Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Syntheses and Structures of Two Chiral Zincophosphite Compounds [C8H8N2][Zn(HPO3)] and [C6H13N2][C6H12N2][Zn3(HPO3)3(H2PO3)] ; _publ_contact_author_name 'Prof. Yunling Liu' _publ_contact_author_email YUNLING@JLU.EDU.CN loop_ _publ_author_name 'Yun Liu' 'Guanghua Li' 'Li Liu' 'Wenqin Pang' 'Xiaofeng Wang' ; Li-Rong Zhang ; # Attachment 'CIF.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 651960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C8 H9 N2 O3 P Zn' _chemical_formula_sum 'C8 H9 N2 O3 P Zn' _chemical_formula_weight 277.51 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.3295(5) _cell_length_b 10.6246(17) _cell_length_c 17.877(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1012.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2541 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.52 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2272 _exptl_absorpt_correction_T_max 0.2840 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7311 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1280 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.52 _reflns_number_total 2541 _reflns_number_gt 1467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _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^)+(0.0258P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 2541 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _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 0.59296(12) 0.30534(6) 0.40577(3) 0.02924(17) Uani 1 1 d . . . P1 P 0.0925(3) 0.15212(11) 0.40746(8) 0.0260(3) Uani 1 1 d . . . H1 H 0.151(8) 0.031(4) 0.389(2) 0.034(14) Uiso 1 1 d . . . O1 O 0.2816(7) 0.2349(4) 0.36668(19) 0.0342(10) Uani 1 1 d . . . O2 O 0.6200(8) 0.3420(4) 0.50977(18) 0.0494(12) Uani 1 1 d . . . O3 O 0.8305(6) 0.1753(4) 0.3785(2) 0.0364(10) Uani 1 1 d . . . N1 N 0.6935(8) 0.4672(4) 0.3561(2) 0.0305(12) Uani 1 1 d . . . N2 N 0.7276(9) 0.6268(4) 0.2772(2) 0.0341(11) Uani 1 1 d . . . H2 H 0.6974 0.6748 0.2395 0.080 Uiso 1 1 calc . . . C1 C 0.8831(11) 0.5470(5) 0.3818(3) 0.0309(12) Uani 1 1 d . . . C2 C 0.9112(13) 0.6471(5) 0.3318(3) 0.0320(12) Uani 1 1 d . . . C3 C 0.6058(12) 0.5186(5) 0.2938(3) 0.0316(12) Uani 1 1 d . . . C4 C 1.0452(11) 0.5401(6) 0.4426(3) 0.0379(15) Uani 1 1 d . . . H4 H 1.0365 0.4728 0.4758 0.080 Uiso 1 1 calc . . . C5 C 1.2169(12) 0.6334(7) 0.4527(4) 0.0507(17) Uani 1 1 d . . . H5 H 1.3241 0.6302 0.4937 0.080 Uiso 1 1 calc . . . C6 C 1.2347(11) 0.7338(6) 0.4027(4) 0.0525(16) Uani 1 1 d . . . H6 H 1.3548 0.7958 0.4111 0.080 Uiso 1 1 calc . . . C7 C 1.0803(14) 0.7439(6) 0.3416(3) 0.0467(15) Uani 1 1 d . . . H7 H 1.0892 0.8117 0.3088 0.080 Uiso 1 1 calc . . . C8 C 0.4046(12) 0.4667(5) 0.2465(3) 0.0409(14) Uani 1 1 d . . . H8A H 0.4655 0.3938 0.2205 0.080 Uiso 1 1 calc R . . H8B H 0.3526 0.5290 0.2108 0.080 Uiso 1 1 calc R . . H8C H 0.2644 0.4436 0.2773 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0283(3) 0.0347(3) 0.0247(3) 0.0043(3) -0.0021(4) -0.0037(3) P1 0.0266(6) 0.0275(7) 0.0238(6) -0.0013(6) 0.0004(10) 0.0011(7) O1 0.029(2) 0.047(3) 0.027(2) -0.0020(17) -0.0003(16) -0.0033(19) O2 0.055(2) 0.068(3) 0.025(2) 0.0049(18) -0.002(2) 0.001(3) O3 0.024(2) 0.049(3) 0.037(2) -0.010(2) -0.0002(15) -0.0103(18) N1 0.034(3) 0.031(3) 0.027(3) 0.004(2) -0.002(2) -0.003(2) N2 0.043(3) 0.030(3) 0.029(3) 0.010(2) 0.005(2) -0.002(2) C1 0.029(3) 0.037(3) 0.027(3) -0.003(2) 0.002(3) 0.004(3) C2 0.035(3) 0.028(3) 0.033(3) 0.005(2) 0.003(3) 0.003(3) C3 0.039(3) 0.034(3) 0.022(3) -0.001(2) 0.003(3) 0.009(3) C4 0.043(4) 0.042(4) 0.029(3) 0.005(3) -0.002(3) 0.001(3) C5 0.038(4) 0.062(5) 0.053(4) -0.003(4) -0.014(3) -0.011(4) C6 0.045(3) 0.045(4) 0.067(4) -0.003(4) -0.002(4) -0.016(3) C7 0.048(4) 0.037(4) 0.055(4) 0.002(3) 0.012(4) -0.007(4) C8 0.046(3) 0.038(4) 0.038(3) 0.006(3) -0.006(4) 0.007(4) _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 1.905(3) . ? Zn1 O3 1.936(4) . ? Zn1 O1 1.950(4) . ? Zn1 N1 2.008(4) . ? P1 O2 1.488(3) 4_456 ? P1 O3 1.509(3) 1_455 ? P1 O1 1.524(4) . ? P1 H1 1.36(4) . ? O2 P1 1.488(3) 4_556 ? O3 P1 1.509(3) 1_655 ? N1 C3 1.326(6) . ? N1 C1 1.397(7) . ? N2 C3 1.353(7) . ? N2 C2 1.399(7) . ? N2 H2 0.8600 . ? C1 C4 1.391(7) . ? C1 C2 1.397(7) . ? C2 C7 1.379(8) . ? C3 C8 1.473(8) . ? C4 C5 1.361(9) . ? C4 H4 0.9300 . ? C5 C6 1.396(9) . ? C5 H5 0.9300 . ? C6 C7 1.373(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O3 110.00(16) . . ? O2 Zn1 O1 119.50(17) . . ? O3 Zn1 O1 101.10(14) . . ? O2 Zn1 N1 103.69(17) . . ? O3 Zn1 N1 108.98(17) . . ? O1 Zn1 N1 113.39(16) . . ? O2 P1 O3 115.2(2) 4_456 1_455 ? O2 P1 O1 112.7(2) 4_456 . ? O3 P1 O1 110.7(2) 1_455 . ? O2 P1 H1 104.6(19) 4_456 . ? O3 P1 H1 106.6(18) 1_455 . ? O1 P1 H1 106.3(18) . . ? P1 O1 Zn1 127.8(2) . . ? P1 O2 Zn1 166.3(3) 4_556 . ? P1 O3 Zn1 129.4(2) 1_655 . ? C3 N1 C1 106.3(4) . . ? C3 N1 Zn1 129.1(4) . . ? C1 N1 Zn1 124.6(3) . . ? C3 N2 C2 108.3(4) . . ? C3 N2 H2 125.9 . . ? C2 N2 H2 125.9 . . ? C4 C1 C2 118.3(5) . . ? C4 C1 N1 132.4(5) . . ? C2 C1 N1 109.2(5) . . ? C7 C2 C1 123.9(5) . . ? C7 C2 N2 131.3(5) . . ? C1 C2 N2 104.7(5) . . ? N1 C3 N2 111.4(5) . . ? N1 C3 C8 125.8(5) . . ? N2 C3 C8 122.8(5) . . ? C5 C4 C1 118.9(5) . . ? C5 C4 H4 120.6 . . ? C1 C4 H4 120.6 . . ? C4 C5 C6 121.2(6) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 121.9(5) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C2 115.7(5) . . ? C6 C7 H7 122.1 . . ? C2 C7 H7 122.1 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 N2 H2 O1 0.86 2.01 2.817(5) 156.8 3_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.458 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.102 #========================== End ========================== data_2 _database_code_depnum_ccdc_archive 'CCDC 651961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C12 H30 N4 O12 P4 Zn3' _chemical_formula_sum 'C12 H30 N4 O12 P4 Zn3' _chemical_formula_weight 742.39 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.985(2) _cell_length_b 13.573(3) _cell_length_c 18.444(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2499.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5699 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.175 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5731 _exptl_absorpt_correction_T_max 0.7059 _exptl_absorpt_process_details Process-auto _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24464 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5699 _reflns_number_gt 4819 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _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^)+(0.0745P)^2^+4.5694P] 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 0.00 _refine_ls_number_reflns 5699 _refine_ls_number_parameters 313 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _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 0.83356(8) 0.41811(6) 0.22618(4) 0.03812(19) Uani 1 1 d . . . Zn2 Zn 0.67107(8) 0.14032(6) 0.31122(4) 0.03889(19) Uani 1 1 d . . . Zn3 Zn 0.69176(9) 0.37721(5) 0.54608(4) 0.0408(2) Uani 1 1 d . . . P1 P 0.6835(2) 0.36368(13) 0.36819(8) 0.0411(4) Uani 1 1 d D . . H1 H 0.583(7) 0.408(7) 0.336(5) 0.080 Uiso 1 1 d D . . P2 P 0.7680(2) 0.21058(14) 0.15344(10) 0.0421(4) Uani 1 1 d D . . H2 H 0.673(7) 0.239(7) 0.107(4) 0.080 Uiso 1 1 d D . . P3 P 0.59190(19) 0.52201(16) 0.14218(11) 0.0489(5) Uani 1 1 d D . . H3 H 0.551(9) 0.434(3) 0.124(5) 0.080 Uiso 1 1 d D . . P4 P 0.95420(18) 0.06397(14) 0.34046(9) 0.0406(4) Uani 1 1 d D . . H4 H 0.984(9) 0.138(5) 0.297(4) 0.080 Uiso 1 1 d D . . O1 O 0.8039(6) 0.4005(6) 0.3298(3) 0.078(2) Uani 1 1 d . . . O2 O 0.8551(8) 0.2922(5) 0.1849(5) 0.096(3) Uani 1 1 d . . . O3 O 0.7014(8) 0.5089(7) 0.2006(4) 0.107(3) Uani 1 1 d . . . O4 O 1.0020(6) 0.4834(6) 0.2095(3) 0.077(2) Uani 1 1 d . . . O5 O 0.6437(8) 0.2593(6) 0.3632(4) 0.0805(11) Uani 1 1 d U . . O6 O 0.6924(7) 0.1516(6) 0.2079(4) 0.0805(11) Uani 1 1 d . . . O7 O 0.8061(7) 0.0562(6) 0.3540(4) 0.0805(11) Uani 1 1 d . . . O8 O 0.4946(15) 0.1145(12) 0.3391(8) 0.0805(11) Uani 0.50 1 d PU . . O8' O 0.5205(15) 0.0435(12) 0.3105(8) 0.0805(11) Uani 0.50 1 d PU . . O9 O 0.6732(9) 0.3981(5) 0.4435(3) 0.085(2) Uani 1 1 d . . . O10 O 0.8594(7) 0.4295(7) 0.5762(4) 0.098(3) Uani 1 1 d . . . O11 O 0.5341(6) 0.4284(5) 0.5902(3) 0.0592(15) Uani 1 1 d . . . O12 O 0.8567(5) 0.1459(4) 0.1067(3) 0.0536(14) Uani 1 1 d . . . H12 H 0.8500 0.0885 0.1200 0.080 Uiso 1 1 calc . . . N1 N 0.7005(5) 0.2240(4) 0.5690(3) 0.0321(11) Uani 1 1 d . . . N2 N 0.6993(5) 0.0406(4) 0.5947(3) 0.0383(12) Uani 1 1 d . . . N3 N 0.6324(7) -0.2644(6) 0.4079(4) 0.063(2) Uani 1 1 d . . . N4 N 0.8764(6) -0.3025(5) 0.3971(3) 0.0450(14) Uani 1 1 d . . . H4C H 0.9653 -0.3164 0.3937 0.080 Uiso 1 1 calc . . . C1 C 0.5719(7) 0.1800(5) 0.5431(5) 0.0479(18) Uani 1 1 d . . . H1A H 0.5651 0.1867 0.4908 0.080 Uiso 1 1 calc . . . H1B H 0.4968 0.2141 0.5650 0.080 Uiso 1 1 calc . . . C2 C 0.5690(8) 0.0701(6) 0.5642(6) 0.063(2) Uani 1 1 d . . . H2A H 0.4989 0.0589 0.5997 0.080 Uiso 1 1 calc . . . H2B H 0.5493 0.0304 0.5218 0.080 Uiso 1 1 calc . . . C3 C 0.8133(7) 0.1752(5) 0.5316(4) 0.0417(15) Uani 1 1 d . . . H3A H 0.8970 0.2008 0.5504 0.080 Uiso 1 1 calc . . . H3B H 0.8093 0.1904 0.4802 0.080 Uiso 1 1 calc . . . C4 C 0.8100(7) 0.0637(5) 0.5417(5) 0.0496(17) Uani 1 1 d . . . H4A H 0.7930 0.0314 0.4957 0.080 Uiso 1 1 calc . . . H4B H 0.8952 0.0406 0.5603 0.080 Uiso 1 1 calc . . . C5 C 0.7169(10) 0.2062(6) 0.6478(4) 0.057(2) Uani 1 1 d . . . H5A H 0.6417 0.2340 0.6740 0.080 Uiso 1 1 calc . . . H5B H 0.7981 0.2377 0.6650 0.080 Uiso 1 1 calc . . . C6 C 0.7247(11) 0.0936(7) 0.6618(4) 0.064(2) Uani 1 1 d . . . H6A H 0.8127 0.0766 0.6802 0.080 Uiso 1 1 calc . . . H6B H 0.6588 0.0750 0.6979 0.080 Uiso 1 1 calc . . . C7 C 0.6682(10) -0.3436(7) 0.4583(6) 0.072(2) Uani 1 1 d . . . H7A H 0.6137 -0.4012 0.4482 0.080 Uiso 1 1 calc . . . H7B H 0.6499 -0.3226 0.5075 0.080 Uiso 1 1 calc . . . C8 C 0.8139(10) -0.3702(7) 0.4512(7) 0.079(3) Uani 1 1 d . . . H8A H 0.8583 -0.3634 0.4978 0.080 Uiso 1 1 calc . . . H8B H 0.8229 -0.4380 0.4353 0.080 Uiso 1 1 calc . . . C9 C 0.7097(9) -0.1776(6) 0.4226(6) 0.065(2) Uani 1 1 d . . . H9A H 0.6821 -0.1502 0.4689 0.080 Uiso 1 1 calc . . . H9B H 0.6916 -0.1287 0.3855 0.080 Uiso 1 1 calc . . . C10 C 0.8595(9) -0.1986(7) 0.4247(6) 0.066(2) Uani 1 1 d . . . H10A H 0.9076 -0.1525 0.3941 0.080 Uiso 1 1 calc . . . H10B H 0.8933 -0.1930 0.4738 0.080 Uiso 1 1 calc . . . C11 C 0.6667(15) -0.2936(11) 0.3323(8) 0.106(4) Uani 1 1 d U . . H11A H 0.6426 -0.2410 0.2992 0.080 Uiso 1 1 calc . . . H11B H 0.6163 -0.3519 0.3189 0.080 Uiso 1 1 calc . . . C12 C 0.8155(14) -0.3146(10) 0.3265(7) 0.096(3) Uani 1 1 d U . . H12A H 0.8295 -0.3814 0.3093 0.080 Uiso 1 1 calc . . . H12B H 0.8563 -0.2696 0.2921 0.080 Uiso 1 1 calc . . . 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 0.0492(4) 0.0380(4) 0.0271(3) 0.0032(3) 0.0065(3) -0.0041(4) Zn2 0.0345(4) 0.0465(4) 0.0357(4) -0.0025(3) 0.0088(3) -0.0045(3) Zn3 0.0616(5) 0.0328(4) 0.0279(3) -0.0016(3) 0.0124(3) -0.0079(4) P1 0.0591(11) 0.0374(9) 0.0267(7) 0.0014(6) 0.0129(7) -0.0005(9) P2 0.0530(10) 0.0382(9) 0.0351(8) -0.0032(7) 0.0078(8) 0.0028(8) P3 0.0400(9) 0.0513(11) 0.0553(12) -0.0031(9) 0.0069(9) 0.0092(9) P4 0.0419(9) 0.0474(10) 0.0324(8) -0.0061(7) 0.0016(7) 0.0103(8) O1 0.070(4) 0.136(6) 0.028(2) 0.015(3) 0.008(2) -0.042(4) O2 0.103(5) 0.061(4) 0.126(6) -0.055(4) 0.046(5) -0.029(4) O3 0.106(6) 0.146(8) 0.068(5) 0.033(5) -0.002(4) 0.051(6) O4 0.066(4) 0.101(5) 0.064(4) 0.045(4) -0.019(3) -0.033(4) O5 0.0809(12) 0.0804(12) 0.0800(12) -0.0001(6) 0.0021(6) -0.0008(6) O6 0.0809(12) 0.0804(12) 0.0800(12) -0.0001(6) 0.0021(6) -0.0008(6) O7 0.0809(12) 0.0804(12) 0.0800(12) -0.0001(6) 0.0021(6) -0.0008(6) O8 0.0809(12) 0.0804(12) 0.0800(12) -0.0001(6) 0.0021(6) -0.0008(6) O8' 0.0809(12) 0.0804(12) 0.0800(12) -0.0001(6) 0.0021(6) -0.0008(6) O9 0.168(7) 0.058(4) 0.027(2) -0.005(2) 0.022(4) -0.017(4) O10 0.082(5) 0.141(7) 0.072(4) -0.046(5) 0.033(4) -0.053(5) O11 0.065(3) 0.071(4) 0.041(3) -0.017(3) 0.004(3) 0.012(3) O12 0.059(3) 0.036(3) 0.065(3) -0.012(2) 0.017(3) -0.007(2) N1 0.034(3) 0.034(3) 0.029(2) 0.001(2) 0.007(2) -0.008(2) N2 0.036(3) 0.034(3) 0.044(3) 0.008(2) 0.005(2) -0.002(2) N3 0.049(4) 0.077(5) 0.062(4) -0.013(4) 0.006(3) 0.019(4) N4 0.040(3) 0.051(4) 0.044(3) -0.002(3) 0.008(3) 0.011(3) C1 0.033(3) 0.034(4) 0.077(5) 0.012(4) -0.005(4) -0.003(3) C2 0.043(4) 0.048(5) 0.096(7) 0.019(5) -0.015(4) -0.005(3) C3 0.045(4) 0.040(3) 0.041(3) 0.007(3) 0.008(3) -0.001(3) C4 0.047(4) 0.037(4) 0.065(4) 0.001(3) 0.017(4) 0.006(3) C5 0.100(6) 0.046(4) 0.027(3) 0.006(3) 0.009(4) -0.009(4) C6 0.102(7) 0.056(5) 0.035(3) 0.020(3) 0.001(4) 0.002(5) C7 0.063(5) 0.065(5) 0.088(6) -0.004(5) 0.023(6) 0.000(5) C8 0.073(6) 0.055(5) 0.110(8) 0.016(5) 0.027(6) 0.009(5) C9 0.065(5) 0.043(5) 0.088(6) 0.003(4) 0.012(5) 0.017(4) C10 0.068(5) 0.045(5) 0.084(6) 0.006(4) 0.012(5) -0.009(4) C11 0.106(4) 0.107(4) 0.105(4) -0.0005(10) -0.0003(10) 0.0001(10) C12 0.096(4) 0.097(4) 0.095(4) -0.0012(10) 0.0000(10) 0.0006(10) _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 O3 1.866(7) . ? Zn1 O2 1.884(6) . ? Zn1 O4 1.926(6) . ? Zn1 O1 1.948(5) . ? Zn2 O8 1.868(15) . ? Zn2 O5 1.898(7) . ? Zn2 O6 1.923(7) . ? Zn2 O7 1.934(7) . ? Zn2 O8' 1.997(15) . ? Zn3 O10 1.901(7) . ? Zn3 O11 1.904(6) . ? Zn3 O9 1.922(5) . ? Zn3 N1 2.124(5) . ? P1 O9 1.470(5) . ? P1 O5 1.474(8) . ? P1 O1 1.483(6) . ? P1 H1 1.31(2) . ? P2 O6 1.490(7) . ? P2 O12 1.516(5) . ? P2 O2 1.523(7) . ? P2 H2 1.33(2) . ? P3 O8' 1.451(15) 3_655 ? P3 O10 1.467(7) 2_664 ? P3 O3 1.545(8) . ? P3 O8 1.563(15) 3_655 ? P3 H3 1.30(2) . ? P4 O4 1.495(6) 3_745 ? P4 O7 1.504(8) . ? P4 O11 1.511(5) 4_556 ? P4 H4 1.32(2) . ? O4 P4 1.495(6) 3_755 ? O8 O8' 1.129(19) . ? O8 P3 1.563(15) 3_645 ? O8' P3 1.451(15) 3_645 ? O10 P3 1.467(7) 2_665 ? O11 P4 1.511(5) 4_456 ? O12 H12 0.8200 . ? N1 C3 1.477(9) . ? N1 C5 1.484(8) . ? N1 C1 1.494(8) . ? N2 C6 1.453(10) . ? N2 C2 1.473(10) . ? N2 C4 1.509(9) . ? N3 C9 1.435(12) . ? N3 C7 1.465(13) . ? N3 C11 1.489(15) . ? N4 C12 1.446(15) . ? N4 C8 1.493(11) . ? N4 C10 1.509(11) . ? N4 H4C 0.9100 . ? C1 C2 1.542(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.525(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.551(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.505(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.523(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.517(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 Zn1 O2 125.3(4) . . ? O3 Zn1 O4 105.9(4) . . ? O2 Zn1 O4 104.7(3) . . ? O3 Zn1 O1 102.8(3) . . ? O2 Zn1 O1 107.6(4) . . ? O4 Zn1 O1 110.2(3) . . ? O8 Zn2 O5 83.4(5) . . ? O8 Zn2 O6 113.1(5) . . ? O5 Zn2 O6 116.6(3) . . ? O8 Zn2 O7 115.8(5) . . ? O5 Zn2 O7 113.4(3) . . ? O6 Zn2 O7 111.9(3) . . ? O8 Zn2 O8' 33.8(6) . . ? O5 Zn2 O8' 117.1(5) . . ? O6 Zn2 O8' 97.4(5) . . ? O7 Zn2 O8' 98.0(5) . . ? O10 Zn3 O11 117.8(3) . . ? O10 Zn3 O9 108.5(3) . . ? O11 Zn3 O9 106.7(3) . . ? O10 Zn3 N1 105.8(3) . . ? O11 Zn3 N1 107.9(2) . . ? O9 Zn3 N1 110.1(2) . . ? O9 P1 O5 110.3(4) . . ? O9 P1 O1 113.7(4) . . ? O5 P1 O1 120.8(5) . . ? O9 P1 H1 103(4) . . ? O5 P1 H1 102(4) . . ? O1 P1 H1 105(4) . . ? O6 P2 O12 111.6(4) . . ? O6 P2 O2 115.0(5) . . ? O12 P2 O2 107.7(4) . . ? O6 P2 H2 103(4) . . ? O12 P2 H2 102(4) . . ? O2 P2 H2 116(4) . . ? O8' P3 O10 131.7(7) 3_655 2_664 ? O8' P3 O3 98.7(7) 3_655 . ? O10 P3 O3 113.3(4) 2_664 . ? O8' P3 O8 43.8(7) 3_655 3_655 ? O10 P3 O8 90.4(7) 2_664 3_655 ? O3 P3 O8 109.3(7) . 3_655 ? O8' P3 H3 96(4) 3_655 . ? O10 P3 H3 108(4) 2_664 . ? O3 P3 H3 107(4) . . ? O8 P3 H3 128(4) 3_655 . ? O4 P4 O7 109.8(4) 3_745 . ? O4 P4 O11 114.6(3) 3_745 4_556 ? O7 P4 O11 112.6(4) . 4_556 ? O4 P4 H4 97(4) 3_745 . ? O7 P4 H4 112(4) . . ? O11 P4 H4 110(4) 4_556 . ? P1 O1 Zn1 129.3(4) . . ? P2 O2 Zn1 138.5(5) . . ? P3 O3 Zn1 138.9(6) . . ? P4 O4 Zn1 133.7(4) 3_755 . ? P1 O5 Zn2 144.2(5) . . ? P2 O6 Zn2 140.1(5) . . ? P4 O7 Zn2 125.2(4) . . ? O8' O8 P3 62.8(11) . 3_645 ? O8' O8 Zn2 79.4(12) . . ? P3 O8 Zn2 137.1(10) 3_645 . ? O8 O8' P3 73.4(11) . 3_645 ? O8 O8' Zn2 66.9(11) . . ? P3 O8' Zn2 135.3(10) 3_645 . ? P1 O9 Zn3 151.3(5) . . ? P3 O10 Zn3 134.6(4) 2_665 . ? P4 O11 Zn3 145.5(4) 4_456 . ? P2 O12 H12 109.5 . . ? C3 N1 C5 107.5(6) . . ? C3 N1 C1 109.1(5) . . ? C5 N1 C1 110.1(6) . . ? C3 N1 Zn3 112.2(4) . . ? C5 N1 Zn3 111.0(4) . . ? C1 N1 Zn3 107.0(4) . . ? C6 N2 C2 110.1(7) . . ? C6 N2 C4 108.8(6) . . ? C2 N2 C4 110.0(6) . . ? C9 N3 C7 110.6(8) . . ? C9 N3 C11 105.8(9) . . ? C7 N3 C11 110.0(8) . . ? C12 N4 C8 110.9(8) . . ? C12 N4 C10 111.3(8) . . ? C8 N4 C10 107.6(6) . . ? C12 N4 H4C 109.0 . . ? C8 N4 H4C 109.0 . . ? C10 N4 H4C 109.0 . . ? N1 C1 C2 108.8(6) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 110.0(6) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C4 111.8(5) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C3 107.5(6) . . ? N2 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? N2 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N1 C5 C6 109.2(6) . . ? N1 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N1 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? N2 C6 C5 109.8(6) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 C8 110.9(8) . . ? N3 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C7 108.3(8) . . ? N4 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? N4 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N3 C9 C10 112.2(7) . . ? N3 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N3 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N4 C10 C9 106.1(7) . . ? N4 C10 H10A 110.5 . . ? C9 C10 H10A 110.5 . . ? N4 C10 H10B 110.5 . . ? C9 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? N3 C11 C12 110.0(11) . . ? N3 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N3 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N4 C12 C11 109.1(11) . . ? N4 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N4 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? 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 O12 H12 N2 0.82 1.88 2.602(7) 146.5 2_654 N4 H4C O12 0.91 1.85 2.757(8) 174.5 3_745 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.559 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.116 #====================== End ============================