Audit Creation Method SHELXL-97 s1

data_1

_audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C5 H10 N2 O8 Zn), 3(H2 O)' _chemical_formula_sum 'C10 H26 N4 O19 Zn2' _chemical_formula_weight 637.09 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' '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 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2'

_cell_length_a 20.3821(10) _cell_length_b 11.6308(5) _cell_length_c 9.5513(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2264.23(19) _cell_formula_units_Z 4 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 2123 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 25.03

_exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.205 _exptl_crystal_size_min 0.091 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 2.217 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details 'SADABS'

_exptl_special_details ; ? ;

_diffrn_ambient_temperature 292(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8149 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1995 _reflns_number_gt 1347 _reflns_threshold_expression >2sigma(I)

_computing_data_collection 'CrysAlis' _computing_cell_refinement 'CrysAlis' _computing_data_reduction 'CrysAlis' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'publCIF (Westrip, 2008)'

_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^)+(0.0158P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1995 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0430 _refine_ls_wR_factor_gt 0.0415 _refine_ls_goodness_of_fit_ref 0.783 _refine_ls_restrained_S_all 0.783 _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 Zn Zn 0.352285(14) 0.76712(2) 0.28659(3) 0.02177(9) Uani 1 1 d . . . C1 C 0.35799(12) 0.52822(18) 0.1876(2) 0.0166(6) Uani 1 1 d . . . C2 C 0.37348(12) 0.41311(18) 0.2100(3) 0.0202(6) Uani 1 1 d . . . H2 H 0.3571 0.3498 0.1619 0.024 Uiso 1 1 calc R . . C3 C 0.41809(12) 0.41250(19) 0.3179(3) 0.0186(6) Uani 1 1 d . . . C4 C 0.31157(12) 0.5850(2) 0.0901(3) 0.0191(6) Uani 1 1 d . . . C5 C 0.45208(13) 0.3167(2) 0.3936(3) 0.0204(6) Uani 1 1 d . . . N1 N 0.39145(10) 0.59582(15) 0.2771(2) 0.0189(5) Uani 1 1 d . . . N2 N 0.42774(10) 0.52360(16) 0.3539(2) 0.0203(5) Uani 1 1 d . . . H1 H 0.4542 0.5454 0.4189 0.024 Uiso 1 1 calc R . . O2 O 0.28403(9) 0.52693(13) -0.00156(18) 0.0245(4) Uani 1 1 d . . . O1 O 0.30303(8) 0.69221(13) 0.11012(17) 0.0236(4) Uani 1 1 d . . . O1W O 0.41593(10) 0.85260(15) 0.15419(19) 0.0419(6) Uani 1 1 d . . . H1WA H 0.4234 0.8335 0.0773 0.063 Uiso 1 1 d R . . H1WB H 0.4353 0.8996 0.1787 0.063 Uiso 1 1 d R . . O3 O 0.43153(9) 0.21675(14) 0.37112(18) 0.0302(5) Uani 1 1 d . . . O2W O 0.27730(9) 0.69732(13) 0.42087(18) 0.0328(5) Uani 1 1 d . . . H2WA H 0.2560 0.7296 0.4746 0.049 Uiso 1 1 d R . . H2WB H 0.2823 0.6371 0.4397 0.049 Uiso 1 1 d R . . O4 O 0.49748(9) 0.34201(13) 0.4748(2) 0.0296(5) Uani 1 1 d . . . O3W O 0.41030(9) 0.82306(14) 0.45263(18) 0.0326(5) Uani 1 1 d . . . H3WB H 0.4349 0.7849 0.4754 0.049 Uiso 1 1 d R . . H3WA H 0.3875 0.8353 0.5158 0.049 Uiso 1 1 d R . . O4W O 0.29451(8) 0.90850(13) 0.2843(2) 0.0316(5) Uani 1 1 d . . . H4WA H 0.2715 0.9292 0.3546 0.047 Uiso 1 1 d R . . H4WB H 0.3082 0.9627 0.2533 0.047 Uiso 1 1 d R . . O5W O 0.33719(9) 0.12740(13) 0.20195(19) 0.0347(5) Uani 1 1 d . . . H5WA H 0.3610 0.1531 0.2594 0.052 Uiso 1 1 d R . . H5WB H 0.2988 0.1598 0.2115 0.052 Uiso 1 1 d R . . O6W O 0.5000 0.0255(2) 0.2500 0.0417(8) Uani 1 2 d S . . H6WA H 0.5140 0.0672 0.1972 0.062 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02515(16) 0.01609(15) 0.02407(17) -0.00226(14) -0.00239(16) 0.00185(14) C1 0.0188(14) 0.0157(13) 0.0153(16) -0.0019(10) 0.0000(13) -0.0009(12) C2 0.0258(16) 0.0146(13) 0.0200(15) -0.0043(12) -0.0008(14) 0.0006(11) C3 0.0218(15) 0.0138(13) 0.0203(17) -0.0032(11) 0.0003(12) 0.0011(11) C4 0.0187(15) 0.0210(16) 0.0177(16) 0.0030(12) 0.0054(13) 0.0009(13) C5 0.0233(16) 0.0195(15) 0.0183(16) 0.0002(12) 0.0036(13) 0.0032(13) N1 0.0214(12) 0.0155(10) 0.0197(13) 0.0008(10) -0.0027(11) 0.0037(9) N2 0.0196(12) 0.0230(12) 0.0183(13) -0.0024(10) -0.0062(10) 0.0009(10) O2 0.0322(11) 0.0172(10) 0.0241(12) -0.0051(8) -0.0099(9) 0.0011(8) O1 0.0315(11) 0.0141(10) 0.0250(11) -0.0038(8) -0.0088(9) 0.0042(8) O1W 0.0511(14) 0.0419(12) 0.0327(13) -0.0152(9) 0.0152(11) -0.0196(11) O3 0.0347(12) 0.0187(10) 0.0373(12) 0.0000(8) -0.0109(9) 0.0011(9) O2W 0.0413(12) 0.0178(10) 0.0391(13) 0.0045(8) 0.0172(10) 0.0059(9) O4 0.0292(11) 0.0239(10) 0.0359(14) 0.0000(9) -0.0156(10) 0.0015(9) O3W 0.0327(12) 0.0353(11) 0.0299(12) -0.0023(9) -0.0089(10) 0.0067(9) O4W 0.0376(12) 0.0198(9) 0.0375(12) 0.0064(9) 0.0158(11) 0.0081(8) O5W 0.0307(12) 0.0297(10) 0.0437(13) 0.0024(9) -0.0083(10) -0.0062(8) O6W 0.0429(18) 0.0280(14) 0.054(2) 0.000 0.0047(15) 0.000

_geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O4W 2.0227(15) . ? Zn O1W 2.0665(18) . ? Zn O3W 2.0824(17) . ? Zn O1 2.1466(16) . ? Zn N1 2.1482(18) . ? Zn O2W 2.1541(17) . ? C1 N1 1.347(3) . ? C1 C2 1.392(3) . ? C1 C4 1.482(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9300 . ? C3 N2 1.352(3) . ? C3 C5 1.499(3) . ? C4 O2 1.240(3) . ? C4 O1 1.274(3) . ? C5 O4 1.243(3) . ? C5 O3 1.254(3) . ? N1 N2 1.339(3) . ? N2 H1 0.8600 . ? O1W H1WA 0.7824 . ? O1W H1WB 0.7138 . ? O2W H2WA 0.7693 . ? O2W H2WB 0.7299 . ? O3W H3WB 0.7039 . ? O3W H3WA 0.7752 . ? O4W H4WA 0.8544 . ? O4W H4WB 0.7503 . ? O5W H5WA 0.7912 . ? O5W H5WB 0.8738 . ? O6W H6WA 0.7550 . ? 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 O4W Zn O1W 88.15(7) . . ? O4W Zn O3W 94.86(7) . . ? O1W Zn O3W 87.67(7) . . ? O4W Zn O1 92.82(7) . . ? O1W Zn O1 90.48(7) . . ? O3W Zn O1 172.03(7) . . ? O4W Zn N1 165.90(7) . . ? O1W Zn N1 100.78(8) . . ? O3W Zn N1 96.38(7) . . ? O1 Zn N1 76.36(7) . . ? O4W Zn O2W 84.24(7) . . ? O1W Zn O2W 172.34(7) . . ? O3W Zn O2W 93.85(7) . . ? O1 Zn O2W 89.01(7) . . ? N1 Zn O2W 86.52(7) . . ? N1 C1 C2 110.4(2) . . ? N1 C1 C4 117.5(2) . . ? C2 C1 C4 132.0(2) . . ? C3 C2 C1 105.7(2) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? N2 C3 C2 106.4(2) . . ? N2 C3 C5 121.4(2) . . ? C2 C3 C5 132.2(2) . . ? O2 C4 O1 125.2(2) . . ? O2 C4 C1 119.3(2) . . ? O1 C4 C1 115.4(2) . . ? O4 C5 O3 125.1(2) . . ? O4 C5 C3 118.0(2) . . ? O3 C5 C3 116.9(2) . . ? N2 N1 C1 105.16(18) . . ? N2 N1 Zn 139.83(16) . . ? C1 N1 Zn 112.35(15) . . ? N1 N2 C3 112.3(2) . . ? N1 N2 H1 123.8 . . ? C3 N2 H1 123.8 . . ? C4 O1 Zn 116.82(15) . . ? Zn O1W H1WA 124.0 . . ? Zn O1W H1WB 121.0 . . ? H1WA O1W H1WB 114.7 . . ? Zn O2W H2WA 127.8 . . ? Zn O2W H2WB 114.2 . . ? H2WA O2W H2WB 112.5 . . ? Zn O3W H3WB 116.3 . . ? Zn O3W H3WA 108.0 . . ? H3WB O3W H3WA 107.6 . . ? Zn O4W H4WA 122.7 . . ? Zn O4W H4WB 118.2 . . ? H4WA O4W H4WB 106.1 . . ? H5WA O5W H5WB 108.4 . . ? 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 O5W H5WA O3 0.79 1.94 2.718(2) 168.9 . N2 H1 O4 0.86 1.93 2.728(3) 154.2 5_666 O1W H1WA O3 0.78 2.06 2.839(2) 173.5 8_565 O2W H2WA O1 0.77 1.99 2.757(2) 176.9 2_565 O2W H2WB O2 0.73 1.99 2.715(2) 172.7 8_566 O3W H3WB O4 0.70 2.07 2.775(2) 172.9 5_666 O3W H3WA O5W 0.78 2.10 2.868(3) 172.4 8_566 O4W H4WA O2 0.85 1.85 2.704(2) 175.6 2_565 O4W H4WB O5W 0.75 2.06 2.803(2) 168.6 1_565 O6W H6WA O3 0.75 2.17 2.870(2) 155.6 4_655

_diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.296 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.060