Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Guo-Yu Yang' 'Zhi-En Lin' 'You-Wei Yao' 'Jie Zhang' _publ_contact_author_name 'Prof Guo-Yu Yang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter 155, West Yangqiao Road Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email YGY@MS.FJIRSM.AC.CN _publ_section_title ; Isolation of a monomeric hybrid zinc phosphate and its one-dimensional relative ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; data_1 _database_code_CSD 208837 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 N4 O12 P3 Zn2' _chemical_formula_weight 781.10 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 40.391(3) _cell_length_b 7.4568(4) _cell_length_c 17.4247(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5248.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.07 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5985 _exptl_absorpt_correction_T_max 1.0000 _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 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3813 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2024 _reflns_number_gt 1898 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0422P)^2^+37.2335P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(18) _refine_ls_number_reflns 2024 _refine_ls_number_parameters 204 _refine_ls_number_restraints 1 _refine_ls_r_factor_ref 0.0382 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.070 _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 0.705257(14) 0.61587(8) 0.34954(4) 0.01949(16) Uani 1 1 d . . . P1 P 0.76635(3) 0.51926(18) 0.45156(8) 0.0180(3) Uani 1 1 d . . . P2 P 0.7500 0.7500 0.20168(11) 0.0215(4) Uani 1 2 d S . . O1 O 0.72221(10) 0.6686(6) 0.2467(2) 0.0346(10) Uani 1 1 d . . . O2 O 0.78513(9) 0.6559(5) 0.4068(2) 0.0272(9) Uani 1 1 d . . . O3 O 0.73497(8) 0.4536(5) 0.4111(2) 0.0247(9) Uani 1 1 d . . . O4 O 0.75848(9) 0.5889(5) 0.5336(2) 0.0254(9) Uani 1 1 d . . . O5 O 0.78900(9) 0.3503(5) 0.4654(2) 0.0277(9) Uani 1 1 d . . . H1 H 0.7800 0.2612 0.4473 0.042 Uiso 1 1 calc R . . O6 O 0.73290(10) 0.8891(6) 0.1479(3) 0.0424(13) Uani 1 1 d . . . H2 H 0.7466 0.9307 0.1181 0.064 Uiso 1 1 calc R . . N1 N 0.65346(10) 0.6726(6) 0.3638(2) 0.0202(9) Uani 1 1 d . . . N2 N 0.68023(10) 0.3720(6) 0.3087(3) 0.0221(10) Uani 1 1 d . . . C1 C 0.64047(13) 0.8215(8) 0.3931(3) 0.0247(12) Uani 1 1 d . . . H3 H 0.6547 0.9101 0.4110 0.030 Uiso 1 1 calc R . . C2 C 0.60610(15) 0.8511(8) 0.3982(4) 0.0321(15) Uani 1 1 d . . . H4 H 0.5979 0.9563 0.4197 0.039 Uiso 1 1 calc R . . C3 C 0.58495(13) 0.7237(8) 0.3712(3) 0.0291(13) Uani 1 1 d . . . H5 H 0.5622 0.7440 0.3721 0.035 Uiso 1 1 calc R . . C4 C 0.59748(12) 0.5603(8) 0.3416(3) 0.0235(11) Uani 1 1 d . . . C5 C 0.57738(13) 0.4154(9) 0.3156(3) 0.0290(13) Uani 1 1 d . . . H6 H 0.5545 0.4270 0.3168 0.035 Uiso 1 1 calc R . . C6 C 0.59097(13) 0.2612(8) 0.2890(3) 0.0290(13) Uani 1 1 d . . . H7 H 0.5773 0.1673 0.2738 0.035 Uiso 1 1 calc R . . C7 C 0.62620(13) 0.2414(8) 0.2843(3) 0.0224(11) Uani 1 1 d . . . C8 C 0.64183(14) 0.0873(8) 0.2556(3) 0.0284(13) Uani 1 1 d . . . H8 H 0.6292 -0.0083 0.2376 0.034 Uiso 1 1 calc R . . C9 C 0.67571(15) 0.0783(8) 0.2542(4) 0.0327(14) Uani 1 1 d . . . H9 H 0.6864 -0.0234 0.2355 0.039 Uiso 1 1 calc R . . C10 C 0.69393(14) 0.2234(8) 0.2811(3) 0.0283(13) Uani 1 1 d . . . H10 H 0.7169 0.2161 0.2798 0.034 Uiso 1 1 calc R . . C11 C 0.64664(13) 0.3790(8) 0.3102(3) 0.0208(12) Uani 1 1 d . . . C12 C 0.63270(11) 0.5443(7) 0.3391(3) 0.0194(11) Uani 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 0.0148(2) 0.0202(3) 0.0235(3) 0.0015(3) -0.0027(2) -0.0020(2) P1 0.0148(6) 0.0158(7) 0.0233(7) 0.0025(6) -0.0032(5) -0.0022(5) P2 0.0195(9) 0.0248(10) 0.0201(9) 0.000 0.000 0.0004(8) O1 0.030(2) 0.044(3) 0.030(2) 0.006(2) 0.0007(18) -0.0164(19) O2 0.0229(19) 0.025(2) 0.033(2) 0.0059(19) 0.0047(16) -0.0052(16) O3 0.0229(18) 0.0173(19) 0.034(2) 0.0046(18) -0.0113(16) -0.0044(15) O4 0.031(2) 0.024(2) 0.021(2) 0.0047(17) 0.0008(16) -0.0005(17) O5 0.0214(19) 0.019(2) 0.043(3) -0.0001(18) -0.0105(16) 0.0019(15) O6 0.031(2) 0.058(3) 0.039(3) 0.028(2) 0.0105(19) 0.015(2) N1 0.017(2) 0.019(2) 0.024(3) 0.0024(19) 0.0005(17) -0.0010(17) N2 0.011(2) 0.031(3) 0.024(2) 0.009(2) -0.0054(17) -0.0012(18) C1 0.025(3) 0.026(3) 0.024(3) 0.001(2) -0.001(2) 0.000(2) C2 0.033(3) 0.030(4) 0.033(3) -0.001(3) 0.004(3) 0.011(3) C3 0.019(3) 0.039(4) 0.029(3) 0.003(3) -0.001(2) 0.006(2) C4 0.015(2) 0.033(3) 0.023(3) 0.001(3) 0.001(2) 0.001(2) C5 0.015(2) 0.044(4) 0.028(3) 0.002(3) -0.001(2) -0.004(2) C6 0.018(3) 0.032(3) 0.037(3) 0.002(3) -0.008(2) -0.006(2) C7 0.021(3) 0.025(3) 0.021(3) 0.005(2) -0.003(2) -0.005(2) C8 0.029(3) 0.026(3) 0.029(3) -0.003(3) -0.005(2) 0.000(2) C9 0.037(3) 0.026(3) 0.036(4) -0.001(3) -0.002(3) 0.008(3) C10 0.022(3) 0.028(3) 0.035(3) -0.001(3) -0.004(2) 0.004(2) C11 0.018(2) 0.026(3) 0.019(3) 0.004(2) -0.001(2) 0.002(2) C12 0.014(2) 0.027(3) 0.017(2) 0.003(2) 0.0011(19) -0.001(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 1.958(4) . ? Zn1 O2 2.010(4) 14_665 ? Zn1 O3 2.014(4) . ? Zn1 N1 2.149(4) . ? Zn1 N2 2.199(5) . ? P1 O2 1.491(4) . ? P1 O3 1.530(3) . ? P1 O4 1.554(4) . ? P1 O5 1.575(4) . ? P2 O1 1.498(4) 14_665 ? P2 O1 1.498(4) . ? P2 O6 1.560(4) 14_665 ? P2 O6 1.560(4) . ? O2 Zn1 2.010(4) 14_665 ? O5 H1 0.8200 . ? O6 H2 0.8200 . ? N1 C1 1.330(7) . ? N1 C12 1.343(7) . ? N2 C10 1.328(7) . ? N2 C11 1.358(6) . ? C1 C2 1.408(8) . ? C1 H3 0.9300 . ? C2 C3 1.361(9) . ? C2 H4 0.9300 . ? C3 C4 1.416(8) . ? C3 H5 0.9300 . ? C4 C5 1.426(8) . ? C4 C12 1.428(7) . ? C5 C6 1.356(9) . ? C5 H6 0.9300 . ? C6 C7 1.433(7) . ? C6 H7 0.9300 . ? C7 C11 1.392(8) . ? C7 C8 1.403(8) . ? C8 C9 1.370(8) . ? C8 H8 0.9300 . ? C9 C10 1.390(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.446(7) . ? 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 O2 102.51(17) . 14_665 ? O1 Zn1 O3 113.57(17) . . ? O2 Zn1 O3 97.41(15) 14_665 . ? O1 Zn1 N1 114.01(17) . . ? O2 Zn1 N1 87.94(16) 14_665 . ? O3 Zn1 N1 129.55(16) . . ? O1 Zn1 N2 91.75(17) . . ? O2 Zn1 N2 161.70(16) 14_665 . ? O3 Zn1 N2 87.12(15) . . ? N1 Zn1 N2 75.68(16) . . ? O2 P1 O3 113.5(2) . . ? O2 P1 O4 110.9(2) . . ? O3 P1 O4 111.2(2) . . ? O2 P1 O5 109.3(2) . . ? O3 P1 O5 107.2(2) . . ? O4 P1 O5 104.2(2) . . ? O1 P2 O1 116.8(3) 14_665 . ? O1 P2 O6 104.6(2) 14_665 14_665 ? O1 P2 O6 112.2(3) . 14_665 ? O1 P2 O6 112.2(3) 14_665 . ? O1 P2 O6 104.6(2) . . ? O6 P2 O6 106.1(4) 14_665 . ? P2 O1 Zn1 145.3(3) . . ? P1 O2 Zn1 159.5(2) . 14_665 ? P1 O3 Zn1 123.2(2) . . ? P1 O5 H1 109.5 . . ? P2 O6 H2 109.5 . . ? C1 N1 C12 118.1(4) . . ? C1 N1 Zn1 126.4(4) . . ? C12 N1 Zn1 115.5(3) . . ? C10 N2 C11 117.1(5) . . ? C10 N2 Zn1 128.0(4) . . ? C11 N2 Zn1 114.9(4) . . ? N1 C1 C2 122.9(5) . . ? N1 C1 H3 118.5 . . ? C2 C1 H3 118.5 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H4 120.4 . . ? C1 C2 H4 120.4 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H5 119.9 . . ? C4 C3 H5 119.9 . . ? C3 C4 C5 124.4(5) . . ? C3 C4 C12 116.1(5) . . ? C5 C4 C12 119.6(5) . . ? C6 C5 C4 121.4(5) . . ? C6 C5 H6 119.3 . . ? C4 C5 H6 119.3 . . ? C5 C6 C7 120.6(5) . . ? C5 C6 H7 119.7 . . ? C7 C6 H7 119.7 . . ? C11 C7 C8 116.9(5) . . ? C11 C7 C6 119.6(5) . . ? C8 C7 C6 123.5(5) . . ? C9 C8 C7 119.7(6) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.0(6) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 123.4(5) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N2 C11 C7 123.9(5) . . ? N2 C11 C12 115.4(5) . . ? C7 C11 C12 120.7(5) . . ? N1 C12 C4 123.5(5) . . ? N1 C12 C11 118.4(4) . . ? C4 C12 C11 118.0(5) . . ? 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 H1 O3 0.82 1.82 2.640(5) 172.3 14_655 O6 H2 O4 0.82 1.95 2.692(5) 151.0 5_554 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.436 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.087 data_znpphen _database_code_CSD 208838 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 N4 O12.50 P3 Zn2' _chemical_formula_weight 790.11 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 10.3179(2) _cell_length_b 12.4168(2) _cell_length_c 12.9696(2) _cell_angle_alpha 65.057(2) _cell_angle_beta 74.625(2) _cell_angle_gamma 71.593(2) _cell_volume 1412.62(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 25.15 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 1.943 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6794 _exptl_absorpt_correction_T_max 1.0000 _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 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7199 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.15 _reflns_number_total 4868 _reflns_number_gt 3555 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0701P)^2^+1.8501P] 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 4868 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0720 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.38843(6) 0.19549(5) 0.48919(5) 0.02555(18) Uani 1 1 d . . . Zn2 Zn 0.70594(6) 0.32608(5) 0.05994(5) 0.02722(18) Uani 1 1 d . . . P1 P 0.68691(13) 0.22179(12) 0.32450(11) 0.0265(3) Uani 1 1 d . . . P2 P 0.37461(13) 0.40029(12) 0.13420(12) 0.0272(3) Uani 1 1 d . . . P3 P 0.40362(14) 0.02527(12) 0.34900(11) 0.0268(3) Uani 1 1 d . . . O1 O 0.7378(3) 0.3110(3) 0.2112(3) 0.0300(8) Uani 1 1 d . . . O2 O 0.5355(3) 0.2675(3) 0.3689(3) 0.0300(8) Uani 1 1 d . . . O3 O 0.5017(3) 0.3045(3) 0.1164(3) 0.0317(8) Uani 1 1 d . . . O4 O 0.3240(4) 0.5004(3) 0.0297(3) 0.0392(9) Uani 1 1 d . . . O5 O 0.5429(4) -0.0380(3) 0.3941(3) 0.0306(8) Uani 1 1 d . . . O6 O 0.3376(4) 0.1390(3) 0.3794(3) 0.0305(8) Uani 1 1 d . . . O7 O 0.7768(4) 0.1981(4) 0.4144(4) 0.0426(10) Uani 1 1 d . . . O8 O 0.7114(4) 0.1002(4) 0.3088(4) 0.0464(11) Uani 1 1 d . . . O9 O 0.4005(4) 0.4585(4) 0.2116(4) 0.0403(10) Uani 1 1 d . . . O10 O 0.2526(4) 0.3362(3) 0.2026(3) 0.0363(9) Uani 1 1 d . . . H1 H 0.2791 0.2751 0.2573 0.054 Uiso 1 1 calc R . . O11 O 0.4391(4) 0.0718(3) 0.2123(3) 0.0361(9) Uani 1 1 d . . . O12 O 0.3115(4) -0.0607(3) 0.3853(3) 0.0358(9) Uani 1 1 d . . . N1 N 0.1750(4) 0.2662(4) 0.5336(4) 0.0314(10) Uani 1 1 d . . . N2 N 0.3859(4) 0.3122(4) 0.5782(4) 0.0309(10) Uani 1 1 d . . . N3 N 0.7310(4) 0.2209(4) -0.0407(4) 0.0318(10) Uani 1 1 d . . . N4 N 0.9293(5) 0.2728(4) 0.0147(4) 0.0359(11) Uani 1 1 d . . . C1 C 0.0708(6) 0.2399(6) 0.5130(6) 0.0466(16) Uani 1 1 d . . . C2 C -0.0658(6) 0.2878(7) 0.5499(6) 0.0533(18) Uani 1 1 d . . . C3 C -0.0985(7) 0.3595(7) 0.6114(6) 0.0541(19) Uani 1 1 d . . . C4 C 0.0084(6) 0.3880(5) 0.6380(5) 0.0421(15) Uani 1 1 d . . . C5 C -0.0129(8) 0.4624(6) 0.7023(6) 0.0538(19) Uani 1 1 d . . . C6 C 0.0918(8) 0.4861(6) 0.7248(6) 0.0518(17) Uani 1 1 d . . . C7 C 0.2325(6) 0.4359(5) 0.6846(5) 0.0405(14) Uani 1 1 d . . . C8 C 0.3481(7) 0.4538(6) 0.7073(6) 0.0506(17) Uani 1 1 d . . . C9 C 0.4755(8) 0.4019(6) 0.6656(7) 0.0526(18) Uani 1 1 d . . . C10 C 0.4930(7) 0.3323(6) 0.6007(6) 0.0467(16) Uani 1 1 d . . . C11 C 0.2581(5) 0.3629(5) 0.6194(5) 0.0309(12) Uani 1 1 d . . . C12 C 0.1441(5) 0.3381(5) 0.5955(4) 0.0313(12) Uani 1 1 d . . . C13 C 0.6312(7) 0.1956(6) -0.0674(6) 0.0447(15) Uani 1 1 d . . . C14 C 0.6598(8) 0.1249(7) -0.1336(7) 0.0574(19) Uani 1 1 d . . . C15 C 0.7913(7) 0.0800(6) -0.1740(6) 0.0493(16) Uani 1 1 d . . . C16 C 0.8997(6) 0.1053(5) -0.1484(5) 0.0391(14) Uani 1 1 d . . . C17 C 1.0436(7) 0.0624(6) -0.1867(5) 0.0460(16) Uani 1 1 d . . . C18 C 1.1423(7) 0.0884(6) -0.1599(6) 0.0463(16) Uani 1 1 d . . . C19 C 1.1100(6) 0.1617(5) -0.0909(5) 0.0400(14) Uani 1 1 d . . . C20 C 1.2079(8) 0.1924(8) -0.0591(7) 0.059(2) Uani 1 1 d . . . C21 C 1.1662(7) 0.2604(8) 0.0086(7) 0.063(2) Uani 1 1 d . . . C22 C 1.0262(7) 0.2988(7) 0.0440(6) 0.0523(17) Uani 1 1 d . . . C23 C 0.9714(5) 0.2058(5) -0.0517(4) 0.0326(12) Uani 1 1 d . . . C24 C 0.8637(5) 0.1769(4) -0.0811(4) 0.0289(12) Uani 1 1 d . . . OW1 O 0.953(2) -0.0865(18) -0.3336(17) 0.171(7) Uiso 0.50 1 d P . . H2 H 0.757(6) 0.150(5) 0.474(5) 0.027(16) Uiso 1 1 d . . . H3 H 0.654(6) 0.064(5) 0.343(5) 0.036(18) Uiso 1 1 d . . . H4 H 0.447(9) 0.401(8) 0.262(7) 0.10(3) Uiso 1 1 d . . . H5 H 0.477(7) 0.138(7) 0.188(6) 0.08(2) Uiso 1 1 d . . . H6 H 0.086(5) 0.200(5) 0.468(5) 0.031(15) Uiso 1 1 d . . . H7 H -0.128(6) 0.267(5) 0.535(5) 0.044(18) Uiso 1 1 d . . . H8 H -0.184(7) 0.379(6) 0.642(6) 0.06(2) Uiso 1 1 d . . . H9 H -0.098(6) 0.491(5) 0.724(5) 0.040(17) Uiso 1 1 d . . . H10 H 0.078(6) 0.535(5) 0.773(5) 0.044(16) Uiso 1 1 d . . . H11 H 0.328(5) 0.503(5) 0.761(5) 0.036(15) Uiso 1 1 d . . . H12 H 0.540(6) 0.408(5) 0.682(5) 0.036(18) Uiso 1 1 d . . . H13 H 0.588(8) 0.295(6) 0.570(6) 0.08(2) Uiso 1 1 d . . . H14 H 0.533(6) 0.239(5) -0.041(5) 0.043(16) Uiso 1 1 d . . . H15 H 0.587(7) 0.119(6) -0.152(6) 0.06(2) Uiso 1 1 d . . . H16 H 0.816(6) 0.036(5) -0.222(5) 0.048(17) Uiso 1 1 d . . . H17 H 1.065(6) 0.015(6) -0.232(5) 0.052(19) Uiso 1 1 d . . . H18 H 1.227(6) 0.067(5) -0.184(5) 0.039(17) Uiso 1 1 d . . . H19 H 1.280(7) 0.186(6) -0.089(6) 0.06(2) Uiso 1 1 d . . . H20 H 1.229(7) 0.278(6) 0.023(6) 0.07(2) Uiso 1 1 d . . . H21 H 0.992(5) 0.349(4) 0.093(4) 0.027(13) 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 0.0264(3) 0.0264(3) 0.0246(3) -0.0123(3) -0.0025(2) -0.0042(2) Zn2 0.0273(3) 0.0292(3) 0.0240(3) -0.0114(3) -0.0022(2) -0.0044(3) P1 0.0279(7) 0.0301(7) 0.0235(7) -0.0110(6) -0.0028(5) -0.0085(6) P2 0.0259(7) 0.0248(7) 0.0287(8) -0.0098(6) -0.0046(6) -0.0027(6) P3 0.0329(7) 0.0267(7) 0.0239(7) -0.0109(6) -0.0069(6) -0.0068(6) O1 0.0307(19) 0.038(2) 0.0220(19) -0.0100(16) -0.0020(15) -0.0116(16) O2 0.030(2) 0.0330(19) 0.027(2) -0.0128(16) -0.0005(15) -0.0081(16) O3 0.030(2) 0.034(2) 0.031(2) -0.0128(17) -0.0003(16) -0.0081(16) O4 0.044(2) 0.034(2) 0.033(2) -0.0017(17) -0.0114(18) -0.0106(18) O5 0.036(2) 0.0263(18) 0.028(2) -0.0047(16) -0.0103(16) -0.0084(16) O6 0.033(2) 0.0333(19) 0.027(2) -0.0139(16) -0.0065(15) -0.0035(16) O7 0.042(2) 0.055(3) 0.029(2) -0.005(2) -0.0133(19) -0.018(2) O8 0.034(2) 0.039(2) 0.069(3) -0.030(2) 0.008(2) -0.013(2) O9 0.049(3) 0.034(2) 0.044(3) -0.022(2) -0.019(2) 0.0016(19) O10 0.032(2) 0.0293(19) 0.040(2) -0.0071(17) -0.0030(17) -0.0063(16) O11 0.053(2) 0.033(2) 0.025(2) -0.0115(17) -0.0065(17) -0.0117(19) O12 0.045(2) 0.038(2) 0.032(2) -0.0118(17) -0.0104(17) -0.0169(18) N1 0.028(2) 0.038(3) 0.030(3) -0.014(2) -0.0043(19) -0.007(2) N2 0.031(3) 0.028(2) 0.034(3) -0.014(2) -0.001(2) -0.007(2) N3 0.030(2) 0.038(3) 0.029(2) -0.017(2) -0.0044(19) -0.004(2) N4 0.031(3) 0.049(3) 0.032(3) -0.023(2) 0.002(2) -0.008(2) C1 0.035(4) 0.062(4) 0.048(4) -0.024(4) -0.007(3) -0.011(3) C2 0.027(3) 0.080(5) 0.059(5) -0.030(4) -0.007(3) -0.015(3) C3 0.025(3) 0.064(4) 0.056(4) -0.016(4) 0.002(3) -0.004(3) C4 0.026(3) 0.043(3) 0.039(3) -0.012(3) 0.001(3) 0.005(3) C5 0.041(4) 0.049(4) 0.056(4) -0.031(3) 0.011(3) 0.010(3) C6 0.062(5) 0.041(4) 0.046(4) -0.027(3) 0.004(3) 0.001(3) C7 0.051(4) 0.032(3) 0.038(3) -0.019(3) 0.002(3) -0.009(3) C8 0.072(5) 0.046(4) 0.053(4) -0.033(3) -0.007(3) -0.021(4) C9 0.053(4) 0.055(4) 0.070(5) -0.037(4) -0.010(4) -0.018(4) C10 0.040(4) 0.049(4) 0.063(4) -0.031(3) -0.004(3) -0.015(3) C11 0.031(3) 0.025(3) 0.032(3) -0.012(2) 0.000(2) -0.004(2) C12 0.031(3) 0.030(3) 0.024(3) -0.011(2) 0.002(2) -0.001(2) C13 0.038(4) 0.053(4) 0.051(4) -0.030(3) -0.011(3) -0.004(3) C14 0.049(4) 0.076(5) 0.067(5) -0.042(4) -0.005(4) -0.020(4) C15 0.059(4) 0.057(4) 0.043(4) -0.030(3) -0.002(3) -0.018(3) C16 0.047(4) 0.035(3) 0.031(3) -0.013(3) -0.002(3) -0.006(3) C17 0.050(4) 0.039(3) 0.037(4) -0.018(3) -0.002(3) 0.007(3) C18 0.034(4) 0.048(4) 0.043(4) -0.020(3) 0.004(3) 0.005(3) C19 0.031(3) 0.046(3) 0.031(3) -0.009(3) -0.004(2) -0.002(3) C20 0.033(4) 0.088(6) 0.054(5) -0.035(4) 0.001(3) -0.007(4) C21 0.043(4) 0.107(6) 0.058(5) -0.039(5) -0.013(3) -0.026(4) C22 0.043(4) 0.078(5) 0.053(4) -0.042(4) 0.000(3) -0.019(4) C23 0.033(3) 0.031(3) 0.027(3) -0.010(2) -0.005(2) 0.001(2) C24 0.035(3) 0.027(3) 0.022(3) -0.009(2) 0.001(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 O5 1.953(3) 2_656 ? Zn1 O2 1.990(3) . ? Zn1 O6 2.065(3) . ? Zn1 N1 2.118(4) . ? Zn1 N2 2.192(4) . ? Zn2 O4 1.936(4) 2_665 ? Zn2 O1 1.996(3) . ? Zn2 O3 2.103(3) . ? Zn2 N3 2.127(4) . ? Zn2 N4 2.178(4) . ? P1 O1 1.499(4) . ? P1 O2 1.528(4) . ? P1 O8 1.542(4) . ? P1 O7 1.556(4) . ? P2 O4 1.483(4) . ? P2 O3 1.508(4) . ? P2 O10 1.565(4) . ? P2 O9 1.575(4) . ? P3 O12 1.498(4) . ? P3 O6 1.528(4) . ? P3 O5 1.540(4) . ? P3 O11 1.593(4) . ? O4 Zn2 1.936(4) 2_665 ? O5 Zn1 1.953(3) 2_656 ? O7 H2 0.78(5) . ? O8 H3 0.78(5) . ? O9 H4 0.85(8) . ? O10 H1 0.8200 . ? O11 H5 0.92(7) . ? N1 C1 1.334(7) . ? N1 C12 1.354(7) . ? N2 C10 1.332(7) . ? N2 C11 1.344(7) . ? N3 C13 1.328(7) . ? N3 C24 1.354(7) . ? N4 C22 1.325(7) . ? N4 C23 1.342(7) . ? C1 C2 1.386(9) . ? C1 H6 0.87(5) . ? C2 C3 1.345(10) . ? C2 H7 0.86(6) . ? C3 C4 1.418(9) . ? C3 H8 0.87(7) . ? C4 C12 1.407(7) . ? C4 C5 1.423(9) . ? C5 C6 1.334(10) . ? C5 H9 0.85(6) . ? C6 C7 1.438(9) . ? C6 H10 1.00(6) . ? C7 C8 1.403(9) . ? C7 C11 1.409(7) . ? C8 C9 1.348(9) . ? C8 H11 1.05(5) . ? C9 C10 1.386(9) . ? C9 H12 0.78(6) . ? C10 H13 1.00(8) . ? C11 C12 1.441(8) . ? C13 C14 1.390(9) . ? C13 H14 1.03(6) . ? C14 C15 1.348(10) . ? C14 H15 0.88(7) . ? C15 C16 1.402(9) . ? C15 H16 0.94(6) . ? C16 C24 1.402(7) . ? C16 C17 1.437(8) . ? C17 C18 1.325(9) . ? C17 H17 0.94(6) . ? C18 C19 1.440(9) . ? C18 H18 0.84(6) . ? C19 C20 1.390(9) . ? C19 C23 1.400(8) . ? C20 C21 1.366(11) . ? C20 H19 0.74(7) . ? C21 C22 1.387(10) . ? C21 H20 0.83(7) . ? C22 H21 1.00(5) . ? C23 C24 1.449(8) . ? 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 O5 Zn1 O2 114.28(14) 2_656 . ? O5 Zn1 O6 100.54(14) 2_656 . ? O2 Zn1 O6 91.63(14) . . ? O5 Zn1 N1 111.84(16) 2_656 . ? O2 Zn1 N1 133.01(15) . . ? O6 Zn1 N1 88.49(15) . . ? O5 Zn1 N2 97.88(15) 2_656 . ? O2 Zn1 N2 88.69(15) . . ? O6 Zn1 N2 159.61(15) . . ? N1 Zn1 N2 76.55(16) . . ? O4 Zn2 O1 103.96(15) 2_665 . ? O4 Zn2 O3 101.33(15) 2_665 . ? O1 Zn2 O3 95.77(14) . . ? O4 Zn2 N3 112.74(16) 2_665 . ? O1 Zn2 N3 141.85(16) . . ? O3 Zn2 N3 87.18(15) . . ? O4 Zn2 N4 99.45(17) 2_665 . ? O1 Zn2 N4 87.72(15) . . ? O3 Zn2 N4 157.40(16) . . ? N3 Zn2 N4 76.64(16) . . ? O1 P1 O2 112.7(2) . . ? O1 P1 O8 107.3(2) . . ? O2 P1 O8 111.7(2) . . ? O1 P1 O7 108.7(2) . . ? O2 P1 O7 108.8(2) . . ? O8 P1 O7 107.4(3) . . ? O4 P2 O3 117.1(2) . . ? O4 P2 O10 106.2(2) . . ? O3 P2 O10 108.45(19) . . ? O4 P2 O9 108.4(2) . . ? O3 P2 O9 109.3(2) . . ? O10 P2 O9 106.9(2) . . ? O12 P3 O6 114.5(2) . . ? O12 P3 O5 112.6(2) . . ? O6 P3 O5 109.5(2) . . ? O12 P3 O11 106.8(2) . . ? O6 P3 O11 106.6(2) . . ? O5 P3 O11 106.2(2) . . ? P1 O1 Zn2 123.6(2) . . ? P1 O2 Zn1 136.6(2) . . ? P2 O3 Zn2 126.6(2) . . ? P2 O4 Zn2 145.7(3) . 2_665 ? P3 O5 Zn1 133.7(2) . 2_656 ? P3 O6 Zn1 130.3(2) . . ? P1 O7 H2 113(4) . . ? P1 O8 H3 115(4) . . ? P2 O9 H4 107(6) . . ? P2 O10 H1 109.5 . . ? P3 O11 H5 108(5) . . ? C1 N1 C12 118.1(5) . . ? C1 N1 Zn1 126.2(4) . . ? C12 N1 Zn1 115.5(3) . . ? C10 N2 C11 118.0(5) . . ? C10 N2 Zn1 128.3(4) . . ? C11 N2 Zn1 113.6(3) . . ? C13 N3 C24 118.2(5) . . ? C13 N3 Zn2 126.8(4) . . ? C24 N3 Zn2 115.1(3) . . ? C22 N4 C23 117.3(5) . . ? C22 N4 Zn2 128.2(4) . . ? C23 N4 Zn2 114.5(4) . . ? N1 C1 C2 121.6(7) . . ? N1 C1 H6 121(4) . . ? C2 C1 H6 117(4) . . ? C3 C2 C1 121.1(7) . . ? C3 C2 H7 122(4) . . ? C1 C2 H7 117(4) . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H8 119(5) . . ? C4 C3 H8 121(5) . . ? C12 C4 C3 115.9(6) . . ? C12 C4 C5 119.3(6) . . ? C3 C4 C5 124.8(6) . . ? C6 C5 C4 122.2(6) . . ? C6 C5 H9 123(4) . . ? C4 C5 H9 115(4) . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H10 123(3) . . ? C7 C6 H10 117(3) . . ? C8 C7 C11 117.0(5) . . ? C8 C7 C6 124.0(6) . . ? C11 C7 C6 119.0(6) . . ? C9 C8 C7 119.0(6) . . ? C9 C8 H11 125(3) . . ? C7 C8 H11 116(3) . . ? C8 C9 C10 120.9(6) . . ? C8 C9 H12 119(4) . . ? C10 C9 H12 120(5) . . ? N2 C10 C9 121.9(6) . . ? N2 C10 H13 118(4) . . ? C9 C10 H13 120(4) . . ? N2 C11 C7 123.2(5) . . ? N2 C11 C12 116.9(5) . . ? C7 C11 C12 119.9(5) . . ? N1 C12 C4 123.7(5) . . ? N1 C12 C11 117.3(4) . . ? C4 C12 C11 119.0(5) . . ? N3 C13 C14 121.8(6) . . ? N3 C13 H14 114(3) . . ? C14 C13 H14 124(3) . . ? C15 C14 C13 120.7(6) . . ? C15 C14 H15 124(5) . . ? C13 C14 H15 115(5) . . ? C14 C15 C16 119.2(6) . . ? C14 C15 H16 124(4) . . ? C16 C15 H16 116(4) . . ? C24 C16 C15 117.1(5) . . ? C24 C16 C17 118.8(6) . . ? C15 C16 C17 124.1(6) . . ? C18 C17 C16 121.8(6) . . ? C18 C17 H17 121(4) . . ? C16 C17 H17 117(4) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 123(4) . . ? C19 C18 H18 115(4) . . ? C20 C19 C23 116.4(6) . . ? C20 C19 C18 124.5(6) . . ? C23 C19 C18 119.1(6) . . ? C21 C20 C19 119.8(7) . . ? C21 C20 H19 118(6) . . ? C19 C20 H19 120(6) . . ? C20 C21 C22 119.3(7) . . ? C20 C21 H20 116(5) . . ? C22 C21 H20 124(5) . . ? N4 C22 C21 122.9(6) . . ? N4 C22 H21 116(3) . . ? C21 C22 H21 122(3) . . ? N4 C23 C19 124.2(5) . . ? N4 C23 C24 116.3(5) . . ? C19 C23 C24 119.5(5) . . ? N3 C24 C16 122.9(5) . . ? N3 C24 C23 117.5(4) . . ? C16 C24 C23 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.080 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.105