# Electronic Supplementary Material for CrystEngComm # This Journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Jihong Yu' 'Peng Chen' 'Zhaojun Dong' 'Jiyang Li' 'Ruren Xu' 'Lang Zhao' _publ_contact_author_name 'Jihong Yu' _publ_contact_author_email JIHONG@JLU.EDU.CN data_ZnPO-CJ36-Jihong _database_code_depnum_ccdc_archive 'CCDC 668032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnPO-CJ36 _chemical_melting_point ? _chemical_formula_moiety (C6H10N3O2)[Zn2(HPO4)(PO4)]H2O _chemical_formula_sum 'C6 H13 N3 O11 P2 Zn2' _chemical_formula_weight 495.87 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6010(8) _cell_length_b 9.0012(8) _cell_length_c 9.9080(10) _cell_angle_alpha 84.754(2) _cell_angle_beta 83.338(2) _cell_angle_gamma 74.795(2) _cell_volume 733.73(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3356 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 3.553 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details Process-auto _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4544 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3356 _reflns_number_gt 2922 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0366P)^2^+0.5985P] 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 3356 _refine_ls_number_parameters 269 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.58151(4) -0.11622(3) -0.30908(3) 0.01638(9) Uani 1 1 d . . . Zn2 Zn 0.24127(4) 0.51856(4) -0.49494(3) 0.01787(9) Uani 1 1 d . . . P1 P 0.52898(8) 0.24342(8) -0.45569(7) 0.01467(15) Uani 1 1 d . . . P2 P 0.91828(8) -0.36372(8) -0.29461(7) 0.01697(15) Uani 1 1 d . . . O1 O 0.3510(2) 0.3211(2) -0.4093(2) 0.0250(5) Uani 1 1 d . . . O1W O 0.3377(3) -0.3969(3) -0.1747(3) 0.0375(6) Uani 1 1 d D . . O2 O 0.6365(3) 0.3418(3) -0.4222(2) 0.0259(5) Uani 1 1 d . . . O3 O 0.5761(3) 0.0881(2) -0.3793(2) 0.0330(5) Uani 1 1 d . . . O4 O 0.4550(3) -0.2257(2) -0.3898(2) 0.0245(5) Uani 1 1 d . . . O5 O 0.8167(2) -0.1984(2) -0.3219(2) 0.0235(4) Uani 1 1 d . . . O6 O 0.1569(3) 0.4827(2) -0.6603(2) 0.0266(5) Uani 1 1 d . . . O7 O 0.9276(3) -0.3918(3) -0.1355(2) 0.0301(5) Uani 1 1 d . . . H7O H 0.848(5) -0.374(5) -0.102(4) 0.036(12) Uiso 1 1 d . . . O8 O 0.0915(2) 0.6212(3) -0.3517(2) 0.0296(5) Uani 1 1 d . . . O9 O 0.4763(3) -0.1007(2) -0.1204(2) 0.0278(5) Uani 1 1 d . . . O10 O 0.6233(3) -0.3208(3) -0.0277(3) 0.0432(7) Uani 1 1 d . . . C1 C 0.5020(4) -0.2116(3) -0.0322(3) 0.0231(6) Uani 1 1 d . . . C2 C 0.3703(4) -0.2087(4) 0.0867(3) 0.0293(7) Uani 1 1 d . . . H2 H 0.392(6) -0.162(5) 0.170(5) 0.069(15) Uiso 1 1 d . . . C3 C 0.2062(4) -0.1123(4) 0.0550(4) 0.0365(8) Uani 1 1 d . . . H32 H 0.220(5) -0.010(5) 0.048(4) 0.042(11) Uiso 1 1 d . . . H31 H 0.171(7) -0.163(6) -0.036(6) 0.098(19) Uiso 1 1 d . . . C4 C 0.0710(4) -0.1173(3) 0.1642(3) 0.0259(7) Uani 1 1 d . . . N2 N 0.0279(3) -0.0221(3) 0.2711(3) 0.0297(6) Uani 1 1 d . . . C5 C -0.0980(4) -0.0541(4) 0.3459(4) 0.0351(8) Uani 1 1 d . . . H5 H -0.147(5) -0.007(4) 0.422(4) 0.035(10) Uiso 1 1 d . . . C6 C -0.0332(4) -0.2076(4) 0.1794(4) 0.0289(7) Uani 1 1 d . . . H6 H -0.033(4) -0.282(4) 0.131(4) 0.023(9) Uiso 1 1 d . . . N1 N 0.3718(4) -0.3707(3) 0.1324(3) 0.0317(7) Uani 1 1 d D . . H3N H 0.457(5) -0.428(5) 0.149(4) 0.043(12) Uiso 1 1 d . . . H2N H 0.346(6) -0.410(6) 0.065(6) 0.075(18) Uiso 1 1 d . . . H1N H 0.309(6) -0.380(6) 0.221(3) 0.091(18) Uiso 1 1 d D . . N3 N -0.1369(3) -0.1662(3) 0.2934(3) 0.0312(6) Uani 1 1 d . . . H1O H 0.377(5) -0.341(5) -0.254(4) 0.081(17) Uiso 1 1 d D . . H2O H 0.242(5) -0.420(7) -0.205(5) 0.12(2) Uiso 1 1 d D . . H4N H -0.203(5) -0.208(4) 0.321(4) 0.034(11) Uiso 1 1 d . . . H5N H 0.074(5) 0.046(5) 0.291(5) 0.056(14) 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 0.01769(17) 0.01413(16) 0.01652(17) 0.00091(12) 0.00107(12) -0.00442(12) Zn2 0.01606(17) 0.01683(16) 0.02118(18) -0.00242(13) 0.00132(12) -0.00596(12) P1 0.0160(3) 0.0118(3) 0.0167(3) 0.0013(3) -0.0007(2) -0.0054(2) P2 0.0144(3) 0.0167(3) 0.0197(4) -0.0045(3) -0.0004(3) -0.0031(3) O1 0.0166(10) 0.0241(11) 0.0311(12) 0.0040(9) 0.0050(8) -0.0047(8) O1W 0.0428(15) 0.0402(14) 0.0349(14) 0.0109(11) -0.0115(11) -0.0214(12) O2 0.0298(12) 0.0304(11) 0.0246(11) -0.0002(9) -0.0021(9) -0.0211(9) O3 0.0438(14) 0.0166(10) 0.0380(14) 0.0104(10) -0.0105(11) -0.0079(10) O4 0.0279(11) 0.0304(11) 0.0194(11) -0.0016(9) 0.0016(8) -0.0163(9) O5 0.0160(10) 0.0169(10) 0.0361(12) -0.0023(9) 0.0009(8) -0.0030(8) O6 0.0318(12) 0.0205(10) 0.0319(12) -0.0005(9) -0.0112(9) -0.0112(9) O7 0.0259(13) 0.0408(14) 0.0219(12) -0.0042(10) -0.0023(10) -0.0045(11) O8 0.0165(10) 0.0348(13) 0.0363(13) -0.0132(10) 0.0052(9) -0.0041(9) O9 0.0362(12) 0.0264(11) 0.0177(11) -0.0001(9) 0.0094(9) -0.0084(9) O10 0.0293(13) 0.0384(14) 0.0500(16) 0.0123(12) 0.0151(11) -0.0008(11) C1 0.0258(15) 0.0246(15) 0.0183(14) -0.0013(12) 0.0065(11) -0.0088(12) C2 0.0279(16) 0.0283(16) 0.0251(17) 0.0036(13) 0.0101(13) -0.0027(13) C3 0.0310(18) 0.0313(18) 0.038(2) 0.0104(16) 0.0101(15) -0.0029(14) C4 0.0226(15) 0.0199(14) 0.0300(17) 0.0057(12) 0.0033(12) -0.0010(11) N2 0.0286(14) 0.0254(14) 0.0370(16) -0.0041(12) 0.0023(12) -0.0118(11) C5 0.0314(18) 0.0360(19) 0.036(2) -0.0055(16) 0.0087(15) -0.0085(15) C6 0.0306(17) 0.0215(15) 0.0339(18) 0.0012(14) -0.0012(14) -0.0072(13) N1 0.0312(16) 0.0224(14) 0.0336(17) 0.0056(13) 0.0122(13) -0.0021(12) N3 0.0223(14) 0.0289(15) 0.0418(17) 0.0050(13) 0.0052(12) -0.0116(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 O3 1.897(2) . ? Zn1 O4 1.925(2) . ? Zn1 O5 1.956(2) . ? Zn1 O9 1.980(2) . ? Zn2 O2 1.914(2) 2_664 ? Zn2 O8 1.928(2) . ? Zn2 O1 1.949(2) . ? Zn2 O6 1.953(2) . ? P1 O3 1.507(2) . ? P1 O2 1.518(2) . ? P1 O4 1.540(2) 2_654 ? P1 O1 1.542(2) . ? P2 O8 1.507(2) 1_645 ? P2 O6 1.510(2) 2_654 ? P2 O5 1.533(2) . ? P2 O7 1.582(2) . ? O1W H1O 0.972(19) . ? O1W H2O 0.988(19) . ? O2 Zn2 1.914(2) 2_664 ? O4 P1 1.540(2) 2_654 ? O6 P2 1.510(2) 2_654 ? O7 H7O 0.71(4) . ? O8 P2 1.507(2) 1_465 ? O9 C1 1.256(4) . ? O10 C1 1.234(4) . ? C1 C2 1.534(4) . ? C2 N1 1.484(4) . ? C2 C3 1.501(5) . ? C2 H2 1.02(5) . ? C3 C4 1.501(4) . ? C3 H32 0.96(4) . ? C3 H31 1.15(6) . ? C4 C6 1.347(4) . ? C4 N2 1.380(4) . ? N2 C5 1.320(4) . ? N2 H5N 0.86(5) . ? C5 N3 1.309(5) . ? C5 H5 0.90(4) . ? C6 N3 1.371(4) . ? C6 H6 0.86(4) . ? N1 H3N 0.80(4) . ? N1 H2N 0.86(6) . ? N1 H1N 0.98(2) . ? N3 H4N 0.77(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 117.72(10) . . ? O3 Zn1 O5 98.03(9) . . ? O4 Zn1 O5 118.37(9) . . ? O3 Zn1 O9 106.58(10) . . ? O4 Zn1 O9 101.88(9) . . ? O5 Zn1 O9 114.33(10) . . ? O2 Zn2 O8 107.96(10) 2_664 . ? O2 Zn2 O1 120.13(9) 2_664 . ? O8 Zn2 O1 104.73(9) . . ? O2 Zn2 O6 96.87(9) 2_664 . ? O8 Zn2 O6 118.75(10) . . ? O1 Zn2 O6 109.21(9) . . ? O3 P1 O2 108.90(13) . . ? O3 P1 O4 110.76(13) . 2_654 ? O2 P1 O4 110.43(12) . 2_654 ? O3 P1 O1 108.52(13) . . ? O2 P1 O1 109.48(13) . . ? O4 P1 O1 108.72(12) 2_654 . ? O8 P2 O6 114.25(13) 1_645 2_654 ? O8 P2 O5 110.28(12) 1_645 . ? O6 P2 O5 112.44(12) 2_654 . ? O8 P2 O7 104.06(14) 1_645 . ? O6 P2 O7 107.82(13) 2_654 . ? O5 P2 O7 107.39(13) . . ? P1 O1 Zn2 120.66(12) . . ? H1O O1W H2O 103(2) . . ? P1 O2 Zn2 141.88(14) . 2_664 ? P1 O3 Zn1 162.37(16) . . ? P1 O4 Zn1 122.01(12) 2_654 . ? P2 O5 Zn1 129.91(12) . . ? P2 O6 Zn2 136.52(14) 2_654 . ? P2 O7 H7O 109(3) . . ? P2 O8 Zn2 138.48(15) 1_465 . ? C1 O9 Zn1 122.5(2) . . ? O10 C1 O9 127.5(3) . . ? O10 C1 C2 115.9(3) . . ? O9 C1 C2 116.6(3) . . ? N1 C2 C3 113.3(3) . . ? N1 C2 C1 107.9(3) . . ? C3 C2 C1 113.7(3) . . ? N1 C2 H2 105(3) . . ? C3 C2 H2 104(3) . . ? C1 C2 H2 113(3) . . ? C4 C3 C2 115.4(3) . . ? C4 C3 H32 107(3) . . ? C2 C3 H32 103(2) . . ? C4 C3 H31 104(3) . . ? C2 C3 H31 107(3) . . ? H32 C3 H31 121(4) . . ? C6 C4 N2 105.9(3) . . ? C6 C4 C3 129.5(3) . . ? N2 C4 C3 124.5(3) . . ? C5 N2 C4 108.9(3) . . ? C5 N2 H5N 123(3) . . ? C4 N2 H5N 128(3) . . ? N3 C5 N2 109.0(3) . . ? N3 C5 H5 126(2) . . ? N2 C5 H5 125(2) . . ? C4 C6 N3 107.6(3) . . ? C4 C6 H6 127(2) . . ? N3 C6 H6 125(2) . . ? C2 N1 H3N 117(3) . . ? C2 N1 H2N 106(4) . . ? H3N N1 H2N 104(4) . . ? C2 N1 H1N 113(3) . . ? H3N N1 H1N 100(4) . . ? H2N N1 H1N 117(5) . . ? C5 N3 C6 108.6(3) . . ? C5 N3 H4N 128(3) . . ? C6 N3 H4N 123(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7O O10 0.71(4) 1.94(4) 2.645(3) 174(5) . N1 H3N O1W 0.80(4) 2.06(5) 2.852(4) 170(4) 2_645 N1 H2N O10 0.86(6) 2.42(5) 3.041(4) 129(4) 2_645 N1 H2N O1W 0.86(6) 2.38(6) 3.127(5) 146(5) . N1 H1N O2 0.98(2) 2.17(5) 2.897(4) 129(4) 2_655 N1 H1N O6 0.98(2) 2.21(4) 3.046(4) 143(4) 1_546 O1W H1O O4 0.972(19) 1.797(19) 2.766(3) 174(5) . O1W H2O O8 0.988(19) 2.00(4) 2.866(3) 145(4) 1_545 N3 H4N O1 0.77(4) 1.92(4) 2.687(3) 172(4) 2 N2 H5N O5 0.86(5) 1.91(5) 2.776(3) 176(4) 2_655 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.852 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.096