Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full J.Mater.Chem. _audit_creation_method SHELXL-97 _journal_coden_Cambridge 1145 loop_ _publ_author_name 'M. Stanley Whittingham' 'Yanning Song' 'Peter Y. Zavalij' _publ_contact_author_name 'Prof M Stanley Whittingham' _publ_contact_author_address ; Department of Chemistry SUNY at Binghamton Vestal Parkway East Binghamton New York 13902-6000 UNITED STATES OF AMERICA ; _publ_contact_author_email STANWHIT@BINGHAMTON.EDU _publ_section_title ; Two novel open-framework zinc phosphates: (CH3NH3)Zn4(PO4)3 and (CH3NH3)2Zn5(PO4)4 ; _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Dowty, E. (1999). ATOMS for Windows and Macintosh. Version 5. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA. Farrugia, L. J. (1997). J. Appl. Cryst., 30, 565-565. Spek A. L. (1990) Acta Cryst., A46, C-34. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of Gottingen, Germany. ; data_Zn4P3-0235 _database_code_CSD 208053 _audit_creation_method 'SHELXL-97 and ZCIF by Peter Y. Zavalij' _chemical_name_systematic ; ? ; _chemical_name_common 'methylammonium zinc phosphate' _chemical_formula_moiety '(C H3 N H3), Zn4 (P O4)3' _chemical_formula_sum 'C H6 N O12 P3 Zn4' _chemical_formula_weight 578.46 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.6797(6) _cell_length_b 10.1204(4) _cell_length_c 16.6015(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2466.39(17) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7051 _cell_measurement_theta_min 5.471 _cell_measurement_theta_max 62.610 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 3.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 8.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2750 _exptl_absorpt_correction_T_max 0.4807 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 295(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 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.05 _diffrn_reflns_number 27937 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.51 _reflns_number_total 3750 _reflns_number_gt 3409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+3.1020P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00128(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3750 _refine_ls_number_parameters 217 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.143310(17) 0.87693(2) 0.226671(15) 0.01001(7) Uani 1 1 d . . . Zn2 Zn 0.365668(17) 0.89255(2) 0.195273(16) 0.00995(7) Uani 1 1 d . . . Zn3 Zn 0.448530(18) 1.15139(2) 0.089206(16) 0.01154(7) Uani 1 1 d . . . Zn4 Zn 0.431142(18) 0.65219(3) 0.058045(16) 0.01128(7) Uani 1 1 d . . . P1 P 0.25741(4) 0.62824(5) 0.16315(3) 0.00832(10) Uani 1 1 d . . . P2 P 0.55109(4) 0.88202(5) 0.10500(3) 0.00902(11) Uani 1 1 d . . . P3 P 0.53918(4) 0.39803(5) 0.12570(3) 0.00910(11) Uani 1 1 d . . . O1 O 0.25332(10) 0.77675(16) 0.18759(10) 0.0119(3) Uani 1 1 d . . . O2 O 0.05174(11) 0.82628(17) 0.14889(11) 0.0159(3) Uani 1 1 d . . . O3 O 0.19700(12) 1.05113(16) 0.23111(10) 0.0159(3) Uani 1 1 d . . . O4 O 0.11792(11) 0.82320(17) 0.33431(10) 0.0149(3) Uani 1 1 d . . . O5 O 0.34181(10) 1.07592(15) 0.15445(10) 0.0114(3) Uani 1 1 d . . . O6 O 0.45376(11) 0.82081(16) 0.11795(10) 0.0135(3) Uani 1 1 d . . . O7 O 0.39314(13) 0.89155(19) 0.30601(10) 0.0209(4) Uani 1 1 d . . . O8 O 0.54329(12) 1.02991(16) 0.11857(12) 0.0189(4) Uani 1 1 d . . . O9 O 0.41612(12) 1.15847(19) -0.02184(10) 0.0192(4) Uani 1 1 d . . . O10 O 0.30641(12) 0.61394(17) 0.08388(11) 0.0173(3) Uani 1 1 d . . . O11 O 0.52127(13) 0.53793(16) 0.10017(12) 0.0218(4) Uani 1 1 d . . . O12 O 0.42425(11) 0.68738(17) -0.05594(9) 0.0145(3) Uani 1 1 d . . . C1 C 0.2458(2) 0.5902(4) 0.4616(2) 0.0314(7) Uani 1 1 d D . . H1C H 0.297(3) 0.544(4) 0.477(3) 0.078(15) Uiso 1 1 d D . . H2C H 0.220(4) 0.645(4) 0.500(3) 0.09(2) Uiso 1 1 d D . . H3C H 0.205(3) 0.526(4) 0.442(3) 0.084(17) Uiso 1 1 d D . . N1 N 0.26675(16) 0.6706(2) 0.39028(14) 0.0199(4) Uani 1 1 d D . . H1N H 0.3098(18) 0.719(3) 0.3998(19) 0.026(9) Uiso 1 1 d D . . H2N H 0.2212(19) 0.713(3) 0.378(2) 0.038(10) Uiso 1 1 d D . . H3N H 0.284(2) 0.627(3) 0.3522(18) 0.032(10) Uiso 1 1 d 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 0.00913(12) 0.01139(12) 0.00950(12) 0.00012(9) 0.00052(9) -0.00084(9) Zn2 0.00925(12) 0.01063(12) 0.00998(12) 0.00013(9) -0.00003(9) 0.00008(9) Zn3 0.01341(13) 0.01137(12) 0.00984(12) -0.00063(9) 0.00031(9) 0.00149(9) Zn4 0.01215(13) 0.01184(12) 0.00986(12) -0.00049(9) 0.00123(9) 0.00008(9) P1 0.0075(2) 0.0074(2) 0.0101(2) -0.00065(18) -0.00002(19) -0.00014(17) P2 0.0083(2) 0.0101(2) 0.0087(2) -0.00063(18) -0.00071(19) 0.00063(18) P3 0.0092(2) 0.0093(2) 0.0088(2) -0.00031(18) -0.00020(19) 0.00007(19) O1 0.0094(7) 0.0094(7) 0.0168(8) -0.0010(6) 0.0000(6) -0.0007(5) O2 0.0133(8) 0.0154(8) 0.0189(8) -0.0042(6) -0.0072(6) 0.0036(6) O3 0.0182(8) 0.0127(7) 0.0169(8) 0.0000(6) 0.0065(7) -0.0039(6) O4 0.0155(8) 0.0189(8) 0.0105(7) 0.0033(6) 0.0048(6) 0.0057(6) O5 0.0093(7) 0.0103(7) 0.0147(8) 0.0023(6) 0.0003(6) 0.0019(6) O6 0.0096(7) 0.0138(7) 0.0170(8) -0.0050(6) 0.0034(6) -0.0022(6) O7 0.0209(9) 0.0296(10) 0.0122(8) 0.0019(7) -0.0065(7) -0.0021(7) O8 0.0147(8) 0.0098(7) 0.0323(10) -0.0016(7) -0.0045(7) 0.0013(6) O9 0.0165(8) 0.0333(10) 0.0078(7) -0.0018(7) 0.0017(6) 0.0008(7) O10 0.0134(8) 0.0232(9) 0.0151(8) -0.0057(6) 0.0064(6) -0.0056(7) O11 0.0199(9) 0.0115(8) 0.0340(11) 0.0048(7) -0.0046(8) 0.0019(7) O12 0.0170(8) 0.0180(8) 0.0084(7) -0.0015(6) 0.0019(6) 0.0036(6) C1 0.0273(15) 0.0343(16) 0.0326(16) 0.0136(13) 0.0003(13) 0.0006(13) N1 0.0174(11) 0.0214(11) 0.0209(11) 0.0028(9) 0.0000(9) 0.0023(9) _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 1.9047(16) . ? Zn1 O3 1.9325(16) . ? Zn1 O2 1.9331(16) . ? Zn1 O1 2.0141(15) . ? Zn2 O7 1.8821(17) . ? Zn2 O6 1.9614(16) . ? Zn2 O5 2.0065(15) . ? Zn2 O1 2.0272(15) . ? Zn3 O9 1.9053(17) . ? Zn3 O8 1.9195(17) . ? Zn3 O2 2.0284(17) 8_665 ? Zn3 O5 2.0520(16) . ? Zn4 O11 1.8912(17) . ? Zn4 O10 1.9201(17) . ? Zn4 O12 1.9283(16) . ? Zn4 O6 2.0029(16) . ? P1 O10 1.5066(17) . ? P1 O3 1.5265(17) 8_655 ? P1 O5 1.5565(16) 8_655 ? P1 O1 1.5580(16) . ? P2 O8 1.5179(17) . ? P2 O9 1.5183(18) 5_675 ? P2 O4 1.5270(17) 6_656 ? P2 O6 1.5721(16) . ? P3 O11 1.5011(17) . ? P3 O7 1.5089(18) 3_645 ? P3 O12 1.5417(17) 5_665 ? P3 O2 1.5675(17) 8_655 ? P3 Zn3 2.8928(6) 1_545 ? C1 N1 1.469(4) . ? C1 H1C 0.93(3) . ? C1 H2C 0.93(3) . ? C1 H3C 0.93(3) . ? N1 H1N 0.82(2) . ? N1 H2N 0.82(2) . ? N1 H3N 0.81(2) . ? 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 107.72(7) . . ? O4 Zn1 O2 114.51(8) . . ? O3 Zn1 O2 123.43(7) . . ? O4 Zn1 O1 108.39(7) . . ? O3 Zn1 O1 98.31(7) . . ? O2 Zn1 O1 102.06(7) . . ? O7 Zn2 O6 119.74(8) . . ? O7 Zn2 O5 111.85(7) . . ? O6 Zn2 O5 103.67(7) . . ? O7 Zn2 O1 103.46(7) . . ? O6 Zn2 O1 106.33(6) . . ? O5 Zn2 O1 111.80(6) . . ? O9 Zn3 O8 116.79(8) . . ? O9 Zn3 O2 116.06(8) . 8_665 ? O8 Zn3 O2 115.86(7) . 8_665 ? O9 Zn3 O5 109.52(7) . . ? O8 Zn3 O5 100.42(7) . . ? O2 Zn3 O5 93.75(6) 8_665 . ? O11 Zn4 O10 117.47(8) . . ? O11 Zn4 O12 120.84(8) . . ? O10 Zn4 O12 101.91(7) . . ? O11 Zn4 O6 102.79(7) . . ? O10 Zn4 O6 102.65(7) . . ? O12 Zn4 O6 109.79(7) . . ? O10 P1 O3 112.78(10) . 8_655 ? O10 P1 O5 109.46(9) . 8_655 ? O3 P1 O5 107.76(9) 8_655 8_655 ? O10 P1 O1 109.79(9) . . ? O3 P1 O1 108.52(9) 8_655 . ? O5 P1 O1 108.43(8) 8_655 . ? O8 P2 O9 115.15(11) . 5_675 ? O8 P2 O4 109.56(10) . 6_656 ? O9 P2 O4 106.93(10) 5_675 6_656 ? O8 P2 O6 107.44(9) . . ? O9 P2 O6 107.83(10) 5_675 . ? O4 P2 O6 109.88(10) 6_656 . ? O11 P3 O7 111.62(11) . 3_645 ? O11 P3 O12 112.19(10) . 5_665 ? O7 P3 O12 108.10(10) 3_645 5_665 ? O11 P3 O2 110.92(10) . 8_655 ? O7 P3 O2 110.86(10) 3_645 8_655 ? O12 P3 O2 102.78(9) 5_665 8_655 ? O11 P3 Zn3 132.39(8) . 1_545 ? O7 P3 Zn3 115.01(8) 3_645 1_545 ? O12 P3 Zn3 61.25(7) 5_665 1_545 ? O2 P3 Zn3 42.27(6) 8_655 1_545 ? P1 O1 Zn1 126.90(9) . . ? P1 O1 Zn2 122.87(9) . . ? Zn1 O1 Zn2 109.94(7) . . ? P3 O2 Zn1 129.29(10) 8_665 . ? P3 O2 Zn3 106.42(9) 8_665 8_655 ? Zn1 O2 Zn3 123.99(8) . 8_655 ? P1 O3 Zn1 128.10(10) 8_665 . ? P2 O4 Zn1 129.31(10) 6_556 . ? P1 O5 Zn2 116.53(9) 8_665 . ? P1 O5 Zn3 129.55(9) 8_665 . ? Zn2 O5 Zn3 112.91(7) . . ? P2 O6 Zn2 122.88(9) . . ? P2 O6 Zn4 114.74(9) . . ? Zn2 O6 Zn4 122.08(8) . . ? P3 O7 Zn2 151.02(13) 3_655 . ? P2 O8 Zn3 130.43(11) . . ? P2 O9 Zn3 142.23(12) 5_675 . ? P1 O10 Zn4 129.13(11) . . ? P3 O11 Zn4 143.48(12) . . ? P3 O12 Zn4 127.98(10) 5_665 . ? N1 C1 H1C 110(3) . . ? N1 C1 H2C 108(3) . . ? H1C C1 H2C 117(5) . . ? N1 C1 H3C 104(3) . . ? H1C C1 H3C 105(4) . . ? H2C C1 H3C 113(5) . . ? C1 N1 H1N 110(2) . . ? C1 N1 H2N 108(3) . . ? H1N N1 H2N 111(3) . . ? C1 N1 H3N 113(2) . . ? H1N N1 H3N 104(3) . . ? H2N N1 H3N 110(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 P1 O1 Zn1 132.59(12) . . . . ? O3 P1 O1 Zn1 -103.74(12) 8_655 . . . ? O5 P1 O1 Zn1 13.05(14) 8_655 . . . ? O10 P1 O1 Zn2 -54.26(13) . . . . ? O3 P1 O1 Zn2 69.41(13) 8_655 . . . ? O5 P1 O1 Zn2 -173.80(10) 8_655 . . . ? O4 Zn1 O1 P1 73.71(13) . . . . ? O3 Zn1 O1 P1 -174.41(12) . . . . ? O2 Zn1 O1 P1 -47.50(13) . . . . ? O4 Zn1 O1 Zn2 -100.18(9) . . . . ? O3 Zn1 O1 Zn2 11.71(9) . . . . ? O2 Zn1 O1 Zn2 138.62(8) . . . . ? O7 Zn2 O1 P1 -98.07(12) . . . . ? O6 Zn2 O1 P1 28.91(13) . . . . ? O5 Zn2 O1 P1 141.40(10) . . . . ? O7 Zn2 O1 Zn1 76.11(9) . . . . ? O6 Zn2 O1 Zn1 -156.91(8) . . . . ? O5 Zn2 O1 Zn1 -44.42(9) . . . . ? O4 Zn1 O2 P3 84.56(15) . . . 8_665 ? O3 Zn1 O2 P3 -50.03(17) . . . 8_665 ? O1 Zn1 O2 P3 -158.57(13) . . . 8_665 ? O4 Zn1 O2 Zn3 -88.24(12) . . . 8_655 ? O3 Zn1 O2 Zn3 137.17(10) . . . 8_655 ? O1 Zn1 O2 Zn3 28.63(12) . . . 8_655 ? O4 Zn1 O3 P1 169.65(12) . . . 8_665 ? O2 Zn1 O3 P1 -53.22(16) . . . 8_665 ? O1 Zn1 O3 P1 57.23(14) . . . 8_665 ? O3 Zn1 O4 P2 64.98(15) . . . 6_556 ? O2 Zn1 O4 P2 -76.41(15) . . . 6_556 ? O1 Zn1 O4 P2 170.42(12) . . . 6_556 ? O7 Zn2 O5 P1 -86.24(11) . . . 8_665 ? O6 Zn2 O5 P1 143.40(10) . . . 8_665 ? O1 Zn2 O5 P1 29.26(12) . . . 8_665 ? O7 Zn2 O5 Zn3 104.16(9) . . . . ? O6 Zn2 O5 Zn3 -26.20(9) . . . . ? O1 Zn2 O5 Zn3 -140.34(7) . . . . ? O9 Zn3 O5 P1 -59.44(14) . . . 8_665 ? O8 Zn3 O5 P1 177.09(12) . . . 8_665 ? O2 Zn3 O5 P1 59.92(13) 8_665 . . 8_665 ? P3 Zn3 O5 P1 67.88(13) 1_565 . . 8_665 ? O9 Zn3 O5 Zn2 108.47(9) . . . . ? O8 Zn3 O5 Zn2 -15.00(9) . . . . ? O2 Zn3 O5 Zn2 -132.16(8) 8_665 . . . ? P3 Zn3 O5 Zn2 -124.20(6) 1_565 . . . ? O8 P2 O6 Zn2 -32.66(15) . . . . ? O9 P2 O6 Zn2 -157.33(11) 5_675 . . . ? O4 P2 O6 Zn2 86.47(13) 6_656 . . . ? O8 P2 O6 Zn4 153.58(10) . . . . ? O9 P2 O6 Zn4 28.90(13) 5_675 . . . ? O4 P2 O6 Zn4 -87.30(11) 6_656 . . . ? O7 Zn2 O6 P2 -63.24(14) . . . . ? O5 Zn2 O6 P2 62.22(12) . . . . ? O1 Zn2 O6 P2 -179.77(11) . . . . ? O7 Zn2 O6 Zn4 110.08(11) . . . . ? O5 Zn2 O6 Zn4 -124.46(10) . . . . ? O1 Zn2 O6 Zn4 -6.45(12) . . . . ? O11 Zn4 O6 P2 60.44(12) . . . . ? O10 Zn4 O6 P2 -177.17(10) . . . . ? O12 Zn4 O6 P2 -69.37(11) . . . . ? O11 Zn4 O6 Zn2 -113.38(11) . . . . ? O10 Zn4 O6 Zn2 9.01(12) . . . . ? O12 Zn4 O6 Zn2 116.80(10) . . . . ? O6 Zn2 O7 P3 31.1(3) . . . 3_655 ? O5 Zn2 O7 P3 -90.4(3) . . . 3_655 ? O1 Zn2 O7 P3 149.1(2) . . . 3_655 ? O9 P2 O8 Zn3 81.32(17) 5_675 . . . ? O4 P2 O8 Zn3 -158.14(14) 6_656 . . . ? O6 P2 O8 Zn3 -38.81(18) . . . . ? O9 Zn3 O8 P2 -55.98(18) . . . . ? O2 Zn3 O8 P2 161.66(13) 8_665 . . . ? O5 Zn3 O8 P2 62.28(16) . . . . ? P3 Zn3 O8 P2 -170.12(14) 1_565 . . . ? O8 Zn3 O9 P2 -15.0(2) . . . 5_675 ? O2 Zn3 O9 P2 127.24(18) 8_665 . . 5_675 ? O5 Zn3 O9 P2 -128.25(18) . . . 5_675 ? P3 Zn3 O9 P2 95.09(19) 1_565 . . 5_675 ? O3 P1 O10 Zn4 -56.55(16) 8_655 . . . ? O5 P1 O10 Zn4 -176.49(12) 8_655 . . . ? O1 P1 O10 Zn4 64.59(16) . . . . ? O11 Zn4 O10 P1 71.24(16) . . . . ? O12 Zn4 O10 P1 -154.32(13) . . . . ? O6 Zn4 O10 P1 -40.62(15) . . . . ? O7 P3 O11 Zn4 -148.0(2) 3_645 . . . ? O12 P3 O11 Zn4 90.5(2) 5_665 . . . ? O2 P3 O11 Zn4 -23.8(3) 8_655 . . . ? O10 Zn4 O11 P3 30.1(2) . . . . ? O12 Zn4 O11 P3 -95.5(2) . . . . ? O6 Zn4 O11 P3 141.9(2) . . . . ? O11 Zn4 O12 P3 22.76(16) . . . 5_665 ? O10 Zn4 O12 P3 -109.69(13) . . . 5_665 ? O6 Zn4 O12 P3 142.03(12) . . . 5_665 ? H1N N1 C1 H1C -56(4) . . . . ? H1N N1 C1 H2C 72(5) . . . . ? H1N N1 C1 H3C -168(4) . . . . ? H2N N1 C1 H1C -178(4) . . . . ? H2N N1 C1 H2C -50(5) . . . . ? H2N N1 C1 H3C 70(4) . . . . ? H3N N1 C1 H1C 59(4) . . . . ? H3N N1 C1 H2C -173(5) . . . . ? H3N N1 C1 H3C -53(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O12 0.82(2) 2.06(2) 2.865(3) 167(3) 7_576 N1 H1N O7 0.82(2) 2.64(3) 3.225(3) 130(3) . N1 H2N O4 0.82(2) 2.02(2) 2.832(3) 172(4) . N1 H3N O3 0.81(2) 2.17(3) 2.954(3) 163(3) 8_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.591 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.124 data_Zn5P4-0237 _database_code_CSD 208054 _audit_creation_method 'SHELXL-97 and ZCIF by Peter Y. Zavalij' _chemical_name_common 'methylammonium zinc phosphate' _chemical_formula_moiety '(C H3 N H3)2, Zn5 (P O4)4' _chemical_formula_sum 'C2 H12 N2 O16 P4 Zn5' _chemical_formula_weight 770.87 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2590(19) _cell_length_b 13.407(4) _cell_length_c 18.031(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1754.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _cell_measurement_reflns_used 3475 _cell_measurement_theta_min 4.518 _cell_measurement_theta_max 59.063 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 7.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_T_max 0.8661 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 296 _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 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 11139 _diffrn_reflns_av_R_equivalents 0.1392 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.72 _reflns_number_total 2336 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.1P)^2^+5.0P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.089(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(8) _refine_ls_number_reflns 2336 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1765 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Zn1 Zn 0.4865(3) 0.61494(16) 0.20659(13) 0.0161(6) Uani 1 1 d . . . Zn2 Zn 0.4992(3) 0.37066(17) 0.22291(12) 0.0175(6) Uani 1 1 d . . . Zn3 Zn 0.1428(3) -0.00154(18) 0.08123(12) 0.0164(5) Uani 1 1 d . . . Zn4 Zn -0.0536(3) 0.35794(18) 0.19721(13) 0.0176(6) Uani 1 1 d . . . Zn5 Zn -0.0576(3) 0.61190(17) 0.18609(13) 0.0176(6) Uani 1 1 d . . . P1 P 0.6823(6) 0.4804(4) 0.0934(3) 0.0143(12) Uani 1 1 d . . . P2 P 0.2604(8) 0.1908(4) 0.1709(3) 0.0166(13) Uani 1 1 d . . . P3 P 0.2404(7) -0.2113(4) 0.1526(3) 0.0150(13) Uani 1 1 d . . . P4 P 0.1895(6) 0.4961(4) 0.2930(3) 0.0167(12) Uani 1 1 d . . . O1 O 0.406(2) 0.7209(11) 0.1423(8) 0.026(4) Uiso 1 1 d . . . O2 O 0.5313(17) 0.4855(11) 0.1569(7) 0.022(3) Uiso 1 1 d . . . O3 O 0.303(2) 0.5893(11) 0.2814(9) 0.027(4) Uiso 1 1 d . . . O4 O 0.3046(19) 0.4033(11) 0.2904(8) 0.022(3) Uiso 1 1 d . . . O5 O 0.427(2) 0.2642(11) 0.1609(8) 0.026(4) Uiso 1 1 d . . . O6 O 0.2882(17) 0.1122(10) 0.1135(7) 0.014(3) Uiso 1 1 d . . . O7 O 0.0819(19) 0.0233(11) -0.0212(8) 0.029(4) Uiso 1 1 d . . . O8 O 0.2384(18) -0.1371(10) 0.0911(8) 0.021(3) Uiso 1 1 d . . . O9 O -0.0936(16) 0.0052(11) 0.1334(7) 0.020(3) Uiso 1 1 d . . . O10 O 0.071(2) 0.2405(11) 0.1645(8) 0.027(4) Uiso 1 1 d . . . O11 O -0.2590(19) 0.3408(11) 0.2713(8) 0.021(3) Uiso 1 1 d . . . O12 O -0.2015(18) 0.3872(10) 0.1099(7) 0.017(3) Uiso 1 1 d . . . O13 O 0.0434(17) 0.4888(10) 0.2306(7) 0.021(3) Uiso 1 1 d . . . O14 O -0.2010(19) 0.5719(11) 0.0987(8) 0.022(3) Uiso 1 1 d . . . O15 O -0.2737(19) 0.6479(10) 0.2495(8) 0.022(3) Uiso 1 1 d . . . O16 O 0.060(2) 0.7309(10) 0.1525(7) 0.018(3) Uiso 1 1 d . . . N1 N 0.721(3) 0.7805(16) 0.0614(13) 0.049(7) Uani 1 1 d . . . H1A H 0.7383 0.7275 0.0326 0.073 Uiso 1 1 calc R . . H1B H 0.6243 0.7698 0.0909 0.073 Uiso 1 1 calc R . . H1C H 0.8206 0.7909 0.0889 0.073 Uiso 1 1 calc R . . C1 C 0.688(4) 0.8629(19) 0.0179(13) 0.039(7) Uani 1 1 d . . . H1D H 0.7579 0.8578 -0.0271 0.058 Uiso 1 1 calc R . . H1E H 0.7235 0.9220 0.0443 0.058 Uiso 1 1 calc R . . H1F H 0.5589 0.8663 0.0061 0.058 Uiso 1 1 calc R . . N2 N 0.713(3) 0.1844(13) 0.0715(10) 0.028(5) Uani 1 1 d . . . H2A H 0.8264 0.1633 0.0812 0.042 Uiso 1 1 calc R . . H2B H 0.6339 0.1556 0.1027 0.042 Uiso 1 1 calc R . . H2C H 0.7074 0.2503 0.0770 0.042 Uiso 1 1 calc R . . C2 C 0.665(5) 0.159(4) -0.0023(16) 0.104(16) Uani 1 1 d . . . H2D H 0.5770 0.2061 -0.0210 0.156 Uiso 1 1 calc R . . H2E H 0.6128 0.0933 -0.0033 0.156 Uiso 1 1 calc R . . H2F H 0.7737 0.1604 -0.0328 0.156 Uiso 1 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 0.0155(12) 0.0153(12) 0.0174(12) -0.0020(10) 0.0002(10) 0.0010(10) Zn2 0.0150(12) 0.0182(13) 0.0193(13) 0.0007(10) -0.0003(10) 0.0007(11) Zn3 0.0169(11) 0.0179(12) 0.0143(12) 0.0030(11) 0.0032(9) 0.0005(12) Zn4 0.0120(11) 0.0193(12) 0.0215(13) 0.0021(10) -0.0014(10) 0.0034(11) Zn5 0.0189(12) 0.0140(12) 0.0199(14) 0.0011(10) -0.0011(10) -0.0025(11) P1 0.012(2) 0.017(3) 0.015(3) 0.003(2) -0.0018(19) 0.000(2) P2 0.016(3) 0.014(3) 0.020(3) 0.004(2) -0.005(2) -0.003(2) P3 0.006(3) 0.017(3) 0.022(3) 0.000(2) 0.000(2) -0.001(2) P4 0.016(2) 0.021(3) 0.013(3) -0.001(3) 0.0015(19) -0.003(3) N1 0.039(13) 0.052(13) 0.054(15) 0.042(12) 0.007(12) 0.009(12) C1 0.053(16) 0.046(16) 0.018(13) 0.009(12) -0.012(12) 0.003(15) N2 0.034(11) 0.028(10) 0.021(11) 0.011(9) 0.014(9) 0.030(10) C2 0.10(3) 0.19(4) 0.021(18) 0.00(2) 0.028(18) 0.09(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 1.924(15) . ? Zn1 O3 1.926(16) . ? Zn1 O15 1.956(14) 1_655 ? Zn1 O2 1.980(14) . ? Zn2 O5 1.887(15) . ? Zn2 O4 1.915(14) . ? Zn2 O2 1.959(14) . ? Zn2 O11 2.001(14) 1_655 ? Zn3 O7 1.928(14) . ? Zn3 O6 1.943(13) . ? Zn3 O8 1.953(14) . ? Zn3 O9 1.959(12) . ? Zn4 O10 1.908(15) . ? Zn4 O12 1.946(14) . ? Zn4 O13 1.984(14) . ? Zn4 O11 2.015(14) . ? Zn5 O16 1.907(14) . ? Zn5 O14 1.963(15) . ? Zn5 O13 1.976(14) . ? Zn5 O15 2.001(14) . ? P1 O7 1.493(15) 4 ? P1 O14 1.493(15) 1_655 ? P1 O12 1.537(15) 1_655 ? P1 O2 1.587(14) . ? P2 O6 1.491(14) . ? P2 O10 1.535(16) . ? P2 O15 1.548(15) 3_545 ? P2 O5 1.570(16) . ? P3 O8 1.490(15) . ? P3 O1 1.519(16) 1_545 ? P3 O16 1.523(15) 1_545 ? P3 O11 1.545(15) 3_545 ? P4 O4 1.500(15) . ? P4 O9 1.504(14) 3 ? P4 O3 1.511(16) . ? P4 O13 1.550(14) . ? N1 C1 1.38(3) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C1 H1F 0.9600 . ? N2 C2 1.42(4) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C2 H2F 0.9600 . ? 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 110.1(6) . . ? O1 Zn1 O15 110.0(6) . 1_655 ? O3 Zn1 O15 112.2(6) . 1_655 ? O1 Zn1 O2 115.1(6) . . ? O3 Zn1 O2 105.9(6) . . ? O15 Zn1 O2 103.4(6) 1_655 . ? O5 Zn2 O4 110.1(6) . . ? O5 Zn2 O2 105.5(6) . . ? O4 Zn2 O2 107.1(6) . . ? O5 Zn2 O11 110.6(6) . 1_655 ? O4 Zn2 O11 114.6(6) . 1_655 ? O2 Zn2 O11 108.5(6) . 1_655 ? O7 Zn3 O6 106.0(6) . . ? O7 Zn3 O8 109.3(6) . . ? O6 Zn3 O8 120.6(6) . . ? O7 Zn3 O9 104.5(6) . . ? O6 Zn3 O9 107.2(6) . . ? O8 Zn3 O9 108.1(6) . . ? O10 Zn4 O12 100.2(6) . . ? O10 Zn4 O13 131.0(6) . . ? O12 Zn4 O13 105.2(6) . . ? O10 Zn4 O11 117.4(6) . . ? O12 Zn4 O11 98.7(5) . . ? O13 Zn4 O11 99.3(6) . . ? O16 Zn5 O14 102.2(6) . . ? O16 Zn5 O13 131.4(6) . . ? O14 Zn5 O13 107.1(6) . . ? O16 Zn5 O15 109.3(6) . . ? O14 Zn5 O15 96.3(6) . . ? O13 Zn5 O15 105.1(6) . . ? O7 P1 O14 111.2(9) 4 1_655 ? O7 P1 O12 114.1(8) 4 1_655 ? O14 P1 O12 110.1(7) 1_655 1_655 ? O7 P1 O2 107.1(8) 4 . ? O14 P1 O2 108.1(8) 1_655 . ? O12 P1 O2 105.9(8) 1_655 . ? O6 P2 O10 112.1(8) . . ? O6 P2 O15 111.9(8) . 3_545 ? O10 P2 O15 106.6(8) . 3_545 ? O6 P2 O5 105.0(8) . . ? O10 P2 O5 114.2(8) . . ? O15 P2 O5 107.0(8) 3_545 . ? O8 P3 O1 108.5(9) . 1_545 ? O8 P3 O16 109.3(8) . 1_545 ? O1 P3 O16 112.0(8) 1_545 1_545 ? O8 P3 O11 111.1(8) . 3_545 ? O1 P3 O11 108.0(8) 1_545 3_545 ? O16 P3 O11 107.9(8) 1_545 3_545 ? O4 P4 O9 110.6(8) . 3 ? O4 P4 O3 112.2(8) . . ? O9 P4 O3 107.9(9) 3 . ? O4 P4 O13 107.9(8) . . ? O9 P4 O13 109.3(7) 3 . ? O3 P4 O13 109.0(8) . . ? P3 O1 Zn1 127.6(9) 1_565 . ? P1 O2 Zn2 119.1(8) . . ? P1 O2 Zn1 118.5(8) . . ? Zn2 O2 Zn1 113.3(6) . . ? P4 O3 Zn1 128.4(10) . . ? P4 O4 Zn2 128.3(9) . . ? P2 O5 Zn2 128.3(9) . . ? P2 O6 Zn3 133.5(8) . . ? P1 O7 Zn3 135.8(9) 4_455 . ? P3 O8 Zn3 133.8(9) . . ? P4 O9 Zn3 145.6(8) 3_545 . ? P2 O10 Zn4 139.4(10) . . ? P3 O11 Zn2 123.7(8) 3 1_455 ? P3 O11 Zn4 125.1(8) 3 . ? Zn2 O11 Zn4 109.7(7) 1_455 . ? P1 O12 Zn4 128.6(8) 1_455 . ? P4 O13 Zn5 119.7(8) . . ? P4 O13 Zn4 121.3(8) . . ? Zn5 O13 Zn4 119.0(6) . . ? P1 O14 Zn5 125.2(9) 1_455 . ? P2 O15 Zn1 120.4(8) 3 1_455 ? P2 O15 Zn5 124.8(8) 3 . ? Zn1 O15 Zn5 114.6(7) 1_455 . ? P3 O16 Zn5 144.1(9) 1_565 . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? C2 N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C2 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? N2 C2 H2D 109.5 . . ? N2 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N2 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 P3 9.5(13) . . . 1_565 ? O15 Zn1 O1 P3 -114.7(11) 1_655 . . 1_565 ? O2 Zn1 O1 P3 129.0(10) . . . 1_565 ? O7 P1 O2 Zn2 111.2(9) 4 . . . ? O14 P1 O2 Zn2 -129.0(9) 1_655 . . . ? O12 P1 O2 Zn2 -11.0(11) 1_655 . . . ? O7 P1 O2 Zn1 -104.0(9) 4 . . . ? O14 P1 O2 Zn1 15.8(11) 1_655 . . . ? O12 P1 O2 Zn1 133.8(8) 1_655 . . . ? O5 Zn2 O2 P1 -61.8(10) . . . . ? O4 Zn2 O2 P1 -179.1(8) . . . . ? O11 Zn2 O2 P1 56.7(10) 1_655 . . . ? O5 Zn2 O2 Zn1 151.7(7) . . . . ? O4 Zn2 O2 Zn1 34.4(8) . . . . ? O11 Zn2 O2 Zn1 -89.8(7) 1_655 . . . ? O1 Zn1 O2 P1 60.1(10) . . . . ? O3 Zn1 O2 P1 -178.0(8) . . . . ? O15 Zn1 O2 P1 -59.8(9) 1_655 . . . ? O1 Zn1 O2 Zn2 -153.1(7) . . . . ? O3 Zn1 O2 Zn2 -31.3(8) . . . . ? O15 Zn1 O2 Zn2 86.9(7) 1_655 . . . ? O4 P4 O3 Zn1 47.1(14) . . . . ? O9 P4 O3 Zn1 169.3(10) 3 . . . ? O13 P4 O3 Zn1 -72.2(13) . . . . ? O1 Zn1 O3 P4 115.3(12) . . . . ? O15 Zn1 O3 P4 -121.8(11) 1_655 . . . ? O2 Zn1 O3 P4 -9.7(13) . . . . ? O9 P4 O4 Zn2 -163.1(9) 3 . . . ? O3 P4 O4 Zn2 -42.5(13) . . . . ? O13 P4 O4 Zn2 77.5(12) . . . . ? O5 Zn2 O4 P4 -112.1(11) . . . . ? O2 Zn2 O4 P4 2.2(12) . . . . ? O11 Zn2 O4 P4 122.5(11) 1_655 . . . ? O6 P2 O5 Zn2 -170.6(10) . . . . ? O10 P2 O5 Zn2 66.2(13) . . . . ? O15 P2 O5 Zn2 -51.5(13) 3_545 . . . ? O4 Zn2 O5 P2 -15.1(13) . . . . ? O2 Zn2 O5 P2 -130.3(11) . . . . ? O11 Zn2 O5 P2 112.6(11) 1_655 . . . ? O10 P2 O6 Zn3 -50.4(13) . . . . ? O15 P2 O6 Zn3 69.4(13) 3_545 . . . ? O5 P2 O6 Zn3 -174.9(10) . . . . ? O7 Zn3 O6 P2 117.6(11) . . . . ? O8 Zn3 O6 P2 -117.8(11) . . . . ? O9 Zn3 O6 P2 6.4(13) . . . . ? O6 Zn3 O7 P1 74.8(14) . . . 4_455 ? O8 Zn3 O7 P1 -56.6(15) . . . 4_455 ? O9 Zn3 O7 P1 -172.1(13) . . . 4_455 ? O1 P3 O8 Zn3 -152.7(11) 1_545 . . . ? O16 P3 O8 Zn3 84.8(12) 1_545 . . . ? O11 P3 O8 Zn3 -34.1(14) 3_545 . . . ? O7 Zn3 O8 P3 -152.2(11) . . . . ? O6 Zn3 O8 P3 84.8(12) . . . . ? O9 Zn3 O8 P3 -39.0(13) . . . . ? O7 Zn3 O9 P4 178.8(16) . . . 3_545 ? O6 Zn3 O9 P4 -69.0(18) . . . 3_545 ? O8 Zn3 O9 P4 62.4(17) . . . 3_545 ? O6 P2 O10 Zn4 -162.8(13) . . . . ? O15 P2 O10 Zn4 74.4(16) 3_545 . . . ? O5 P2 O10 Zn4 -43.5(17) . . . . ? O12 Zn4 O10 P2 142.6(14) . . . . ? O13 Zn4 O10 P2 21.9(19) . . . . ? O11 Zn4 O10 P2 -111.9(15) . . . . ? O10 Zn4 O11 P3 56.1(12) . . . 3 ? O12 Zn4 O11 P3 162.4(10) . . . 3 ? O13 Zn4 O11 P3 -90.4(10) . . . 3 ? O10 Zn4 O11 Zn2 -110.3(8) . . . 1_455 ? O12 Zn4 O11 Zn2 -3.9(8) . . . 1_455 ? O13 Zn4 O11 Zn2 103.2(7) . . . 1_455 ? O10 Zn4 O12 P1 -171.1(10) . . . 1_455 ? O13 Zn4 O12 P1 -33.4(11) . . . 1_455 ? O11 Zn4 O12 P1 68.8(11) . . . 1_455 ? O4 P4 O13 Zn5 -152.8(8) . . . . ? O9 P4 O13 Zn5 86.9(10) 3 . . . ? O3 P4 O13 Zn5 -30.8(11) . . . . ? O4 P4 O13 Zn4 30.0(11) . . . . ? O9 P4 O13 Zn4 -90.3(10) 3 . . . ? O3 P4 O13 Zn4 152.0(9) . . . . ? O16 Zn5 O13 P4 45.5(12) . . . . ? O14 Zn5 O13 P4 170.0(8) . . . . ? O15 Zn5 O13 P4 -88.4(9) . . . . ? O16 Zn5 O13 Zn4 -137.2(7) . . . . ? O14 Zn5 O13 Zn4 -12.8(9) . . . . ? O15 Zn5 O13 Zn4 88.8(8) . . . . ? O10 Zn4 O13 P4 -53.1(12) . . . . ? O12 Zn4 O13 P4 -171.8(8) . . . . ? O11 Zn4 O13 P4 86.4(9) . . . . ? O10 Zn4 O13 Zn5 129.7(8) . . . . ? O12 Zn4 O13 Zn5 11.0(8) . . . . ? O11 Zn4 O13 Zn5 -90.7(7) . . . . ? O16 Zn5 O14 P1 178.3(10) . . . 1_455 ? O13 Zn5 O14 P1 37.6(11) . . . 1_455 ? O15 Zn5 O14 P1 -70.4(11) . . . 1_455 ? O16 Zn5 O15 P2 -72.6(11) . . . 3 ? O14 Zn5 O15 P2 -177.8(10) . . . 3 ? O13 Zn5 O15 P2 72.6(11) . . . 3 ? O16 Zn5 O15 Zn1 112.2(7) . . . 1_455 ? O14 Zn5 O15 Zn1 6.9(8) . . . 1_455 ? O13 Zn5 O15 Zn1 -102.7(7) . . . 1_455 ? O14 Zn5 O16 P3 -138.0(15) . . . 1_565 ? O13 Zn5 O16 P3 -11.8(19) . . . 1_565 ? O15 Zn5 O16 P3 120.8(15) . . . 1_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O14 0.89 2.44 2.93(2) 115.0 1_655 N1 H1A O8 0.89 2.54 3.36(3) 153.5 4 N1 H1B O1 0.89 1.95 2.83(3) 167.7 . N1 H1C O16 0.89 2.23 3.03(3) 149.8 1_655 N1 H1C O4 0.89 2.80 3.14(3) 104.7 3_655 N2 H2A O9 0.89 2.39 3.00(2) 125.8 1_655 N2 H2A O10 0.89 2.54 3.18(3) 129.3 1_655 N2 H2B O5 0.89 2.34 2.84(2) 115.1 . N2 H2B O3 0.89 2.32 2.95(2) 127.6 3_645 N2 H2C O12 0.89 2.04 2.87(2) 155.8 1_655 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 22.72 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.158 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.304