# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1146 data_crystal #================================== # CRYSTAL DATA _chemical_name_systematic ; Lithium zinc monohydrogenphosphate phosphate ethylenediamine dication hydrate ; _chemical_formula_structural 'LiZn(HPO~4~)(PO~4~).enH~2~.H~2~O' _chemical_formula_sum 'C2 H13 Li N2 O9 P2 Zn' _chemical_formula_weight 343.41 _symmetry_cell_setting 'Monoclinic, b-unique' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '+x,-y,1/2+z' '-x,-y,-z' '-x,+y,1/2-z' '1/2+x,1/2+y,+z' '1/2+x,1/2-y,1/2+z' '1/2-x,1/2-y,-z' '1/2-x,1/2+y,1/2-z' _cell_length_a 18.068(2) _cell_length_b 5.3034(6) _cell_length_c 21.065(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.992(2) _cell_angle_gamma 90.00 _cell_volume 2017.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description 'triangle, plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.794 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.93 #================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120(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 SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_reflns_number 4108 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.038 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 25 _diffrn_reflns_reduction_process 4108 _reflns_number_total 1616 _reflns_number_observed 1122 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR92 Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Burla,M.C., Polidori,G. & Camalli,M. (1994). J.Appl. Cryst. 27, 435. ; _computing_structure_refinement ; KRYSTAL Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. Modified ORFLS(1962) Busing,W.T., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. ; _computing_molecular_graphics ; ATOMS ver. 4.0 E. Dowty (1997), Program ATOMS 4.0, Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # REFINEMENT DATA _refine_ls_structure_factor_coef Fsq _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/[\s~cs~(F^2^)+0.03F^2^]^2^ ; _refine_ls_hydrogen_treatment calc _refine_ls_extinction_method ; Becker-Coppens type 1, Lorentzian isotropic Becker,P.J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. ; _refine_ls_extinction_coef 95(19) _refine_ls_number_reflns 1122 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_number_constraints 8 _refine_ls_R_factor_obs 0.027 _refine_ls_wR_factor_obs 0.035 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.25(6) _refine_diff_density_min -0.22(6) #========================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 Zn 0.03911(3) 0.19605(9) 0.57437(2) 0.0066(3) Uij 1. P1 -0.06006(6) -0.29998(22) 0.57040(5) 0.0053(6) Uij 1. P2 0.19355(6) 0.19421(21) 0.65331(5) 0.0051(6) Uij 1. O1 -0.1179(2) -0.2435(5) 0.6203(1) 0.012(2) Uij 1. O2 -0.0458(1) -0.5860(5) 0.5729(1) 0.011(2) Uij 1. O3 -0.0927(2) -0.2264(5) 0.5047(1) 0.009(2) Uij 1. O4 0.0123(2) -0.1560(5) 0.5849(1) 0.009(2) Uij 1. O5 0.1941(1) -0.0916(5) 0.6626(1) 0.008(2) Uij 1. O6 0.1149(1) 0.2920(5) 0.6381(1) 0.009(2) Uij 1. O7 0.2285(1) 0.3357(5) 0.7097(1) 0.007(2) Uij 1. O8 0.2393(1) 0.2568(5) 0.5926(1) 0.009(2) Uij 1. Ow 0.1351(2) -0.2066(7) 0.3279(2) 0.013(2) Uij 1. LI 0.2654(4) -0.3066(14) 0.7060(3) 0.011(4) Uij 1. N1 0.1589(2) -0.3016(9) 0.5384(2) 0.008(2) Uij 1. C1 0.2115(2) -0.2037(9) 0.4916(2) 0.007(2) Uij 1. HO8 0.287 0.257 0.602 0.01 Uiso 1. Hw1 0.126(3) -0.063(13) 0.343(3) 0.06(2) Uiso 1. Hw2 0.114(3) -0.312(12) 0.359(3) 0.06(2) Uiso 1. H1a 0.199(2) -0.274(8) 0.452(2) 0.00 Uiso 1. H1b 0.210(2) -0.018(8) 0.494(2) 0.00 Uiso 1. HN1a 0.160(2) -0.459(10) 0.536(2) 0.01(1) Uiso 1. HN1b 0.115(3) -0.245(10) 0.531(3) 0.03(2) Uiso 1. HN1c 0.175(2) -0.256(7) 0.577(2) 0.00 Uiso 1. N21 0.1056(7) -0.3452(25) 0.7504(6) 0.009(1) Uiso 0.5 C21 0.0263(4) -0.4321(18) 0.7402(4) 0.011(4) Uij 0.5 N22 -0.1008(7) -0.3252(25) 0.7604(6) 0.009 Uiso 0.5 C22 -0.0237(4) -0.2218(17) 0.7604(4) 0.007 Uiso 0.5 H21a 0.018 -0.579 0.766 0.03(2) Uiso 0.5 H21b 0.017 -0.470 0.698 0.03 Uiso 0.5 H22a -0.021 -0.084 0.733 0.03 Uiso 0.5 H22b -0.010 -0.167 0.803 0.03 Uiso 0.5 HN21a 0.137 -0.479 0.739 0.03(1) Uiso 0.5 HN21b 0.115 -0.309 0.795 0.03 Uiso 0.5 HN21c 0.114 -0.201 0.727 0.03 Uiso 0.5 HN22a -0.133 -0.191 0.774 0.03 Uiso 0.5 HN22b -0.104 -0.461 0.790 0.03 Uiso 0.5 HN22c -0.115 -0.378 0.719 0.03 Uiso 0.5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn 0.0055(3) 0.0047(3) 0.0097(3) 0.0004(2) -0.0007(2) 0.0004(2) P1 0.0047(6) 0.0042(6) 0.0071(7) 0.0011(5) 0.0003(5) -0.0001(5) P2 0.0050(6) 0.0034(6) 0.0067(6) -0.0009(5) -0.0009(5) 0.0000(5) O1 0.009(2) 0.016(2) 0.011(2) 0.002(1) 0.002(1) -0.001(1) O2 0.006(2) 0.004(2) 0.022(2) 0.001(1) 0.000(1) 0.000(1) O3 0.008(2) 0.010(2) 0.010(2) 0.002(1) -0.003(1) 0.001(1) O4 0.008(2) 0.004(2) 0.017(2) -0.001(1) -0.001(1) 0.001(1) O5 0.011(2) 0.003(2) 0.010(2) -0.001(1) 0.000(1) 0.000(1) O6 0.006(2) 0.007(2) 0.012(2) 0.002(1) -0.002(1) -0.001(1) O7 0.009(2) 0.003(2) 0.009(2) -0.002(1) -0.002(1) -0.001(1) O8 0.004(2) 0.011(2) 0.011(2) 0.000(1) -0.001(1) 0.001(1) Ow 0.016(2) 0.008(2) 0.015(2) -0.002(2) 0.004(1) -0.002(2) LI 0.008(4) 0.013(4) 0.012(4) 0.001(3) -0.005(3) 0.003(3) N1 0.008(2) 0.005(2) 0.013(2) 0.004(2) -0.001(2) -0.002(2) C1 0.009(2) 0.006(3) 0.007(3) -0.003(2) 0.002(2) -0.001(2) C21 0.007(4) 0.014(4) 0.012(4) -0.004(2) 0.000(3) -0.001(2) #================================= # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Zn O2 1.921(3) . 1_565 Zn O4 1.943(3) . . Zn O6 1.952(3) . . Zn O3 1.961(3) . 3_556 P1 O3 1.536(3) . . P1 O4 1.536(3) . . P1 O1 1.538(3) . . P1 O2 1.539(3) . . P2 O7 1.523(3) . . P2 O5 1.528(3) . . P2 O6 1.536(3) . . P2 O8 1.582(3) . . O5 LI 1.928(8) . . O7 LI 1.929(8) . 8_556 Ow LI 1.959(8) . 7_546 N1 C1 1.487(6) . . C1 C1 1.505(9) . 7_546 N21 C21 1.514(16) . . C21 C22 1.506(11) . . N22 C22 1.497(16) . . O8 HO8 0.868(3) . . Ow Hw1 0.85(7) . . Ow Hw2 0.95(7) . . N1 HN1a 0.84(5) . . N1 HN1b 0.86(6) . . N1 HN1c 0.895(49) . . C1 H1a 0.926(46) . . C1 H1b 0.988(45) . . N21 HN21a 0.948(14) . . N21 HN21b 0.967(13) . . N21 HN21c 0.931(13) . . C21 H21a 0.964(10) . . C21 H21b 0.929(10) . . N22 HN22a 0.963(14) . . N22 HN22b 0.952(14) . . N22 HN22c 0.935(12) . . C22 H22a 0.935(10) . . C22 H22b 0.974(10) . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 HN21b 1.819(3) . 4_556 O1 Hw1 1.81(7) . 3_556 O5 HN22a 1.847(3) . 4_556 O1 HO8 1.756(3) . 5_445 O1 HN22c 2.206(3) . . O1 Hw2 2.40(7) . 3_546 O1 O8 2.624(4) . 5_445 O1 Ow 2.648(5) . 3_556 O1 N21 2.778(13) . 4_556 O1 N22 2.988(13) . . O2 Hw2 2.00(7) . 3_546 O2 Ow 2.899(5) . 3_546 O3 HN1a 2.22(5) . 3_546 O3 N1 2.906(6) . 3_546 O4 HN1b 2.26(6) . . O4 N1 2.959(5) . . O5 HN22a 1.847(3) . 4_556 O5 HN1c 2.01(5) . . O5 HN21c 2.093(3) . . O5 N22 2.682(14) . 4_556 O5 N21 2.825(14) . . O5 N1 2.894(5) . . O6 HN22b 2.023(3) . 4_566 O6 N22 2.967(14) . 4_566 O6 HO8 3.226(3) . . O7 HN21a 2.034(3) . 1_565 O7 N21 2.943(14) . 1_565 O8 HN1a 2.37(5) . 1_565 O8 N1 2.964(6) . 1_565 Ow HN22c 2.439(4) . 3_546 Ow HN21a 2.516(4) . 2_544 Ow N21 2.923(14) . 2_544 Ow N22 3.152(13) . 3_546 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_2 _geom_angle_site_symmetry_3 O2 Zn O4 112.2(1) 1_565 . . O2 Zn O6 113.3(1) 1_565 . . O2 Zn O3 110.8(1) 1_565 . 3_556 O4 Zn O6 110.1(1) . . . O4 Zn O3 107.9(1) . . 3_556 O3 Zn O6 102.0(1) 3_556 . . O3 P1 O4 110.5(2) . . . O1 P1 O3 108.5(2) . . . O2 P1 O3 109.9(2) . . . O1 P1 O4 111.2(2) . . . O2 P1 O4 110.0(2) . . . O1 P1 O2 106.6(2) . . . O5 P2 O7 112.9(2) . . . O6 P2 O7 110.6(2) . . . O7 P2 O8 108.2(2) . . . O5 P2 O6 111.3(2) . . . O5 P2 O8 108.0(2) . . . O6 P2 O8 105.5(2) . . . Zn O2 P1 136.6(2) 1_545 . . Zn O3 P1 126.9(2) 3_556 . . Zn O4 P1 131.9(2) . . . P2 O5 LI 130.4(3) . . . Zn O6 P2 132.6(2) . . . P2 O7 LI 122.3(3) . . 8_556 O5 LI O7 102.8(4) . . 8_546 O7 LI Ow 107.3(4) 8_546 . 7_546 O5 LI Ow 114.4(4) . . 7_546 N1 C1 C1 109.7(5) . . 7_546 N21 C21 C22 108.0(8) . . . C21 C22 N22 107.2(8) . . . P1 O1 HN21b 129.5(2) . . 4_556 P1 O1 Hw1 122.3(19) . . 3_556 Hw1 O1 HN21b 75.8(21) 3_556 . 4_556 P2 O5 HN22a 112.0(2) . . 4_556 LI O5 HN22a 84.1(3) . . 4_556 P2 O8 HO8 110.9(3) . . . Hw1 Ow Hw2 100(6) . . . LI Ow Hw1 107(4) 7_546 . . LI Ow Hw2 132(4) 7_546 . . HN1a N1 HN1b 111(5) . . . HN1a N1 HN1c 109(4) . . . C1 N1 HN1a 106.3(31) . . . H1a N1 HN1a 89.9(34) . . . HN1b N1 HN1c 110(5) . . . C1 N1 HN1b 111(4) . . . H1a N1 HN1b 100(4) . . . C1 N1 HN1c 108.9(28) . . . H1a N1 HN1c 135.0(31) . . . C1 N1 H1a 26.5(12) . . . H1a C1 H1b 116(4) . . . N1 C1 H1a 107.6(26) . . . C1 C1 H1a 106.3(26) 7_546 . . H1a C1 HN1a 92.0(30) . . . H1a C1 HN1c 132.7(30) . . . N1 C1 H1b 106.8(23) . . . C1 C1 H1b 110.5(24) 7_546 . . H1b C1 HN1a 131.8(28) . . . H1b C1 HN1c 94.6(27) . . . N1 C1 HN1a 25.0(15) . . . N1 C1 HN1c 25.5(13) . . . C1 C1 HN1a 96.6(15) 7_546 . . C1 C1 HN1c 94.4(13) 7_546 . . HN1a C1 HN1c 42.7(19) . . . HN1a C1 HN1c 42.7(19) . . . HN21a N21 HN21c 111.6(14) . . . HN21b N21 HN21c 109.6(14) . . . C21 N21 HN21c 110.0(11) . . . HN21a N21 HN21b 108.6(12) . . . C21 N21 HN21a 107.8(12) . . . C21 N21 HN21b 109.2(12) . . . H21a C21 H21b 110.1(10) . . . C22 C21 H21b 110.2(9) . . . N21 C21 H21b 109.9(8) . . . C22 C21 H21a 109.5(8) . . . N21 C21 H21a 109.2(9) . . . HN22b N22 HN22c 110.6(13) . . . HN22a N22 HN22c 110.1(13) . . . C22 N22 HN22c 109.8(12) . . . HN22a N22 HN22b 108.7(13) . . . C22 N22 HN22b 110.4(11) . . . C22 N22 HN22a 107.0(11) . . . H22a C22 H22b 108.7(9) . . . N22 C22 H22a 110.7(9) . . . C21 C22 H22a 111.2(8) . . . N22 C22 H22b 108.9(8) . . . C21 C22 H22b 110.2(8) . . . #================================= # TITLE AND AUTHOR LIST _publ_section_title ; A novel layered templated lithium zinc phosphate prepared by an unusual solution mediated technique ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. loop_ _publ_author_name _publ_author_address 'Jensen, Torben R.' ; Chemistry Department University of Odense DK-5230 Odense M Denmark ; 'Hazell, Rita G.' ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; _publ_contact_author ; Torben R. Jensen Chemistry Department University of Odense DK-5230 Odense M Denmark ; _publ_contact_author_phone '+45 6557 2579' _publ_contact_author_fax '+45 6615 8780' _publ_contact_author_email trj@gamma.dou.dk