#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2013252.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2013252
_journal_name_full  'Acta Crystallographica, Section C'
_journal_year  2003
_journal_volume  59
_journal_page_first  m168
_journal_page_last  m170
_publ_section_title
;
Monoclinic polymorph of
rac-5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane
bis(hexafluorogermanate) tetrahydrate
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
loop_
_publ_author_name
  'Fonari, Marina S.'
  'Simonov, Yurii A.'
  'Chumakov, Yurii M.'
  'Bocelli, Gabriele'
  'Ganin, Eduard V.'
  'Gelmboldt, Vladimir O.'
_chemical_name_common
;
(H4-tet b) bis(hexafluorogermanate)tetrahydrate
;
_chemical_formula_moiety  'C16 H40 N4 4+, 2F6 Ge 2-, 4H2 O'
_chemical_formula_sum  'C16 H48 F12 Ge2 N4 O4'
_chemical_formula_iupac  '(C16 H40 N4) [Ge F6]2, 4H2 O'
_chemical_formula_weight  733.76
_chemical_melting_point  70
_symmetry_cell_setting  monoclinic
loop_
_symmetry_equiv_pos_as_xyz
  'x, y, z'
  '-x, y+1/2, -z+1/2'
  '-x, -y, -z'
  'x, -y-1/2, z-1/2'
_cell_length_a  9.5650(19)
_cell_length_b  16.522(3)
_cell_length_c  9.0210(18)
_cell_angle_alpha  90.00
_cell_angle_beta  96.28(3)
_cell_angle_gamma  90.00
_cell_volume  1417.1(5)
_cell_formula_units_Z  2
_cell_measurement_temperature  293(2)
_exptl_crystal_density_diffrn  1.720
_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
  N1 0.65202(15) 0.48758(9) 0.28844(16) 0.0170(3) Uani d . 1 . . N
  H1N 0.665(2) 0.4808(14) 0.377(3) 0.038(7) Uiso d . 1 . . H
  H2N 0.583(2) 0.5204(12) 0.273(2) 0.019(5) Uiso d . 1 . . H
  C2 0.61510(18) 0.40828(10) 0.21150(19) 0.0201(3) Uani d . 1 . . C
  H2A 0.6883 0.3692 0.2423 0.024 Uiso calc R 1 . . H
  H2B 0.6135 0.4159 0.1047 0.024 Uiso calc R 1 . . H
  C3 0.47415(18) 0.37364(10) 0.24386(18) 0.0209(3) Uani d . 1 . . C
  H3A 0.4769 0.3154 0.2307 0.025 Uiso calc R 1 . . H
  H3B 0.4630 0.3839 0.3478 0.025 Uiso calc R 1 . . H
  N4 0.34695(15) 0.40574(9) 0.15045(16) 0.0176(3) Uani d . 1 . . N
  H3N 0.272(3) 0.3778(13) 0.180(3) 0.031(6) Uiso d . 1 . . H
  H4N 0.339(2) 0.4523(15) 0.173(2) 0.029(6) Uiso d . 1 . . H
  C5 0.34726(18) 0.40030(10) -0.01641(17) 0.0174(3) Uani d . 1 . . C
  H5 0.4316 0.4279 -0.0431 0.021 Uiso calc R 1 . . H
  C51 0.3563(2) 0.31189(12) -0.0614(2) 0.0343(5) Uani d . 1 . . C
  H51A 0.4383 0.2877 -0.0084 0.051 Uiso calc R 1 . . H
  H51B 0.3624 0.3084 -0.1667 0.051 Uiso calc R 1 . . H
  H51C 0.2738 0.2837 -0.0376 0.051 Uiso calc R 1 . . H
  C6 0.21803(17) 0.44708(10) -0.08745(18) 0.0188(3) Uani d . 1 . . C
  H6A 0.2103 0.4961 -0.0298 0.023 Uiso calc R 1 . . H
  H6B 0.1356 0.4145 -0.0754 0.023 Uiso calc R 1 . . H
  C7 0.21032(17) 0.47177(10) -0.25352(18) 0.0185(3) Uani d . 1 . . C
  C71 0.09110(19) 0.53334(12) -0.2851(2) 0.0312(4) Uani d . 1 . . C
  H71A 0.0945 0.5563 -0.3824 0.047 Uiso calc R 1 . . H
  H71B 0.1017 0.5755 -0.2116 0.047 Uiso calc R 1 . . H
  H71C 0.0023 0.5068 -0.2811 0.047 Uiso calc R 1 . . H
  C72 0.1857(2) 0.40094(12) -0.3625(2) 0.0291(4) Uani d . 1 . . C
  H72A 0.1058 0.3702 -0.3390 0.044 Uiso calc R 1 . . H
  H72B 0.2674 0.3668 -0.3543 0.044 Uiso calc R 1 . . H
  H72C 0.1685 0.4213 -0.4624 0.044 Uiso calc R 1 . . H
  Ge1 0.310989(19) 0.621276(10) 0.316046(19) 0.01870(7) Uani d . 1 . . Ge
  F1 0.24643(18) 0.65746(9) 0.48029(16) 0.0585(4) Uani d . 1 . . F
  F2 0.29704(16) 0.52018(7) 0.38974(14) 0.0471(4) Uani d . 1 . . F
  F3 0.13940(14) 0.61257(9) 0.22150(18) 0.0503(4) Uani d . 1 . . F
  F4 0.38129(13) 0.57228(7) 0.15877(12) 0.0336(3) Uani d . 1 . . F
  F5 0.32908(15) 0.71764(7) 0.24103(17) 0.0474(4) Uani d . 1 . . F
  F6 0.48772(15) 0.62380(10) 0.40165(17) 0.0563(4) Uani d . 1 . . F
  O1W 0.12041(17) 0.31098(10) 0.20649(19) 0.0376(4) Uani d D 1 . . O
  H1W 0.077(2) 0.3026(15) 0.283(2) 0.044(7) Uiso d D 1 . . H
  H2W 0.067(2) 0.2972(16) 0.135(2) 0.046(8) Uiso d D 1 . . H
  O2W 0.03232(17) 0.74663(11) 0.05757(19) 0.0397(4) Uani d D 1 . . O
  H3W 0.068(3) 0.7104(14) 0.109(3) 0.054(9) Uiso d D 1 . . H
  H4W 0.098(3) 0.7706(19) 0.022(4) 0.088(12) 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
  N1 0.0179(7) 0.0173(7) 0.0154(7) -0.0014(5) 0.0004(5) 0.0021(5)
  C2 0.0212(8) 0.0171(7) 0.0211(8) -0.0001(6) -0.0015(6) -0.0013(6)
  C3 0.0255(8) 0.0188(8) 0.0174(7) -0.0044(7) -0.0020(6) 0.0050(6)
  N4 0.0204(7) 0.0162(6) 0.0162(6) -0.0030(5) 0.0026(5) -0.0006(5)
  C5 0.0192(8) 0.0196(7) 0.0137(7) 0.0012(6) 0.0032(6) 0.0029(6)
  C51 0.0517(13) 0.0254(9) 0.0247(9) 0.0143(9) -0.0006(9) -0.0065(7)
  C6 0.0181(7) 0.0201(8) 0.0183(7) 0.0001(6) 0.0030(6) 0.0026(6)
  C7 0.0158(7) 0.0200(8) 0.0189(8) -0.0027(6) -0.0012(6) 0.0044(6)
  C71 0.0179(8) 0.0337(10) 0.0408(11) 0.0030(7) -0.0024(8) 0.0146(9)
  C72 0.0348(10) 0.0290(10) 0.0222(8) -0.0117(8) -0.0026(7) -0.0002(7)
  Ge1 0.02193(10) 0.01746(10) 0.01710(9) 0.00349(7) 0.00387(6) 0.00024(7)
  F1 0.0845(12) 0.0531(9) 0.0435(8) 0.0186(8) 0.0328(8) -0.0117(7)
  F2 0.0837(10) 0.0255(6) 0.0368(7) 0.0096(6) 0.0277(7) 0.0138(5)
  F3 0.0231(6) 0.0586(9) 0.0663(10) -0.0104(6) -0.0080(6) 0.0156(7)
  F4 0.0524(7) 0.0281(6) 0.0237(5) -0.0062(5) 0.0192(5) -0.0048(5)
  F5 0.0588(9) 0.0199(6) 0.0646(9) -0.0062(6) 0.0111(7) 0.0078(6)
  F6 0.0339(7) 0.0848(12) 0.0458(8) 0.0079(7) -0.0159(6) -0.0109(8)
  O1W 0.0339(8) 0.0413(9) 0.0385(9) -0.0119(7) 0.0078(7) 0.0017(7)
  O2W 0.0311(8) 0.0450(10) 0.0423(9) -0.0011(7) 0.0008(7) 0.0122(8)
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
  N1 C2 . 1.506(2) no
  N1 C7 3_665 1.541(2) no
  N1 H1N . 0.81(2) no
  N1 H2N . 0.85(2) no
  C2 C3 . 1.522(2) no
  C2 H2A . 0.9700 no
  C2 H2B . 0.9700 no
  C3 N4 . 1.499(2) no
  C3 H3A . 0.9700 no
  C3 H3B . 0.9700 no
  N4 C5 . 1.508(2) no
  N4 H3N . 0.92(2) no
  N4 H4N . 0.80(2) no
  C5 C51 . 1.521(2) no
  C5 C6 . 1.537(2) no
  C5 H5 . 0.9800 no
  C51 H51A . 0.9600 no
  C51 H51B . 0.9600 no
  C51 H51C . 0.9600 no
  C6 C7 . 1.547(2) no
  C6 H6A . 0.9700 no
  C6 H6B . 0.9700 no
  C7 C72 . 1.530(2) no
  C7 C71 . 1.531(2) no
  C7 N1 3_665 1.541(2) no
  C71 H71A . 0.9600 no
  C71 H71B . 0.9600 no
  C71 H71C . 0.9600 no
  C72 H72A . 0.9600 no
  C72 H72B . 0.9600 no
  C72 H72C . 0.9600 no
  Ge1 F5 . 1.7459(12) yes
  Ge1 F1 . 1.7703(13) yes
  Ge1 F3 . 1.7708(14) yes
  Ge1 F6 . 1.7805(15) yes
  Ge1 F2 . 1.8081(12) yes
  Ge1 F4 . 1.8246(11) yes
  O1W H1W . 0.854(16) no
  O1W H2W . 0.814(16) no
  O2W H3W . 0.811(17) no
  O2W H4W . 0.835(18) no
_cod_database_code 2013252