Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_sad1 _database_code_CSD 172864 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Choudhury, Amitava' 'Natarajan, Srinivasan' 'Neeraj, S.' 'Rao, C. N. R.' _publ_contact_author_name 'Prof C N R Rao' _publ_contact_author_address ; Prof C. N. R. Rao Chemistry and Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jakkur P.O. Bangalore - 560 064 INDIA ; _publ_contact_author_email 'CNRRAO@JNCASR.AC.IN' _publ_section_title ; Transformations of Two-Dimensional Layered Zinc Phosphates to Three-Dimensional and One-Dimensional Structures ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C1.50 N O4.50 P Zn' _chemical_formula_weight 200.36 _chemical_melting_point ? _chemical_compound_source ? 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' '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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.9824(5) _cell_length_b 7.6791(3) _cell_length_c 6.6178(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1167.94(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.279 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 4.420 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.823248 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4347 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.25 _reflns_number_total 844 _reflns_number_observed 671 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.040' _computing_cell_refinement ? _computing_data_reduction 'SAINT software V4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+16.5597P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 844 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_obs 0.0564 _refine_ls_wR_factor_all 0.1285 _refine_ls_wR_factor_obs 0.1188 _refine_ls_goodness_of_fit_all 1.230 _refine_ls_goodness_of_fit_obs 1.290 _refine_ls_restrained_S_all 1.230 _refine_ls_restrained_S_obs 1.290 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.73810(5) 0.5054(2) 0.09403(15) 0.0169(4) Uani 1 d . . P1 P 0.82695(11) 0.7044(3) 0.3405(4) 0.0152(6) Uani 1 d . . O1 O 0.6879(3) 0.3084(9) 0.1502(10) 0.024(2) Uani 1 d . . O2 O 0.6830(3) 0.6901(9) 0.0344(10) 0.021(2) Uani 1 d . . O3 O 0.7820(3) 0.5476(8) 0.3471(10) 0.017(2) Uani 1 d . . O4 O 0.8881(3) 0.6336(9) 0.3290(10) 0.023(2) Uani 1 d . . N1 N -0.1034(4) 0.2821(12) 0.3653(14) 0.031(2) Uiso 1 d . . C2 C 0.0000 0.2770(25) 0.2500 0.051(5) Uiso 1 d S . O20 O 0.0216(6) 0.2188(19) 0.4861(24) 0.034(4) Uiso 0.50 d P . C1 C -0.0468(9) 0.2137(28) 0.3786(39) 0.027(8) Uiso 0.52(4) d P . C1A C -0.0550(9) 0.2053(27) 0.2430(39) 0.020(8) Uiso 0.48(4) d P . 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 0.0185(7) 0.0186(6) 0.0135(6) 0.0012(5) -0.0004(5) 0.0001(6) P1 0.0169(13) 0.0138(13) 0.0150(14) 0.0010(11) 0.0008(12) 0.0010(11) O1 0.029(4) 0.022(4) 0.020(4) 0.012(4) -0.006(4) -0.007(3) O2 0.020(4) 0.024(4) 0.018(4) -0.001(3) 0.002(3) 0.004(3) O3 0.021(4) 0.017(4) 0.015(3) 0.004(3) -0.004(3) -0.006(3) O4 0.018(4) 0.024(4) 0.027(4) -0.006(3) 0.004(3) 0.005(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 O1 1.938(6) . ? Zn1 O2 1.942(6) . ? Zn1 O3 1.963(6) 7_565 ? Zn1 O3 1.981(6) . ? P1 O4 1.510(7) . ? P1 O1 1.530(7) 8_765 ? P1 O2 1.535(7) 2_665 ? P1 O3 1.588(6) . ? O1 P1 1.530(7) 8_755 ? O2 P1 1.535(7) 2_664 ? O3 Zn1 1.963(6) 7_566 ? N1 C1 1.40(2) . ? N1 C1A 1.50(2) . ? C2 C1A 1.38(2) . ? C2 C1A 1.38(2) 3 ? C2 C1 1.46(2) . ? C2 C1 1.46(2) 3 ? C2 O20 1.70(2) 3 ? C2 O20 1.70(2) . ? O20 C1A 1.70(3) 3 ? O20 C1 1.73(3) . ? C1 C1A 0.92(2) . ? C1A O20 1.70(3) 3 ? 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 102.8(3) . . ? O1 Zn1 O3 107.7(3) . 7_565 ? O2 Zn1 O3 108.5(3) . 7_565 ? O1 Zn1 O3 105.6(3) . . ? O2 Zn1 O3 112.6(3) . . ? O3 Zn1 O3 118.5(3) 7_565 . ? O4 P1 O1 110.8(4) . 8_765 ? O4 P1 O2 111.8(4) . 2_665 ? O1 P1 O2 112.3(4) 8_765 2_665 ? O4 P1 O3 109.6(4) . . ? O1 P1 O3 105.9(4) 8_765 . ? O2 P1 O3 106.3(4) 2_665 . ? P1 O1 Zn1 134.3(4) 8_755 . ? P1 O2 Zn1 130.8(4) 2_664 . ? P1 O3 Zn1 121.0(4) . 7_566 ? P1 O3 Zn1 115.6(4) . . ? Zn1 O3 Zn1 114.1(3) 7_566 . ? C1 N1 C1A 36.8(10) . . ? C1A C2 C1A 133.0(24) . 3 ? C1A C2 C1 37.7(10) . . ? C1A C2 C1 121.6(15) 3 . ? C1A C2 C1 121.6(15) . 3 ? C1A C2 C1 37.7(10) 3 3 ? C1 C2 C1 141.0(23) . 3 ? C1A C2 O20 66.2(12) . 3 ? C1A C2 O20 101.2(13) 3 3 ? C1 C2 O20 103.5(12) . 3 ? C1 C2 O20 65.8(11) 3 3 ? C1A C2 O20 101.2(13) . . ? C1A C2 O20 66.2(12) 3 . ? C1 C2 O20 65.8(11) . . ? C1 C2 O20 103.5(12) 3 . ? O20 C2 O20 149.5(17) 3 . ? C2 O20 C1A 47.9(9) . 3 ? C2 O20 C1 50.3(9) . . ? C1A O20 C1 92.5(12) 3 . ? C1A C1 N1 77.0(22) . . ? C1A C1 C2 66.7(20) . . ? N1 C1 C2 121.5(17) . . ? C1A C1 O20 126.2(25) . . ? N1 C1 O20 149.3(18) . . ? C2 C1 O20 63.9(10) . . ? C1 C1A C2 75.6(21) . . ? C1 C1A N1 66.2(20) . . ? C2 C1A N1 120.3(17) . . ? C1 C1A O20 140.6(25) . 3 ? C2 C1A O20 65.9(11) . 3 ? N1 C1A O20 142.5(16) . 3 ? _refine_diff_density_max 0.963 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.160