data_2011343 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1092 _journal_page_last 1094 _publ_section_title ; A three-dimensional open-framework germanate containing four-, five- and six-coordinated germanium ; loop_ _publ_author_name 'Sun, Kai' 'Dadachov, Mike S.' 'Conradsson, Tony' 'Zou, Xiaodong' _chemical_name_common '[(H2NC2H4NH2)(H3NC2H4NH3)2][Ge9O18(OH)4]' _chemical_formula_moiety 'C6 H32 Ge9 N6 O22' _chemical_formula_sum 'C6 H32 Ge9 N6 O22' _chemical_formula_iupac '(C2 H8 N2 )(C2 H10 N2 )2 [H4 Ge9 O22 ]' _chemical_formula_weight 1193.68 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.1958(15) _cell_length_b 9.9753(10) _cell_length_c 13.1655(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.695(17) _cell_angle_gamma 90.00 _cell_volume 1338.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.961 _diffrn_ambient_temperature 293(2) 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 Ge1 .5000 .0000 .0000 .00530(14) Uani d S 1 . . Ge Ge2 .66385(4) .11685(4) .22083(3) .00670(12) Uani d . 1 . . Ge Ge3 .38181(4) .16338(4) .22955(3) .00800(12) Uani d . 1 . . Ge Ge4 .37016(4) .17895(4) -.16785(3) .00633(12) Uani d . 1 . . Ge Ge5 .66835(4) .13366(4) -.16933(3) .00673(12) Uani d . 1 . . Ge O1 .3862(3) .1442(3) -.0388(2) .0099(6) Uani d . 1 . . O O2 .5145(3) .0677(3) .1338(2) .0073(6) Uani d . 1 . . O O3 .7882(3) .1684(3) .3194(2) .0113(6) Uani d . 1 . . O O4 .6463(3) .1004(3) -.0407(2) .0102(6) Uani d . 1 . . O O5 .2897(3) .0122(3) .2377(2) .0143(7) Uani d . 1 . . O O6 .7432(3) .2095(3) .1243(2) .0139(7) Uani d . 1 . . O H1 .7163 .1846 .0685 .017 Uiso calc R 1 . . H O7 .5342(3) .1864(3) .2947(2) .0129(7) Uani d . 1 . . O O8 .5254(3) .2072(3) -.2226(2) .0128(6) Uani d . 1 . . O O9 .3406(3) .2767(3) .1307(2) .0173(7) Uani d . 1 . . O H2 .3454 .2383 .0758 .021 Uiso calc R 1 . . H O10 .2939(3) .2503(3) .3284(2) .0132(7) Uani d . 1 . . O O11 .7151(3) -.0528(3) .2336(2) .0127(7) Uani d . 1 . . O C1 .5575(5) .4524(5) .0077(4) .0273(12) Uani d . 1 . . C H1A .5368 .3653 -.0209 .033 Uiso calc R 1 . . H H1B .6346 .4871 -.0258 .033 Uiso calc R 1 . . H N1 .5825(5) .4405(5) .1180(3) .0293(11) Uani d . 1 . . N H1C .6178 .5164 .1411 .035 Uiso calc R 1 . . H H1D .6376 .3729 .1297 .035 Uiso calc R 1 . . H H1E .5073 .4251 .1495 .035 Uiso calc R 1 . . H C2 .4830(7) .0688(7) .5199(5) .0409(16) Uani d . 1 . . C H2A .4136 .1064 .4777 .049 Uiso calc R 1 . . H H2B .4494 .0598 .5882 .049 Uiso calc R 1 . . H N2 .5918(6) .1605(6) -.4781(4) .0471(15) Uani d . 1 . . N H2C .6557 .1274 -.4388 .057 Uiso calc R 1 . . H H2D .5658 .2390 -.4533 .057 Uiso calc R 1 . . H H2E .6214 .1719 -.5408 .057 Uiso calc R 1 . . H C3 .5232(13) .5073(10) -.4518(6) .092(4) Uani d . 1 . . C H3A .4699 .5747 -.4188 .110 Uiso calc R 1 . . H H3B .6114 .5432 -.4558 .110 Uiso calc R 1 . . H N3 .5281(6) .3920(7) -.3866(5) .0487(15) Uani d D 1 . . N H3C .449(3) .366(7) -.366(4) .058 Uiso d D 1 . . H H3D .580(5) .402(8) -.331(3) .058 Uiso d D 1 . . H 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 Ge1 .0061(3) .0048(3) .0050(3) -.0004(2) -.0009(2) .0004(2) Ge2 .0065(2) .0050(2) .0086(2) -.00009(16) -.00103(16) -.00059(17) Ge3 .0073(2) .0067(2) .0100(2) .00070(16) -.00015(17) -.00085(18) Ge4 .0077(2) .0043(2) .0069(2) .00008(16) -.00225(16) .00046(17) Ge5 .0071(2) .0062(2) .0069(2) -.00028(16) .00108(17) .00076(17) O1 .0113(15) .0091(16) .0092(15) .0027(12) -.0003(12) .0030(12) O2 .0066(14) .0101(16) .0052(14) .0014(11) .0007(11) .0004(12) O3 .0124(15) .0070(16) .0144(15) -.0017(12) -.0084(12) .0020(12) O4 .0098(15) .0119(16) .0088(15) -.0044(12) -.0020(12) .0027(12) O5 .0145(16) .0105(17) .0180(16) -.0040(12) .0078(13) -.0047(13) O6 .0185(16) .0157(17) .0075(15) -.0092(13) -.0025(12) .0005(13) O7 .0079(14) .0180(18) .0126(15) .0019(13) -.0019(12) -.0091(13) O8 .0125(15) .0146(17) .0113(15) .0004(13) .0005(12) .0055(13) O9 .0241(18) .0136(18) .0143(16) .0096(14) -.0009(14) .0010(13) O10 .0154(16) .0126(17) .0115(16) .0047(12) -.0006(13) -.0015(13) O11 .0126(16) .0088(16) .0165(16) .0007(12) -.0090(13) -.0010(13) C1 .030(3) .018(3) .033(3) .004(2) -.013(2) .001(2) N1 .036(3) .017(2) .035(3) -.0064(19) -.020(2) .006(2) C2 .046(4) .048(4) .029(3) -.003(3) -.004(3) .006(3) N2 .057(4) .053(4) .031(3) -.008(3) .008(3) -.004(3) C3 .178(12) .058(6) .040(4) -.013(7) -.011(6) .015(4) N3 .036(3) .062(4) .048(3) -.004(3) -.003(3) .015(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 Ge1 O4 . 1.880(3) yes Ge1 O4 3_655 1.880(3) ? Ge1 O2 3_655 1.890(3) ? Ge1 O2 . 1.890(3) yes Ge1 O1 3_655 1.914(3) ? Ge1 O1 . 1.914(3) yes Ge2 O6 . 1.774(3) yes Ge2 O11 . 1.778(3) yes Ge2 O7 . 1.790(3) yes Ge2 O3 . 1.874(3) yes Ge2 O2 . 1.957(3) yes Ge2 Ge3 . 2.9165(7) ? Ge3 O9 . 1.770(3) yes Ge3 O7 . 1.781(3) yes Ge3 O5 . 1.781(3) yes Ge3 O10 . 1.810(3) yes Ge3 O2 . 2.091(3) yes Ge4 O1 . 1.739(3) yes Ge4 O3 4_565 1.744(3) yes Ge4 O11 3_655 1.752(3) yes Ge4 O8 . 1.770(3) yes Ge5 O10 4_665 1.726(3) yes Ge5 O4 . 1.743(3) yes Ge5 O5 3_655 1.766(3) yes Ge5 O8 . 1.769(3) yes O3 Ge4 4_666 1.744(3) ? O5 Ge5 3_655 1.766(3) ? O6 H1 . .8200 ? O9 H2 . .8200 ? O10 Ge5 4_566 1.726(3) ? O11 Ge4 3_655 1.752(3) ? C1 N1 . 1.475(7) ? C1 C1 3_665 1.520(10) ? C1 H1A . .9700 ? C1 H1B . .9700 ? N1 H1C . .8900 ? N1 H1D . .8900 ? N1 H1E . .8900 ? C2 N2 1_556 1.438(9) ? C2 C2 3_656 1.511(14) ? C2 H2A . .9700 ? C2 H2B . .9700 ? N2 C2 1_554 1.438(9) ? N2 H2C . .8900 ? N2 H2D . .8900 ? N2 H2E . .8900 ? C3 C3 3_664 1.357(16) ? C3 N3 . 1.436(10) ? C3 H3A . .9700 ? C3 H3B . .9700 ? N3 H3C . .90(2) ? N3 H3D . .90(2) ?