# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2176 data_2 _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_email 'igor.fritsky@urz.uni-heidelberg.de' loop_ _publ_author_name ; J.Swiatek-Kozlowska, I.O.Fritsky, A.Dobosz, A.Karaczyn, N.M.Dudarenko,T.Yu.Sliva, E.Gumienna-Kontecka, L.Jerzykiewicz ; _journal_name_full 'J. Chem. Soc., Dalton Trans.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; dipotassium bis(oxalodihydroxamato)nickolate(II) dihydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H4 K N2 Ni0.50 O5' _chemical_formula_weight 204.53 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 3.7290(10) _cell_length_b 19.753(4) _cell_length_c 8.203(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.91(3) _cell_angle_gamma 90.00 _cell_volume 591.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type 'empirical (Starynowicz, 1999)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.92 _diffrn_ambient_temperature 300(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 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 1138 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1012 _reflns_number_gt 882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-97 (Keller, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.4728P] 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 1012 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.0000 0.0000 0.01473(18) Uani 1 d S . . K K -0.46264(16) -0.23378(3) -0.34725(8) 0.0249(2) Uani 1 d . . . O1 O 0.5628(5) -0.16206(9) 0.1954(2) 0.0230(4) Uani 1 d . . . O2 O 0.1516(5) -0.19017(9) -0.1242(2) 0.0233(4) Uani 1 d . . . O3 O 0.4774(6) -0.03910(11) 0.3201(2) 0.0259(5) Uani 1 d . . . O4 O -0.2430(6) -0.08729(10) -0.2897(2) 0.0242(5) Uani 1 d . . . N1 N 0.3056(6) -0.05549(11) 0.1543(3) 0.0185(5) Uani 1 d . . . N2 N -0.0148(6) -0.07776(12) -0.1298(3) 0.0195(5) Uani 1 d . . . C1 C 0.3691(7) -0.11704(13) 0.1112(3) 0.0168(5) Uani 1 d . . . C2 C 0.1558(7) -0.13247(13) -0.0642(3) 0.0172(5) Uani 1 d . . . O5 O -0.9235(7) -0.13806(14) -0.5285(3) 0.0319(5) Uani 1 d . . . H1 H -0.116(14) -0.102(2) -0.360(6) 0.063(14) Uiso 1 d . . . H2 H 0.405(15) 0.005(3) 0.330(7) 0.074(16) Uiso 1 d . . . H3 H -0.816(16) -0.113(3) -0.555(7) 0.069(19) Uiso 1 d . . . H4 H -1.105(14) -0.145(2) -0.613(6) 0.055(12) Uiso 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 Ni 0.0180(3) 0.0132(3) 0.0113(3) -0.00083(17) -0.00077(18) 0.00172(17) K 0.0230(3) 0.0243(4) 0.0265(4) -0.0053(3) 0.0032(3) 0.0017(2) O1 0.0251(10) 0.0179(10) 0.0231(10) 0.0024(8) -0.0023(8) 0.0040(8) O2 0.0307(10) 0.0162(10) 0.0223(10) -0.0029(8) 0.0040(8) 0.0017(8) O3 0.0364(11) 0.0214(11) 0.0140(10) -0.0052(8) -0.0084(8) 0.0052(8) O4 0.0293(11) 0.0261(11) 0.0130(10) -0.0070(8) -0.0052(8) 0.0037(8) N1 0.0235(11) 0.0184(12) 0.0107(11) -0.0014(8) -0.0035(8) 0.0005(9) N2 0.0244(11) 0.0205(11) 0.0105(11) -0.0041(9) -0.0035(9) 0.0014(9) C1 0.0176(12) 0.0177(13) 0.0148(13) 0.0022(11) 0.0024(10) -0.0007(10) C2 0.0176(12) 0.0177(14) 0.0169(13) 0.0002(11) 0.0049(10) -0.0003(10) O5 0.0319(12) 0.0398(14) 0.0201(11) 0.0033(10) -0.0036(10) 0.0063(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 Ni N2 1.863(2) . ? Ni N2 1.863(2) 3 ? Ni N1 1.873(2) . ? Ni N1 1.873(2) 3 ? K O2 2.692(2) 1_455 ? K O2 2.758(2) . ? K O5 2.772(2) . ? K O1 2.783(2) 4_455 ? K O1 2.813(2) 4 ? K O2 2.828(2) 4 ? K O4 3.018(2) . ? K C1 3.241(3) 4 ? K C2 3.266(3) 4 ? K O5 3.326(3) 1_655 ? K C2 3.536(3) . ? K K 3.7290(10) 1_455 ? O1 C1 1.258(3) . ? O1 K 2.783(2) 4_756 ? O1 K 2.813(2) 4_656 ? O2 C2 1.240(3) . ? O2 K 2.692(2) 1_655 ? O2 K 2.828(2) 4_656 ? O3 N1 1.416(3) . ? O4 N2 1.421(3) . ? N1 C1 1.301(4) . ? N2 C2 1.312(4) . ? C1 C2 1.524(4) . ? C1 K 3.241(3) 4_656 ? C2 K 3.266(3) 4_656 ? O5 K 3.326(3) 1_455 ? 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 N2 Ni N2 180.0 . 3 ? N2 Ni N1 81.13(10) . . ? N2 Ni N1 98.87(10) 3 . ? N2 Ni N1 98.87(10) . 3 ? N2 Ni N1 81.13(10) 3 3 ? N1 Ni N1 180.0 . 3 ? O2 K O2 86.35(6) 1_455 . ? O2 K O5 77.71(7) 1_455 . ? O2 K O5 118.74(8) . . ? O2 K O1 73.04(6) 1_455 4_455 ? O2 K O1 127.61(6) . 4_455 ? O5 K O1 103.40(8) . 4_455 ? O2 K O1 127.29(6) 1_455 4 ? O2 K O1 71.59(6) . 4 ? O5 K O1 154.75(7) . 4 ? O1 K O1 83.59(6) 4_455 4 ? O2 K O2 154.99(7) 1_455 4 ? O2 K O2 117.17(7) . 4 ? O5 K O2 96.37(7) . 4 ? O1 K O2 85.03(6) 4_455 4 ? O1 K O2 59.66(6) 4 4 ? O2 K O4 75.67(6) 1_455 . ? O2 K O4 55.61(5) . . ? O5 K O4 63.14(8) . . ? O1 K O4 148.04(6) 4_455 . ? O1 K O4 121.49(6) 4 . ? O2 K O4 123.64(6) 4 . ? O2 K C1 129.17(6) 1_455 4 ? O2 K C1 94.07(6) . 4 ? O5 K C1 140.49(8) . 4 ? O1 K C1 66.88(6) 4_455 4 ? O1 K C1 22.60(6) 4 4 ? O2 K C1 46.26(6) 4 4 ? O4 K C1 142.29(7) . 4 ? O2 K C2 141.32(7) 1_455 4 ? O2 K C2 115.27(6) . 4 ? O5 K C2 113.46(7) . 4 ? O1 K C2 68.37(6) 4_455 4 ? O1 K C2 46.13(6) 4 4 ? O2 K C2 22.02(6) 4 4 ? O4 K C2 142.95(6) . 4 ? C1 K C2 27.09(7) 4 4 ? O2 K O5 125.38(6) 1_455 1_655 ? O2 K O5 67.86(6) . 1_655 ? O5 K O5 74.78(7) . 1_655 ? O1 K O5 159.29(6) 4_455 1_655 ? O1 K O5 90.10(6) 4 1_655 ? O2 K O5 74.79(6) 4 1_655 ? O4 K O5 49.85(6) . 1_655 ? C1 K O5 101.00(7) 4 1_655 ? C2 K O5 93.10(7) 4 1_655 ? O2 K C2 74.94(6) 1_455 . ? O2 K C2 17.79(6) . . ? O5 K C2 102.38(8) . . ? O1 K C2 132.95(6) 4_455 . ? O1 K C2 89.38(6) 4 . ? O2 K C2 129.95(6) 4 . ? O4 K C2 40.13(6) . . ? C1 K C2 111.86(7) 4 . ? C2 K C2 132.25(8) 4 . ? O5 K C2 66.38(6) 1_655 . ? O2 K K 47.57(5) 1_455 1_455 ? O2 K K 133.92(4) . 1_455 ? O5 K K 59.38(7) . 1_455 ? O1 K K 48.55(4) 4_455 1_455 ? O1 K K 132.14(4) 4 1_455 ? O2 K K 108.44(5) 4 1_455 ? O4 K K 103.84(4) . 1_455 ? C1 K K 113.79(5) 4 1_455 ? C2 K K 104.34(5) 4 1_455 ? O5 K K 134.16(4) 1_655 1_455 ? C2 K K 121.11(4) . 1_455 ? C1 O1 K 139.59(17) . 4_756 ? C1 O1 K 98.19(15) . 4_656 ? K O1 K 83.59(6) 4_756 4_656 ? C2 O2 K 126.82(16) . 1_655 ? C2 O2 K 119.42(17) . . ? K O2 K 86.35(6) 1_655 . ? C2 O2 K 99.25(16) . 4_656 ? K O2 K 124.49(7) 1_655 4_656 ? K O2 K 97.17(6) . 4_656 ? N2 O4 K 111.29(14) . . ? C1 N1 O3 113.8(2) . . ? C1 N1 Ni 118.86(18) . . ? O3 N1 Ni 127.36(17) . . ? C2 N2 O4 114.6(2) . . ? C2 N2 Ni 119.33(17) . . ? O4 N2 Ni 125.32(17) . . ? O1 C1 N1 128.8(2) . . ? O1 C1 C2 120.4(2) . . ? N1 C1 C2 110.8(2) . . ? O1 C1 K 59.21(14) . 4_656 ? N1 C1 K 136.57(18) . 4_656 ? C2 C1 K 77.37(14) . 4_656 ? O2 C2 N2 128.9(2) . . ? O2 C2 C1 121.3(2) . . ? N2 C2 C1 109.7(2) . . ? O2 C2 K 58.74(14) . 4_656 ? N2 C2 K 141.38(18) . 4_656 ? C1 C2 K 75.54(14) . 4_656 ? O2 C2 K 42.79(13) . . ? N2 C2 K 90.08(15) . . ? C1 C2 K 151.11(16) . . ? K C2 K 75.92(6) 4_656 . ? K O5 K 74.78(7) . 1_455 ? loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_contact_distance_DH _geom_contact_distance_HA _geom_angle_DHA _geom_contact_distance_DA _geom_contact_site_symmetry_A O4 H1 O5 0.86(5) 1.83(5) 2.69(4) 170(5) 1_655 O3 H2 O4 0.92(6) 1.74(6) 2.64(3) 164(6) 2_555 O5 H3 O3 0.69(6) 2.21(6) 2.89(4) 170(7) 1_454 O5 H4 O1 0.87(5) 1.82(6) 2.70(4) 172(5) 1_354 # $1 x+1, y, z # $2 -x, -y, -z # $3 x-1, y, z-1 # $4 x-2, y, z-1 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.285 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.089