16) 3_545 ? P1 O2 1.5088(17) . ? P1 O1 1.5174(16) . ? P1 O3 1.5208(17) . ? P1 C1 1.813(2) . ? O1 Zn1 1.9225(16) 5_766 ? O4 C7 1.265(3) . ? O4 Zn2 1.9844(16) 3_455 ? O5 C7 1.240(3) . ? O5 Zn1 2.1409(18) 3_455 ? C1 C6 1.388(3) . ? C1 C2 1.396(3) . ? C2 C3 1.386(3) . ? C2 H2 0.9500 . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 C7 1.505(3) . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N1 C8 1.338(3) . ? N1 C12 1.345(3) . ? N2 C17 1.329(3) . ? N2 C13 1.337(3) . ? C8 C9 1.379(4) . ? C8 H8 0.9500 . ? C9 C10 1.359(4) . ? C9 H9 0.9500 . ? C10 C11 1.371(4) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 C13 1.474(4) . ? C13 C14 1.389(3) . ? C14 C15 1.367(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(5) . ? C15 H15 0.9500 . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? 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 O2 123.79(8) 5_766 . ? O1 Zn1 N1 106.33(7) 5_766 . ? O2 Zn1 N1 128.53(8) . . ? O1 Zn1 O5 96.37(7) 5_766 3_545 ? O2 Zn1 O5 96.45(6) . 3_545 ? N1 Zn1 O5 88.28(7) . 3_545 ? O1 Zn1 N2 100.21(7) 5_766 . ? O2 Zn1 N2 83.95(7) . . ? N1 Zn1 N2 75.96(8) . . ? O5 Zn1 N2 159.73(8) 3_545 . ? O3 Zn2 O3 100.99(10) . 2_755 ? O3 Zn2 O4 114.67(7) . 4_645 ? O3 Zn2 O4 105.40(7) 2_755 4_645 ? O3 Zn2 O4 105.40(7) . 3_545 ? O3 Zn2 O4 114.67(7) 2_755 3_545 ? O4 Zn2 O4 115.07(9) 4_645 3_545 ? O2 P1 O1 113.33(10) . . ? O2 P1 O3 113.85(9) . . ? O1 P1 O3 111.24(10) . . ? O2 P1 C1 106.46(10) . . ? O1 P1 C1 105.43(10) . . ? O3 P1 C1 105.74(9) . . ? P1 O1 Zn1 136.86(11) . 5_766 ? P1 O2 Zn1 144.04(11) . . ? P1 O3 Zn2 130.94(9) . . ? C7 O4 Zn2 114.30(14) . 3_455 ? C7 O5 Zn1 167.57(17) . 3_455 ? C6 C1 C2 117.6(2) . . ? C6 C1 P1 121.44(17) . . ? C2 C1 P1 120.95(17) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.6(2) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 C7 121.3(2) . . ? C5 C4 C7 119.8(2) . . ? C6 C5 C4 120.0(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 121.7(2) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O5 C7 O4 123.8(2) . . ? O5 C7 C4 119.0(2) . . ? O4 C7 C4 117.17(19) . . ? C8 N1 C12 118.6(2) . . ? C8 N1 Zn1 124.03(16) . . ? C12 N1 Zn1 117.35(16) . . ? C17 N2 C13 119.4(2) . . ? C17 N2 Zn1 125.22(18) . . ? C13 N2 Zn1 114.36(16) . . ? N1 C8 C9 122.5(2) . . ? N1 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N1 C12 C11 121.0(2) . . ? N1 C12 C13 115.9(2) . . ? C11 C12 C13 123.1(2) . . ? N2 C13 C14 121.2(2) . . ? N2 C13 C12 115.5(2) . . ? C14 C13 C12 123.3(2) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 118.1(3) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? N2 C17 C16 122.5(3) . . ? N2 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.419 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.095 # Attachment '- 2.cif' data_a00426e _database_code_depnum_ccdc_archive 'CCDC 777257' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H9.50 N0.50 O5.50 P Zn' _chemical_formula_weight 297.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.804(6) _cell_length_b 19.340(12) _cell_length_c 10.242(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.51(5) _cell_angle_gamma 90.00 _cell_volume 3069(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 851 _cell_measurement_theta_min 2.153 _cell_measurement_theta_max 20.001 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7262 _exptl_absorpt_correction_T_max 0.8754 _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 6447 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2669 _reflns_number_gt 2111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2669 _refine_ls_number_parameters 156 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1991 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.61068(4) 0.55091(3) 0.47772(7) 0.0306(3) Uani 1 1 d . . . P1 P 0.40667(9) 0.57122(6) 0.34552(16) 0.0291(4) Uani 1 1 d . . . O1 O 0.5006(2) 0.58139(19) 0.4573(5) 0.0456(11) Uani 1 1 d . . . O2 O 0.3915(3) 0.53038(19) 0.2081(5) 0.0441(10) Uani 1 1 d . . . O3 O 0.3584(3) 0.53791(19) 0.4175(5) 0.0425(10) Uani 1 1 d . . . O4 O 0.3031(4) 0.9092(3) 0.1356(8) 0.092(2) Uani 1 1 d . . . O5 O 0.1759(3) 0.8672(2) 0.0854(6) 0.0607(13) Uani 1 1 d . . . C1 C 0.3626(3) 0.6576(2) 0.2892(6) 0.0320(12) Uani 1 1 d . . . C2 C 0.4154(4) 0.7136(3) 0.3126(9) 0.0488(16) Uani 1 1 d . . . H2 H 0.4750 0.7077 0.3637 0.059 Uiso 1 1 calc R . . C3 C 0.3804(4) 0.7804(3) 0.2597(8) 0.0560(18) Uani 1 1 d . . . H3 H 0.4167 0.8174 0.2718 0.067 Uiso 1 1 calc R . . C4 C 0.2940(4) 0.7900(3) 0.1916(7) 0.0425(14) Uani 1 1 d . . . C5 C 0.2410(4) 0.7355(3) 0.1706(8) 0.0488(16) Uani 1 1 d . . . H5 H 0.1817 0.7426 0.1242 0.059 Uiso 1 1 calc R . . C6 C 0.2748(4) 0.6682(3) 0.2184(8) 0.0470(15) Uani 1 1 d . . . H6 H 0.2377 0.6312 0.2019 0.056 Uiso 1 1 calc R . . C7 C 0.2563(5) 0.8616(3) 0.1352(8) 0.0532(17) Uani 1 1 d . . . C8 C 0.5835(10) 0.6528(10) 0.7996(17) 0.187(7) Uani 1 1 d U . . H8A H 0.6279 0.6188 0.8252 0.280 Uiso 1 1 calc R . . H8B H 0.5973 0.6809 0.8858 0.280 Uiso 1 1 calc R . . H8C H 0.5796 0.6815 0.7199 0.280 Uiso 1 1 calc R . . O6 O 0.9430(17) 0.5901(14) 0.570(4) 0.116(11) Uani 0.25 1 d P . . O7 O 0.805(2) 0.472(2) 0.434(4) 0.141(12) Uani 0.25 1 d PU . . N1 N 0.5000 0.6177(9) 0.7500 0.148(6) Uiso 1 2 d S . . H1 H 0.4920 0.5898 0.6739 0.177 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 0.0417(5) 0.0196(4) 0.0298(5) -0.0008(2) 0.0171(3) -0.0033(2) P1 0.0413(8) 0.0200(7) 0.0300(8) 0.0040(5) 0.0206(6) 0.0061(5) O1 0.042(2) 0.029(2) 0.055(3) 0.0003(19) 0.015(2) 0.0092(16) O2 0.073(3) 0.0262(19) 0.039(2) 0.0021(18) 0.033(2) 0.0091(19) O3 0.064(3) 0.0292(19) 0.051(3) 0.0165(18) 0.042(2) 0.0153(18) O4 0.087(4) 0.035(3) 0.130(6) 0.026(3) 0.036(4) 0.006(3) O5 0.083(3) 0.039(2) 0.065(3) 0.025(2) 0.041(3) 0.032(2) C1 0.046(3) 0.021(2) 0.034(3) 0.003(2) 0.024(2) 0.006(2) C2 0.042(3) 0.030(3) 0.071(5) 0.011(3) 0.025(3) 0.005(2) C3 0.058(4) 0.027(3) 0.077(5) 0.015(3) 0.028(4) 0.003(3) C4 0.059(4) 0.026(3) 0.042(4) 0.007(2) 0.025(3) 0.012(2) C5 0.044(3) 0.033(3) 0.066(5) 0.010(3) 0.025(3) 0.015(2) C6 0.043(3) 0.032(3) 0.063(4) 0.008(3) 0.023(3) 0.002(2) C7 0.074(5) 0.031(3) 0.052(4) 0.013(3) 0.029(4) 0.020(3) C8 0.209(15) 0.210(15) 0.179(14) 0.011(11) 0.125(12) 0.049(11) O6 0.094(18) 0.10(2) 0.19(3) -0.06(2) 0.10(2) -0.034(15) O7 0.114(17) 0.144(18) 0.144(19) -0.068(14) 0.048(13) 0.043(13) _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 O2 1.926(4) 2_655 ? Zn1 O5 1.953(4) 8_566 ? Zn1 O3 1.955(4) 5_666 ? Zn1 O1 1.957(4) . ? P1 O1 1.503(4) . ? P1 O2 1.518(4) . ? P1 O3 1.523(4) . ? P1 C1 1.814(5) . ? O2 Zn1 1.926(4) 2_655 ? O3 Zn1 1.955(4) 5_666 ? O4 C7 1.241(8) . ? O5 C7 1.265(8) . ? O5 Zn1 1.953(4) 8_465 ? C1 C6 1.376(8) . ? C1 C2 1.377(8) . ? C2 C3 1.421(8) . ? C2 H2 0.9300 . ? C3 C4 1.353(9) . ? C3 H3 0.9300 . ? C4 C5 1.358(9) . ? C4 C7 1.523(8) . ? C5 C6 1.417(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 N1 1.478(17) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 C8 1.478(17) 2_656 ? N1 H1 0.8999 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O5 116.23(19) 2_655 8_566 ? O2 Zn1 O3 102.96(18) 2_655 5_666 ? O5 Zn1 O3 118.3(2) 8_566 5_666 ? O2 Zn1 O1 115.17(19) 2_655 . ? O5 Zn1 O1 95.85(19) 8_566 . ? O3 Zn1 O1 108.64(17) 5_666 . ? O1 P1 O2 113.4(2) . . ? O1 P1 O3 111.6(3) . . ? O2 P1 O3 110.1(3) . . ? O1 P1 C1 105.4(2) . . ? O2 P1 C1 109.4(2) . . ? O3 P1 C1 106.5(2) . . ? P1 O1 Zn1 136.2(3) . . ? P1 O2 Zn1 135.8(3) . 2_655 ? P1 O3 Zn1 124.3(2) . 5_666 ? C7 O5 Zn1 122.5(4) . 8_465 ? C6 C1 C2 118.4(5) . . ? C6 C1 P1 120.4(4) . . ? C2 C1 P1 121.2(4) . . ? C1 C2 C3 121.0(6) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 C7 119.7(6) . . ? C5 C4 C7 120.2(6) . . ? C4 C5 C6 120.9(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.9(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? O4 C7 O5 124.2(6) . . ? O4 C7 C4 120.3(6) . . ? O5 C7 C4 115.4(6) . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8 N1 C8 125(2) . 2_656 ? C8 N1 H1 106.0 . . ? C8 N1 H1 105.9 2_656 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.90 2.30 3.084(7) 145.0 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.403 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.218 # Attachment '- 2a.cif' data_a00911a _database_code_depnum_ccdc_archive 'CCDC 794593' #TrackingRef '- 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10.50 H19.50 N1.50 O7.50 P Zn' _chemical_formula_weight 383.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.372(8) _cell_length_b 19.143(8) _cell_length_c 10.534(5) _cell_angle_alpha 90.00 _cell_angle_beta 124.353(10) _cell_angle_gamma 90.00 _cell_volume 3059(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 957 _cell_measurement_theta_min 3.165 _cell_measurement_theta_max 27.007 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6693 _exptl_absorpt_correction_T_max 0.7797 _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 6145 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2686 _reflns_number_gt 2166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0724P)^2^+3.5286P] 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 2686 _refine_ls_number_parameters 209 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.093 _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 0.60731(3) 0.55123(2) 0.49305(5) 0.02652(18) Uani 1 1 d . . . P1 P 0.39324(6) 0.56333(5) 0.30395(11) 0.0260(2) Uani 1 1 d . . . O1 O 0.48964(16) 0.57263(14) 0.4161(3) 0.0366(7) Uani 1 1 d . . . O2 O 0.36965(17) 0.52680(14) 0.1583(3) 0.0327(6) Uani 1 1 d . . . O3 O 0.34940(16) 0.52721(14) 0.3706(3) 0.0306(6) Uani 1 1 d . . . O4 O 0.29414(19) 0.90542(15) 0.1631(3) 0.0448(8) Uani 1 1 d . . . O5 O 0.16642(18) 0.86179(14) 0.0905(3) 0.0385(7) Uani 1 1 d . . . C1 C 0.3486(2) 0.64982(19) 0.2559(4) 0.0278(8) Uani 1 1 d . . . C2 C 0.4033(3) 0.7059(2) 0.2879(6) 0.0488(12) Uani 1 1 d . . . H2 H 0.4632 0.6986 0.3343 0.059 Uiso 1 1 calc R . . C3 C 0.3702(3) 0.7719(2) 0.2523(6) 0.0504(12) Uani 1 1 d . . . H3 H 0.4078 0.8093 0.2738 0.060 Uiso 1 1 calc R . . C4 C 0.2824(2) 0.78383(19) 0.1852(4) 0.0296(8) Uani 1 1 d . . . C5 C 0.2283(2) 0.7285(2) 0.1517(5) 0.0327(9) Uani 1 1 d . . . H5 H 0.1682 0.7359 0.1043 0.039 Uiso 1 1 calc R . . C6 C 0.2609(2) 0.6620(2) 0.1867(5) 0.0318(9) Uani 1 1 d . . . H6 H 0.2229 0.6247 0.1629 0.038 Uiso 1 1 calc R . . C7 C 0.2466(3) 0.8560(2) 0.1443(4) 0.0321(9) Uani 1 1 d . . . N1 N 0.2167(4) 0.4481(2) -0.0386(6) 0.0682(14) Uani 1 1 d . . . H1A H 0.2631 0.4772 0.0002 0.082 Uiso 1 1 calc R . . H1B H 0.1863 0.4504 -0.1418 0.082 Uiso 1 1 calc R . . C9 C 0.1618(4) 0.4718(4) 0.0073(7) 0.0717(16) Uani 1 1 d . . . H9A H 0.1435 0.5189 -0.0275 0.107 Uiso 1 1 calc R . . H9B H 0.1938 0.4703 0.1174 0.107 Uiso 1 1 calc R . . H9C H 0.1108 0.4423 -0.0369 0.107 Uiso 1 1 calc R . . C8 C 0.2490(4) 0.3779(4) 0.0096(7) 0.0767(17) Uani 1 1 d . . . H8A H 0.2856 0.3656 -0.0253 0.115 Uiso 1 1 calc R . . H8B H 0.2001 0.3462 -0.0336 0.115 Uiso 1 1 calc R . . H8C H 0.2828 0.3752 0.1197 0.115 Uiso 1 1 calc R . . O7 O 0.0730(3) 0.5876(3) 0.1483(5) 0.0980(15) Uani 1 1 d . . . H7A H 0.0388 0.5914 0.0495 0.147 Uiso 1 1 d R . . H7B H 0.0516 0.6159 0.1808 0.147 Uiso 1 1 d R . . O8 O 0.4653(3) 0.9375(2) 0.3413(5) 0.0858(14) Uani 1 1 d . . . H8D H 0.4676 0.9817 0.3300 0.129 Uiso 1 1 d R . . H8E H 0.4904 0.9064 0.3211 0.129 Uiso 1 1 d R . . N2 N 0.9610(7) 0.7603(7) 0.2939(13) 0.142(7) Uani 0.50 1 d PD . . O9 O 1.0000 0.8732(5) 0.2500 0.172(4) Uani 1 2 d SD . . C10 C 0.886(2) 0.7720(16) 0.272(7) 0.43(4) Uani 0.50 1 d PDU . . C11 C 0.9753(9) 0.6893(5) 0.2625(16) 0.074(4) Uani 0.50 1 d PD . . C12 C 1.0000 0.8011(3) 0.2500 0.0418(14) Uani 1 2 d SD . . 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 0.0203(3) 0.0226(3) 0.0272(3) 0.00111(16) 0.0077(2) -0.00045(15) P1 0.0200(5) 0.0239(5) 0.0262(5) 0.0027(4) 0.0083(4) 0.0037(3) O1 0.0205(13) 0.0341(15) 0.0401(16) 0.0020(12) 0.0079(12) 0.0052(11) O2 0.0377(15) 0.0276(14) 0.0307(15) -0.0006(11) 0.0180(13) -0.0001(12) O3 0.0278(13) 0.0279(13) 0.0324(14) 0.0076(11) 0.0148(12) 0.0056(11) O4 0.0411(17) 0.0290(16) 0.0482(19) 0.0041(13) 0.0155(15) 0.0043(13) O5 0.0352(16) 0.0301(14) 0.0418(17) 0.0093(12) 0.0167(13) 0.0128(12) C1 0.0262(18) 0.0241(18) 0.0284(19) 0.0035(15) 0.0125(16) 0.0046(14) C2 0.022(2) 0.031(2) 0.074(3) 0.005(2) 0.016(2) 0.0052(16) C3 0.035(2) 0.028(2) 0.074(3) 0.002(2) 0.022(2) -0.0022(17) C4 0.033(2) 0.0270(19) 0.0268(19) 0.0040(15) 0.0155(17) 0.0068(15) C5 0.0240(19) 0.031(2) 0.040(2) 0.0040(17) 0.0162(18) 0.0073(15) C6 0.0274(19) 0.027(2) 0.037(2) 0.0029(16) 0.0157(17) -0.0003(15) C7 0.036(2) 0.030(2) 0.024(2) 0.0029(16) 0.0127(18) 0.0069(17) N1 0.085(4) 0.060(3) 0.061(3) -0.002(2) 0.042(3) -0.022(2) C9 0.057(3) 0.089(4) 0.059(4) 0.001(3) 0.027(3) -0.007(3) C8 0.070(4) 0.092(5) 0.058(4) 0.006(3) 0.030(3) -0.003(3) O7 0.069(3) 0.120(4) 0.074(3) 0.017(3) 0.022(2) -0.010(3) O8 0.063(3) 0.084(3) 0.076(3) 0.005(2) 0.018(2) -0.018(2) N2 0.073(8) 0.212(17) 0.067(8) 0.071(9) -0.006(6) -0.074(9) O9 0.182(10) 0.116(8) 0.174(10) 0.000 0.074(8) 0.000 C10 0.43(4) 0.42(4) 0.42(4) 0.003(10) 0.24(2) 0.000(10) C11 0.097(11) 0.039(5) 0.081(8) 0.014(6) 0.047(8) -0.027(6) C12 0.044(3) 0.037(3) 0.041(3) 0.000 0.022(3) 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 1.876(3) . ? Zn1 O3 1.913(3) 5_666 ? Zn1 O2 1.924(3) 2_655 ? Zn1 O5 1.936(3) 8_566 ? P1 O1 1.484(3) . ? P1 O3 1.502(3) . ? P1 O2 1.510(3) . ? P1 C1 1.789(4) . ? O2 Zn1 1.924(3) 2_655 ? O3 Zn1 1.913(3) 5_666 ? O4 C7 1.227(5) . ? O5 C7 1.249(5) . ? O5 Zn1 1.936(3) 8_465 ? C1 C6 1.362(5) . ? C1 C2 1.376(6) . ? C2 C3 1.359(6) . ? C2 H2 0.9300 . ? C3 C4 1.366(6) . ? C3 H3 0.9300 . ? C4 C5 1.357(6) . ? C4 C7 1.485(5) . ? C5 C6 1.366(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N1 C9 1.417(7) . ? N1 C8 1.441(7) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O7 H7A 0.8635 . ? O7 H7B 0.8465 . ? O8 H8D 0.8577 . ? O8 H8E 0.8504 . ? N2 C10 1.281(16) . ? N2 C12 1.308(9) . ? N2 C11 1.457(15) . ? O9 C12 1.380(10) . ? C11 C11 1.08(2) 2_755 ? C12 N2 1.308(10) 2_755 ? 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 112.66(12) . 5_666 ? O1 Zn1 O2 115.69(12) . 2_655 ? O3 Zn1 O2 103.82(12) 5_666 2_655 ? O1 Zn1 O5 101.89(12) . 8_566 ? O3 Zn1 O5 113.93(13) 5_666 8_566 ? O2 Zn1 O5 109.19(12) 2_655 8_566 ? O1 P1 O3 113.39(17) . . ? O1 P1 O2 113.18(17) . . ? O3 P1 O2 109.83(16) . . ? O1 P1 C1 105.35(17) . . ? O3 P1 C1 106.08(16) . . ? O2 P1 C1 108.56(16) . . ? P1 O1 Zn1 152.2(2) . . ? P1 O2 Zn1 131.16(17) . 2_655 ? P1 O3 Zn1 127.35(15) . 5_666 ? C7 O5 Zn1 118.8(3) . 8_465 ? C6 C1 C2 118.5(3) . . ? C6 C1 P1 121.7(3) . . ? C2 C1 P1 119.9(3) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 C7 120.7(3) . . ? C3 C4 C7 120.5(4) . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 120.7(4) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? O4 C7 O5 123.7(4) . . ? O4 C7 C4 120.8(4) . . ? O5 C7 C4 115.5(4) . . ? C9 N1 C8 114.1(5) . . ? C9 N1 H1A 108.7 . . ? C8 N1 H1A 108.7 . . ? C9 N1 H1B 108.7 . . ? C8 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H7A O7 H7B 104.1 . . ? H8D O8 H8E 125.3 . . ? C10 N2 C12 125.4(18) . . ? C10 N2 C11 115.9(17) . . ? C12 N2 C11 105.8(11) . . ? C11 C11 N2 109.9(6) 2_755 . ? N2 C12 N2 106.6(15) 2_755 . ? N2 C12 O9 126.7(8) 2_755 . ? N2 C12 O9 126.7(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O7 0.90 2.13 2.913(7) 144.4 6_565 N1 H1A O3 0.90 2.61 3.116(6) 116.1 6_565 N1 H1A O2 0.90 1.96 2.808(6) 157.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.019 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.105