data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof Guo-Yu Yang' _publ_contact_author_address ; State Key Lab of Structural Chemistry Fujian Institute of Research on the Structure of Matter Fuzhou 155, West Yangqiao Road Fujian 350002 CHINA ; _publ_contact_author_email YGY@FJIRSM.AC.CN _publ_section_title ; Synthesis and characterization of a novel open-framework nickel-zinc phosphite with intersecting three-dimensional 16-ring channels ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; loop_ _publ_author_name 'Guo-Yu Yang' 'Zhi-En Lin' 'Jie Zhang' 'Shou-Tian Zheng' data_2 _database_code_depnum_ccdc_archive 'CCDC 231297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 N3 Ni O10 P3 Zn2' _chemical_formula_weight 550.57 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5848(6) _cell_length_b 9.1884(6) _cell_length_c 11.9256(8) _cell_angle_alpha 102.997(2) _cell_angle_beta 94.614(2) _cell_angle_gamma 115.952(2) _cell_volume 806.81(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 25.07 _exptl_crystal_description prism _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 4.452 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.4245 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _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_% 0 _diffrn_reflns_number 4202 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2825 _reflns_number_gt 2696 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+3.0685P] 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 SHELXL _refine_ls_extinction_coef 0.0286(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2825 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0406 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 0.50585(8) 0.23840(7) -0.02556(5) 0.0212(2) Uani 1 1 d . . . Zn2 Zn 0.53693(7) 0.37852(6) 0.34219(5) 0.0187(2) Uani 1 1 d . . . Ni1 Ni 1.00808(7) 0.91191(7) 0.36856(5) 0.0163(2) Uani 1 1 d . . . P1 P 0.35005(17) 0.44077(15) 0.13437(11) 0.0202(3) Uani 1 1 d . . . H1 H 0.199(7) 0.377(7) 0.169(5) 0.022(13) Uiso 1 1 d . . . P2 P 0.66091(17) 0.14658(15) 0.18613(11) 0.0200(3) Uani 1 1 d . . . H2 H 0.819(9) 0.241(8) 0.246(6) 0.045(18) Uiso 1 1 d . . . P3 P 0.81303(16) 0.68659(14) 0.54436(10) 0.0179(3) Uani 1 1 d . . . H3 H 0.895(8) 0.682(8) 0.639(5) 0.033(16) Uiso 1 1 d . . . O1 O 0.3558(6) 0.5865(5) 0.0945(3) 0.0336(9) Uani 1 1 d . . . O2 O 0.5017(5) 0.5014(5) 0.2377(3) 0.0353(9) Uani 1 1 d . . . O3 O 0.3323(5) 0.2922(5) 0.0393(4) 0.0357(9) Uani 1 1 d . . . O4 O 0.6629(5) 0.2093(5) 0.0800(3) 0.0327(9) Uani 1 1 d . . . O5 O 0.6346(5) -0.0343(5) 0.1579(3) 0.0310(9) Uani 1 1 d . . . O6 O 0.5346(5) 0.1693(4) 0.2620(3) 0.0308(8) Uani 1 1 d . . . O7 O 0.7672(5) 0.5351(4) 0.4414(3) 0.0267(8) Uani 1 1 d . . . O8 O 0.6525(6) 0.6988(5) 0.5765(4) 0.0432(11) Uani 1 1 d . . . O9 O 0.9483(4) 0.8518(4) 0.5273(3) 0.0177(7) Uani 1 1 d . . . OW1 O 0.7355(5) 0.8431(5) 0.3222(3) 0.0260(8) Uani 1 1 d . . . H4 H 0.655(8) 0.743(8) 0.299(5) 0.021(14) Uiso 1 1 d . . . H5 H 0.697(8) 0.886(8) 0.267(6) 0.033(16) Uiso 1 1 d . . . N1 N 1.2630(6) 0.9590(6) 0.4286(5) 0.0277(10) Uani 1 1 d . . . H6 H 1.299(11) 1.028(11) 0.500(8) 0.06(2) Uiso 1 1 d . . . H7 H 1.343(11) 1.026(10) 0.407(7) 0.05(2) Uiso 1 1 d . . . N2 N 0.9849(7) 0.6796(6) 0.2762(4) 0.0267(10) Uani 1 1 d . . . H8 H 0.912(8) 0.630(8) 0.295(5) 0.018(16) Uiso 1 1 d . . . N3 N 1.0444(7) 0.9653(6) 0.2063(4) 0.0340(11) Uani 1 1 d . . . H9 H 0.932(10) 0.965(9) 0.165(6) 0.047(19) Uiso 1 1 d . . . H10 H 1.135(16) 1.061(14) 0.213(10) 0.11(4) Uiso 1 1 d . . . C1 C 1.2548(17) 0.7986(18) 0.4376(11) 0.029(3) Uani 0.50 1 d P . . C1' C 1.2876(19) 0.8076(18) 0.3783(18) 0.048(4) Uani 0.50 1 d P . . C2 C 1.1407(11) 0.6657(9) 0.3215(7) 0.055(2) Uani 1 1 d . . . C3 C 0.9588(9) 0.6661(8) 0.1504(5) 0.0390(14) Uani 1 1 d . . . H11 H 0.992(9) 0.577(9) 0.104(6) 0.045(19) Uiso 1 1 d . . . H12 H 0.823(10) 0.622(9) 0.118(6) 0.047(19) Uiso 1 1 d . . . C4 C 1.0745(9) 0.8326(8) 0.1299(5) 0.0403(14) Uani 1 1 d . . . H13 H 1.046(9) 0.832(8) 0.047(6) 0.042(18) Uiso 1 1 d . . . H14 H 1.198(10) 0.865(9) 0.146(6) 0.044(19) 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 0.0338(4) 0.0188(3) 0.0175(3) 0.0057(2) 0.0059(2) 0.0176(3) Zn2 0.0228(3) 0.0123(3) 0.0200(3) 0.0049(2) 0.0088(2) 0.0064(2) Ni1 0.0191(3) 0.0132(3) 0.0162(3) 0.0044(2) 0.0058(2) 0.0069(2) P1 0.0266(7) 0.0172(6) 0.0213(6) 0.0075(5) 0.0093(5) 0.0125(5) P2 0.0280(7) 0.0151(6) 0.0178(6) 0.0027(5) 0.0004(5) 0.0125(5) P3 0.0222(6) 0.0127(6) 0.0170(6) 0.0075(5) 0.0055(5) 0.0049(5) O1 0.048(2) 0.031(2) 0.035(2) 0.0198(17) 0.0138(18) 0.0250(19) O2 0.045(2) 0.0198(18) 0.034(2) 0.0105(16) -0.0019(18) 0.0099(17) O3 0.037(2) 0.032(2) 0.037(2) -0.0047(17) 0.0034(17) 0.0230(18) O4 0.037(2) 0.042(2) 0.036(2) 0.0241(18) 0.0127(17) 0.0263(19) O5 0.054(2) 0.0243(19) 0.0214(18) 0.0016(15) -0.0007(16) 0.0279(18) O6 0.048(2) 0.0172(17) 0.031(2) 0.0053(15) 0.0178(17) 0.0178(17) O7 0.0271(18) 0.0156(17) 0.033(2) 0.0034(15) 0.0093(15) 0.0071(14) O8 0.039(2) 0.021(2) 0.067(3) 0.0123(19) 0.038(2) 0.0077(17) O9 0.0185(16) 0.0114(15) 0.0211(17) 0.0062(13) 0.0078(13) 0.0040(13) OW1 0.0243(19) 0.0178(19) 0.029(2) 0.0073(15) -0.0021(15) 0.0053(16) N1 0.020(2) 0.023(2) 0.039(3) 0.006(2) 0.008(2) 0.0096(19) N2 0.032(3) 0.023(2) 0.027(2) 0.0075(19) 0.013(2) 0.013(2) N3 0.039(3) 0.033(3) 0.028(2) 0.015(2) 0.012(2) 0.010(2) C1 0.032(6) 0.044(7) 0.021(6) 0.013(6) 0.012(5) 0.023(5) C1' 0.036(8) 0.035(7) 0.072(12) -0.004(8) -0.011(8) 0.027(6) C2 0.070(5) 0.041(4) 0.059(4) -0.008(3) -0.008(4) 0.044(4) C3 0.052(4) 0.033(3) 0.019(3) -0.004(2) 0.007(3) 0.014(3) C4 0.047(4) 0.047(4) 0.020(3) 0.007(3) 0.015(3) 0.017(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 O4 1.915(4) . ? Zn1 O3 1.929(4) . ? Zn1 O1 1.937(4) 2_665 ? Zn1 O5 1.961(4) 2_655 ? Zn2 O8 1.909(4) 2_666 ? Zn2 O7 1.936(4) . ? Zn2 O6 1.936(3) . ? Zn2 O2 1.947(4) . ? Ni1 N1 2.067(5) . ? Ni1 N2 2.084(4) . ? Ni1 O9 2.097(3) 2_776 ? Ni1 N3 2.114(5) . ? Ni1 OW1 2.126(4) . ? Ni1 O9 2.129(3) . ? P1 O1 1.502(4) . ? P1 O3 1.506(4) . ? P1 O2 1.524(4) . ? P1 H1 1.32(5) . ? P2 O4 1.503(4) . ? P2 O6 1.519(4) . ? P2 O5 1.528(4) . ? P2 H2 1.28(7) . ? P3 O8 1.503(4) . ? P3 O7 1.508(4) . ? P3 O9 1.526(3) . ? P3 H3 1.30(6) . ? O1 Zn1 1.937(4) 2_665 ? O5 Zn1 1.961(4) 2_655 ? O8 Zn2 1.909(4) 2_666 ? O9 Ni1 2.097(3) 2_776 ? OW1 H4 0.83(6) . ? OW1 H5 0.94(7) . ? N1 C1 1.474(14) . ? N1 C1' 1.498(14) . ? N1 H6 0.88(9) . ? N1 H7 0.81(9) . ? N2 C3 1.468(7) . ? N2 C2 1.470(8) . ? N2 H8 0.68(6) . ? N3 C4 1.482(8) . ? N3 H9 1.05(7) . ? N3 H10 0.86(12) . ? C1 C1' 0.790(19) . ? C1 C2 1.530(15) . ? C1' C2 1.333(16) . ? C3 C4 1.504(9) . ? C3 H11 1.04(7) . ? C3 H12 1.06(7) . ? C4 H13 1.00(7) . ? C4 H14 0.95(7) . ? 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 O4 Zn1 O3 116.69(17) . . ? O4 Zn1 O1 109.01(17) . 2_665 ? O3 Zn1 O1 108.41(17) . 2_665 ? O4 Zn1 O5 112.16(16) . 2_655 ? O3 Zn1 O5 104.15(17) . 2_655 ? O1 Zn1 O5 105.79(17) 2_665 2_655 ? O8 Zn2 O7 115.26(19) 2_666 . ? O8 Zn2 O6 101.87(16) 2_666 . ? O7 Zn2 O6 110.06(16) . . ? O8 Zn2 O2 112.0(2) 2_666 . ? O7 Zn2 O2 103.89(16) . . ? O6 Zn2 O2 114.10(16) . . ? N1 Ni1 N2 82.13(19) . . ? N1 Ni1 O9 92.81(16) . 2_776 ? N2 Ni1 O9 174.53(16) . 2_776 ? N1 Ni1 N3 97.7(2) . . ? N2 Ni1 N3 82.9(2) . . ? O9 Ni1 N3 99.91(17) 2_776 . ? N1 Ni1 OW1 172.34(18) . . ? N2 Ni1 OW1 95.90(18) . . ? O9 Ni1 OW1 88.85(14) 2_776 . ? N3 Ni1 OW1 89.34(18) . . ? N1 Ni1 O9 87.11(18) . . ? N2 Ni1 O9 97.44(16) . . ? O9 Ni1 O9 80.17(13) 2_776 . ? N3 Ni1 O9 175.15(18) . . ? OW1 Ni1 O9 85.81(14) . . ? O1 P1 O3 115.8(2) . . ? O1 P1 O2 110.9(2) . . ? O3 P1 O2 112.7(2) . . ? O1 P1 H1 105(2) . . ? O3 P1 H1 102(2) . . ? O2 P1 H1 109(2) . . ? O4 P2 O6 114.3(2) . . ? O4 P2 O5 113.6(2) . . ? O6 P2 O5 111.1(2) . . ? O4 P2 H2 103(3) . . ? O6 P2 H2 108(3) . . ? O5 P2 H2 106(3) . . ? O8 P3 O7 112.8(2) . . ? O8 P3 O9 111.3(2) . . ? O7 P3 O9 112.69(19) . . ? O8 P3 H3 106(3) . . ? O7 P3 H3 112(3) . . ? O9 P3 H3 102(3) . . ? P1 O1 Zn1 143.6(3) . 2_665 ? P1 O2 Zn2 129.0(2) . . ? P1 O3 Zn1 132.1(3) . . ? P2 O4 Zn1 138.8(2) . . ? P2 O5 Zn1 133.6(2) . 2_655 ? P2 O6 Zn2 127.8(2) . . ? P3 O7 Zn2 127.6(2) . . ? P3 O8 Zn2 146.0(3) . 2_666 ? P3 O9 Ni1 121.91(18) . 2_776 ? P3 O9 Ni1 129.23(19) . . ? Ni1 O9 Ni1 99.83(13) 2_776 . ? Ni1 OW1 H4 124(4) . . ? Ni1 OW1 H5 120(4) . . ? H4 OW1 H5 99(5) . . ? C1 N1 C1' 30.8(7) . . ? C1 N1 Ni1 107.6(6) . . ? C1' N1 Ni1 110.8(6) . . ? C1 N1 H6 107(6) . . ? C1' N1 H6 130(6) . . ? Ni1 N1 H6 107(5) . . ? C1 N1 H7 122(6) . . ? C1' N1 H7 97(6) . . ? Ni1 N1 H7 119(6) . . ? H6 N1 H7 91(7) . . ? C3 N2 C2 114.4(5) . . ? C3 N2 Ni1 108.0(4) . . ? C2 N2 Ni1 109.1(4) . . ? C3 N2 H8 116(5) . . ? C2 N2 H8 111(5) . . ? Ni1 N2 H8 97(5) . . ? C4 N3 Ni1 108.4(4) . . ? C4 N3 H9 109(4) . . ? Ni1 N3 H9 110(4) . . ? C4 N3 H10 107(7) . . ? Ni1 N3 H10 113(8) . . ? H9 N3 H10 109(9) . . ? C1' C1 N1 76.3(15) . . ? C1' C1 C2 60.5(16) . . ? N1 C1 C2 106.0(8) . . ? C1 C1' C2 88(2) . . ? C1 C1' N1 72.9(16) . . ? C2 C1' N1 115.8(10) . . ? C1' C2 N2 118.3(7) . . ? C1' C2 C1 31.1(9) . . ? N2 C2 C1 114.8(6) . . ? N2 C3 C4 110.8(5) . . ? N2 C3 H11 111(4) . . ? C4 C3 H11 107(4) . . ? N2 C3 H12 108(4) . . ? C4 C3 H12 112(4) . . ? H11 C3 H12 107(5) . . ? N3 C4 C3 108.4(5) . . ? N3 C4 H13 107(4) . . ? C3 C4 H13 112(4) . . ? N3 C4 H14 109(4) . . ? C3 C4 H14 114(4) . . ? H13 C4 H14 106(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.792 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.134