Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Natarajan, Srinivasan' _publ_contact_author_name 'Dr Srinivasan Natarajan' _publ_contact_author_address ; Chemistry & Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jakkur P.O. Bangalore 560 064 INDIA ; _publ_contact_author_email 'RAJ@JNCASR.AC.IN' _publ_section_title ; Synthesis of a Layered Zinc Phosphate, [NH3(CH2)2NH2(CH2)3NH3[Zn2(PO4)(HOP4)2].H2O and its Transformation to a Extra Large Pore three-dimensional zinc phosphate, [NH3(CH2)2NH2(CH2)3NH3[Zn3(PO4)(HPO4)3] ; #COMPOUND I (Layered Zinc Phosphate) data_junk _database_code_CSD 177589 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H22 N3 O13 P3 Zn2' _chemical_formula_weight 555.91 _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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3980(3) _cell_length_b 13.76560(10) _cell_length_c 8.9235(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.8370(10) _cell_angle_gamma 90.00 _cell_volume 1737.07(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Colorless _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 3.109 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.742537 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7042 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2479 _reflns_number_observed 1934 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXTL-PLUS' _computing_structure_refinement 'SHELXTL-PLUS' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0378P)^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 2479 _refine_ls_number_parameters 243 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_obs 0.0376 _refine_ls_wR_factor_all 0.0881 _refine_ls_wR_factor_obs 0.0810 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.008 _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 0.36684(4) 0.46445(4) 0.06483(7) 0.0172(2) Uani 1 d . . Zn2 Zn 0.31792(4) 0.76538(4) 0.01370(7) 0.0174(2) Uani 1 d . . P1 P 0.23674(10) 0.88974(10) -0.2940(2) 0.0170(3) Uani 1 d . . P2 P 0.42862(10) 0.62051(10) -0.1726(2) 0.0146(3) Uani 1 d . . P3 P 0.19363(10) 0.31569(11) 0.0370(2) 0.0195(4) Uani 1 d . . O1 O 0.3230(3) 0.5464(3) 0.2114(4) 0.0247(9) Uani 1 d . . O2 O 0.4669(2) 0.3880(3) 0.1877(4) 0.0217(9) Uani 1 d . . O3 O 0.3937(2) 0.5224(2) -0.1203(4) 0.0224(9) Uani 1 d . . O4 O 0.2751(3) 0.3638(3) -0.0240(4) 0.0229(9) Uani 1 d . . O5 O 0.2369(2) 0.8355(3) -0.1470(4) 0.0240(9) Uani 1 d . . O6 O 0.4224(2) 0.6995(3) -0.0530(4) 0.0251(9) Uani 1 d . . O7 O 0.2231(2) 0.6787(3) 0.0691(4) 0.0226(9) Uani 1 d . . O8 O 0.3697(2) 0.8558(3) 0.1733(4) 0.0256(10) Uani 1 d . . O9 O 0.1464(3) 0.9559(3) -0.3140(5) 0.0300(10) Uani 1 d . . H30 H 0.0993(3) 0.9217(3) -0.3188(5) 0.045 Uiso 1 calc R . O10 O 0.2277(3) 0.2620(3) 0.1851(4) 0.0300(10) Uani 1 d . . O11 O 0.1153(2) 0.3882(3) 0.0502(4) 0.0280(10) Uani 1 d . . O12 O 0.1494(3) 0.2376(3) -0.0853(4) 0.0325(10) Uani 1 d . . H20 H 0.1302(3) 0.2646(3) -0.1672(4) 0.049 Uiso 1 calc R . O100 O -0.0016(3) 0.8642(3) -0.2182(6) 0.0442(12) Uani 1 d D . N1 N 0.5847(3) 0.7998(3) 0.0590(5) 0.0260(12) Uani 1 d . . H1 H 0.5338(3) 0.7634(3) 0.0268(5) 0.039 Uiso 1 calc R . H2 H 0.5755(3) 0.8358(3) 0.1377(5) 0.039 Uiso 1 calc R . H3 H 0.6347(3) 0.7616(3) 0.0879(5) 0.039 Uiso 1 calc R . C1 C 0.6013(4) 0.8636(4) -0.0656(7) 0.032(2) Uani 1 d . . H4 H 0.5463(4) 0.9043(4) -0.0981(7) 0.038 Uiso 1 calc R . H5 H 0.6102(4) 0.8241(4) -0.1519(7) 0.038 Uiso 1 calc R . C2 C 0.6884(4) 0.9279(4) -0.0158(6) 0.0248(14) Uani 1 d . . H6 H 0.6690(4) 0.9906(4) 0.0173(6) 0.030 Uiso 1 calc R . H7 H 0.7304(4) 0.8980(4) 0.0694(6) 0.030 Uiso 1 calc R . N2 N 0.7390(3) 0.9414(3) -0.1446(5) 0.0197(11) Uani 1 d . . H8 H 0.6994(3) 0.9691(3) -0.2230(5) 0.024 Uiso 1 calc R . H9 H 0.7553(3) 0.8827(3) -0.1759(5) 0.024 Uiso 1 calc R . C3 C 0.8267(4) 1.0032(4) -0.1047(6) 0.0236(14) Uani 1 d . . H10 H 0.8799(4) 0.9627(4) -0.0602(6) 0.028 Uiso 1 calc R . H11 H 0.8176(4) 1.0515(4) -0.0295(6) 0.028 Uiso 1 calc R . C4 C 0.8483(4) 1.0539(4) -0.2458(6) 0.0253(14) Uani 1 d . . H12 H 0.8648(4) 1.0055(4) -0.3153(6) 0.030 Uiso 1 calc R . H13 H 0.7920(4) 1.0874(4) -0.2973(6) 0.030 Uiso 1 calc R . C5 C 0.9267(4) 1.1249(4) -0.2086(7) 0.037(2) Uani 1 d . . H14 H 0.9833(4) 1.0916(4) -0.1576(7) 0.045 Uiso 1 calc R . H15 H 0.9103(4) 1.1735(4) -0.1393(7) 0.045 Uiso 1 calc R . N3 N 0.9462(3) 1.1735(3) -0.3484(5) 0.0275(12) Uani 1 d . . H16 H 0.9935(3) 1.2155(3) -0.3228(5) 0.041 Uiso 1 calc R . H17 H 0.8947(3) 1.2049(3) -0.3945(5) 0.041 Uiso 1 calc R . H18 H 0.9622(3) 1.1291(3) -0.4115(5) 0.041 Uiso 1 calc R . H102 H 0.0509(32) 0.9041(43) -0.2231(88) 0.080(27) Uiso 1 d D . H101 H -0.0451(51) 0.8675(66) -0.3117(54) 0.126(41) Uiso 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 0.0182(4) 0.0178(4) 0.0153(4) 0.0019(3) 0.0025(3) 0.0014(3) Zn2 0.0192(4) 0.0169(4) 0.0157(4) -0.0017(3) 0.0024(3) -0.0008(3) P1 0.0192(8) 0.0173(8) 0.0148(8) 0.0019(6) 0.0041(7) 0.0023(6) P2 0.0156(8) 0.0134(8) 0.0146(8) 0.0010(6) 0.0022(6) 0.0008(6) P3 0.0234(8) 0.0175(8) 0.0183(8) 0.0005(6) 0.0057(7) -0.0033(7) O1 0.030(2) 0.027(2) 0.018(2) -0.003(2) 0.006(2) 0.007(2) O2 0.020(2) 0.025(2) 0.021(2) 0.006(2) 0.006(2) 0.005(2) O3 0.032(2) 0.018(2) 0.018(2) 0.006(2) 0.006(2) -0.003(2) O4 0.021(2) 0.025(2) 0.023(2) -0.002(2) 0.004(2) -0.009(2) O5 0.029(2) 0.027(2) 0.016(2) 0.008(2) 0.005(2) 0.001(2) O6 0.023(2) 0.023(2) 0.031(2) -0.010(2) 0.009(2) -0.001(2) O7 0.017(2) 0.028(2) 0.022(2) 0.007(2) 0.001(2) -0.007(2) O8 0.028(2) 0.027(2) 0.019(2) -0.009(2) -0.005(2) 0.002(2) O9 0.026(2) 0.026(2) 0.043(3) 0.005(2) 0.017(2) 0.003(2) O10 0.041(3) 0.026(2) 0.023(2) 0.007(2) 0.008(2) 0.005(2) O11 0.021(2) 0.021(2) 0.042(3) -0.001(2) 0.007(2) 0.001(2) O12 0.039(2) 0.034(3) 0.026(2) -0.011(2) 0.009(2) -0.017(2) O100 0.029(3) 0.034(3) 0.068(4) 0.002(3) 0.006(3) 0.000(2) N1 0.022(3) 0.028(3) 0.030(3) -0.003(2) 0.010(2) -0.003(2) C1 0.036(4) 0.037(4) 0.023(4) -0.001(3) 0.008(3) -0.008(3) C2 0.031(4) 0.020(3) 0.025(4) -0.003(3) 0.008(3) -0.001(3) N2 0.024(3) 0.020(3) 0.017(3) -0.003(2) 0.006(2) 0.002(2) C3 0.022(3) 0.030(4) 0.019(3) 0.000(3) 0.005(3) 0.000(3) C4 0.031(3) 0.025(4) 0.019(3) 0.003(3) 0.003(3) -0.001(3) C5 0.041(4) 0.043(4) 0.028(4) -0.002(3) 0.004(3) -0.017(3) N3 0.026(3) 0.026(3) 0.030(3) 0.002(2) 0.005(2) 0.003(2) _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 1.921(3) . ? Zn1 O3 1.938(3) . ? Zn1 O2 1.947(3) . ? Zn1 O4 1.975(3) . ? Zn2 O5 1.929(4) . ? Zn2 O8 1.932(3) . ? Zn2 O6 1.943(3) . ? Zn2 O7 1.945(3) . ? P1 O5 1.509(4) . ? P1 O1 1.516(4) 4_575 ? P1 O7 1.526(4) 4_575 ? P1 O9 1.570(4) . ? P2 O8 1.510(4) 4_575 ? P2 O6 1.538(4) . ? P2 O2 1.540(4) 3_665 ? P2 O3 1.543(4) . ? P3 O10 1.513(4) . ? P3 O11 1.528(4) . ? P3 O4 1.533(4) . ? P3 O12 1.578(4) . ? O1 P1 1.516(4) 4_576 ? O2 P2 1.540(4) 3_665 ? O7 P1 1.526(4) 4_576 ? O8 P2 1.510(4) 4_576 ? O9 H30 0.82 . ? O12 H20 0.82 . ? O100 H102 0.943(10) . ? O100 H101 0.946(10) . ? N1 C1 1.471(7) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? C1 C2 1.531(8) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 N2 1.483(7) . ? C2 H6 0.97 . ? C2 H7 0.97 . ? N2 C3 1.509(6) . ? N2 H8 0.90 . ? N2 H9 0.90 . ? C3 C4 1.522(7) . ? C3 H10 0.97 . ? C3 H11 0.97 . ? C4 C5 1.482(7) . ? C4 H12 0.97 . ? C4 H13 0.97 . ? C5 N3 1.488(7) . ? C5 H14 0.97 . ? C5 H15 0.97 . ? N3 H16 0.89 . ? N3 H17 0.89 . ? N3 H18 0.89 . ? 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 118.8(2) . . ? O1 Zn1 O2 103.70(15) . . ? O3 Zn1 O2 117.23(15) . . ? O1 Zn1 O4 113.9(2) . . ? O3 Zn1 O4 99.92(15) . . ? O2 Zn1 O4 102.4(2) . . ? O5 Zn2 O8 108.7(2) . . ? O5 Zn2 O6 113.6(2) . . ? O8 Zn2 O6 108.23(15) . . ? O5 Zn2 O7 98.07(15) . . ? O8 Zn2 O7 113.6(2) . . ? O6 Zn2 O7 114.3(2) . . ? O5 P1 O1 113.1(2) . 4_575 ? O5 P1 O7 111.7(2) . 4_575 ? O1 P1 O7 111.4(2) 4_575 4_575 ? O5 P1 O9 104.6(2) . . ? O1 P1 O9 108.9(2) 4_575 . ? O7 P1 O9 106.7(2) 4_575 . ? O8 P2 O6 112.5(2) 4_575 . ? O8 P2 O2 109.1(2) 4_575 3_665 ? O6 P2 O2 107.4(2) . 3_665 ? O8 P2 O3 107.7(2) 4_575 . ? O6 P2 O3 110.2(2) . . ? O2 P2 O3 109.8(2) 3_665 . ? O10 P3 O11 112.0(2) . . ? O10 P3 O4 112.1(2) . . ? O11 P3 O4 111.8(2) . . ? O10 P3 O12 107.1(2) . . ? O11 P3 O12 106.9(2) . . ? O4 P3 O12 106.5(2) . . ? P1 O1 Zn1 133.7(2) 4_576 . ? P2 O2 Zn1 128.6(2) 3_665 . ? P2 O3 Zn1 138.3(2) . . ? P3 O4 Zn1 131.3(2) . . ? P1 O5 Zn2 142.7(2) . . ? P2 O6 Zn2 133.8(2) . . ? P1 O7 Zn2 126.3(2) 4_576 . ? P2 O8 Zn2 152.1(2) 4_576 . ? P1 O9 H30 109.47(15) . . ? P3 O12 H20 109.5(2) . . ? H102 O100 H101 109.5(72) . . ? C1 N1 H1 109.5(3) . . ? C1 N1 H2 109.5(3) . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5(3) . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? N1 C1 C2 111.5(5) . . ? N1 C1 H4 109.3(3) . . ? C2 C1 H4 109.3(3) . . ? N1 C1 H5 109.3(3) . . ? C2 C1 H5 109.3(3) . . ? H4 C1 H5 108.0 . . ? N2 C2 C1 110.0(4) . . ? N2 C2 H6 109.7(3) . . ? C1 C2 H6 109.7(3) . . ? N2 C2 H7 109.7(3) . . ? C1 C2 H7 109.7(3) . . ? H6 C2 H7 108.2 . . ? C2 N2 C3 113.5(4) . . ? C2 N2 H8 108.9(3) . . ? C3 N2 H8 108.9(3) . . ? C2 N2 H9 108.9(3) . . ? C3 N2 H9 108.9(3) . . ? H8 N2 H9 107.7 . . ? N2 C3 C4 110.8(4) . . ? N2 C3 H10 109.5(3) . . ? C4 C3 H10 109.5(3) . . ? N2 C3 H11 109.5(3) . . ? C4 C3 H11 109.5(3) . . ? H10 C3 H11 108.1 . . ? C5 C4 C3 112.5(5) . . ? C5 C4 H12 109.1(4) . . ? C3 C4 H12 109.1(3) . . ? C5 C4 H13 109.1(4) . . ? C3 C4 H13 109.1(3) . . ? H12 C4 H13 107.8 . . ? C4 C5 N3 111.4(5) . . ? C4 C5 H14 109.3(3) . . ? N3 C5 H14 109.3(3) . . ? C4 C5 H15 109.3(4) . . ? N3 C5 H15 109.3(3) . . ? H14 C5 H15 108.0 . . ? C5 N3 H16 109.5(3) . . ? C5 N3 H17 109.5(3) . . ? H16 N3 H17 109.5 . . ? C5 N3 H18 109.5(3) . . ? H16 N3 H18 109.5 . . ? H17 N3 H18 109.5 . . ? _refine_diff_density_max 0.564 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.114 EOF #COMPOUND II (Three-dimensional Zinc Phosphate) data_sad _database_code_CSD 177590 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H21 N3 O16 P4 Zn3' _chemical_formula_weight 699.24 _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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4557(2) _cell_length_b 9.28440(10) _cell_length_c 13.8599(3) _cell_angle_alpha 81.1140(10) _cell_angle_beta 83.6420(10) _cell_angle_gamma 72.626(2) _cell_volume 1023.57(3) _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 colorless _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_method ? _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 3.882 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.681841 _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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4348 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.23 _reflns_number_total 2904 _reflns_number_observed 2484 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXTL-PLUS' _computing_structure_refinement 'SHELXTL-PLUS' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0427P)^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 2904 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_all 0.0808 _refine_ls_wR_factor_obs 0.0752 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.061 _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 0.29367(6) 0.91830(6) 0.51946(4) 0.0175(2) Uani 1 d . . Zn2 Zn 0.74556(6) 1.49370(6) -0.02699(4) 0.0160(2) Uani 1 d . . Zn3 Zn 0.63779(6) 0.88788(6) 0.12587(4) 0.0158(2) Uani 1 d . . P1 P 0.58114(14) 1.21710(13) 0.01996(8) 0.0141(3) Uani 1 d . . P2 P 0.58470(14) 0.86461(13) 0.36397(8) 0.0159(3) Uani 1 d . . P3 P 0.90460(14) 1.56629(13) 0.14874(8) 0.0154(3) Uani 1 d . . P4 P 0.01690(14) 1.20793(14) 0.42267(8) 0.0178(3) Uani 1 d . . O1 O 0.1668(4) 1.0703(4) 0.4238(2) 0.0295(8) Uani 1 d . . O2 O 0.4718(4) 0.7992(3) 0.4396(2) 0.0237(8) Uani 1 d . . O3 O 0.4033(4) 0.9820(3) 0.6163(2) 0.0226(7) Uani 1 d . . O4 O 0.1403(4) 0.8210(4) 0.6032(2) 0.0247(8) Uani 1 d . . O5 O 0.8141(4) 1.4767(4) 0.1035(2) 0.0287(8) Uani 1 d . . O6 O 0.9089(4) 1.5020(4) -0.1349(2) 0.0273(8) Uani 1 d . . O7 O 0.7098(4) 1.2965(3) -0.0300(2) 0.0227(7) Uani 1 d . . O8 O 0.5648(4) 1.6714(4) -0.0697(2) 0.0266(8) Uani 1 d . . O9 O 0.6642(4) 1.0918(3) 0.1018(2) 0.0199(7) Uani 1 d . . O10 O 0.8500(4) 0.7362(3) 0.1126(2) 0.0229(7) Uani 1 d . . O11 O 0.4689(4) 0.8557(4) 0.0581(2) 0.0248(8) Uani 1 d . . O12 O 0.5306(4) 0.8757(4) 0.2614(2) 0.0216(7) Uani 1 d . . O13 O 0.7678(4) 0.7538(4) 0.3695(2) 0.0281(8) Uani 1 d . . H20 H 0.7690(4) 0.6694(4) 0.3580(2) 0.042 Uiso 1 calc R . O14 O 0.8576(4) 1.5443(3) 0.2622(2) 0.0227(7) Uani 1 d . . H30 H 0.8847(4) 1.4533(3) 0.2829(2) 0.034 Uiso 1 calc R . O15 O 0.0579(4) 1.3336(4) 0.3493(3) 0.0319(9) Uani 1 d . . O16 O -0.0235(4) 1.2597(4) 0.5276(2) 0.0374(9) Uani 1 d . . H20' H 0.0562(4) 1.2812(4) 0.5438(2) 0.056 Uiso 1 calc R . N1 N 0.9045(5) 1.1629(4) 0.1865(3) 0.0260(10) Uani 1 d . . H1 H 0.8982(5) 1.2513(4) 0.1493(3) 0.039 Uiso 1 calc R . H2 H 0.8869(5) 1.1776(4) 0.2492(3) 0.039 Uiso 1 calc R . H3 H 0.8279(5) 1.1240(4) 0.1708(3) 0.039 Uiso 1 calc R . C1 C 1.0732(6) 1.0550(6) 0.1700(4) 0.0297(12) Uani 1 d . . H4 H 1.1575(6) 1.0968(6) 0.1866(4) 0.036 Uiso 1 calc R . H5 H 1.0936(6) 1.0387(6) 0.1017(4) 0.036 Uiso 1 calc R . C2 C 1.0802(6) 0.9046(5) 0.2346(4) 0.0251(11) Uani 1 d . . H6 H 1.0567(6) 0.9225(5) 0.3025(4) 0.030 Uiso 1 calc R . H7 H 0.9958(6) 0.8636(5) 0.2173(4) 0.030 Uiso 1 calc R . N2 N 1.2453(5) 0.7927(4) 0.2230(3) 0.0239(9) Uani 1 d . . H8 H 1.3227(5) 0.8337(4) 0.2370(3) 0.029 Uiso 1 calc R . H9 H 1.2651(5) 0.7768(4) 0.1598(3) 0.029 Uiso 1 calc R . C3 C 1.2665(6) 0.6428(5) 0.2847(3) 0.0244(11) Uani 1 d . . H10 H 1.1858(6) 0.5956(5) 0.2696(3) 0.029 Uiso 1 calc R . H11 H 1.2478(6) 0.6573(5) 0.3533(3) 0.029 Uiso 1 calc R . C4 C 1.4402(6) 0.5406(5) 0.2654(4) 0.0285(12) Uani 1 d . . H12 H 1.4606(6) 0.5343(5) 0.1958(4) 0.034 Uiso 1 calc R . H13 H 1.5194(6) 0.5864(5) 0.2844(4) 0.034 Uiso 1 calc R . C5 C 1.4699(6) 0.3822(6) 0.3193(4) 0.0323(13) Uani 1 d . . H14 H 1.5887(6) 0.3336(6) 0.3186(4) 0.039 Uiso 1 calc R . H15 H 1.4284(6) 0.3892(6) 0.3870(4) 0.039 Uiso 1 calc R . N3 N 1.3906(5) 0.2847(4) 0.2779(3) 0.0254(9) Uani 1 d . . H16 H 1.4130(5) 0.1931(4) 0.3131(3) 0.038 Uiso 1 calc R . H17 H 1.4300(5) 0.2754(4) 0.2162(3) 0.038 Uiso 1 calc R . H18 H 1.2811(5) 0.3270(4) 0.2797(3) 0.038 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 0.0168(3) 0.0202(3) 0.0165(3) -0.0012(2) -0.0042(2) -0.0065(2) Zn2 0.0159(3) 0.0166(3) 0.0168(3) -0.0012(2) -0.0048(2) -0.0058(2) Zn3 0.0177(3) 0.0161(3) 0.0156(3) -0.0011(2) -0.0059(2) -0.0064(2) P1 0.0144(6) 0.0147(6) 0.0143(6) -0.0006(5) -0.0056(5) -0.0048(5) P2 0.0166(6) 0.0185(6) 0.0140(6) -0.0036(5) -0.0046(5) -0.0049(5) P3 0.0153(6) 0.0160(6) 0.0147(6) -0.0020(5) -0.0033(5) -0.0036(5) P4 0.0163(6) 0.0227(6) 0.0152(6) 0.0023(5) -0.0051(5) -0.0077(5) O1 0.023(2) 0.032(2) 0.026(2) 0.005(2) -0.0097(15) 0.000(2) O2 0.028(2) 0.021(2) 0.020(2) -0.0017(14) 0.0023(14) -0.0074(15) O3 0.026(2) 0.021(2) 0.023(2) -0.0048(14) -0.0113(14) -0.0067(14) O4 0.022(2) 0.036(2) 0.019(2) 0.0038(15) -0.0039(14) -0.015(2) O5 0.046(2) 0.028(2) 0.019(2) 0.0022(15) -0.013(2) -0.021(2) O6 0.017(2) 0.031(2) 0.025(2) 0.005(2) 0.0025(14) 0.0010(15) O7 0.026(2) 0.025(2) 0.023(2) -0.0019(14) -0.0024(14) -0.0160(15) O8 0.027(2) 0.026(2) 0.021(2) -0.0013(15) -0.0032(14) 0.0015(15) O9 0.025(2) 0.016(2) 0.021(2) 0.0038(14) -0.0135(14) -0.0089(14) O10 0.018(2) 0.020(2) 0.027(2) -0.0001(14) -0.0029(14) -0.0020(14) O11 0.030(2) 0.031(2) 0.020(2) -0.0031(14) -0.0131(14) -0.014(2) O12 0.022(2) 0.033(2) 0.015(2) -0.0037(14) -0.0032(13) -0.0134(15) O13 0.021(2) 0.032(2) 0.033(2) -0.015(2) -0.0100(15) -0.0009(15) O14 0.028(2) 0.020(2) 0.016(2) 0.0011(14) -0.0053(14) -0.0012(14) O15 0.022(2) 0.031(2) 0.039(2) 0.015(2) -0.007(2) -0.009(2) O16 0.023(2) 0.069(3) 0.029(2) -0.019(2) -0.002(2) -0.019(2) N1 0.030(2) 0.021(2) 0.028(2) -0.001(2) -0.011(2) -0.006(2) C1 0.026(3) 0.030(3) 0.032(3) 0.003(2) -0.004(2) -0.010(2) C2 0.021(3) 0.024(3) 0.030(3) -0.004(2) -0.001(2) -0.006(2) N2 0.020(2) 0.029(2) 0.023(2) -0.003(2) -0.004(2) -0.007(2) C3 0.020(3) 0.027(3) 0.027(3) -0.005(2) 0.003(2) -0.008(2) C4 0.023(3) 0.029(3) 0.036(3) -0.004(2) -0.003(2) -0.011(2) C5 0.028(3) 0.037(3) 0.031(3) 0.002(2) -0.011(2) -0.007(2) N3 0.023(2) 0.026(2) 0.026(2) 0.002(2) -0.004(2) -0.007(2) _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 O2 1.932(3) . ? Zn1 O1 1.932(3) . ? Zn1 O3 1.964(3) . ? Zn1 O4 1.971(3) . ? Zn2 O5 1.928(3) . ? Zn2 O6 1.929(3) . ? Zn2 O7 1.950(3) . ? Zn2 O8 1.949(3) . ? Zn3 O11 1.910(3) . ? Zn3 O10 1.932(3) . ? Zn3 O9 1.945(3) . ? Zn3 O12 1.996(3) . ? P1 O11 1.518(3) 2_675 ? P1 O8 1.530(3) 2_685 ? P1 O7 1.537(3) . ? P1 O9 1.553(3) . ? P2 O2 1.519(3) . ? P2 O12 1.520(3) . ? P2 O3 1.526(3) 2_676 ? P2 O13 1.585(3) . ? P3 O6 1.517(3) 2_785 ? P3 O5 1.523(3) . ? P3 O10 1.524(3) 1_565 ? P3 O14 1.576(3) . ? P4 O1 1.507(3) . ? P4 O15 1.521(3) . ? P4 O4 1.522(3) 2_576 ? P4 O16 1.572(3) . ? O3 P2 1.526(3) 2_676 ? O4 P4 1.522(3) 2_576 ? O6 P3 1.517(3) 2_785 ? O8 P1 1.530(3) 2_685 ? O10 P3 1.524(3) 1_545 ? O11 P1 1.518(3) 2_675 ? O13 H20 0.82 . ? O14 H30 0.82 . ? O16 H20 0.82 . ? N1 C1 1.495(6) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? C1 C2 1.526(6) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 N2 1.480(6) . ? C2 H6 0.97 . ? C2 H7 0.97 . ? N2 C3 1.489(6) . ? N2 H8 0.90 . ? N2 H9 0.90 . ? C3 C4 1.512(6) . ? C3 H10 0.97 . ? C3 H11 0.97 . ? C4 C5 1.504(7) . ? C4 H12 0.97 . ? C4 H13 0.97 . ? C5 N3 1.486(6) . ? C5 H14 0.97 . ? C5 H15 0.97 . ? N3 H16 0.89 . ? N3 H17 0.89 . ? N3 H18 0.89 . ? 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 Zn1 O1 102.76(13) . . ? O2 Zn1 O3 105.32(13) . . ? O1 Zn1 O3 119.38(14) . . ? O2 Zn1 O4 120.06(14) . . ? O1 Zn1 O4 108.21(14) . . ? O3 Zn1 O4 102.12(13) . . ? O5 Zn2 O6 117.70(14) . . ? O5 Zn2 O7 102.87(13) . . ? O6 Zn2 O7 102.16(14) . . ? O5 Zn2 O8 117.37(14) . . ? O6 Zn2 O8 100.39(13) . . ? O7 Zn2 O8 115.94(14) . . ? O11 Zn3 O10 113.52(14) . . ? O11 Zn3 O9 115.96(13) . . ? O10 Zn3 O9 110.82(13) . . ? O11 Zn3 O12 98.74(13) . . ? O10 Zn3 O12 112.98(13) . . ? O9 Zn3 O12 103.85(13) . . ? O11 P1 O8 113.7(2) 2_675 2_685 ? O11 P1 O7 106.7(2) 2_675 . ? O8 P1 O7 111.1(2) 2_685 . ? O11 P1 O9 109.6(2) 2_675 . ? O8 P1 O9 106.8(2) 2_685 . ? O7 P1 O9 108.7(2) . . ? O2 P2 O12 110.7(2) . . ? O2 P2 O3 113.2(2) . 2_676 ? O12 P2 O3 110.7(2) . 2_676 ? O2 P2 O13 108.4(2) . . ? O12 P2 O13 108.3(2) . . ? O3 P2 O13 105.3(2) 2_676 . ? O6 P3 O5 110.6(2) 2_785 . ? O6 P3 O10 112.3(2) 2_785 1_565 ? O5 P3 O10 112.9(2) . 1_565 ? O6 P3 O14 106.7(2) 2_785 . ? O5 P3 O14 105.9(2) . . ? O10 P3 O14 108.0(2) 1_565 . ? O1 P4 O15 107.7(2) . . ? O1 P4 O4 113.8(2) . 2_576 ? O15 P4 O4 109.9(2) . 2_576 ? O1 P4 O16 109.6(2) . . ? O15 P4 O16 110.2(2) . . ? O4 P4 O16 105.7(2) 2_576 . ? P4 O1 Zn1 138.0(2) . . ? P2 O2 Zn1 124.6(2) . . ? P2 O3 Zn1 134.0(2) 2_676 . ? P4 O4 Zn1 129.2(2) 2_576 . ? P3 O5 Zn2 132.0(2) . . ? P3 O6 Zn2 134.3(2) 2_785 . ? P1 O7 Zn2 134.5(2) . . ? P1 O8 Zn2 136.2(2) 2_685 . ? P1 O9 Zn3 124.5(2) . . ? P3 O10 Zn3 131.3(2) 1_545 . ? P1 O11 Zn3 150.0(2) 2_675 . ? P2 O12 Zn3 135.9(2) . . ? P2 O13 H20 109.47(13) . . ? P3 O14 H30 109.47(12) . . ? P4 O16 H20 109.47(13) . . ? C1 N1 H1 109.5(2) . . ? C1 N1 H2 109.5(3) . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5(3) . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? N1 C1 C2 108.3(4) . . ? N1 C1 H4 110.0(3) . . ? C2 C1 H4 110.0(3) . . ? N1 C1 H5 110.0(3) . . ? C2 C1 H5 110.0(3) . . ? H4 C1 H5 108.4 . . ? N2 C2 C1 111.2(4) . . ? N2 C2 H6 109.4(2) . . ? C1 C2 H6 109.4(3) . . ? N2 C2 H7 109.4(2) . . ? C1 C2 H7 109.4(3) . . ? H6 C2 H7 108.0 . . ? C2 N2 C3 115.5(4) . . ? C2 N2 H8 108.4(2) . . ? C3 N2 H8 108.4(2) . . ? C2 N2 H9 108.4(2) . . ? C3 N2 H9 108.4(2) . . ? H8 N2 H9 107.5 . . ? N2 C3 C4 109.8(4) . . ? N2 C3 H10 109.7(2) . . ? C4 C3 H10 109.7(3) . . ? N2 C3 H11 109.7(2) . . ? C4 C3 H11 109.7(3) . . ? H10 C3 H11 108.2 . . ? C5 C4 C3 113.7(4) . . ? C5 C4 H12 108.8(3) . . ? C3 C4 H12 108.8(3) . . ? C5 C4 H13 108.8(3) . . ? C3 C4 H13 108.8(3) . . ? H12 C4 H13 107.7 . . ? N3 C5 C4 114.2(4) . . ? N3 C5 H14 108.7(2) . . ? C4 C5 H14 108.7(3) . . ? N3 C5 H15 108.7(2) . . ? C4 C5 H15 108.7(3) . . ? H14 C5 H15 107.6 . . ? C5 N3 H16 109.5(2) . . ? C5 N3 H17 109.5(2) . . ? H16 N3 H17 109.5 . . ? C5 N3 H18 109.5(2) . . ? H16 N3 H18 109.5 . . ? H17 N3 H18 109.5 . . ? _refine_diff_density_max 0.690 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.111