# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xintao Wu' _publ_contact_author_email WXT@FJIRSM.AC.CN _publ_section_title ; Syntheses, crystal structures, thermal stabilities and luminescence of two new zinc phosphonates ; loop_ _publ_author_name 'Xintao Wu.' 'Ruibiao Fu.' 'Sheng-min Hu.' # Attachment 'crystal-data-1.CIF' data_f1 _database_code_depnum_ccdc_archive 'CCDC 691730' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10.50 H24 N O28 P4 Zn5' _chemical_formula_weight 1063.04 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' 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1800(14) _cell_length_b 11.0600(16) _cell_length_c 14.0137(15) _cell_angle_alpha 68.297(4) _cell_angle_beta 78.859(5) _cell_angle_gamma 72.300(7) _cell_volume 1390.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3892 _cell_measurement_theta_min 2.0487 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 4.603 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5231 _exptl_absorpt_correction_T_max 1.0000 _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 'Rotating Anode' _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 10113 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6155 _reflns_number_gt 5154 _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^)+(0.0384P)^2^+0.7557P] 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 6155 _refine_ls_number_parameters 519 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.07753(3) -0.14624(3) -0.08602(2) 0.01052(9) Uani 1 1 d . . . Zn2 Zn -0.07846(3) -0.35199(3) 0.08304(2) 0.01113(9) Uani 1 1 d . . . Zn3 Zn -0.37564(3) -0.01330(3) -0.17730(2) 0.01258(9) Uani 1 1 d . . . Zn4 Zn 0.02476(12) 0.22077(11) -0.51149(10) 0.01121(17) Uani 0.75 1 d P . . Zn4A Zn 0.0056(5) 0.2425(5) -0.5039(3) 0.0705(18) Uani 0.25 1 d P . . Zn5 Zn 0.38149(3) 0.50945(3) -0.82359(2) 0.01268(9) Uani 1 1 d . . . P1 P 0.22506(7) -0.46867(7) -0.01775(5) 0.00877(15) Uani 1 1 d . . . P2 P -0.22200(7) -0.03026(7) 0.01563(5) 0.00916(15) Uani 1 1 d . . . P3 P -0.15964(7) 0.01356(7) -0.38524(6) 0.01232(16) Uani 1 1 d . . . P4 P 0.15665(8) 0.47441(7) -0.62009(6) 0.01349(16) Uani 1 1 d . . . O1W O -0.3144(3) -0.2111(2) -0.1581(2) 0.0250(6) Uani 1 1 d . . . H18 H -0.365(5) -0.238(5) -0.160(4) 0.048(16) Uiso 1 1 d . . . H19 H -0.257(5) -0.269(5) -0.114(4) 0.048(13) Uiso 1 1 d . . . O1 O 0.3342(2) -0.4942(2) 0.05102(17) 0.0190(5) Uani 1 1 d . . . O2 O 0.1813(2) -0.59497(19) -0.00086(15) 0.0130(4) Uani 1 1 d . . . O2W O 0.3146(3) 0.7069(2) -0.8402(2) 0.0243(5) Uani 1 1 d . . . H20 H 0.379(5) 0.738(5) -0.837(4) 0.057(15) Uiso 1 1 d . . . H21 H 0.269(4) 0.750(4) -0.874(3) 0.023(12) Uiso 1 1 d . . . O3 O 0.1015(2) -0.34952(19) -0.01357(15) 0.0129(4) Uani 1 1 d . . . O3W O 0.4192(4) 0.6266(4) -0.6090(3) 0.0586(10) Uani 1 1 d D . . H22 H 0.507(5) 0.559(7) -0.611(5) 0.18(4) Uiso 1 1 d D . . H23 H 0.418(4) 0.642(4) -0.547(2) 0.028(10) Uiso 1 1 d D . . O4 O 0.5842(2) 0.5232(2) -0.83028(19) 0.0197(5) Uani 1 1 d . . . H15 H 0.611(5) 0.584(5) -0.838(4) 0.053(15) Uiso 1 1 d . . . O4W O 0.3788(4) 0.6683(4) -0.4146(3) 0.0692(11) Uani 1 1 d D . . H24 H 0.455(7) 0.593(7) -0.425(8) 0.20(5) Uiso 1 1 d D . . H25 H 0.301(7) 0.630(10) -0.396(13) 0.43(10) Uiso 1 1 d D . . O5 O 0.5111(2) 0.30865(19) -0.79784(16) 0.0152(4) Uani 1 1 d . . . O6 O 0.2780(2) -0.18695(19) -0.17230(16) 0.0157(4) Uani 1 1 d . . . O7 O -0.0996(2) -0.15040(18) 0.01260(15) 0.0125(4) Uani 1 1 d . . . O8 O -0.1776(2) 0.09497(19) 0.00075(15) 0.0127(4) Uani 1 1 d . . . O9 O -0.3285(2) -0.0027(2) -0.05536(17) 0.0209(5) Uani 1 1 d . . . O10 O -0.5808(2) -0.0300(2) -0.15960(18) 0.0189(5) Uani 1 1 d . . . H13 H -0.617(5) -0.082(4) -0.155(3) 0.042(13) Uiso 1 1 d . . . O11 O -0.5088(2) 0.1866(2) -0.19989(17) 0.0175(4) Uani 1 1 d . . . O12 O -0.2805(2) -0.3098(2) 0.17054(17) 0.0171(4) Uani 1 1 d . . . O13 O -0.2868(2) 0.0543(2) -0.31540(16) 0.0196(5) Uani 1 1 d . . . O14 O -0.1725(2) -0.0974(2) -0.42081(16) 0.0183(5) Uani 1 1 d . . . O15 O -0.1320(2) 0.1346(2) -0.47591(16) 0.0181(5) Uani 1 1 d . . . O16 O -0.0238(2) -0.1596(2) -0.21489(17) 0.0183(5) Uani 1 1 d . . . H14 H -0.007(5) -0.218(5) -0.229(4) 0.051(16) Uiso 1 1 d . . . O17 O 0.0289(2) 0.0404(2) -0.19302(15) 0.0151(4) Uani 1 1 d . . . O18 O 0.0613(3) 0.1502(2) -0.35864(16) 0.0247(5) Uani 1 1 d . . . O19 O 0.1270(2) 0.3586(2) -0.52815(16) 0.0202(5) Uani 1 1 d . . . O20 O 0.1722(2) 0.5874(2) -0.58456(19) 0.0237(5) Uani 1 1 d . . . H17 H 0.259(6) 0.598(5) -0.606(4) 0.081(18) Uiso 1 1 d . . . O21 O 0.2801(2) 0.4346(2) -0.69124(16) 0.0209(5) Uani 1 1 d . . . O22 O 0.0161(2) -0.3402(2) 0.21726(18) 0.0217(5) Uani 1 1 d . . . H16 H 0.004(5) -0.287(4) 0.241(3) 0.039(13) Uiso 1 1 d . . . O23 O -0.0668(2) 0.3454(2) -0.64714(17) 0.0239(5) Uani 1 1 d . . . O24 O -0.0332(2) -0.5387(2) 0.18916(15) 0.0163(4) Uani 1 1 d . . . N1 N -0.4302(4) -0.1313(4) -0.4317(3) 0.0451(9) Uani 1 1 d . . . H6 H -0.4310 -0.2160 -0.3910 0.054 Uiso 1 1 calc R . . H5 H -0.3477 -0.1183 -0.4298 0.054 Uiso 1 1 calc R . . C1 C -0.3749(8) -0.1938(8) -0.5807(6) 0.0312(17) Uani 0.50 1 d P . . H1 H -0.3979 -0.1698 -0.6498 0.047 Uiso 0.50 1 calc PR . . H2 H -0.3879 -0.2816 -0.5409 0.047 Uiso 0.50 1 calc PR . . H3 H -0.2800 -0.1945 -0.5823 0.047 Uiso 0.50 1 calc PR . . C2 C -0.4496(6) -0.1119(5) -0.5417(4) 0.0612(16) Uani 1 1 d . . . H4 H -0.5431 -0.1220 -0.5379 0.073 Uiso 1 1 calc R . . C3 C -0.5422(6) -0.0351(5) -0.3929(3) 0.0550(13) Uani 1 1 d . . . H7 H -0.5279 -0.0485 -0.3228 0.066 Uiso 1 1 calc R . . H8 H -0.6299 -0.0539 -0.3910 0.066 Uiso 1 1 calc R . . C4 C 0.3050(3) -0.4171(3) -0.1508(2) 0.0106(5) Uani 1 1 d . . . H9 H 0.235(3) -0.387(3) -0.197(2) 0.008(7) Uiso 1 1 d . . . C5 C 0.6382(3) 0.2965(3) -0.8232(2) 0.0110(5) Uani 1 1 d . . . C6 C -0.3066(3) -0.0798(3) 0.1475(2) 0.0114(5) Uani 1 1 d . . . H10 H -0.241(3) -0.105(3) 0.197(2) 0.010(8) Uiso 1 1 d . . . C7 C -0.6355(3) 0.2000(3) -0.1739(2) 0.0109(5) Uani 1 1 d . . . C8 C -0.0058(3) -0.0565(3) -0.3103(2) 0.0120(6) Uani 1 1 d . . . H11 H 0.069(4) -0.088(3) -0.356(3) 0.022(9) Uiso 1 1 d . . . C9 C 0.0308(3) 0.0525(3) -0.2863(2) 0.0124(6) Uani 1 1 d . . . C10 C -0.0005(3) -0.4481(3) 0.3106(2) 0.0146(6) Uani 1 1 d . . . H12 H -0.078(4) -0.422(3) 0.358(3) 0.014(8) Uiso 1 1 d . . . C11 C -0.0361(3) -0.5544(3) 0.2823(2) 0.0131(6) 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 0.00869(16) 0.00978(17) 0.01125(17) -0.00213(13) 0.00043(12) -0.00229(12) Zn2 0.00955(17) 0.00973(17) 0.01201(17) -0.00188(13) 0.00054(13) -0.00262(12) Zn3 0.01220(17) 0.01372(18) 0.01206(17) -0.00428(13) -0.00095(13) -0.00378(12) Zn4 0.0113(3) 0.0125(3) 0.0094(4) -0.0045(3) 0.0016(2) -0.0029(2) Zn4A 0.062(3) 0.105(4) 0.032(2) 0.048(2) -0.037(2) -0.073(3) Zn5 0.01104(17) 0.01343(18) 0.01300(17) -0.00384(13) -0.00091(13) -0.00314(12) P1 0.0064(3) 0.0088(3) 0.0103(3) -0.0033(3) -0.0009(3) -0.0005(2) P2 0.0069(3) 0.0098(3) 0.0106(3) -0.0044(3) -0.0007(3) -0.0006(2) P3 0.0096(3) 0.0161(4) 0.0095(3) -0.0024(3) 0.0003(3) -0.0039(3) P4 0.0125(4) 0.0152(4) 0.0115(4) -0.0027(3) 0.0000(3) -0.0046(3) O1W 0.0260(14) 0.0108(11) 0.0371(15) -0.0016(10) -0.0163(12) -0.0029(10) O1 0.0147(11) 0.0239(12) 0.0205(11) -0.0093(9) -0.0086(9) -0.0011(8) O2 0.0145(10) 0.0105(10) 0.0136(10) -0.0023(8) -0.0035(8) -0.0035(7) O2W 0.0233(13) 0.0144(12) 0.0357(15) -0.0038(11) -0.0145(12) -0.0039(10) O3 0.0091(9) 0.0097(10) 0.0150(10) -0.0024(8) 0.0037(8) -0.0008(7) O3W 0.066(2) 0.081(3) 0.0417(19) -0.0082(18) -0.0033(17) -0.052(2) O4 0.0110(10) 0.0159(11) 0.0369(14) -0.0187(10) 0.0094(9) -0.0049(8) O4W 0.046(2) 0.097(3) 0.056(2) -0.011(2) -0.0103(18) -0.021(2) O5 0.0075(9) 0.0141(10) 0.0243(11) -0.0067(9) 0.0012(8) -0.0044(7) O6 0.0114(10) 0.0120(10) 0.0235(11) -0.0085(9) 0.0047(8) -0.0033(8) O7 0.0097(9) 0.0081(9) 0.0150(10) -0.0031(8) 0.0062(8) -0.0009(7) O8 0.0139(10) 0.0101(10) 0.0134(10) -0.0035(8) -0.0010(8) -0.0029(7) O9 0.0165(11) 0.0273(12) 0.0227(11) -0.0121(10) -0.0088(9) -0.0021(9) O10 0.0123(11) 0.0154(11) 0.0332(13) -0.0163(10) 0.0079(9) -0.0056(8) O11 0.0086(10) 0.0142(10) 0.0299(12) -0.0089(9) 0.0022(9) -0.0037(8) O12 0.0120(10) 0.0139(11) 0.0252(12) -0.0095(9) 0.0047(9) -0.0034(8) O13 0.0144(11) 0.0219(11) 0.0156(11) -0.0032(9) 0.0034(9) -0.0018(8) O14 0.0145(11) 0.0220(11) 0.0202(11) -0.0087(9) -0.0007(9) -0.0057(8) O15 0.0145(11) 0.0238(12) 0.0124(10) 0.0004(9) -0.0010(8) -0.0079(8) O16 0.0266(12) 0.0118(11) 0.0161(11) 0.0004(9) -0.0069(9) -0.0075(9) O17 0.0179(11) 0.0164(10) 0.0114(10) -0.0041(8) -0.0030(8) -0.0046(8) O18 0.0386(14) 0.0244(12) 0.0130(11) 0.0032(9) -0.0066(10) -0.0195(10) O19 0.0230(12) 0.0248(12) 0.0128(10) -0.0007(9) -0.0017(9) -0.0129(9) O20 0.0190(12) 0.0289(13) 0.0303(13) -0.0164(10) 0.0012(10) -0.0099(9) O21 0.0182(11) 0.0218(12) 0.0160(11) -0.0028(9) 0.0042(9) -0.0038(9) O22 0.0282(13) 0.0140(11) 0.0220(12) -0.0020(10) -0.0062(10) -0.0069(9) O23 0.0315(13) 0.0210(12) 0.0180(11) 0.0066(9) -0.0102(10) -0.0162(10) O24 0.0204(11) 0.0137(10) 0.0138(10) -0.0026(8) -0.0042(9) -0.0037(8) N1 0.050(2) 0.052(2) 0.0319(19) 0.0049(16) -0.0085(17) -0.0318(18) C1 0.029(4) 0.032(4) 0.035(4) -0.017(3) -0.012(3) 0.002(3) C2 0.100(4) 0.066(3) 0.035(2) 0.005(2) -0.029(3) -0.058(3) C3 0.071(3) 0.071(3) 0.028(2) 0.001(2) -0.009(2) -0.045(3) C4 0.0056(12) 0.0112(13) 0.0166(14) -0.0092(11) 0.0011(11) 0.0001(10) C5 0.0120(13) 0.0116(13) 0.0085(13) -0.0023(11) 0.0003(10) -0.0038(10) C6 0.0081(13) 0.0139(14) 0.0149(14) -0.0088(11) 0.0001(11) -0.0023(10) C7 0.0119(13) 0.0131(14) 0.0097(13) -0.0064(11) 0.0007(10) -0.0037(10) C8 0.0109(13) 0.0150(14) 0.0086(13) -0.0024(11) -0.0011(11) -0.0030(10) C9 0.0102(13) 0.0128(14) 0.0138(14) -0.0029(11) -0.0026(11) -0.0031(10) C10 0.0142(14) 0.0129(14) 0.0142(14) -0.0036(11) -0.0001(12) -0.0017(11) C11 0.0097(13) 0.0135(14) 0.0128(14) -0.0004(11) -0.0034(11) -0.0018(10) _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 O8 2.028(2) 2 ? Zn1 O17 2.032(2) . ? Zn1 O7 2.0501(19) . ? Zn1 O3 2.0541(19) . ? Zn1 O6 2.172(2) . ? Zn1 O16 2.315(2) . ? Zn2 O24 2.025(2) . ? Zn2 O2 2.026(2) 2_545 ? Zn2 O7 2.0382(19) . ? Zn2 O3 2.058(2) . ? Zn2 O12 2.195(2) . ? Zn2 O22 2.332(2) . ? Zn3 O9 1.914(2) . ? Zn3 O13 1.946(2) . ? Zn3 O1W 2.012(2) . ? Zn3 O10 2.111(2) . ? Zn3 O11 2.157(2) . ? Zn4 O15 1.993(3) . ? Zn4 O19 2.017(3) . ? Zn4 O14 2.045(2) 2_554 ? Zn4 O18 2.057(2) . ? Zn4 O23 2.085(2) . ? Zn4A O19 1.942(5) . ? Zn4A O15 2.000(5) . ? Zn4A O18 2.016(5) . ? Zn4A O23 2.060(5) . ? Zn4A O14 2.340(6) 2_554 ? Zn5 O1 1.927(2) 1_564 ? Zn5 O21 1.958(2) . ? Zn5 O2W 2.017(2) . ? Zn5 O4 2.097(2) . ? Zn5 O5 2.148(2) . ? P1 O1 1.505(2) . ? P1 O2 1.516(2) . ? P1 O3 1.5308(19) . ? P1 C4 1.837(3) . ? P2 O9 1.500(2) . ? P2 O8 1.515(2) . ? P2 O7 1.5281(19) . ? P2 C6 1.839(3) . ? P3 O15 1.522(2) . ? P3 O13 1.523(2) . ? P3 O14 1.532(2) . ? P3 C8 1.858(3) . ? P4 O19 1.502(2) . ? P4 O21 1.507(2) . ? P4 O20 1.564(2) . ? P4 C10 1.840(3) 1_564 ? O1 Zn5 1.927(2) 1_546 ? O2 Zn2 2.026(2) 2_545 ? O4 C4 1.425(3) 2_654 ? O5 C5 1.253(3) . ? O6 C5 1.268(3) 2_654 ? O8 Zn1 2.028(2) 2 ? O10 C6 1.431(3) 2_455 ? O11 C7 1.250(3) . ? O12 C7 1.267(3) 2_455 ? O14 Zn4 2.045(2) 2_554 ? O14 Zn4A 2.340(6) 2_554 ? O16 C8 1.424(3) . ? O17 C9 1.260(3) . ? O18 C9 1.250(3) . ? O22 C10 1.430(4) . ? O23 C11 1.259(3) 1_564 ? O24 C11 1.247(3) . ? N1 C3 1.476(6) . ? N1 C2 1.520(5) . ? C1 C2 1.218(8) . ? C2 C3 1.528(7) 2_454 ? C3 C2 1.528(7) 2_454 ? C4 O4 1.425(3) 2_654 ? C4 C5 1.509(4) 2_654 ? C5 O6 1.268(3) 2_654 ? C5 C4 1.509(4) 2_654 ? C6 O10 1.431(3) 2_455 ? C6 C7 1.510(4) 2_455 ? C7 O12 1.267(3) 2_455 ? C7 C6 1.510(4) 2_455 ? C8 C9 1.526(4) . ? C10 C11 1.527(4) . ? C10 P4 1.840(3) 1_546 ? C11 O23 1.259(3) 1_546 ? 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 O8 Zn1 O17 95.34(8) 2 . ? O8 Zn1 O7 95.69(8) 2 . ? O17 Zn1 O7 102.89(8) . . ? O8 Zn1 O3 103.78(8) 2 . ? O17 Zn1 O3 160.65(8) . . ? O7 Zn1 O3 78.48(8) . . ? O8 Zn1 O6 85.15(8) 2 . ? O17 Zn1 O6 89.04(8) . . ? O7 Zn1 O6 167.88(7) . . ? O3 Zn1 O6 89.57(7) . . ? O8 Zn1 O16 166.04(8) 2 . ? O17 Zn1 O16 71.87(8) . . ? O7 Zn1 O16 92.71(8) . . ? O3 Zn1 O16 88.80(8) . . ? O6 Zn1 O16 88.97(8) . . ? O24 Zn2 O2 93.57(8) . 2_545 ? O24 Zn2 O7 160.56(8) . . ? O2 Zn2 O7 105.53(8) 2_545 . ? O24 Zn2 O3 102.71(8) . . ? O2 Zn2 O3 97.74(8) 2_545 . ? O7 Zn2 O3 78.67(8) . . ? O24 Zn2 O12 88.61(8) . . ? O2 Zn2 O12 84.45(8) 2_545 . ? O7 Zn2 O12 89.63(7) . . ? O3 Zn2 O12 168.26(7) . . ? O24 Zn2 O22 71.93(8) . . ? O2 Zn2 O22 163.13(8) 2_545 . ? O7 Zn2 O22 88.64(8) . . ? O3 Zn2 O22 93.96(8) . . ? O12 Zn2 O22 86.56(8) . . ? O9 Zn3 O13 125.00(10) . . ? O9 Zn3 O1W 104.05(10) . . ? O13 Zn3 O1W 98.78(10) . . ? O9 Zn3 O10 111.39(9) . . ? O13 Zn3 O10 119.25(9) . . ? O1W Zn3 O10 86.97(10) . . ? O9 Zn3 O11 86.54(9) . . ? O13 Zn3 O11 88.34(8) . . ? O1W Zn3 O11 160.09(10) . . ? O10 Zn3 O11 73.39(8) . . ? O15 Zn4 O19 158.36(9) . . ? O15 Zn4 O14 101.69(10) . 2_554 ? O19 Zn4 O14 99.83(10) . 2_554 ? O15 Zn4 O18 90.48(10) . . ? O19 Zn4 O18 85.70(10) . . ? O14 Zn4 O18 106.18(10) 2_554 . ? O15 Zn4 O23 86.58(10) . . ? O19 Zn4 O23 89.33(10) . . ? O14 Zn4 O23 94.96(10) 2_554 . ? O18 Zn4 O23 158.81(10) . . ? O19 Zn4A O15 175.3(3) . . ? O19 Zn4A O18 88.9(2) . . ? O15 Zn4A O18 91.5(2) . . ? O19 Zn4A O23 92.2(2) . . ? O15 Zn4A O23 87.10(19) . . ? O18 Zn4A O23 175.1(3) . . ? O19 Zn4A O14 92.6(2) . 2_554 ? O15 Zn4A O14 92.0(2) . 2_554 ? O18 Zn4A O14 97.4(2) . 2_554 ? O23 Zn4A O14 87.3(2) . 2_554 ? O1 Zn5 O21 120.36(10) 1_564 . ? O1 Zn5 O2W 102.27(10) 1_564 . ? O21 Zn5 O2W 99.88(10) . . ? O1 Zn5 O4 114.46(9) 1_564 . ? O21 Zn5 O4 120.84(9) . . ? O2W Zn5 O4 88.39(10) . . ? O1 Zn5 O5 88.81(8) 1_564 . ? O21 Zn5 O5 86.21(8) . . ? O2W Zn5 O5 162.06(10) . . ? O4 Zn5 O5 74.09(8) . . ? O1 P1 O2 112.16(12) . . ? O1 P1 O3 113.49(12) . . ? O2 P1 O3 112.49(12) . . ? O1 P1 C4 106.45(13) . . ? O2 P1 C4 106.96(12) . . ? O3 P1 C4 104.58(12) . . ? O9 P2 O8 111.98(12) . . ? O9 P2 O7 113.32(12) . . ? O8 P2 O7 112.86(11) . . ? O9 P2 C6 106.49(13) . . ? O8 P2 C6 106.39(12) . . ? O7 P2 C6 105.08(12) . . ? O15 P3 O13 111.48(12) . . ? O15 P3 O14 111.88(12) . . ? O13 P3 O14 110.95(13) . . ? O15 P3 C8 106.50(12) . . ? O13 P3 C8 108.59(12) . . ? O14 P3 C8 107.19(12) . . ? O19 P4 O21 113.87(13) . . ? O19 P4 O20 110.25(13) . . ? O21 P4 O20 110.95(13) . . ? O19 P4 C10 106.72(13) . 1_564 ? O21 P4 C10 110.33(13) . 1_564 ? O20 P4 C10 104.20(13) . 1_564 ? P1 O1 Zn5 149.08(14) . 1_546 ? P1 O2 Zn2 133.96(12) . 2_545 ? P1 O3 Zn1 130.70(12) . . ? P1 O3 Zn2 127.88(12) . . ? Zn1 O3 Zn2 101.02(8) . . ? C4 O4 Zn5 117.72(17) 2_654 . ? C5 O5 Zn5 117.02(17) . . ? C5 O6 Zn1 131.44(19) 2_654 . ? P2 O7 Zn2 130.99(12) . . ? P2 O7 Zn1 126.52(12) . . ? Zn2 O7 Zn1 101.82(8) . . ? P2 O8 Zn1 134.02(12) . 2 ? P2 O9 Zn3 149.72(15) . . ? C6 O10 Zn3 119.36(17) 2_455 . ? C7 O11 Zn3 118.73(18) . . ? C7 O12 Zn2 131.44(19) 2_455 . ? P3 O13 Zn3 140.77(13) . . ? P3 O14 Zn4 129.80(13) . 2_554 ? P3 O14 Zn4A 130.77(17) . 2_554 ? Zn4 O14 Zn4A 1.25(15) 2_554 2_554 ? P3 O15 Zn4 130.62(13) . . ? P3 O15 Zn4A 132.10(18) . . ? Zn4 O15 Zn4A 8.60(16) . . ? C8 O16 Zn1 111.47(17) . . ? C9 O17 Zn1 119.63(18) . . ? C9 O18 Zn4A 132.2(2) . . ? C9 O18 Zn4 129.8(2) . . ? Zn4A O18 Zn4 8.35(16) . . ? P4 O19 Zn4A 132.09(18) . . ? P4 O19 Zn4 131.39(13) . . ? Zn4A O19 Zn4 8.40(17) . . ? P4 O21 Zn5 141.45(14) . . ? C10 O22 Zn2 111.11(18) . . ? C11 O23 Zn4A 129.7(2) 1_564 . ? C11 O23 Zn4 130.7(2) 1_564 . ? Zn4A O23 Zn4 8.25(16) . . ? C11 O24 Zn2 120.87(18) . . ? C3 N1 C2 110.0(4) . . ? C1 C2 N1 118.0(5) . . ? C1 C2 C3 114.8(6) . 2_454 ? N1 C2 C3 108.4(4) . 2_454 ? N1 C3 C2 113.4(4) . 2_454 ? O4 C4 C5 107.5(2) 2_654 2_654 ? O4 C4 P1 111.4(2) 2_654 . ? C5 C4 P1 112.90(19) 2_654 . ? O5 C5 O6 123.0(3) . 2_654 ? O5 C5 C4 118.8(2) . 2_654 ? O6 C5 C4 118.1(2) 2_654 2_654 ? O10 C6 C7 107.5(2) 2_455 2_455 ? O10 C6 P2 109.2(2) 2_455 . ? C7 C6 P2 113.56(19) 2_455 . ? O11 C7 O12 123.7(3) . 2_455 ? O11 C7 C6 118.5(2) . 2_455 ? O12 C7 C6 117.7(2) 2_455 2_455 ? O16 C8 C9 107.4(2) . . ? O16 C8 P3 113.19(19) . . ? C9 C8 P3 111.47(19) . . ? O18 C9 O17 122.2(3) . . ? O18 C9 C8 119.6(2) . . ? O17 C9 C8 118.2(2) . . ? O22 C10 C11 107.7(2) . . ? O22 C10 P4 112.7(2) . 1_546 ? C11 C10 P4 109.15(19) . 1_546 ? O24 C11 O23 122.2(3) . 1_546 ? O24 C11 C10 118.4(2) . . ? O23 C11 C10 119.4(3) 1_546 . ? 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 O1W H18 O5 0.69(5) 2.13(5) 2.800(3) 168(6) 2_554 O1W H19 O2 0.86(5) 1.86(5) 2.696(3) 164(4) 2_545 O2W H20 O11 0.84(5) 1.99(5) 2.818(3) 168(5) 2_564 O2W H21 O8 0.67(4) 2.09(4) 2.742(3) 163(5) 2_564 O3W H22 O4W 0.98(2) 2.34(5) 3.219(6) 148(7) 2_664 O3W H23 O4W 0.939(18) 1.94(2) 2.861(6) 168(3) . O4 H15 O12 0.76(5) 1.89(5) 2.622(3) 162(5) 1_664 O4W H24 O3W 0.99(2) 2.29(5) 3.219(6) 156(8) 2_664 O10 H13 O6 0.75(4) 1.90(4) 2.638(3) 167(5) 1_455 O16 H14 O24 0.70(5) 2.46(5) 3.101(3) 153(5) 2_545 O16 H14 O23 0.70(5) 2.50(5) 3.148(3) 154(5) 2_554 O20 H17 O3W 0.90(5) 1.75(6) 2.617(4) 161(5) . O22 H16 O17 0.74(4) 2.49(4) 3.102(3) 141(4) 2 O22 H16 O18 0.74(4) 2.50(4) 3.230(3) 166(5) 2 N1 H6 O21 0.90 2.43 3.191(4) 142.6 2_554 N1 H6 O5 0.90 2.53 3.188(4) 130.6 2_554 N1 H5 O14 0.90 1.90 2.800(4) 177.6 . _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.647 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.101 data_f1 _database_code_depnum_ccdc_archive 'CCDC 729406' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 N2 O12 P2 Zn2' _chemical_formula_weight 524.91 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.014(6) _cell_length_b 9.526(6) _cell_length_c 17.076(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1629.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1521 _cell_measurement_theta_min 2.1378 _cell_measurement_theta_max 27.4758 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 3.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5483 _exptl_absorpt_correction_T_max 1.0000 _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 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11368 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1853 _reflns_number_gt 1705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0518P)^2^+0.9505P] 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 1853 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 0.15745(3) 0.19834(3) 0.247940(18) 0.01998(14) Uani 1 1 d . . . P1 P 0.09329(6) -0.12160(7) 0.23299(4) 0.01663(17) Uani 1 1 d . . . O1 O -0.0020(2) -0.1952(2) 0.28955(11) 0.0262(4) Uani 1 1 d . . . O2 O 0.1893(2) -0.2245(2) 0.19467(12) 0.0279(4) Uani 1 1 d . . . O3 O 0.16234(18) 0.0009(2) 0.27277(13) 0.0253(4) Uani 1 1 d . . . O4 O 0.0720(2) 0.0516(2) 0.11500(14) 0.0323(5) Uani 1 1 d . . . H2 H 0.047(4) 0.045(4) 0.065(3) 0.047(11) Uiso 1 1 d . . . O5 O 0.14713(19) 0.2524(2) 0.36300(12) 0.0275(4) Uani 1 1 d . . . O6 O 0.0498(3) 0.3470(2) 0.46684(12) 0.0367(5) Uani 1 1 d . . . N1 N 0.0092(3) 0.1110(3) 0.55611(16) 0.0334(6) Uani 1 1 d . . . H7 H 0.006(4) 0.143(4) 0.607(3) 0.050(11) Uiso 1 1 d . . . H8 H 0.027(4) 0.187(4) 0.526(2) 0.044(11) Uiso 1 1 d . . . C1 C -0.0102(3) -0.0446(3) 0.15589(15) 0.0197(5) Uani 1 1 d . . . H1 H -0.081(3) 0.006(3) 0.1754(18) 0.020(7) Uiso 1 1 d . . . C2 C 0.0727(3) 0.3430(3) 0.39536(16) 0.0222(5) Uani 1 1 d . . . C3 C -0.1235(3) 0.0610(4) 0.5272(2) 0.0380(7) Uani 1 1 d . . . H3 H -0.150(4) -0.015(4) 0.568(3) 0.041(10) Uiso 1 1 d . . . H4 H -0.182(4) 0.146(4) 0.526(2) 0.052(12) Uiso 1 1 d . . . C4 C 0.1105(3) -0.0035(4) 0.5545(2) 0.0372(7) Uani 1 1 d . . . H6 H 0.077(4) -0.082(4) 0.590(2) 0.041(10) Uiso 1 1 d . . . H5 H 0.188(4) 0.038(4) 0.573(2) 0.044(10) 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 0.0173(2) 0.0167(2) 0.0260(2) 0.00217(11) 0.00196(11) 0.00081(11) P1 0.0155(3) 0.0143(3) 0.0200(3) 0.0000(2) -0.0014(2) 0.0002(2) O1 0.0260(9) 0.0317(11) 0.0208(10) 0.0026(7) -0.0015(8) -0.0090(8) O2 0.0249(9) 0.0305(10) 0.0283(11) -0.0053(8) -0.0044(8) 0.0101(8) O3 0.0273(11) 0.0166(10) 0.0319(11) -0.0001(8) -0.0098(8) -0.0036(8) O4 0.0395(12) 0.0277(11) 0.0298(11) 0.0075(9) -0.0027(9) -0.0115(9) O5 0.0327(11) 0.0257(10) 0.0241(10) -0.0023(8) -0.0033(8) 0.0079(8) O6 0.0541(13) 0.0357(12) 0.0203(10) -0.0035(9) -0.0009(10) 0.0086(11) N1 0.0418(15) 0.0367(15) 0.0218(12) -0.0008(11) 0.0026(11) -0.0005(12) C1 0.0198(12) 0.0156(12) 0.0236(13) 0.0026(9) -0.0025(10) 0.0018(10) C2 0.0225(12) 0.0211(13) 0.0231(13) -0.0036(10) -0.0039(10) -0.0019(10) C3 0.0279(14) 0.051(2) 0.0354(17) 0.0018(15) 0.0059(13) 0.0098(15) C4 0.0305(16) 0.049(2) 0.0323(17) 0.0062(15) -0.0093(13) -0.0015(15) _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 1.929(2) . ? Zn1 O2 1.929(2) 8_665 ? Zn1 O1 1.965(2) 3 ? Zn1 O5 2.034(2) . ? P1 O3 1.517(2) . ? P1 O2 1.521(2) . ? P1 O1 1.528(2) . ? P1 C1 1.829(3) . ? O1 Zn1 1.965(2) 3_545 ? O2 Zn1 1.929(2) 8_655 ? O4 C1 1.416(3) . ? O5 C2 1.267(3) . ? O6 C2 1.243(3) . ? N1 C4 1.490(5) . ? N1 C3 1.495(5) . ? C1 C2 1.518(4) 3_545 ? C2 C1 1.518(4) 3 ? C3 C4 1.504(5) 5_556 ? C4 C3 1.504(5) 5_556 ? 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 O2 117.05(9) . 8_665 ? O3 Zn1 O1 126.52(8) . 3 ? O2 Zn1 O1 106.25(10) 8_665 3 ? O3 Zn1 O5 92.06(9) . . ? O2 Zn1 O5 113.54(9) 8_665 . ? O1 Zn1 O5 98.26(8) 3 . ? O3 P1 O2 113.60(12) . . ? O3 P1 O1 110.77(12) . . ? O2 P1 O1 111.78(13) . . ? O3 P1 C1 105.80(12) . . ? O2 P1 C1 107.87(13) . . ? O1 P1 C1 106.55(12) . . ? P1 O1 Zn1 121.71(12) . 3_545 ? P1 O2 Zn1 123.05(13) . 8_655 ? P1 O3 Zn1 129.80(13) . . ? C2 O5 Zn1 128.59(18) . . ? C4 N1 C3 111.5(3) . . ? O4 C1 C2 114.3(2) . 3_545 ? O4 C1 P1 106.56(18) . . ? C2 C1 P1 111.48(18) 3_545 . ? O6 C2 O5 123.9(3) . . ? O6 C2 C1 117.9(2) . 3 ? O5 C2 C1 118.1(2) . 3 ? N1 C3 C4 110.2(3) . 5_556 ? N1 C4 C3 110.0(3) . 5_556 ? 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 H8 O6 0.90(4) 1.85(4) 2.747(4) 176(4) . N1 H7 O1 0.92(4) 1.84(4) 2.756(4) 176(4) 5_556 O4 H2 O6 0.89(4) 1.97(4) 2.717(3) 141(4) 7_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.630 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.112