Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'S. Neeraj' 'A.K. Cheetham' _publ_contact_author_name 'Prof A Cheetham' _publ_contact_author_address ; Materials Research Laboratory University of California Santa Barbara California 93106 USA ; _publ_contact_author_email 'CHEETHAM@MRL.UCSB.EDU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis of Open-Framework Zinc Phosphates from Organophosphorus Amides ; data_Compound_I _database_code_CSD 179397 _audit_creation_method SHELXL-97 _chemical_name_systematic ? ; ? ; _chemical_name_common ; Zinc Phosphate with N,N'dimethylamine ; _chemical_melting_point ? _chemical_formula_moiety [C2NH8][Zn3(PO4)(HPO4)2].H2O _chemical_formula_sum 'C2 H10 N O13 P3 Zn3' _chemical_formula_weight 545.13 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 ? _symmetry_space_group_name_H-M ? 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 12.6528(11) _cell_length_b 5.1909(4) _cell_length_c 21.1457(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.088(2) _cell_angle_gamma 90.00 _cell_volume 1383.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Long rod' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 5.575 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 7705 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3171 _reflns_number_gt 2604 _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^)+(0.0491P)^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 SHELXL _refine_ls_extinction_coef 0.0054(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3171 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.00597(3) 0.21510(8) 0.070543(18) 0.01404(12) Uani 1 1 d . . . Zn2 Zn -0.00112(3) 0.73311(7) 0.172723(17) 0.01411(12) Uani 1 1 d . . . Zn3 Zn 0.39935(3) -0.22196(8) 0.054651(18) 0.01604(13) Uani 1 1 d . . . P1 P 0.13998(7) -0.26768(16) 0.05251(4) 0.01173(19) Uani 1 1 d . . . P2 P -0.12672(7) 0.24183(16) 0.18659(4) 0.01230(19) Uani 1 1 d . . . P3 P 0.47221(7) -0.29911(17) -0.08318(4) 0.0155(2) Uani 1 1 d . . . O1 O 0.11566(19) 0.4457(5) 0.04952(11) 0.0216(5) Uani 1 1 d . . . O2 O -0.11773(17) 0.1427(5) 0.01308(10) 0.0181(5) Uani 1 1 d . . . O3 O -0.03717(18) 0.3747(5) 0.15073(10) 0.0174(5) Uani 1 1 d . . . O4 O 0.06544(17) -0.1298(5) 0.09755(10) 0.0151(5) Uani 1 1 d . . . O5 O 0.1017(2) 0.7963(5) 0.24236(11) 0.0221(6) Uani 1 1 d . . . O6 O -0.12340(18) 0.9555(4) 0.17088(11) 0.0183(5) Uani 1 1 d . . . O7 O 0.39430(19) -0.3291(6) -0.03265(12) 0.0289(6) Uani 1 1 d . . . O8 O 0.43111(19) 0.1388(5) 0.06135(13) 0.0266(6) Uani 1 1 d . . . O9 O 0.4950(2) -0.4393(5) 0.10692(11) 0.0230(6) Uani 1 1 d . . . O10 O 0.25407(18) -0.2198(5) 0.07987(11) 0.0191(5) Uani 1 1 d . . . O11 O -0.23193(18) 0.3622(5) 0.16567(12) 0.0240(6) Uani 1 1 d . . . H10 H -0.2773 0.2495 0.1607 0.036 Uiso 1 1 calc R . . O12 O 0.41077(18) -0.1499(5) -0.14023(11) 0.0233(6) Uani 1 1 d . . . H9 H 0.3526 -0.2169 -0.1489 0.035 Uiso 1 1 calc R . . O100 O 0.2666(3) -0.7694(6) -0.06258(17) 0.0483(9) Uani 1 1 d . . . N1 N 0.2855(2) 0.0398(7) 0.19934(15) 0.0319(8) Uani 1 1 d . . . H8 H 0.2743 -0.0263 0.1600 0.038 Uiso 1 1 calc R . . H7 H 0.2401 -0.0377 0.2237 0.038 Uiso 1 1 calc R . . C2 C 0.3947(4) -0.0187(11) 0.2247(2) 0.0511(14) Uani 1 1 d . . . H6 H 0.4049 -0.2020 0.2257 0.077 Uiso 1 1 calc R . . H5 H 0.4069 0.0492 0.2670 0.077 Uiso 1 1 calc R . . H4 H 0.4435 0.0584 0.1981 0.077 Uiso 1 1 calc R . . C1 C 0.2624(5) 0.3139(10) 0.1967(3) 0.0581(15) Uani 1 1 d . . . H3 H 0.1902 0.3400 0.1799 0.087 Uiso 1 1 calc R . . H2 H 0.3092 0.3975 0.1699 0.087 Uiso 1 1 calc R . . H1 H 0.2726 0.3853 0.2387 0.087 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 0.0150(2) 0.0127(2) 0.0148(2) -0.00018(14) 0.00353(15) -0.00095(14) Zn2 0.0158(2) 0.0126(2) 0.0145(2) -0.00029(14) 0.00433(15) -0.00054(14) Zn3 0.0133(2) 0.0166(2) 0.0186(2) -0.00152(15) 0.00378(15) -0.00079(15) P1 0.0106(4) 0.0120(4) 0.0132(4) 0.0002(3) 0.0043(3) -0.0016(3) P2 0.0110(4) 0.0132(5) 0.0130(4) -0.0006(3) 0.0030(3) -0.0003(3) P3 0.0130(4) 0.0150(5) 0.0187(4) -0.0012(3) 0.0024(3) -0.0010(3) O1 0.0231(13) 0.0127(14) 0.0305(14) 0.0013(10) 0.0117(10) -0.0017(10) O2 0.0189(12) 0.0221(14) 0.0134(11) 0.0037(10) 0.0021(9) -0.0047(10) O3 0.0228(12) 0.0121(12) 0.0190(11) -0.0021(10) 0.0112(9) -0.0065(10) O4 0.0166(11) 0.0125(13) 0.0175(11) 0.0019(10) 0.0093(9) 0.0034(9) O5 0.0240(13) 0.0284(16) 0.0141(12) 0.0023(10) 0.0018(10) -0.0044(11) O6 0.0150(11) 0.0116(13) 0.0288(13) -0.0013(10) 0.0058(9) 0.0011(9) O7 0.0219(14) 0.0458(18) 0.0199(13) -0.0081(12) 0.0060(10) -0.0079(12) O8 0.0195(12) 0.0174(14) 0.0418(16) 0.0001(12) -0.0041(11) -0.0033(11) O9 0.0306(14) 0.0142(14) 0.0236(13) -0.0046(10) -0.0018(10) 0.0045(10) O10 0.0109(11) 0.0251(15) 0.0214(12) 0.0000(10) 0.0027(9) -0.0027(9) O11 0.0163(12) 0.0213(14) 0.0336(14) 0.0007(12) -0.0020(10) 0.0018(11) O12 0.0191(12) 0.0212(14) 0.0287(14) 0.0077(12) -0.0023(10) -0.0018(11) O100 0.043(2) 0.049(2) 0.052(2) 0.0011(15) -0.0028(17) -0.0052(15) N1 0.0269(17) 0.039(2) 0.0310(18) -0.0048(16) 0.0113(14) -0.0068(15) C2 0.039(3) 0.068(4) 0.047(3) 0.016(3) 0.007(2) 0.003(2) C1 0.078(4) 0.041(3) 0.056(3) 0.004(3) 0.011(3) 0.013(3) _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 1.915(2) . ? Zn1 O2 1.931(2) . ? Zn1 O4 2.005(2) . ? Zn1 O3 2.006(2) . ? Zn2 O5 1.905(2) . ? Zn2 O6 1.928(2) . ? Zn2 O3 1.961(2) . ? Zn2 O4 1.995(2) 1_565 ? Zn3 O8 1.918(3) . ? Zn3 O7 1.924(3) . ? Zn3 O9 1.929(2) . ? Zn3 O10 1.959(2) . ? P1 O1 1.520(2) 1_545 ? P1 O10 1.527(2) . ? P1 O2 1.534(2) 3 ? P1 O4 1.571(2) . ? P2 O11 1.501(2) . ? P2 O6 1.524(2) 1_545 ? P2 O5 1.534(2) 2_545 ? P2 O3 1.577(2) . ? P3 O8 1.517(3) 3_655 ? P3 O9 1.518(3) 3_645 ? P3 O7 1.525(3) . ? P3 O12 1.579(2) . ? O1 P1 1.520(2) 1_565 ? O2 P1 1.534(2) 3 ? O4 Zn2 1.995(2) 1_545 ? O5 P2 1.534(2) 2 ? O6 P2 1.524(2) 1_565 ? O8 P3 1.517(3) 3_655 ? O9 P3 1.518(3) 3_645 ? N1 C1 1.452(6) . ? N1 C2 1.469(5) . ? 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 122.63(10) . . ? O1 Zn1 O4 111.28(10) . . ? O2 Zn1 O4 105.56(10) . . ? O1 Zn1 O3 101.26(10) . . ? O2 Zn1 O3 110.25(10) . . ? O4 Zn1 O3 104.56(9) . . ? O5 Zn2 O6 113.84(10) . . ? O5 Zn2 O3 118.36(11) . . ? O6 Zn2 O3 113.19(10) . . ? O5 Zn2 O4 104.30(10) . 1_565 ? O6 Zn2 O4 99.50(10) . 1_565 ? O3 Zn2 O4 104.78(9) . 1_565 ? O8 Zn3 O7 110.00(12) . . ? O8 Zn3 O9 114.34(10) . . ? O7 Zn3 O9 110.27(11) . . ? O8 Zn3 O10 99.78(11) . . ? O7 Zn3 O10 108.11(10) . . ? O9 Zn3 O10 113.79(11) . . ? O1 P1 O10 110.87(14) 1_545 . ? O1 P1 O2 110.86(14) 1_545 3 ? O10 P1 O2 111.42(13) . 3 ? O1 P1 O4 109.94(13) 1_545 . ? O10 P1 O4 107.11(13) . . ? O2 P1 O4 106.47(13) 3 . ? O11 P2 O6 112.49(14) . 1_545 ? O11 P2 O5 108.22(14) . 2_545 ? O6 P2 O5 112.70(14) 1_545 2_545 ? O11 P2 O3 109.41(14) . . ? O6 P2 O3 106.67(13) 1_545 . ? O5 P2 O3 107.19(14) 2_545 . ? O8 P3 O9 110.75(15) 3_655 3_645 ? O8 P3 O7 113.37(15) 3_655 . ? O9 P3 O7 110.68(16) 3_645 . ? O8 P3 O12 107.01(14) 3_655 . ? O9 P3 O12 108.47(14) 3_645 . ? O7 P3 O12 106.28(15) . . ? P1 O1 Zn1 138.66(16) 1_565 . ? P1 O2 Zn1 124.06(14) 3 . ? P2 O3 Zn2 117.57(13) . . ? P2 O3 Zn1 119.12(13) . . ? Zn2 O3 Zn1 121.14(11) . . ? P1 O4 Zn2 129.73(14) . 1_545 ? P1 O4 Zn1 117.66(12) . . ? Zn2 O4 Zn1 111.79(10) 1_545 . ? P2 O5 Zn2 142.47(16) 2 . ? P2 O6 Zn2 128.10(14) 1_565 . ? P3 O7 Zn3 132.42(16) . . ? P3 O8 Zn3 135.72(16) 3_655 . ? P3 O9 Zn3 120.64(14) 3_645 . ? P1 O10 Zn3 140.73(15) . . ? C1 N1 C2 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.698 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.162 #======================================================================= data_Compound_II _database_code_CSD 179398 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [(C2NH8)(H3O)][Zn4(PO4)3(H2O)]2.H2O _chemical_formula_sum 'C H4 N0.50 O14 P3 Zn4' _chemical_formula_weight 601.44 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.284(3) _cell_length_b 17.726(3) _cell_length_c 5.1882(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1405.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Long needles' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1162 _exptl_absorpt_coefficient_mu 7.157 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 8025 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.37 _reflns_number_total 3174 _reflns_number_gt 2593 _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^)+(0.1121P)^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 0.00(4) _refine_ls_number_reflns 3174 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _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 0.28064(8) 0.80316(7) 0.6676(3) 0.0151(3) Uani 1 1 d . . . Zn2 Zn 0.10691(9) 0.80464(7) 0.2648(3) 0.0157(3) Uani 1 1 d . . . Zn3 Zn 0.40651(8) 0.75190(7) 1.1726(3) 0.0137(3) Uani 1 1 d . . . Zn4 Zn 0.73316(9) 0.93645(7) 1.3504(3) 0.0171(3) Uani 1 1 d . . . P1 P 0.39952(17) 0.65526(15) 0.6900(6) 0.0112(6) Uani 1 1 d . . . P2 P 0.28031(18) 0.89476(15) 0.1730(7) 0.0130(5) Uani 1 1 d . . . P3 P 0.6121(2) 0.79306(16) 1.2488(7) 0.0136(6) Uani 1 1 d . . . O1 O 0.3050(6) 0.8860(5) 0.8886(16) 0.0182(18) Uani 1 1 d . . . O2 O 0.1601(6) 0.7715(5) 0.6041(18) 0.024(2) Uani 1 1 d . . . O3 O 0.3243(5) 0.8260(5) 0.3229(17) 0.0185(18) Uani 1 1 d . . . O4 O 0.3565(5) 0.7256(4) 0.8313(18) 0.0162(17) Uani 1 1 d . . . O5 O 0.6212(8) 0.7795(6) 1.535(2) 0.032(2) Uani 1 1 d . . . O6 O -0.0062(5) 0.8505(4) 0.284(2) 0.023(2) Uani 1 1 d . . . O7 O 0.1825(5) 0.8909(5) 0.2134(19) 0.026(2) Uani 1 1 d . . . O8 O 0.5197(5) 0.7941(5) 1.146(2) 0.028(2) Uani 1 1 d . . . O9 O 0.3889(6) 0.6671(5) 1.3986(16) 0.0214(19) Uani 1 1 d . . . O10 O 0.6818(5) 1.0315(4) 1.2781(19) 0.0187(18) Uani 1 1 d . . . O11 O 0.8538(6) 0.9175(4) 1.2703(19) 0.0202(18) Uani 1 1 d . . . O12 O 0.6557(6) 0.8678(5) 1.176(2) 0.026(2) Uani 1 1 d . . . O13 O 0.7379(8) 0.9145(9) 1.729(2) 0.053(3) Uani 1 1 d . . . O20 O 0.505(2) 0.9393(18) 1.750(11) 0.27(3) Uani 0.75 1 d P . . N1 N 0.0000 1.0000 0.570(4) 0.049(6) Uani 1 2 d S . . H10B H 0.0237 1.0356 0.4683 0.059 Uiso 0.50 1 calc PR . . H10C H -0.0237 0.9644 0.4683 0.059 Uiso 0.50 1 calc PR . . C1 C 0.0693(12) 0.9657(11) 0.731(4) 0.053(5) Uani 1 1 d . . . H1B H 0.1134 0.9442 0.6217 0.079 Uiso 1 1 calc R . . H1C H 0.0443 0.9269 0.8370 0.079 Uiso 1 1 calc R . . H1D H 0.0951 1.0037 0.8386 0.079 Uiso 1 1 calc R . . O20A O 0.444(3) 0.991(2) 1.745(9) 0.037(10) Uiso 0.25 1 d P . . 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 0.0167(6) 0.0178(6) 0.0108(6) 0.0007(6) -0.0001(6) 0.0027(5) Zn2 0.0154(6) 0.0177(6) 0.0139(6) 0.0006(6) -0.0014(5) 0.0003(5) Zn3 0.0147(6) 0.0151(6) 0.0112(6) -0.0005(6) -0.0014(6) 0.0006(5) Zn4 0.0174(6) 0.0136(6) 0.0205(7) -0.0003(6) -0.0015(6) -0.0001(5) P1 0.0140(12) 0.0107(12) 0.0089(14) 0.0009(12) -0.0015(11) 0.0019(10) P2 0.0160(12) 0.0124(12) 0.0105(13) 0.0007(13) 0.0011(13) 0.0016(10) P3 0.0143(13) 0.0132(13) 0.0131(15) -0.0017(12) 0.0010(11) -0.0018(11) O1 0.034(5) 0.019(4) 0.002(4) 0.004(3) 0.004(4) -0.004(4) O2 0.016(4) 0.028(5) 0.028(6) 0.012(4) -0.002(4) -0.009(4) O3 0.023(4) 0.016(4) 0.016(5) 0.001(4) 0.003(4) 0.009(3) O4 0.016(4) 0.016(4) 0.017(4) -0.004(4) -0.005(3) 0.007(3) O5 0.056(7) 0.027(5) 0.015(5) -0.002(4) 0.002(5) -0.003(5) O6 0.013(4) 0.018(4) 0.038(6) -0.013(4) -0.007(4) 0.003(3) O7 0.013(4) 0.025(5) 0.039(7) 0.007(5) 0.000(4) 0.005(3) O8 0.010(4) 0.025(4) 0.050(6) -0.003(5) -0.007(4) -0.004(3) O9 0.039(5) 0.019(4) 0.006(4) -0.005(4) 0.001(4) 0.001(4) O10 0.018(4) 0.010(4) 0.028(5) 0.001(4) 0.002(4) 0.000(3) O11 0.023(4) 0.012(3) 0.026(5) -0.011(4) 0.000(4) 0.010(3) O12 0.030(5) 0.026(4) 0.022(5) -0.007(4) -0.004(4) -0.016(4) O13 0.048(7) 0.087(9) 0.025(7) 0.017(7) -0.005(5) -0.005(7) O20 0.065(17) 0.16(3) 0.58(10) 0.22(4) -0.03(4) -0.008(18) N1 0.093(17) 0.030(9) 0.024(9) 0.000 0.000 -0.042(11) C1 0.046(9) 0.055(10) 0.057(13) 0.000(10) 0.017(9) 0.010(9) _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 1.900(9) . ? Zn1 O3 1.951(9) . ? Zn1 O2 1.954(9) . ? Zn1 O4 1.988(8) . ? Zn2 O6 1.914(8) . ? Zn2 O5 1.922(11) 3_463 ? Zn2 O7 1.935(9) . ? Zn2 O2 2.026(9) . ? Zn3 O8 1.891(8) . ? Zn3 O9 1.925(9) . ? Zn3 O3 1.978(8) 1_556 ? Zn3 O4 1.984(9) . ? Zn4 O10 1.896(8) . ? Zn4 O11 1.919(8) . ? Zn4 O12 1.923(9) . ? Zn4 O13 2.006(12) . ? P1 O6 1.525(8) 3_565 ? P1 O11 1.525(8) 3_464 ? P1 O9 1.535(9) 1_554 ? P1 O4 1.590(8) . ? P2 O7 1.511(9) . ? P2 O10 1.530(8) 2_674 ? P2 O1 1.531(9) 1_554 ? P2 O3 1.594(9) . ? P3 O8 1.509(9) . ? P3 O5 1.511(11) . ? P3 O12 1.530(9) . ? P3 O2 1.553(9) 3_565 ? O1 P2 1.531(9) 1_556 ? O2 P3 1.553(9) 3_464 ? O3 Zn3 1.978(8) 1_554 ? O5 Zn2 1.922(11) 3_566 ? O6 P1 1.525(8) 3_464 ? O9 P1 1.535(9) 1_556 ? O10 P2 1.530(8) 2_676 ? O11 P1 1.525(8) 3_565 ? O20 O20A 1.30(5) . ? O20 O20A 1.47(5) 2_675 ? N1 C1 1.48(2) 2_575 ? N1 C1 1.48(2) . ? N1 H10B 0.9000 . ? N1 H10C 0.9000 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? O20A O20 1.47(5) 2_675 ? O20A O20A 1.74(8) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 109.0(4) . . ? O1 Zn1 O2 120.6(4) . . ? O3 Zn1 O2 103.2(4) . . ? O1 Zn1 O4 99.3(4) . . ? O3 Zn1 O4 109.6(4) . . ? O2 Zn1 O4 115.0(3) . . ? O6 Zn2 O5 117.8(4) . 3_463 ? O6 Zn2 O7 102.2(4) . . ? O5 Zn2 O7 117.4(4) 3_463 . ? O6 Zn2 O2 116.1(4) . . ? O5 Zn2 O2 105.5(4) 3_463 . ? O7 Zn2 O2 96.3(4) . . ? O8 Zn3 O9 118.9(4) . . ? O8 Zn3 O3 110.3(4) . 1_556 ? O9 Zn3 O3 100.9(4) . 1_556 ? O8 Zn3 O4 112.3(5) . . ? O9 Zn3 O4 107.8(4) . . ? O3 Zn3 O4 105.2(3) 1_556 . ? O10 Zn4 O11 120.7(4) . . ? O10 Zn4 O12 102.4(4) . . ? O11 Zn4 O12 112.2(4) . . ? O10 Zn4 O13 112.4(5) . . ? O11 Zn4 O13 98.2(5) . . ? O12 Zn4 O13 111.1(5) . . ? O6 P1 O11 106.8(5) 3_565 3_464 ? O6 P1 O9 115.2(6) 3_565 1_554 ? O11 P1 O9 109.6(5) 3_464 1_554 ? O6 P1 O4 107.2(5) 3_565 . ? O11 P1 O4 110.4(5) 3_464 . ? O9 P1 O4 107.6(5) 1_554 . ? O7 P2 O10 111.3(5) . 2_674 ? O7 P2 O1 111.9(6) . 1_554 ? O10 P2 O1 109.7(5) 2_674 1_554 ? O7 P2 O3 108.4(5) . . ? O10 P2 O3 108.6(5) 2_674 . ? O1 P2 O3 106.8(5) 1_554 . ? O8 P3 O5 115.9(7) . . ? O8 P3 O12 108.1(5) . . ? O5 P3 O12 109.8(6) . . ? O8 P3 O2 106.3(6) . 3_565 ? O5 P3 O2 108.3(6) . 3_565 ? O12 P3 O2 108.2(6) . 3_565 ? P2 O1 Zn1 127.7(5) 1_556 . ? P3 O2 Zn1 125.2(5) 3_464 . ? P3 O2 Zn2 116.3(5) 3_464 . ? Zn1 O2 Zn2 116.2(4) . . ? P2 O3 Zn1 117.5(5) . . ? P2 O3 Zn3 125.7(5) . 1_554 ? Zn1 O3 Zn3 116.1(4) . 1_554 ? P1 O4 Zn3 115.9(4) . . ? P1 O4 Zn1 125.9(5) . . ? Zn3 O4 Zn1 116.3(4) . . ? P3 O5 Zn2 136.3(7) . 3_566 ? P1 O6 Zn2 143.9(5) 3_464 . ? P2 O7 Zn2 130.2(5) . . ? P3 O8 Zn3 145.5(7) . . ? P1 O9 Zn3 133.8(6) 1_556 . ? P2 O10 Zn4 132.3(5) 2_676 . ? P1 O11 Zn4 130.4(5) 3_565 . ? P3 O12 Zn4 134.5(7) . . ? O20A O20 O20A 78(3) . 2_675 ? C1 N1 C1 111(2) 2_575 . ? C1 N1 H10B 109.4 2_575 . ? C1 N1 H10B 109.4 . . ? C1 N1 H10C 109.4 2_575 . ? C1 N1 H10C 109.4 . . ? H10B N1 H10C 108.0 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O20 O20A O20 102(3) . 2_675 ? O20 O20A O20A 56(3) . 2_675 ? O20 O20A O20A 47(2) 2_675 2_675 ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.187 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.266