Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Microwave-assisted hydrothermal syntheses of metal phosphonates with layered and framework structures ; _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN loop_ _publ_author_name 'Li-Min Zheng' 'Song-Song Bao' 'Yun-Sheng Ma' 'Yi-Fan Yang' # Attachment 'Cd.cif' data_61201cm _database_code_depnum_ccdc_archive 'CCDC 641244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cd N O5 P' _chemical_formula_sum 'C6 H4 Cd N O5 P' _chemical_formula_weight 313.47 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.2706(10) _cell_length_b 8.7918(9) _cell_length_c 9.8810(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.466(2) _cell_angle_gamma 90.00 _cell_volume 786.37(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3558 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 28.24 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 2.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.555 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _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_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 4026 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1543 _reflns_number_gt 1508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0314P)^2^+0.6720P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1543 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Cd1 Cd -0.45492(2) 0.79188(2) 0.518484(19) 0.01449(10) Uani 1 1 d . . . P1 P 0.44649(7) 0.49805(7) 0.70342(7) 0.01227(15) Uani 1 1 d . . . N1 N 0.3133(3) 0.7356(3) 0.5485(3) 0.0182(5) Uani 1 1 d . . . C1 C 0.2883(3) 0.6177(3) 0.6266(3) 0.0150(5) Uani 1 1 d . . . C2 C 0.1478(3) 0.5905(3) 0.6508(3) 0.0178(5) Uani 1 1 d . . . H2A H 0.1310 0.5070 0.7032 0.021 Uiso 1 1 calc R . . C3 C 0.0338(3) 0.6887(3) 0.5961(3) 0.0198(6) Uani 1 1 d . . . C4 C 0.0610(3) 0.8074(4) 0.5124(3) 0.0250(7) Uani 1 1 d . . . H4A H -0.0149 0.8722 0.4708 0.030 Uiso 1 1 calc R . . C5 C 0.2009(3) 0.8275(4) 0.4921(3) 0.0246(6) Uani 1 1 d . . . H5A H 0.2189 0.9080 0.4370 0.029 Uiso 1 1 calc R . . C6 C -0.1186(3) 0.6787(3) 0.6233(3) 0.0202(6) Uani 1 1 d . . . O1 O 0.4601(2) 0.5128(2) 0.85991(19) 0.0166(4) Uani 1 1 d . . . O2 O 0.5764(2) 0.5651(2) 0.6528(2) 0.0180(4) Uani 1 1 d . . . O3 O 0.4082(2) 0.3381(2) 0.6572(2) 0.0215(4) Uani 1 1 d . . . O4 O -0.2004(2) 0.7888(2) 0.5961(3) 0.0252(5) Uani 1 1 d . . . O5 O -0.1525(2) 0.5521(3) 0.6752(2) 0.0288(5) Uani 1 1 d . . . H5D H -0.2417 0.5624 0.6963 0.035 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 Cd1 0.01358(15) 0.01343(14) 0.01723(14) -0.00035(6) 0.00500(9) 0.00086(6) P1 0.0129(3) 0.0122(3) 0.0123(3) 0.0007(2) 0.0042(2) 0.0008(3) N1 0.0176(13) 0.0188(11) 0.0184(12) 0.0037(10) 0.0044(10) 0.0006(10) C1 0.0160(13) 0.0141(12) 0.0152(12) -0.0008(10) 0.0037(10) 0.0009(10) C2 0.0175(14) 0.0184(13) 0.0181(13) 0.0028(10) 0.0050(11) -0.0011(10) C3 0.0158(14) 0.0217(14) 0.0222(14) -0.0009(11) 0.0046(11) -0.0004(10) C4 0.0182(16) 0.0247(16) 0.0321(18) 0.0083(12) 0.0055(14) 0.0068(11) C5 0.0214(15) 0.0239(14) 0.0286(16) 0.0122(13) 0.0056(13) 0.0028(12) C6 0.0148(14) 0.0241(14) 0.0212(14) -0.0016(11) 0.0027(11) -0.0011(11) O1 0.0208(10) 0.0159(9) 0.0130(9) 0.0008(7) 0.0035(7) -0.0020(8) O2 0.0130(9) 0.0211(10) 0.0208(10) 0.0045(8) 0.0055(7) 0.0019(7) O3 0.0300(11) 0.0159(9) 0.0208(10) -0.0018(8) 0.0104(9) -0.0019(9) O4 0.0158(11) 0.0214(11) 0.0389(14) -0.0002(8) 0.0072(10) 0.0029(8) O5 0.0147(10) 0.0300(12) 0.0436(13) 0.0113(10) 0.0103(9) 0.0027(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 Cd1 O3 2.198(2) 3_566 ? Cd1 N1 2.286(2) 1_455 ? Cd1 O1 2.2897(18) 2_556 ? Cd1 O4 2.318(2) . ? Cd1 O1 2.3436(18) 4_475 ? Cd1 O2 2.3779(19) 1_455 ? P1 O3 1.498(2) . ? P1 O2 1.5197(19) . ? P1 O1 1.5295(19) . ? P1 C1 1.831(3) . ? N1 C5 1.341(4) . ? N1 C1 1.342(4) . ? N1 Cd1 2.286(2) 1_655 ? C1 C2 1.395(4) . ? C2 C3 1.381(4) . ? C2 H2A 0.9300 . ? C3 C4 1.387(4) . ? C3 C6 1.496(4) . ? C4 C5 1.366(5) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O4 1.223(4) . ? C6 O5 1.292(4) . ? O1 Cd1 2.2897(18) 2_546 ? O1 Cd1 2.3436(18) 4_676 ? O2 Cd1 2.3779(19) 1_655 ? O3 Cd1 2.198(2) 3_566 ? O5 H5D 0.9004 . ? 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 O3 Cd1 N1 109.95(8) 3_566 1_455 ? O3 Cd1 O1 152.30(7) 3_566 2_556 ? N1 Cd1 O1 89.34(8) 1_455 2_556 ? O3 Cd1 O4 83.98(8) 3_566 . ? N1 Cd1 O4 150.75(9) 1_455 . ? O1 Cd1 O4 88.37(7) 2_556 . ? O3 Cd1 O1 87.03(7) 3_566 4_475 ? N1 Cd1 O1 93.19(7) 1_455 4_475 ? O1 Cd1 O1 71.77(7) 2_556 4_475 ? O4 Cd1 O1 113.65(7) . 4_475 ? O3 Cd1 O2 89.06(7) 3_566 1_455 ? N1 Cd1 O2 75.60(8) 1_455 1_455 ? O1 Cd1 O2 115.61(7) 2_556 1_455 ? O4 Cd1 O2 79.18(7) . 1_455 ? O1 Cd1 O2 166.05(6) 4_475 1_455 ? O3 P1 O2 114.60(12) . . ? O3 P1 O1 110.51(11) . . ? O2 P1 O1 113.70(10) . . ? O3 P1 C1 107.27(12) . . ? O2 P1 C1 105.16(12) . . ? O1 P1 C1 104.74(11) . . ? C5 N1 C1 119.3(2) . . ? C5 N1 Cd1 118.92(19) . 1_655 ? C1 N1 Cd1 121.70(19) . 1_655 ? N1 C1 C2 121.0(2) . . ? N1 C1 P1 117.4(2) . . ? C2 C1 P1 121.6(2) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.8(3) . . ? C2 C3 C6 124.4(3) . . ? C4 C3 C6 116.8(3) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 122.5(3) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? O4 C6 O5 125.1(3) . . ? O4 C6 C3 118.7(3) . . ? O5 C6 C3 116.2(3) . . ? P1 O1 Cd1 116.89(10) . 2_546 ? P1 O1 Cd1 132.88(10) . 4_676 ? Cd1 O1 Cd1 108.23(7) 2_546 4_676 ? P1 O2 Cd1 119.92(10) . 1_655 ? P1 O3 Cd1 130.92(12) . 3_566 ? C6 O4 Cd1 128.40(19) . . ? C6 O5 H5D 108.6 . . ? 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 C5 N1 C1 C2 -0.7(4) . . . . ? Cd1 N1 C1 C2 176.03(19) 1_655 . . . ? C5 N1 C1 P1 -179.0(2) . . . . ? Cd1 N1 C1 P1 -2.3(3) 1_655 . . . ? O3 P1 C1 N1 -123.9(2) . . . . ? O2 P1 C1 N1 -1.5(2) . . . . ? O1 P1 C1 N1 118.6(2) . . . . ? O3 P1 C1 C2 57.8(2) . . . . ? O2 P1 C1 C2 -179.8(2) . . . . ? O1 P1 C1 C2 -59.7(2) . . . . ? N1 C1 C2 C3 -1.5(4) . . . . ? P1 C1 C2 C3 176.7(2) . . . . ? C1 C2 C3 C4 3.3(4) . . . . ? C1 C2 C3 C6 -175.2(3) . . . . ? C2 C3 C4 C5 -3.0(5) . . . . ? C6 C3 C4 C5 175.6(3) . . . . ? C1 N1 C5 C4 1.0(5) . . . . ? Cd1 N1 C5 C4 -175.8(2) 1_655 . . . ? C3 C4 C5 N1 0.9(5) . . . . ? C2 C3 C6 O4 163.9(3) . . . . ? C4 C3 C6 O4 -14.7(4) . . . . ? C2 C3 C6 O5 -15.8(4) . . . . ? C4 C3 C6 O5 165.6(3) . . . . ? O3 P1 O1 Cd1 8.92(15) . . . 2_546 ? O2 P1 O1 Cd1 -121.60(11) . . . 2_546 ? C1 P1 O1 Cd1 124.15(12) . . . 2_546 ? O3 P1 O1 Cd1 170.59(13) . . . 4_676 ? O2 P1 O1 Cd1 40.08(17) . . . 4_676 ? C1 P1 O1 Cd1 -74.18(16) . . . 4_676 ? O3 P1 O2 Cd1 121.96(13) . . . 1_655 ? O1 P1 O2 Cd1 -109.59(12) . . . 1_655 ? C1 P1 O2 Cd1 4.41(15) . . . 1_655 ? O2 P1 O3 Cd1 -22.1(2) . . . 3_566 ? O1 P1 O3 Cd1 -152.12(14) . . . 3_566 ? C1 P1 O3 Cd1 94.25(17) . . . 3_566 ? O5 C6 O4 Cd1 -33.7(4) . . . . ? C3 C6 O4 Cd1 146.7(2) . . . . ? O3 Cd1 O4 C6 -59.8(3) 3_566 . . . ? N1 Cd1 O4 C6 61.1(3) 1_455 . . . ? O1 Cd1 O4 C6 146.8(3) 2_556 . . . ? O1 Cd1 O4 C6 -143.9(3) 4_475 . . . ? O2 Cd1 O4 C6 30.3(3) 1_455 . . . ? 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 O5 H5D O2 0.90 1.65 2.478(3) 152 1_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.475 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.153 # Attachment 'Zn.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 641245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H6 N O6 P Zn' _chemical_formula_sum 'C6 H6 N O6 P Zn' _chemical_formula_weight 284.46 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.137(2) _cell_length_b 6.5104(16) _cell_length_c 9.101(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.664(4) _cell_angle_gamma 90.00 _cell_volume 434.54(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 588 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 3.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.545 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _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_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 2331 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.99 _reflns_number_total 921 _reflns_number_gt 866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0483P)^2^+0.2133P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 921 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 1.21489(6) 0.2500 0.47521(5) 0.0192(2) Uani 1 2 d S . . P1 P 0.84029(14) 0.2500 0.49523(12) 0.0181(3) Uani 1 2 d S . . N1 N 0.9683(5) 0.2500 0.2629(4) 0.0231(8) Uani 1 2 d S . . C1 C 0.8149(5) 0.2500 0.2837(5) 0.0210(9) Uani 1 2 d S . . C2 C 0.6432(6) 0.2500 0.1513(5) 0.0221(9) Uani 1 2 d S . . H2A H 0.5380 0.2500 0.1677 0.027 Uiso 1 2 calc SR . . C3 C 0.6318(6) 0.2500 -0.0051(5) 0.0249(9) Uani 1 2 d S . . C4 C 0.7904(6) 0.2500 -0.0257(6) 0.0325(11) Uani 1 2 d S . . H4A H 0.7858 0.2500 -0.1296 0.039 Uiso 1 2 calc SR . . C5 C 0.9563(6) 0.2500 0.1111(6) 0.0318(11) Uani 1 2 d S . . H5A H 1.0630 0.2500 0.0974 0.038 Uiso 1 2 calc SR . . C6 C 0.4532(6) 0.2500 -0.1522(5) 0.0242(9) Uani 1 2 d S . . O1 O 1.0445(4) 0.2500 0.5959(4) 0.0251(7) Uani 1 2 d S . . O2 O 0.7450(3) 0.0603(4) 0.5142(3) 0.0263(5) Uani 1 1 d . . . O3 O 0.3105(4) 0.2500 -0.1224(4) 0.0304(7) Uani 1 2 d S . . H3D H 0.2120 0.2500 -0.2097 0.037 Uiso 1 2 d SR . . O4 O 0.4486(4) 0.2500 -0.2867(4) 0.0326(8) Uani 1 2 d S . . O1W O 1.3903(4) 0.2500 0.3593(4) 0.0269(7) Uani 1 2 d S . . H1WA H 1.4671 0.1439 0.3994 0.032 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 0.0148(3) 0.0230(3) 0.0187(3) 0.000 0.0063(2) 0.000 P1 0.0134(5) 0.0217(6) 0.0181(5) 0.000 0.0058(4) 0.000 N1 0.0183(18) 0.029(2) 0.0200(18) 0.000 0.0069(15) 0.000 C1 0.015(2) 0.020(2) 0.024(2) 0.000 0.0051(17) 0.000 C2 0.019(2) 0.027(2) 0.022(2) 0.000 0.0104(17) 0.000 C3 0.024(2) 0.026(2) 0.023(2) 0.000 0.0085(18) 0.000 C4 0.025(2) 0.051(3) 0.021(2) 0.000 0.0093(19) 0.000 C5 0.021(2) 0.050(3) 0.025(2) 0.000 0.0103(19) 0.000 C6 0.025(2) 0.020(2) 0.024(2) 0.000 0.0079(18) 0.000 O1 0.0140(14) 0.0422(19) 0.0178(15) 0.000 0.0057(12) 0.000 O2 0.0250(11) 0.0220(12) 0.0351(12) 0.0018(9) 0.0160(10) -0.0013(9) O3 0.0184(15) 0.049(2) 0.0209(15) 0.000 0.0057(13) 0.000 O4 0.0239(17) 0.050(2) 0.0190(16) 0.000 0.0046(13) 0.000 O1W 0.0215(16) 0.0297(18) 0.0308(17) 0.000 0.0127(14) 0.000 _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 2.042(2) 2_756 ? Zn1 O2 2.042(2) 3_756 ? Zn1 N1 2.098(4) . ? Zn1 O1 2.109(3) . ? Zn1 O1W 2.110(3) . ? Zn1 O4 2.177(3) 1_656 ? P1 O2 1.508(2) . ? P1 O2 1.508(2) 4_565 ? P1 O1 1.511(3) . ? P1 C1 1.845(4) . ? N1 C5 1.342(6) . ? N1 C1 1.342(5) . ? C1 C2 1.395(6) . ? C2 C3 1.386(6) . ? C2 H2A 0.9300 . ? C3 C4 1.382(7) . ? C3 C6 1.489(6) . ? C4 C5 1.384(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O4 1.209(5) . ? C6 O3 1.302(5) . ? O2 Zn1 2.042(2) 3_756 ? O3 H3D 0.8499 . ? O4 Zn1 2.177(3) 1_454 ? O1W H1WA 0.8965 . ? 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 O2 163.23(12) 2_756 3_756 ? O2 Zn1 N1 96.50(6) 2_756 . ? O2 Zn1 N1 96.50(6) 3_756 . ? O2 Zn1 O1 95.92(6) 2_756 . ? O2 Zn1 O1 95.92(6) 3_756 . ? N1 Zn1 O1 84.13(12) . . ? O2 Zn1 O1W 83.96(6) 2_756 . ? O2 Zn1 O1W 83.96(6) 3_756 . ? N1 Zn1 O1W 97.10(13) . . ? O1 Zn1 O1W 178.77(11) . . ? O2 Zn1 O4 84.26(6) 2_756 1_656 ? O2 Zn1 O4 84.26(6) 3_756 1_656 ? N1 Zn1 O4 172.39(13) . 1_656 ? O1 Zn1 O4 88.26(12) . 1_656 ? O1W Zn1 O4 90.51(12) . 1_656 ? O2 P1 O2 110.04(18) . 4_565 ? O2 P1 O1 114.57(11) . . ? O2 P1 O1 114.57(11) 4_565 . ? O2 P1 C1 106.77(11) . . ? O2 P1 C1 106.77(11) 4_565 . ? O1 P1 C1 103.29(17) . . ? C5 N1 C1 119.2(4) . . ? C5 N1 Zn1 124.2(3) . . ? C1 N1 Zn1 116.6(3) . . ? N1 C1 C2 121.6(4) . . ? N1 C1 P1 117.2(3) . . ? C2 C1 P1 121.3(3) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C4 C3 C2 119.2(4) . . ? C4 C3 C6 118.9(4) . . ? C2 C3 C6 121.9(4) . . ? C3 C4 C5 118.8(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 122.3(4) . . ? N1 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? O4 C6 O3 124.9(4) . . ? O4 C6 C3 120.0(4) . . ? O3 C6 C3 115.1(4) . . ? P1 O1 Zn1 118.84(17) . . ? P1 O2 Zn1 137.42(13) . 3_756 ? C6 O3 H3D 111.8 . . ? C6 O4 Zn1 129.7(3) . 1_454 ? Zn1 O1W H1WA 107.5 . . ? 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 O2 Zn1 N1 C5 84.69(6) 2_756 . . . ? O2 Zn1 N1 C5 -84.69(6) 3_756 . . . ? O1 Zn1 N1 C5 180.0 . . . . ? O1W Zn1 N1 C5 0.0 . . . . ? O2 Zn1 N1 C1 -95.31(6) 2_756 . . . ? O2 Zn1 N1 C1 95.31(6) 3_756 . . . ? O1 Zn1 N1 C1 0.0 . . . . ? O1W Zn1 N1 C1 180.0 . . . . ? C5 N1 C1 C2 0.0 . . . . ? Zn1 N1 C1 C2 180.0 . . . . ? C5 N1 C1 P1 180.0 . . . . ? Zn1 N1 C1 P1 0.0 . . . . ? O2 P1 C1 N1 -121.16(10) . . . . ? O2 P1 C1 N1 121.16(10) 4_565 . . . ? O1 P1 C1 N1 0.0 . . . . ? O2 P1 C1 C2 58.84(10) . . . . ? O2 P1 C1 C2 -58.84(10) 4_565 . . . ? O1 P1 C1 C2 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? P1 C1 C2 C3 180.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C6 180.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C6 C3 C4 C5 180.0 . . . . ? C1 N1 C5 C4 0.0 . . . . ? Zn1 N1 C5 C4 180.0 . . . . ? C3 C4 C5 N1 0.0 . . . . ? C4 C3 C6 O4 0.0 . . . . ? C2 C3 C6 O4 180.0 . . . . ? C4 C3 C6 O3 180.0 . . . . ? C2 C3 C6 O3 0.0 . . . . ? O2 P1 O1 Zn1 115.72(11) . . . . ? O2 P1 O1 Zn1 -115.72(11) 4_565 . . . ? C1 P1 O1 Zn1 0.0 . . . . ? O2 Zn1 O1 P1 95.95(6) 2_756 . . . ? O2 Zn1 O1 P1 -95.95(6) 3_756 . . . ? N1 Zn1 O1 P1 0.0 . . . . ? O4 Zn1 O1 P1 180.0 1_656 . . . ? O2 P1 O2 Zn1 -174.3(2) 4_565 . . 3_756 ? O1 P1 O2 Zn1 -43.5(3) . . . 3_756 ? C1 P1 O2 Zn1 70.2(2) . . . 3_756 ? O3 C6 O4 Zn1 0.0 . . . 1_454 ? C3 C6 O4 Zn1 180.0 . . . 1_454 ? 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 O3 H3D O1 0.85 1.70 2.539(4) 168 1_454 O1W H1WA O2 0.90 2.11 2.884(4) 144.0 1_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.702 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.094