#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003700.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003700
loop_
_publ_author_name
'Chiang, H.-C.'
'Hwang, S.-F.'
'Ueng, C.-H.'
_publ_section_title
;
 Sodium
 Bis(2,3-dimethylbutane-2,3-diolato)hydroxogermanate(IV)--Methanol
 (1/3)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1258
_journal_page_last               1260
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C15 H37 Ge1 Na1 O8'
_chemical_formula_sum            'C15 H37 Ge Na O8'
_chemical_formula_weight         441.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                86.88(4)
_cell_angle_beta                 80.46(3)
_cell_angle_gamma                66.59(6)
_cell_formula_units_Z            2
_cell_length_a                   10.235(5)
_cell_length_b                   10.249(8)
_cell_length_c                   11.810(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    218
_cell_measurement_theta_max      13.11
_cell_measurement_theta_min      10.12
_cell_volume                     1121.1(12)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2927
_diffrn_reflns_theta_max         22.5
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.40
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_meas      1.3
_exptl_crystal_density_method    'flotation in CH~2~Cl~2~/C~2~H~5~OH'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       2.1(5)\mm
_refine_ls_extinction_method
'secondary extinction (NRCVAX; Larsen et al., 1990)'
_refine_ls_goodness_of_fit_obs   2.59
_refine_ls_hydrogen_treatment
'H-atom positions taken from \DF map and not refined'
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2646
_refine_ls_R_factor_obs          0.032
_refine_ls_shift/esd_max         0.012
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      1/[\s^2^(F)+0.0001F^2^]
_refine_ls_wR_factor_obs         0.039
_reflns_number_observed          2646
_reflns_number_total             2917
_reflns_observed_criterion       >2\s(I)
_[local]_cod_data_source_file    mu1145.cif
_[local]_cod_data_source_block   mu1145a
_[local]_cod_chemical_formula_sum_orig 'C15 H37 Ge1 Na1 O8'
_cod_original_cell_volume        1121.0(10)
_cod_database_code               2003700
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ge .93310(4) .17596(4) .16909(3)
O(1) 1.0425(2) -.0187(2) .1446(2)
O(2) 1.0806(2) .1841(2) .2298(2)
O(3) .7906(2) .1338(2) .2503(2)
O(4) .8222(2) .3657(2) .2114(2)
O(5) .9318(2) .2198(2) .0222(2)
C(1) 1.1884(4) -.0536(4) .1590(4)
C(2) 1.1847(4) .0467(4) .2508(4)
C(3) 1.2711(4) -.0181(5) .0434(4)
C(4) 1.2589(4) -.2089(4) .1796(4)
C(5) 1.1261(5) -.0034(6) .3703(4)
C(6) 1.3230(5) .0580(5) .2614(5)
C(7) .6618(4) .2563(4) .2875(3)
C(8) .7126(4) .3773(4) .3074(3)
C(9) .5828(4) .2176(5) .3954(4)
C(10) .5695(4) .2931(5) .1926(4)
C(11) .7785(4) .3567(5) .4166(3)
C(12) .5937(5) .5237(4) .3081(4)
C(13) 1.2131(8) .1819(6) -.3229(7)
C(14) 1.3053(5) .3645(6) -.0178(5)
C(15) .8698(5) .5367(5) -.3414(4)
O(6) 1.1147(4) .1913(3) -.2319(3)
O(7) 1.1706(3) .4473(3) -.0507(2)
O(8) .9112(4) .5491(3) -.2403(3)
Na .9929(2) .3781(2) -.09980(10)
HO(5) .951 .161 -.014
HO(6) 1.026 .226 -.257
HO(7) 1.184 .501 -.113
HO(8) 1.011 .495 -.266
H(3A) 1.232 .096 .037
H(3B) 1.245 -.061 -.027
H(3C) 1.383 -.067 .052
H(4A) 1.256 -.266 .118
H(4B) 1.358 -.238 .188
H(4C) 1.212 -.236 .250
H(5A) 1.029 -.016 .362
H(5B) 1.102 .079 .433
H(5C) 1.212 -.101 .387
H(6A) 1.313 .123 .319
H(6B) 1.395 -.033 .275
H(6C) 1.363 .090 .188
H(9A) .494 .296 .423
H(9B) .562 .137 .383
H(9C) .641 .195 .457
H(10A) .546 .214 .177
H(10B) .478 .372 .216
H(10C) .615 .318 .124
H(11A) .818 .424 .423
H(11B) .708 .363 .483
H(11C) .854 .262 .416
H(12A) .517 .535 .370
H(12B) .628 .596 .311
H(12C) .551 .536 .237
H(13A) 1.210 .123 -.386
H(13B) 1.312 .133 -.306
H(13C) 1.198 .288 -.356
H(14A) 1.296 .304 .046
H(14B) 1.372 .304 -.079
H(14C) 1.347 .440 .008
H(15A) .887 .604 -.399
H(15B) .768 .558 -.333
H(15C) .932 .430 -.373
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) Ge O(2) . . 87.60(10) yes
O(1) Ge O(3) . . 88.90(10) yes
O(1) Ge O(4) . . 173.50(10) yes
O(1) Ge O(5) . . 95.90(10) yes
O(2) Ge O(3) . . 123.80(10) yes
O(2) Ge O(4) . . 90.00(10) yes
O(2) Ge O(5) . . 115.60(10) yes
O(3) Ge O(4) . . 87.40(10) yes
O(3) Ge O(5) . . 120.60(10) yes
O(4) Ge O(5) . . 90.60(10) yes
Ge O(1) C(1) . . 110.6(2) yes
Ge O(2) C(2) . . 112.8(2) yes
Ge O(3) C(7) . . 113.8(2) yes
Ge O(4) C(8) . . 111.3(2) yes
Ge O(5) Na . . 136.30(10) yes
C(13) O(6) Na . . 128.9(3) yes
C(14) O(7) Na . . 130.2(3) yes
C(14) O(7) Na . 2_765 112.5(3) yes
Na O(7) Na . 2_765 95.70(10) yes
C(15) O(8) Na . . 129.8(3) yes
O(5) Na O(6) . . 87.90(10) yes
O(5) Na O(7) . . 116.40(10) yes
O(5) Na O(7) . 2_765 82.60(10) yes
O(5) Na O(8) . . 143.30(10) yes
O(6) Na O(7) . . 105.80(10) yes
O(6) Na O(7) . 2_765 168.50(10) yes
O(6) Na O(8) . . 94.20(10) yes
O(7) Na O(7) . 2_765 84.30(10) yes
O(7) Na O(8) . . 98.30(10) yes
O(7) Na O(8) 2_765 . 89.50(10) yes
Ge O(5) HO(5) . . 113.7(2) no
Na O(5) HO(5) . . 102.2(2) no
O(1) C(1) C(2) . . 106.9(3) no
O(1) C(1) C(3) . . 108.3(3) no
O(1) C(1) C(4) . . 109.3(3) no
C(2) C(1) C(3) . . 106.7(3) no
C(2) C(1) C(4) . . 117.1(4) no
C(7) C(9) H(9A) . . 111.3(4) no
C(7) C(9) H(9B) . . 111.7(4) no
C(7) C(9) H(9C) . . 110.4(3) no
H(9A) C(9) H(9B) . . 108.9(4) no
H(9A) C(9) H(9C) . . 106.7(4) no
H(9B) C(9) H(9C) . . 107.6(4) no
C(7) C(10) H(10A) . . 110.6(4) no
C(7) C(10) H(10B) . . 110.6(4) no
C(7) C(10) H(10C) . . 112.6(3) no
H(10A) C(10) H(10B) . . 105.9(4) no
H(10A) C(10) H(10C) . . 108.6(4) no
H(10B) C(10) H(10C) . . 108.3(4) no
C(8) C(11) H(11A) . . 111.6(4) no
C(8) C(11) H(11B) . . 110.6(4) no
C(8) C(11) H(11C) . . 109.7(3) no
H(11A) C(11) H(11B) . . 109.4(4) no
H(11A) C(11) H(11C) . . 108.5(4) no
H(11B) C(11) H(11C) . . 106.9(4) no
C(8) C(12) H(12A) . . 111.2(4) no
C(8) C(12) H(12B) . . 111.9(4) no
C(8) C(12) H(12C) . . 109.3(4) no
H(12A) C(12) H(12B) . . 110.3(4) no
C(3) C(1) C(4) . . 108.2(4) no
O(2) C(2) C(1) . . 107.1(3) no
O(2) C(2) C(5) . . 107.1(3) no
O(2) C(2) C(6) . . 109.4(3) no
C(1) C(2) C(5) . . 107.4(4) no
C(1) C(2) C(6) . . 117.5(4) no
C(5) C(2) C(6) . . 107.9(4) no
C(1) C(3) H(3A) . . 107.5(3) no
C(1) C(3) H(3B) . . 107.6(4) no
C(1) C(3) H(3C) . . 104.9(4) no
H(3A) C(3) H(3B) . . 109.9(4) no
H(3A) C(3) H(3C) . . 113.2(4) no
H(3B) C(3) H(3C) . . 113.3(4) no
C(1) C(4) H(4A) . . 112.3(4) no
C(1) C(4) H(4B) . . 112.2(4) no
C(1) C(4) H(4C) . . 111.4(4) no
H(4A) C(4) H(4B) . . 107.4(4) no
H(4A) C(4) H(4C) . . 106.5(4) no
H(4B) C(4) H(4C) . . 106.7(4) no
C(2) C(5) H(5A) . . 108.1(4) no
C(2) C(5) H(5B) . . 107.9(4) no
C(2) C(5) H(5C) . . 104.9(4) no
H(5A) C(5) H(5B) . . 109.6(4) no
H(5A) C(5) H(5C) . . 113.3(5) no
H(5B) C(5) H(5C) . . 112.8(4) no
C(2) C(6) H(6A) . . 113.2(4) no
C(2) C(6) H(6B) . . 111.1(4) no
C(2) C(6) H(6C) . . 110.5(4) no
H(6A) C(6) H(6B) . . 109.5(4) no
H(6A) C(6) H(6C) . . 106.9(5) no
H(6B) C(6) H(6C) . . 105.3(5) no
O(3) C(7) C(8) . . 106.0(3) no
O(3) C(7) C(9) . . 108.0(3) no
O(3) C(7) C(10) . . 107.8(3) no
C(8) C(7) C(9) . . 113.2(3) no
C(8) C(7) C(10) . . 111.7(3) no
C(9) C(7) C(10) . . 109.9(3) no
O(4) C(8) C(7) . . 104.6(3) no
O(4) C(8) C(11) . . 108.5(3) no
O(4) C(8) C(12) . . 108.6(3) no
C(7) C(8) C(11) . . 112.3(3) no
C(7) C(8) C(12) . . 112.8(3) no
C(11) C(8) C(12) . . 109.8(3) no
H(12A) C(12) H(12C) . . 106.3(4) no
H(12B) C(12) H(12C) . . 107.5(4) no
O(6) C(13) H(13A) . . 113.0(6) no
O(6) C(13) H(13B) . . 112.3(8) no
O(6) C(13) H(13C) . . 110.5(5) no
H(13A) C(13) H(13B) . . 103.4(5) no
H(13A) C(13) H(13C) . . 108.2(8) no
H(13B) C(13) H(13C) . . 109.1(6) no
O(7) C(14) H(14A) . . 111.7(5) no
O(7) C(14) H(14B) . . 112.6(5) no
O(7) C(14) H(14C) . . 106.2(4) no
H(14A) C(14) H(14B) . . 107.5(5) no
H(14A) C(14) H(14C) . . 109.0(6) no
H(14B) C(14) H(14C) . . 109.8(5) no
O(8) C(15) H(15A) . . 112.3(4) no
O(8) C(15) H(15B) . . 112.1(5) no
O(8) C(15) H(15C) . . 107.9(4) no
H(15A) C(15) H(15B) . . 105.4(5) no
H(15A) C(15) H(15C) . . 108.7(5) no
H(15B) C(15) H(15C) . . 110.5(4) no
C(13) O(6) HO(6) . . 107.1(5) no
Na O(6) HO(6) . . 81.7(2) no
C(14) O(7) HO(7) . . 108.8(3) no
Na O(7) HO(7) . . 101.50(19) no
Na O(7) HO(7) 2_765 . 105.26(18) no
C(15) O(8) HO(8) . . 94.5(3) no
Na O(8) HO(8) . . 73.09(18) no
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
Ge O(1) . 1.870(3) yes
Ge O(2) . 1.806(2) yes
Ge O(3) . 1.796(2) yes
Ge O(4) . 1.866(3) yes
Ge O(5) . 1.769(2) yes
O(5) Na . 2.313(3) yes
O(6) Na . 2.332(4) yes
O(7) Na . 2.359(3) yes
O(8) Na . 2.347(4) yes
Na O(7) 2_765 2.478(3) yes
O(1) C(1) . 1.428(4) yes
O(2) C(2) . 1.427(4) yes
O(3) C(7) . 1.435(4) yes
O(4) C(8) . 1.430(4) yes
C(13) O(6) . 1.324(8) yes
C(14) O(7) . 1.408(5) yes
C(15) O(8) . 1.359(6) yes
O(5) HO(5) . .703(2) no
C(1) C(2) . 1.520(6) no
C(1) C(3) . 1.587(6) no
C(1) C(4) . 1.489(5) no
C(2) C(5) . 1.581(7) no
C(2) C(6) . 1.490(6) no
C(3) H(3A) . 1.078(5) no
C(3) H(3B) . 1.076(5) no
C(3) H(3C) . 1.077(4) no
C(4) H(4A) . .964(5) no
C(4) H(4B) . .961(4) no
C(4) H(4C) . .972(5) no
C(5) H(5A) . 1.076(6) no
C(5) H(5B) . 1.082(6) no
C(5) H(5C) . 1.073(5) no
C(6) H(6A) . .940(5) no
C(6) H(6B) . .960(5) no
C(6) H(6C) . .991(5) no
C(7) C(8) . 1.564(5) no
C(7) C(9) . 1.514(5) no
C(7) C(10) . 1.521(5) no
C(8) C(11) . 1.519(5) no
C(8) C(12) . 1.510(5) no
C(9) H(9A) . .958(4) no
C(9) H(9B) . .948(5) no
C(9) H(9C) . .975(4) no
C(10) H(10A) . .970(5) no
C(10) H(10B) . .973(4) no
C(10) H(10C) . .941(4) no
C(11) H(11A) . .941(4) no
C(11) H(11B) . .960(4) no
C(11) H(11C) . .971(5) no
C(12) H(12A) . .952(4) no
C(12) H(12B) . .938(5) no
C(12) H(12C) . .986(5) no
C(13) H(13A) . .994(8) no
C(13) H(13B) . .982(8) no
C(13) H(13C) . 1.094(7) no
C(14) H(14A) . .967(5) no
C(14) H(14B) . .956(6) no
C(14) H(14C) . 1.095(6) no
C(15) H(15A) . .987(5) no
C(15) H(15B) . .963(5) no
C(15) H(15C) . 1.074(5) no
O(6) HO(6) . .929(4) no
O(7) HO(7) . .919(2) no
O(8) HO(8) . .950(4) no