Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Guo-Yu Yang' 'Zhi-En Lin' 'Youwei Yao' 'Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Coordination and Hydrothermal Chemi 155 Yangqiao West Road Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email YGY@MS.FJIRSM.AC.CN _publ_contact_author_name 'Prof Guo-Yu Yang' _publ_section_title ; Synthesis and structure of a novel open-framwork zincophosphate with intersecting three-dimensional helical channels ; data_FJ-13 _database_code_CSD 191451 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common FJ-13 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H3 O4.50 P Zn0.50' _chemical_formula_weight 138.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fd2d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, y+1/4, -z+1/4' 'x, y+1/2, z+1/2' '-x, y+1/2, -z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, y+3/4, -z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, y, -z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, y+1/4, -z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, y+3/4, -z+1/4' _cell_length_a 9.8812(7) _cell_length_b 15.1899(10) _cell_length_c 16.0041(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2402.1(3) _cell_formula_units_Z 20 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 2.904 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.721375 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 1785 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.06 _reflns_number_total 877 _reflns_number_gt 865 _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^)+(0.1120P)^2^+6.1118P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 877 _refine_ls_number_parameters 56 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.201 _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 Zn Zn 0.0000 0.959905(17) 0.0000 0.0244(4) Uani 1 2 d S . . P P 0.03418(18) 1.11535(13) 0.12902(10) 0.0286(5) Uani 1 1 d . . . O1 O 0.0805(5) 1.0321(4) 0.0853(3) 0.0349(11) Uani 1 1 d . . . O2 O 0.1398(6) 0.8838(4) -0.0406(3) 0.0459(15) Uani 1 1 d . . . O3 O 0.0434(7) 1.1955(4) 0.0699(3) 0.0436(14) Uani 1 1 d . . . H H -0.0325 1.2159 0.0625 0.080 Uiso 1 1 calc R . . O4 O -0.1211(6) 1.1060(5) 0.1483(5) 0.0550(17) Uani 1 1 d . . . H H -0.1330 1.0653 0.1811 0.080 Uiso 1 1 calc R . . O1W O 0.2500 0.8516(7) 0.2500 0.056(3) Uani 1 2 d S . . 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 Zn 0.0375(6) 0.0160(6) 0.0198(5) 0.000 0.0008(4) 0.000 P 0.0364(9) 0.0205(10) 0.0289(9) -0.0056(7) -0.0037(7) -0.0079(8) O1 0.043(2) 0.030(3) 0.032(3) -0.007(2) -0.005(2) 0.005(2) O2 0.072(4) 0.040(3) 0.026(2) -0.002(2) 0.014(2) 0.026(3) O3 0.066(3) 0.024(3) 0.040(3) 0.003(2) -0.014(3) -0.014(3) O4 0.036(3) 0.036(4) 0.093(5) -0.014(4) 0.012(3) -0.001(2) O1W 0.051(5) 0.041(7) 0.078(8) 0.000 -0.009(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 Zn O2 1.914(5) 2 ? Zn O2 1.914(5) . ? Zn O1 1.924(5) . ? Zn O1 1.924(5) 2 ? P O1 1.515(6) . ? P O2 1.516(5) 3 ? P O3 1.544(6) . ? P O4 1.571(6) . ? O2 P 1.516(5) 7_544 ? O3 H 0.8200 . ? O4 H 0.8200 . ? 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 Zn O2 105.8(4) 2 . ? O2 Zn O1 113.7(2) 2 . ? O2 Zn O1 106.7(3) . . ? O2 Zn O1 106.7(3) 2 2 ? O2 Zn O1 113.7(2) . 2 ? O1 Zn O1 110.5(3) . 2 ? O1 P O2 113.4(3) . 3 ? O1 P O3 110.9(3) . . ? O2 P O3 110.2(3) 3 . ? O1 P O4 108.1(3) . . ? O2 P O4 109.5(4) 3 . ? O3 P O4 104.4(4) . . ? P O1 Zn 132.7(3) . . ? P O2 Zn 139.2(3) 7_544 . ? P O3 H 109.5 . . ? P O4 H 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.980 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.229