data_2012508 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m81 _journal_page_last m83 _publ_section_title ; (\m-oxalato-O,O':O,O')-bis[aqua(diethylenetriamine)nickel(II)] bis(hexafluorophosphate) dihydrate ; loop_ _publ_author_name 'Muga, I\~naki' 'Vitoria, Pablo' "Guti\'errez-Zorrilla, Juan M." 'Luque, Antonio' "Guzm\'an-Miralles, Carmen" "Rom\'an, Pascual" _chemical_formula_moiety 'C10 H30 N6 Ni2 O6 2+, 2(F6 P 1-), 2(H2 O)' _chemical_formula_sum 'C10 H34 F12 N6 Ni2 O8 P2' _chemical_formula_iupac '[Ni2(C2O4)(C4H13N2)(H2O)2].2PF6.2H2O' _chemical_formula_weight 773.79 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.994(3) _cell_length_b 7.1850(10) _cell_length_c 16.806(3) _cell_angle_alpha 90 _cell_angle_beta 98.860(10) _cell_angle_gamma 90 _cell_volume 2743.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_meas 1.860(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ni1 .179352(16) .02743(6) .39461(2) .02721(16) Uani d . 1 A . Ni C1 .24313(13) .3334(4) .47094(18) .0284(5) Uani d . 1 . . C O1 .21024(10) .3027(3) .40594(14) .0339(5) Uani d . 1 . . O O2 .23426(12) .0133(3) .50730(16) .0378(6) Uani d . 1 . . O O3w .25067(13) -.0329(4) .3343(2) .0480(7) Uani d . 1 . . O H31w .2816(18) .024(3) .3488(9) .072 Uiso d . 1 . . H H32w .2607(6) -.144(6) .3308(3) .072 Uiso d . 1 . . H N1 .12576(14) .1058(5) .28923(17) .0406(7) Uani d DU 1 . . N H11A .1464 .1675 .2563 .049 Uiso calc PR .692(14) A 1 H H12A .1086 .0060 .2631 .049 Uiso calc PR .692(14) A 1 H H11B .1368 .2190 .2741 .049 Uiso calc PR .308(14) A 2 H H12B .1302 .0246 .2499 .049 Uiso calc PR .308(14) A 2 H C3 .0565(2) .1434(9) .3844(3) .0612(12) Uani d DU 1 . . C H31A .0304 .0431 .3635 .073 Uiso calc PR .692(14) A 1 H H32A .0337 .2339 .4094 .073 Uiso calc PR .692(14) A 1 H H31B .0536 .2764 .3929 .073 Uiso calc PR .308(14) A 2 H H32B .0195 .0879 .3926 .073 Uiso calc PR .308(14) A 2 H C2A .0803(3) .2316(10) .3181(4) .0486(17) Uani d PDU .692(14) A 1 C H21A .0983 .3496 .3359 .058 Uiso calc PR .692(14) A 1 H H22A .0487 .2560 .2741 .058 Uiso calc PR .692(14) A 1 H C2B .0647(5) .111(2) .2998(7) .050(4) Uani d PDU .308(14) A 2 C H21B .0462 -.0057 .2816 .060 Uiso calc PR .308(14) A 2 H H22B .0450 .2095 .2664 .060 Uiso calc PR .308(14) A 2 H N4 .10349(13) .0688(5) .44557(19) .0363(6) Uani d . 1 A . N H4 .1115 .1538 .4859 .044 Uiso calc R 1 . . H C5 .0891(2) -.1113(7) .4811(3) .0569(11) Uani d . 1 . . C H51 .0482 -.1110 .4889 .068 Uiso calc R 1 A . H H52 .1133 -.1272 .5332 .068 Uiso calc R 1 . . H C6 .0996(2) -.2703(7) .4270(3) .0542(10) Uani d . 1 A . C H61 .0973 -.3873 .4552 .065 Uiso calc R 1 . . H H62 .0697 -.2707 .3796 .065 Uiso calc R 1 . . H N7 .15821(13) -.2510(4) .40288(19) .0375(6) Uani d . 1 . . N H71 .1584 -.3067 .3550 .045 Uiso calc R 1 A . H H72 .1853 -.3074 .4394 .045 Uiso calc R 1 . . H O4w .2765(2) -.3876(5) .3242(2) .0708(12) Uani d . 1 . . O H41w .2699(5) -.442(4) .288(3) .106 Uiso d . 1 . . H H42w .2675(7) -.439(4) .360(3) .106 Uiso d . 1 . . H P1 .41065(5) .12878(17) .35642(6) .0451(3) Uani d . 1 . . P F1 .3949(4) -.0843(7) .3557(4) .145(2) Uani d . 1 . . F F2 .4610(3) .1057(15) .3104(5) .212(5) Uani d . 1 . . F F3 .4523(2) .1217(10) .4397(3) .1198(19) Uani d . 1 . . F F4 .35914(17) .1510(9) .4085(3) .122(2) Uani d . 1 . . F F5 .3672(3) .1400(12) .2780(3) .159(3) Uani d . 1 . . F F6 .4245(3) .3421(7) .3635(4) .148(3) Uani d . 1 . . F loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 .0270(2) .0256(2) .0274(2) -.00334(13) -.00091(15) -.00169(13) C1 .0291(12) .0238(13) .0302(13) -.0018(10) -.0027(10) .0039(10) O1 .0398(11) .0273(10) .0301(10) -.0056(9) -.0085(8) .0033(8) O2 .0420(13) .0269(11) .0385(12) -.0073(9) -.0129(10) .0057(9) O3w .0400(14) .0455(16) .0618(18) -.0048(11) .0182(13) -.0078(13) N1 .0431(15) .0468(18) .0287(12) -.0047(13) -.0044(11) .0007(12) C3 .045(2) .081(3) .057(2) .022(2) .0038(17) .002(2) C2A .037(3) .051(4) .055(3) .004(2) -.003(2) .011(3) C2B .035(5) .063(10) .046(5) .001(6) -.014(4) .011(6) N4 .0388(14) .0351(14) .0358(13) -.0009(11) .0079(11) -.0037(11) C5 .064(3) .052(3) .061(3) -.009(2) .029(2) .003(2) C6 .058(2) .045(2) .062(3) -.0160(18) .015(2) .0014(19) N7 .0402(14) .0285(13) .0427(15) -.0037(11) .0025(11) -.0035(11) O4w .110(3) .054(2) .0584(19) .023(2) .045(2) .0160(16) P1 .0437(5) .0528(6) .0388(5) -.0075(4) .0066(4) -.0010(4) F1 .222(7) .060(3) .160(5) -.029(4) .055(5) -.019(3) F2 .141(5) .338(11) .187(7) -.107(6) .124(5) -.148(7) F3 .082(3) .179(6) .086(3) -.009(3) -.027(2) .007(3) F4 .070(2) .187(6) .117(3) -.038(3) .037(2) -.083(4) F5 .135(4) .262(9) .062(2) -.056(5) -.042(3) .038(4) F6 .210(6) .066(3) .160(6) -.047(4) .001(5) .011(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 N7 . 2.068(3) yes Ni1 N1 . 2.074(3) yes Ni1 N4 . 2.080(3) yes Ni1 O1 . 2.100(2) yes Ni1 O3w . 2.102(3) yes Ni1 O2 . 2.111(2) yes C1 O1 . 1.249(3) no C1 O2 7_556 1.249(4) no C1 C1 7_556 1.547(6) no O2 C1 7_556 1.249(4) no O3w H31w . .82(4) no O3w H32w . .83(4) no N1 C2B . 1.442(11) no N1 C2A . 1.517(7) no N1 H11A . .9000 no N1 H12A . .9000 no N1 H11B . .9000 no N1 H12B . .9000 no C3 C2A . 1.460(8) no C3 N4 . 1.472(5) no C3 C2B . 1.481(13) no C3 H31A . .9700 no C3 H32A . .9700 no C3 H31B . .9700 no C3 H32B . .9700 no C2A H21A . .9700 no C2A H22A . .9700 no C2B H21B . .9700 no C2B H22B . .9700 no N4 C5 . 1.483(6) no N4 H4 . .9100 no C5 C6 . 1.502(7) no C5 H51 . .9700 no C5 H52 . .9700 no C6 N7 . 1.472(5) no C6 H61 . .9700 no C6 H62 . .9700 no N7 H71 . .9000 no N7 H72 . .9000 no O4w H41w . .72(4) no O4w H42w . .76(4) no P1 F2 . 1.498(5) no P1 F5 . 1.528(4) no P1 F6 . 1.567(5) no P1 F3 . 1.570(4) no P1 F1 . 1.573(5) no P1 F4 . 1.586(4) no