Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_sad _database_code_CSD 177858 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Natarajan, Srinivasan' _publ_contact_author_name 'Prof Srinivasan Natarajan' _publ_contact_author_address ; Framework Solids Laboratory, Chemistry and Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jakkur P.O Bangalore 500 064 INDIA ; _publ_contact_author_email 'RAJ@JNCASR.AC.IN' _publ_section_title ; Synthesis and Structure of a Layered Zinc Phosphate-Acetate, [C5H10NH2]2[ZnOOCCH3)(PO4)(HPO4)] ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H28 N2 O10 P2 Zn2' _chemical_formula_weight 553.04 _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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1374(10) _cell_length_b 9.1963(11) _cell_length_c 12.9915(15) _cell_angle_alpha 91.421(2) _cell_angle_beta 104.988(2) _cell_angle_gamma 110.162(2) _cell_volume 982.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method ? _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 2.660 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4129 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 23.32 _reflns_number_total 2767 _reflns_number_observed 1801 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _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^)+(0.0370P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2767 _refine_ls_number_parameters 254 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_obs 0.0448 _refine_ls_wR_factor_all 0.1050 _refine_ls_wR_factor_obs 0.0902 _refine_ls_goodness_of_fit_all 0.933 _refine_ls_goodness_of_fit_obs 1.019 _refine_ls_restrained_S_all 0.996 _refine_ls_restrained_S_obs 1.111 _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 0.24986(10) 0.52302(10) 0.51251(7) 0.0226(3) Uani 1 d . . Zn2 Zn 0.92905(10) 0.92552(9) 0.63995(7) 0.0223(3) Uani 1 d . . P1 P 0.6360(2) 0.6287(2) 0.6533(2) 0.0204(5) Uani 1 d . . P2 P -0.0671(2) 0.2348(2) 0.5041(2) 0.0210(5) Uani 1 d . . O1 O 0.2159(5) 0.7175(5) 0.5103(4) 0.0314(14) Uani 1 d . . O2 O 0.2886(6) 0.4878(5) 0.3750(4) 0.0266(13) Uani 1 d . . O3 O 0.0882(5) 0.3730(5) 0.5667(4) 0.0264(13) Uani 1 d . . O4 O 0.4540(5) 0.5580(6) 0.6207(4) 0.0354(14) Uani 1 d . . O5 O 0.9087(6) 1.0942(6) 0.5643(4) 0.0356(14) Uani 1 d . . O6 O 1.0518(5) 0.8038(5) 0.6075(4) 0.0268(13) Uani 1 d . . O7 O 1.0444(7) 1.0245(7) 0.7888(4) 0.046(2) Uani 1 d . . O8 O 0.6993(5) 0.7820(5) 0.6073(4) 0.0238(12) Uani 1 d . . O9 O 0.6868(6) 0.6614(6) 0.7797(4) 0.0345(14) Uani 1 d . . H30 H 0.7862 0.7005 0.8027 0.052 Uiso 1 calc R . O10 O 1.0031(7) 0.8042(8) 0.8641(5) 0.064(2) Uani 1 d . . C1 C 1.0688(10) 0.9482(12) 0.8661(7) 0.040(2) Uani 1 d . . C2 C 1.1907(10) 1.0363(10) 0.9706(6) 0.048(3) Uani 1 d . . H25 H 1.1829 1.1366 0.9821 0.072 Uiso 1 calc R . H26 H 1.2985 1.0501 0.9675 0.072 Uiso 1 calc R . H27 H 1.1684 0.9782 1.0287 0.072 Uiso 1 calc R . N1 N 0.1048(7) 0.5643(8) 0.7439(5) 0.040(2) Uani 1 d D . H2 H 0.0566 0.6306 0.7160 0.048 Uiso 1 calc R . H1 H 0.1024 0.5022 0.6884 0.048 Uiso 1 calc R . C11 C 0.2749(10) 0.6565(13) 0.7987(8) 0.085(4) Uani 1 d D . H3 H 0.3350 0.6751 0.7458 0.103 Uiso 1 calc R . H4 H 0.2811 0.7572 0.8280 0.103 Uiso 1 calc R . C12 C 0.3547(12) 0.5891(16) 0.8842(10) 0.129(6) Uani 1 d D . H5 H 0.4456 0.6736 0.9318 0.155 Uiso 1 calc R . H6 H 0.3997 0.5238 0.8527 0.155 Uiso 1 calc R . C13 C 0.2566(10) 0.4933(11) 0.9517(7) 0.062(3) Uani 1 d D . H7 H 0.2546 0.5626 1.0084 0.075 Uiso 1 calc R . H8 H 0.3099 0.4247 0.9854 0.075 Uiso 1 calc R . C14 C 0.0836(11) 0.3957(14) 0.8893(10) 0.111(5) Uani 1 d D . H9 H 0.0828 0.2987 0.8576 0.133 Uiso 1 calc R . H10 H 0.0188 0.3694 0.9395 0.133 Uiso 1 calc R . C15 C 0.0058(11) 0.4669(14) 0.8051(8) 0.098(5) Uani 1 d D . H11 H -0.0410 0.5298 0.8371 0.117 Uiso 1 calc R . H12 H -0.0836 0.3842 0.7551 0.117 Uiso 1 calc R . N2 N 0.5193(7) 0.8100(7) 0.3962(5) 0.030(2) Uani 1 d . . H13 H 0.4365 0.7171 0.3810 0.036 Uiso 1 calc R . H14 H 0.5681 0.8254 0.4674 0.036 Uiso 1 calc R . C21 C 0.4538(9) 0.9354(9) 0.3670(6) 0.033(2) Uani 1 d . . H15 H 0.5411 1.0365 0.3901 0.040 Uiso 1 calc R . H16 H 0.3729 0.9305 0.4040 0.040 Uiso 1 calc R . C22 C 0.3771(10) 0.9187(10) 0.2464(7) 0.048(3) Uani 1 d . . H17 H 0.2782 0.8268 0.2257 0.058 Uiso 1 calc R . H18 H 0.3478 1.0089 0.2289 0.058 Uiso 1 calc R . C23 C 0.4908(12) 0.9047(11) 0.1826(7) 0.058(3) Uani 1 d . . H19 H 0.5808 1.0035 0.1934 0.070 Uiso 1 calc R . H20 H 0.4327 0.8812 0.1067 0.070 Uiso 1 calc R . C24 C 0.5569(10) 0.7756(10) 0.2178(7) 0.045(2) Uani 1 d . . H21 H 0.4684 0.6750 0.2003 0.054 Uiso 1 calc R . H22 H 0.6345 0.7732 0.1796 0.054 Uiso 1 calc R . C25 C 0.6385(9) 0.8063(10) 0.3373(7) 0.039(2) Uani 1 d . . H23 H 0.6803 0.7248 0.3594 0.046 Uiso 1 calc R . H24 H 0.7293 0.9054 0.3544 0.046 Uiso 1 calc R . 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 0.0159(5) 0.0179(5) 0.0362(6) 0.0040(4) 0.0086(4) 0.0078(4) Zn2 0.0209(5) 0.0167(5) 0.0295(6) 0.0042(4) 0.0068(4) 0.0072(4) P1 0.0142(11) 0.0175(12) 0.0294(13) 0.0037(9) 0.0060(10) 0.0058(9) P2 0.0158(11) 0.0139(11) 0.0349(13) 0.0038(10) 0.0072(10) 0.0073(9) O1 0.019(3) 0.017(3) 0.067(4) 0.004(3) 0.017(3) 0.015(2) O2 0.027(3) 0.023(3) 0.036(3) 0.007(2) 0.010(3) 0.016(2) O3 0.014(3) 0.025(3) 0.038(3) 0.003(2) 0.010(2) 0.003(2) O4 0.013(3) 0.037(4) 0.050(3) 0.013(3) 0.003(3) 0.006(2) O5 0.041(3) 0.023(3) 0.050(4) 0.020(3) 0.018(3) 0.016(3) O6 0.023(3) 0.029(3) 0.033(3) 0.006(3) 0.009(2) 0.014(2) O7 0.051(4) 0.047(4) 0.029(4) 0.005(3) -0.003(3) 0.016(3) O8 0.021(3) 0.021(3) 0.030(3) 0.006(2) 0.007(2) 0.008(2) O9 0.027(3) 0.044(4) 0.032(3) 0.007(3) 0.010(3) 0.011(3) O10 0.050(4) 0.053(5) 0.058(4) 0.011(4) -0.010(3) -0.001(4) C1 0.023(5) 0.049(7) 0.037(6) -0.005(5) 0.006(4) 0.004(5) C2 0.044(6) 0.056(6) 0.034(5) 0.000(5) 0.001(5) 0.012(5) N1 0.049(5) 0.040(5) 0.033(4) 0.008(4) 0.009(4) 0.020(4) C11 0.049(7) 0.094(10) 0.087(9) 0.033(8) 0.016(7) -0.004(7) C12 0.048(8) 0.159(14) 0.133(12) 0.082(11) -0.010(8) 0.001(9) C13 0.055(7) 0.073(8) 0.047(6) 0.015(6) -0.007(6) 0.024(6) C14 0.061(8) 0.129(12) 0.125(11) 0.083(10) 0.007(8) 0.023(8) C15 0.037(6) 0.128(12) 0.080(8) 0.047(8) 0.003(6) -0.020(7) N2 0.028(4) 0.029(4) 0.029(4) 0.010(3) 0.010(3) 0.003(3) C21 0.033(5) 0.026(5) 0.037(5) 0.007(4) 0.008(4) 0.008(4) C22 0.048(6) 0.048(6) 0.051(6) 0.010(5) -0.001(5) 0.031(5) C23 0.085(8) 0.065(7) 0.041(6) 0.018(5) 0.017(6) 0.047(6) C24 0.048(6) 0.041(6) 0.053(6) -0.002(5) 0.027(5) 0.016(5) C25 0.022(5) 0.033(5) 0.060(6) 0.013(5) 0.008(5) 0.011(4) _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 1.918(5) . ? Zn1 O3 1.940(4) . ? Zn1 O4 1.941(5) . ? Zn1 O2 1.950(5) . ? Zn2 O5 1.894(5) . ? Zn2 O6 1.943(5) . ? Zn2 O7 1.968(5) . ? Zn2 O8 1.982(4) . ? P1 O4 1.498(5) . ? P1 O8 1.529(5) . ? P1 O2 1.542(5) 2_666 ? P1 O9 1.576(5) . ? P2 O5 1.508(5) 1_445 ? P2 O1 1.535(5) 2_566 ? P2 O6 1.537(5) 2_666 ? P2 O3 1.549(5) . ? O1 P2 1.535(5) 2_566 ? O2 P1 1.542(5) 2_666 ? O5 P2 1.508(5) 1_665 ? O6 P2 1.537(5) 2_666 ? O7 C1 1.256(10) . ? O9 H30 0.82 . ? O10 C1 1.248(10) . ? C1 C2 1.511(10) . ? C2 H25 0.96 . ? C2 H26 0.96 . ? C2 H27 0.96 . ? N1 C15 1.449(7) . ? N1 C11 1.460(8) . ? N1 H2 0.90 . ? N1 H1 0.90 . ? C11 C12 1.441(8) . ? C11 H3 0.97 . ? C11 H4 0.97 . ? C12 C13 1.501(8) . ? C12 H5 0.97 . ? C12 H6 0.97 . ? C13 C14 1.511(8) . ? C13 H7 0.97 . ? C13 H8 0.97 . ? C14 C15 1.445(8) . ? C14 H9 0.97 . ? C14 H10 0.97 . ? C15 H11 0.97 . ? C15 H12 0.97 . ? N2 C21 1.488(9) . ? N2 C25 1.494(9) . ? N2 H13 0.90 . ? N2 H14 0.90 . ? C21 C22 1.522(10) . ? C21 H15 0.97 . ? C21 H16 0.97 . ? C22 C23 1.522(12) . ? C22 H17 0.97 . ? C22 H18 0.97 . ? C23 C24 1.537(12) . ? C23 H19 0.97 . ? C23 H20 0.97 . ? C24 C25 1.510(10) . ? C24 H21 0.97 . ? C24 H22 0.97 . ? C25 H23 0.97 . ? C25 H24 0.97 . ? 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 O3 109.7(2) . . ? O1 Zn1 O4 107.1(2) . . ? O3 Zn1 O4 104.1(2) . . ? O1 Zn1 O2 104.8(2) . . ? O3 Zn1 O2 124.4(2) . . ? O4 Zn1 O2 105.7(2) . . ? O5 Zn2 O6 122.0(2) . . ? O5 Zn2 O7 103.7(2) . . ? O6 Zn2 O7 104.8(2) . . ? O5 Zn2 O8 101.9(2) . . ? O6 Zn2 O8 107.0(2) . . ? O7 Zn2 O8 118.4(2) . . ? O4 P1 O8 112.5(3) . . ? O4 P1 O2 111.7(3) . 2_666 ? O8 P1 O2 111.2(3) . 2_666 ? O4 P1 O9 104.8(3) . . ? O8 P1 O9 109.4(3) . . ? O2 P1 O9 106.9(3) 2_666 . ? O5 P2 O1 108.5(3) 1_445 2_566 ? O5 P2 O6 110.7(3) 1_445 2_666 ? O1 P2 O6 108.6(3) 2_566 2_666 ? O5 P2 O3 110.9(3) 1_445 . ? O1 P2 O3 109.4(3) 2_566 . ? O6 P2 O3 108.7(3) 2_666 . ? P2 O1 Zn1 134.9(3) 2_566 . ? P1 O2 Zn1 125.8(3) 2_666 . ? P2 O3 Zn1 129.2(3) . . ? P1 O4 Zn1 148.2(3) . . ? P2 O5 Zn2 166.5(4) 1_665 . ? P2 O6 Zn2 125.9(3) 2_666 . ? C1 O7 Zn2 123.1(6) . . ? P1 O8 Zn2 126.6(3) . . ? P1 O9 H30 109.5 . . ? O10 C1 O7 125.7(8) . . ? O10 C1 C2 116.4(8) . . ? O7 C1 C2 117.9(8) . . ? C1 C2 H25 109.5 . . ? C1 C2 H26 109.5 . . ? H25 C2 H26 109.5 . . ? C1 C2 H27 109.5 . . ? H25 C2 H27 109.5 . . ? H26 C2 H27 109.5 . . ? C15 N1 C11 118.5(7) . . ? C15 N1 H2 107.7 . . ? C11 N1 H2 107.7 . . ? C15 N1 H1 107.7 . . ? C11 N1 H1 107.7 . . ? H2 N1 H1 107.1 . . ? C12 C11 N1 116.1(8) . . ? C12 C11 H3 108.3 . . ? N1 C11 H3 108.3 . . ? C12 C11 H4 108.3 . . ? N1 C11 H4 108.3 . . ? H3 C11 H4 107.4 . . ? C11 C12 C13 118.3(9) . . ? C11 C12 H5 107.7 . . ? C13 C12 H5 107.7 . . ? C11 C12 H6 107.7 . . ? C13 C12 H6 107.7 . . ? H5 C12 H6 107.1 . . ? C12 C13 C14 113.7(8) . . ? C12 C13 H7 108.8 . . ? C14 C13 H7 108.8 . . ? C12 C13 H8 108.8 . . ? C14 C13 H8 108.8 . . ? H7 C13 H8 107.7 . . ? C15 C14 C13 115.9(9) . . ? C15 C14 H9 108.3 . . ? C13 C14 H9 108.3 . . ? C15 C14 H10 108.3 . . ? C13 C14 H10 108.3 . . ? H9 C14 H10 107.4 . . ? C14 C15 N1 117.8(9) . . ? C14 C15 H11 107.9 . . ? N1 C15 H11 107.9 . . ? C14 C15 H12 107.9 . . ? N1 C15 H12 107.9 . . ? H11 C15 H12 107.2 . . ? C21 N2 C25 112.0(6) . . ? C21 N2 H13 109.2 . . ? C25 N2 H13 109.2 . . ? C21 N2 H14 109.2 . . ? C25 N2 H14 109.2 . . ? H13 N2 H14 107.9 . . ? N2 C21 C22 111.1(7) . . ? N2 C21 H15 109.4 . . ? C22 C21 H15 109.4 . . ? N2 C21 H16 109.4 . . ? C22 C21 H16 109.4 . . ? H15 C21 H16 108.0 . . ? C23 C22 C21 112.3(7) . . ? C23 C22 H17 109.2 . . ? C21 C22 H17 109.2 . . ? C23 C22 H18 109.2 . . ? C21 C22 H18 109.2 . . ? H17 C22 H18 107.9 . . ? C22 C23 C24 111.0(7) . . ? C22 C23 H19 109.4 . . ? C24 C23 H19 109.4 . . ? C22 C23 H20 109.4 . . ? C24 C23 H20 109.4 . . ? H19 C23 H20 108.0 . . ? C25 C24 C23 109.7(8) . . ? C25 C24 H21 109.7 . . ? C23 C24 H21 109.7 . . ? C25 C24 H22 109.7 . . ? C23 C24 H22 109.7 . . ? H21 C24 H22 108.2 . . ? N2 C25 C24 109.8(6) . . ? N2 C25 H23 109.7 . . ? C24 C25 H23 109.7 . . ? N2 C25 H24 109.7 . . ? C24 C25 H24 109.7 . . ? H23 C25 H24 108.2 . . ? _refine_diff_density_max 0.747 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.198