# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm # Attachment 'CIF.txt' _journal_coden_Cambridge 1350 _publ_contact_author_name 'Rongshun Wang' _publ_contact_author_address ; Institute of Functional Material Chemistry Faculty of Chemistry Northeast Normal University Changchun 130024 P. R. China ; _publ_contact_author_email FENGJD009@NENU.EDU.CN loop_ _publ_author_name 'Rong-Shun Wang.' 'Jing-Dong Feng.' 'Kui-Zhan Shao.' 'Zhong-Min Su.' ; Shu-Wei Tang ; 'Hai-Ming Xie.' 'Chan Yao.' #complex NIS-4 data_NIS-4 _database_code_depnum_ccdc_archive 'CCDC 737304' #TrackingRef 'CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H14 N2 O8 P2 Zn' _chemical_formula_weight 369.50 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 8.8490(7) _cell_length_b 13.8690(10) _cell_length_c 10.8180(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1327.66(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 164 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 23.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 2.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5975 _exptl_absorpt_correction_T_max 0.6637 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type graphite _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7573 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.51 _reflns_number_total 3013 _reflns_number_gt 2884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0351P)^2^+0.0044P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(10) _refine_ls_number_reflns 3013 _refine_ls_number_parameters 172 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.03756(3) 0.101162(17) 0.32781(3) 0.02015(8) Uani 1 1 d . . . P1 P 0.01052(8) -0.07784(5) 0.12516(6) 0.02192(13) Uani 1 1 d . . . P2 P -0.17102(7) 0.28392(4) 0.38000(7) 0.02293(14) Uani 1 1 d . . . O5 O -0.1013(2) 0.20657(14) 0.30080(17) 0.0334(5) Uani 1 1 d . . . O8 O -0.2725(2) 0.24083(13) 0.48230(18) 0.0295(4) Uani 1 1 d . . . O4 O -0.0103(2) -0.04953(15) -0.00696(18) 0.0314(4) Uani 1 1 d . . . O2 O -0.1000(3) -0.16304(14) 0.1589(2) 0.0385(5) Uani 1 1 d . . . O3 O -0.0160(2) 0.00102(17) 0.2165(2) 0.0381(5) Uani 1 1 d . . . O7 O -0.0405(2) 0.34147(17) 0.4476(2) 0.0427(6) Uani 1 1 d . . . O1 O 0.1750(2) -0.11776(16) 0.1469(2) 0.0418(5) Uani 1 1 d . . . O6 O -0.2571(2) 0.35660(14) 0.30376(19) 0.0342(5) Uani 1 1 d . . . N1 N -0.3832(3) -0.2149(2) 0.4371(2) 0.0425(6) Uani 1 1 d . . . N2 N -0.3918(3) -0.08446(18) 0.3297(3) 0.0434(6) Uani 1 1 d . . . C3 C -0.3321(4) -0.1401(3) 0.5111(4) 0.0525(9) Uani 1 1 d . . . H3 H -0.2998 -0.1449 0.5926 0.063 Uiso 1 1 calc R . . C1 C -0.4169(4) -0.1786(2) 0.3270(4) 0.0415(6) Uani 1 1 d . . . H1 H -0.4522 -0.2134 0.2594 0.050 Uiso 1 1 calc R . . C2 C -0.3383(4) -0.0602(3) 0.4431(3) 0.0517(9) Uani 1 1 d . . . H2 H -0.3108 0.0014 0.4687 0.062 Uiso 1 1 calc R . . C4 C -0.4188(5) -0.0170(3) 0.2264(4) 0.0650(11) Uani 1 1 d . . . H4A H -0.3924 0.0472 0.2515 0.097 Uiso 1 1 calc R . . H4B H -0.5236 -0.0189 0.2036 0.097 Uiso 1 1 calc R . . H4C H -0.3579 -0.0355 0.1568 0.097 Uiso 1 1 calc R . . C5 C -0.3964(4) -0.3170(3) 0.4735(3) 0.0518(9) Uani 1 1 d . . . H5A H -0.4420 -0.3209 0.5549 0.062 Uiso 1 1 calc R . . H5B H -0.4622 -0.3501 0.4158 0.062 Uiso 1 1 calc R . . C6 C -0.2520(6) -0.3638(3) 0.4757(6) 0.0871(18) Uani 1 1 d . . . H6A H -0.2647 -0.4300 0.4994 0.131 Uiso 1 1 calc R . . H6B H -0.1873 -0.3320 0.5341 0.131 Uiso 1 1 calc R . . H6C H -0.2072 -0.3608 0.3949 0.131 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 0.02475(14) 0.02034(13) 0.01535(13) -0.00407(13) 0.00150(13) -0.00122(9) P1 0.0298(3) 0.0209(3) 0.0151(3) -0.0050(3) -0.0017(3) -0.0010(2) P2 0.0222(3) 0.0249(3) 0.0217(3) -0.0004(3) 0.0022(3) 0.0051(2) O5 0.0368(11) 0.0360(10) 0.0273(12) -0.0067(8) -0.0015(8) 0.0148(8) O8 0.0292(10) 0.0333(10) 0.0261(10) 0.0074(8) 0.0056(8) 0.0066(8) O4 0.0494(12) 0.0293(10) 0.0154(10) 0.0018(9) -0.0045(8) -0.0044(9) O2 0.0545(13) 0.0368(11) 0.0241(10) 0.0009(8) -0.0024(9) -0.0178(10) O3 0.0439(12) 0.0383(12) 0.0322(12) -0.0214(10) -0.0033(10) 0.0017(9) O7 0.0343(12) 0.0370(12) 0.0568(16) -0.0162(11) -0.0037(10) -0.0010(9) O1 0.0375(12) 0.0541(12) 0.0337(12) -0.0132(10) -0.0094(10) 0.0116(10) O6 0.0276(9) 0.0391(10) 0.0359(12) 0.0126(9) 0.0087(8) 0.0127(8) N1 0.0462(16) 0.0494(15) 0.0318(13) -0.0032(12) 0.0005(12) -0.0038(12) N2 0.0477(15) 0.0464(13) 0.0360(13) -0.0061(17) 0.0063(16) 0.0004(11) C3 0.053(2) 0.074(2) 0.0304(17) -0.0136(18) -0.0079(15) 0.0002(18) C1 0.0487(16) 0.0451(15) 0.0308(14) -0.0100(18) -0.0011(19) -0.0033(13) C2 0.057(2) 0.0484(19) 0.049(2) -0.0170(17) -0.0103(17) -0.0056(17) C4 0.087(3) 0.059(2) 0.049(2) 0.000(2) -0.005(2) 0.022(2) C5 0.052(2) 0.056(2) 0.047(2) 0.0115(17) 0.0032(17) -0.0150(17) C6 0.060(3) 0.065(2) 0.137(5) 0.044(3) -0.009(3) -0.009(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 O3 1.898(2) . ? Zn1 O6 1.9264(19) 4 ? Zn1 O5 1.9319(19) . ? Zn1 O4 1.941(2) 2 ? P1 O3 1.492(2) . ? P1 O4 1.494(2) . ? P1 O1 1.575(2) . ? P1 O2 1.577(2) . ? P2 O5 1.5052(19) . ? P2 O6 1.5090(19) . ? P2 O8 1.546(2) . ? P2 O7 1.583(2) . ? O4 Zn1 1.941(2) 2_554 ? O6 Zn1 1.9264(19) 4_455 ? N1 C1 1.327(5) . ? N1 C3 1.385(5) . ? N1 C5 1.474(5) . ? N2 C1 1.325(4) . ? N2 C2 1.357(5) . ? N2 C4 1.477(5) . ? C3 C2 1.332(6) . ? C3 H3 0.9300 . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.434(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 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 O3 Zn1 O6 111.85(9) . 4 ? O3 Zn1 O5 107.40(9) . . ? O6 Zn1 O5 110.44(9) 4 . ? O3 Zn1 O4 106.46(10) . 2 ? O6 Zn1 O4 110.73(9) 4 2 ? O5 Zn1 O4 109.84(9) . 2 ? O3 P1 O4 114.92(14) . . ? O3 P1 O1 107.70(12) . . ? O4 P1 O1 110.44(13) . . ? O3 P1 O2 107.37(13) . . ? O4 P1 O2 110.00(12) . . ? O1 P1 O2 105.99(13) . . ? O5 P2 O6 111.84(11) . . ? O5 P2 O8 111.73(11) . . ? O6 P2 O8 110.86(11) . . ? O5 P2 O7 108.85(13) . . ? O6 P2 O7 106.52(12) . . ? O8 P2 O7 106.76(13) . . ? P2 O5 Zn1 135.56(12) . . ? P1 O4 Zn1 143.11(13) . 2_554 ? P1 O3 Zn1 156.48(14) . . ? P2 O6 Zn1 127.27(12) . 4_455 ? C1 N1 C3 107.9(3) . . ? C1 N1 C5 125.9(3) . . ? C3 N1 C5 126.1(3) . . ? C1 N2 C2 108.8(3) . . ? C1 N2 C4 125.5(3) . . ? C2 N2 C4 125.7(3) . . ? C2 C3 N1 106.9(3) . . ? C2 C3 H3 126.5 . . ? N1 C3 H3 126.5 . . ? N2 C1 N1 108.5(3) . . ? N2 C1 H1 125.8 . . ? N1 C1 H1 125.8 . . ? C3 C2 N2 107.9(3) . . ? C3 C2 H2 126.1 . . ? N2 C2 H2 126.1 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N1 111.6(3) . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? N1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 O6 P2 O5 Zn1 172.10(17) . . . . ? O8 P2 O5 Zn1 -63.0(2) . . . . ? O7 P2 O5 Zn1 54.7(2) . . . . ? O3 Zn1 O5 P2 148.02(19) . . . . ? O6 Zn1 O5 P2 -89.8(2) 4 . . . ? O4 Zn1 O5 P2 32.6(2) 2 . . . ? O3 P1 O4 Zn1 -164.1(2) . . . 2_554 ? O1 P1 O4 Zn1 73.9(3) . . . 2_554 ? O2 P1 O4 Zn1 -42.8(3) . . . 2_554 ? O4 P1 O3 Zn1 -99.4(4) . . . . ? O1 P1 O3 Zn1 24.1(5) . . . . ? O2 P1 O3 Zn1 137.9(4) . . . . ? O6 Zn1 O3 P1 16.1(5) 4 . . . ? O5 Zn1 O3 P1 137.4(4) . . . . ? O4 Zn1 O3 P1 -105.0(4) 2 . . . ? O5 P2 O6 Zn1 128.02(16) . . . 4_455 ? O8 P2 O6 Zn1 2.6(2) . . . 4_455 ? O7 P2 O6 Zn1 -113.17(17) . . . 4_455 ? C1 N1 C3 C2 0.6(4) . . . . ? C5 N1 C3 C2 -179.9(3) . . . . ? C2 N2 C1 N1 1.1(4) . . . . ? C4 N2 C1 N1 -178.5(3) . . . . ? C3 N1 C1 N2 -1.1(4) . . . . ? C5 N1 C1 N2 179.5(3) . . . . ? N1 C3 C2 N2 0.0(4) . . . . ? C1 N2 C2 C3 -0.7(4) . . . . ? C4 N2 C2 C3 178.9(4) . . . . ? C1 N1 C5 C6 103.1(5) . . . . ? C3 N1 C5 C6 -76.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.603 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.068