Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Philip Lightfoot' _publ_contact_author_address ; Department of Chemistry University of St Andrews St Andrews Fife KY16 9ST UK ; _publ_contact_author_email PL@ST-ANDREWS.AC.UK _publ_section_title ; The pH-controlled hydrothermal synthesis and crystal structures of two zinc N,N'-piperazinebis(methylenephosphonate) frameworks ; loop_ _publ_author_name 'Philip Lightfoot' 'John A. Groves' 'P. Wright' data_I _database_code_depnum_ccdc_archive 'CCDC 263840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 N4 O14 P4 Zn2' _chemical_formula_weight 711.04 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 8.3172(19) _cell_length_b 8.8825(7) _cell_length_c 8.9558(15) _cell_angle_alpha 64.176(15) _cell_angle_beta 86.29(2) _cell_angle_gamma 79.11(2) _cell_volume 584.72(17) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2140 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.3 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4219 _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 3691 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2017 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.3343P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2017 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.25696(5) 0.07143(5) 0.42647(5) 0.00732(18) Uani 1 1 d . . . P1 P 0.44523(11) 0.02967(11) 0.75076(11) 0.0063(2) Uani 1 1 d . . . P2 P -0.07819(11) 0.25538(11) 0.45647(12) 0.0067(2) Uani 1 1 d . . . O1 O 0.3703(3) 0.1185(3) 0.5770(3) 0.0086(6) Uani 1 1 d . . . O2 O 0.6040(3) -0.0959(3) 0.7628(3) 0.0096(6) Uani 1 1 d . . . O3 O 0.0667(3) 0.2558(3) 0.3406(3) 0.0118(6) Uani 1 1 d . . . O4 O -0.1976(3) 0.1492(3) 0.4472(3) 0.0142(6) Uani 1 1 d . . . O5 O 0.4617(3) 0.1606(3) 0.8105(3) 0.0086(6) Uani 1 1 d . . . O6 O -0.0291(3) 0.2170(3) 0.6298(3) 0.0121(6) Uani 1 1 d . . . O7 O 0.2533(4) 0.4434(3) 0.0545(4) 0.0292(8) Uani 1 1 d . . . C1 C 0.3098(4) -0.1118(4) 0.8851(4) 0.0076(8) Uani 1 1 d . . . H1A H 0.3005 -0.1935 0.8428 0.009 Uiso 1 1 calc R . . H1B H 0.3600 -0.1747 0.9950 0.009 Uiso 1 1 calc R . . C2 C -0.1823(4) 0.4771(4) 0.3503(4) 0.0073(7) Uani 1 1 d . . . H2A H -0.1129 0.5482 0.3613 0.009 Uiso 1 1 calc R . . H2B H -0.1898 0.5056 0.2331 0.009 Uiso 1 1 calc R . . C3 C 0.1429(4) 0.0644(4) 1.0090(5) 0.0085(8) Uani 1 1 d . . . H3A H 0.2134 0.1486 0.9614 0.010 Uiso 1 1 calc R . . H3B H 0.1878 -0.0177 1.1174 0.010 Uiso 1 1 calc R . . N2 N -0.3509(3) 0.5250(4) 0.4061(4) 0.0067(6) Uiso 1 1 d . . . H2 H -0.3799 0.6399 0.3492 0.008 Uiso 1 1 calc R . . C4 C 0.0280(4) -0.1508(4) 0.9716(5) 0.0080(8) Uani 1 1 d . . . H4A H 0.0705 -0.2379 1.0790 0.010 Uiso 1 1 calc R . . H4B H 0.0228 -0.2052 0.8992 0.010 Uiso 1 1 calc R . . C5 C -0.4786(4) 0.4487(4) 0.3651(5) 0.0081(8) Uani 1 1 d . . . H5A H -0.4539 0.3258 0.4250 0.010 Uiso 1 1 calc R . . H5B H -0.4779 0.4783 0.2473 0.010 Uiso 1 1 calc R . . C6 C -0.3536(4) 0.4855(4) 0.5875(4) 0.0078(7) Uani 1 1 d . . . H6A H -0.2722 0.5376 0.6113 0.009 Uiso 1 1 calc R . . H6B H -0.3260 0.3635 0.6532 0.009 Uiso 1 1 calc R . . N1 N 0.1407(3) -0.0240(4) 0.9002(4) 0.0066(6) Uani 1 1 d . . . H1 H 0.1025 0.0544 0.7975 0.008 Uiso 1 1 calc R . . H7 H 0.3470 0.3805 0.0693 0.020 Uiso 1 1 d R . . H8 H 0.1859 0.4221 0.1358 0.020 Uiso 1 1 d 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 0.0041(3) 0.0066(3) 0.0111(3) -0.00379(19) -0.00026(17) -0.00024(17) P1 0.0030(5) 0.0060(5) 0.0086(5) -0.0024(4) 0.0009(4) -0.0003(3) P2 0.0036(5) 0.0041(5) 0.0110(5) -0.0025(4) -0.0005(4) 0.0006(3) O1 0.0067(12) 0.0077(12) 0.0120(14) -0.0041(10) 0.0002(10) -0.0032(10) O2 0.0060(12) 0.0073(12) 0.0147(13) -0.0051(10) 0.0007(10) 0.0010(10) O3 0.0057(12) 0.0150(13) 0.0161(14) -0.0086(11) 0.0024(11) -0.0009(10) O4 0.0099(13) 0.0039(12) 0.0260(16) -0.0036(11) -0.0034(12) -0.0007(10) O5 0.0074(12) 0.0082(12) 0.0104(13) -0.0037(11) -0.0013(10) -0.0025(10) O6 0.0097(13) 0.0095(13) 0.0109(13) -0.0007(11) -0.0013(11) 0.0038(10) O7 0.044(2) 0.0162(16) 0.0206(17) -0.0040(13) 0.0078(15) -0.0017(14) C1 0.0032(17) 0.0068(17) 0.0111(18) -0.0038(14) 0.0009(14) 0.0024(13) C2 0.0045(17) 0.0078(18) 0.0083(18) -0.0024(14) 0.0008(14) -0.0013(13) C3 0.0060(18) 0.0105(18) 0.0119(18) -0.0071(15) 0.0019(14) -0.0032(14) C4 0.0064(17) 0.0053(17) 0.0118(19) -0.0027(14) 0.0009(14) -0.0020(14) C5 0.0058(17) 0.0080(18) 0.0109(18) -0.0042(14) -0.0024(14) -0.0007(14) C6 0.0054(17) 0.0066(17) 0.0114(18) -0.0037(14) 0.0000(14) -0.0015(13) N1 0.0019(14) 0.0073(14) 0.0088(15) -0.0025(12) 0.0001(12) 0.0006(11) _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 1.920(3) . ? Zn1 O4 1.930(3) 2_556 ? Zn1 O2 1.943(3) 2_656 ? Zn1 O3 1.964(3) . ? P1 O5 1.507(3) . ? P1 O1 1.517(3) . ? P1 O2 1.535(2) . ? P1 C1 1.827(4) . ? P2 O6 1.504(3) . ? P2 O4 1.522(3) . ? P2 O3 1.538(3) . ? P2 C2 1.834(3) . ? O2 Zn1 1.943(3) 2_656 ? O4 Zn1 1.930(3) 2_556 ? O7 H7 0.8495 . ? O7 H8 0.8644 . ? C1 N1 1.503(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.506(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.496(5) . ? C3 C4 1.520(5) 2_557 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N2 C5 1.504(5) . ? N2 C6 1.504(5) . ? N2 H2 0.9100 . ? C4 N1 1.500(4) . ? C4 C3 1.520(5) 2_557 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.517(5) 2_466 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.517(5) 2_466 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N1 H1 0.9100 . ? 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 O4 106.72(11) . 2_556 ? O1 Zn1 O2 108.08(11) . 2_656 ? O4 Zn1 O2 116.44(11) 2_556 2_656 ? O1 Zn1 O3 106.00(11) . . ? O4 Zn1 O3 113.18(11) 2_556 . ? O2 Zn1 O3 105.87(10) 2_656 . ? O5 P1 O1 109.33(14) . . ? O5 P1 O2 114.43(15) . . ? O1 P1 O2 112.38(15) . . ? O5 P1 C1 110.50(16) . . ? O1 P1 C1 107.89(16) . . ? O2 P1 C1 101.94(15) . . ? O6 P2 O4 114.50(16) . . ? O6 P2 O3 114.16(15) . . ? O4 P2 O3 111.12(16) . . ? O6 P2 C2 109.77(16) . . ? O4 P2 C2 105.58(15) . . ? O3 P2 C2 100.40(15) . . ? P1 O1 Zn1 140.07(16) . . ? P1 O2 Zn1 122.65(15) . 2_656 ? P2 O3 Zn1 118.18(15) . . ? P2 O4 Zn1 139.60(17) . 2_556 ? H7 O7 H8 119.4 . . ? N1 C1 P1 114.8(2) . . ? N1 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? N2 C2 P2 118.0(2) . . ? N2 C2 H2A 107.8 . . ? P2 C2 H2A 107.8 . . ? N2 C2 H2B 107.8 . . ? P2 C2 H2B 107.8 . . ? H2A C2 H2B 107.1 . . ? N1 C3 C4 111.5(3) . 2_557 ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 2_557 . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 2_557 . ? H3A C3 H3B 108.0 . . ? C5 N2 C6 110.6(3) . . ? C5 N2 C2 113.3(3) . . ? C6 N2 C2 112.3(3) . . ? C5 N2 H2 106.7 . . ? C6 N2 H2 106.7 . . ? C2 N2 H2 106.7 . . ? N1 C4 C3 110.7(3) . 2_557 ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 2_557 . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 2_557 . ? H4A C4 H4B 108.1 . . ? N2 C5 C6 109.9(3) . 2_466 ? N2 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 2_466 . ? N2 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 2_466 . ? H5A C5 H5B 108.2 . . ? N2 C6 C5 110.7(3) . 2_466 ? N2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 2_466 . ? N2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 2_466 . ? H6A C6 H6B 108.1 . . ? C3 N1 C4 109.2(3) . . ? C3 N1 C1 110.9(3) . . ? C4 N1 C1 110.0(3) . . ? C3 N1 H1 108.9 . . ? C4 N1 H1 108.9 . . ? C1 N1 H1 108.9 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.802 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.136 #===end data_II _database_code_depnum_ccdc_archive 'CCDC 263841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 N2 O6 P2 Zn2' _chemical_formula_weight 400.86 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.2531(4) _cell_length_b 10.6598(6) _cell_length_c 8.5163(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.4260(10) _cell_angle_gamma 90.00 _cell_volume 556.42(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 30.5 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 4.619 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.693 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6117 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 30.48 _reflns_number_total 1672 _reflns_number_gt 1484 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1672 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.167 _refine_ls_shift/su_mean 0.015 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 0.15651(4) 0.89560(2) 0.72145(3) 0.01019(10) Uani 1 1 d . . . P1 P 0.25618(9) 0.66097(5) 0.90279(7) 0.01021(13) Uani 1 1 d . . . N1 N 0.0285(3) 0.87672(16) 0.9314(2) 0.0088(3) Uani 1 1 d . . . O1 O 0.3431(3) 0.74973(16) 0.78950(19) 0.0153(3) Uani 1 1 d . . . O2 O 0.1811(3) 0.53594(15) 0.8238(2) 0.0151(3) Uani 1 1 d . . . O3 O 0.4090(3) 0.64670(18) 1.0613(2) 0.0230(4) Uani 1 1 d . . . C1 C 0.0097(4) 0.73700(19) 0.9398(3) 0.0113(4) Uani 1 1 d . . . C2 C -0.1917(4) 0.9333(2) 0.9251(3) 0.0107(4) Uani 1 1 d . . . C3 C 0.1775(4) 0.9252(2) 1.0762(3) 0.0108(4) Uani 1 1 d . . . H11 H -0.109(5) 0.704(3) 0.873(4) 0.014(7) Uiso 1 1 d . . . H12 H -0.024(5) 0.705(3) 1.038(4) 0.024(8) Uiso 1 1 d . . . H21 H -0.293(5) 0.907(2) 0.823(4) 0.010(7) Uiso 1 1 d . . . H22 H -0.242(5) 0.901(2) 1.023(4) 0.015(8) Uiso 1 1 d . . . H31 H 0.312(5) 0.887(3) 1.082(4) 0.018(8) Uiso 1 1 d . . . H32 H 0.129(5) 0.887(3) 1.165(4) 0.018(8) Uiso 1 1 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 0.01353(16) 0.00725(15) 0.00981(15) 0.00069(7) 0.00239(11) -0.00111(8) P1 0.0137(3) 0.0075(2) 0.0093(3) -0.00039(17) 0.0020(2) 0.00231(19) N1 0.0108(9) 0.0066(7) 0.0088(8) -0.0019(6) 0.0013(7) 0.0011(6) O1 0.0181(8) 0.0106(8) 0.0201(9) 0.0039(6) 0.0108(7) 0.0045(6) O2 0.0161(8) 0.0090(7) 0.0206(8) -0.0041(6) 0.0045(7) 0.0028(6) O3 0.0271(10) 0.0248(9) 0.0135(8) -0.0021(7) -0.0044(7) 0.0126(8) C1 0.0148(10) 0.0062(8) 0.0138(10) -0.0009(7) 0.0050(8) -0.0004(7) C2 0.0086(9) 0.0102(9) 0.0130(10) -0.0032(7) 0.0011(8) 0.0009(7) C3 0.0105(10) 0.0093(9) 0.0116(10) -0.0013(7) 0.0000(8) 0.0024(8) _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 1.8900(16) 2_556 ? Zn1 O3 1.9031(18) 4_575 ? Zn1 O1 1.9615(17) . ? Zn1 N1 2.1083(18) . ? P1 O3 1.4994(18) . ? P1 O2 1.5246(17) . ? P1 O1 1.5262(17) . ? P1 C1 1.823(2) . ? N1 C3 1.483(3) . ? N1 C2 1.494(3) . ? N1 C1 1.497(3) . ? O2 Zn1 1.8900(16) 2_546 ? O3 Zn1 1.9031(18) 4_676 ? C1 H11 0.91(3) . ? C1 H12 0.97(3) . ? C2 C3 1.511(3) 3_577 ? C2 H21 1.01(3) . ? C2 H22 1.00(3) . ? C3 C2 1.511(3) 3_577 ? C3 H31 0.93(3) . ? C3 H32 0.96(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 O2 Zn1 O3 115.79(8) 2_556 4_575 ? O2 Zn1 O1 112.06(7) 2_556 . ? O3 Zn1 O1 112.06(8) 4_575 . ? O2 Zn1 N1 123.90(7) 2_556 . ? O3 Zn1 N1 101.16(8) 4_575 . ? O1 Zn1 N1 88.70(7) . . ? O3 P1 O2 113.24(11) . . ? O3 P1 O1 112.88(11) . . ? O2 P1 O1 112.33(10) . . ? O3 P1 C1 107.41(10) . . ? O2 P1 C1 105.54(10) . . ? O1 P1 C1 104.64(9) . . ? C3 N1 C2 108.16(16) . . ? C3 N1 C1 110.44(17) . . ? C2 N1 C1 108.82(17) . . ? C3 N1 Zn1 112.98(13) . . ? C2 N1 Zn1 115.66(14) . . ? C1 N1 Zn1 100.49(12) . . ? P1 O1 Zn1 114.38(9) . . ? P1 O2 Zn1 130.61(10) . 2_546 ? P1 O3 Zn1 162.17(12) . 4_676 ? N1 C1 P1 110.92(15) . . ? N1 C1 H11 114.4(19) . . ? P1 C1 H11 109.4(18) . . ? N1 C1 H12 115.5(19) . . ? P1 C1 H12 109.2(18) . . ? H11 C1 H12 96(2) . . ? N1 C2 C3 110.38(18) . 3_577 ? N1 C2 H21 109.4(16) . . ? C3 C2 H21 107.4(15) 3_577 . ? N1 C2 H22 105.6(16) . . ? C3 C2 H22 112.0(16) 3_577 . ? H21 C2 H22 112(2) . . ? N1 C3 C2 111.67(18) . 3_577 ? N1 C3 H31 108(2) . . ? C2 C3 H31 112.4(18) 3_577 . ? N1 C3 H32 105(2) . . ? C2 C3 H32 117.1(18) 3_577 . ? H31 C3 H32 102(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.861 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.130