#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/91/2019178.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_2019178
loop_
_publ_author_name
'Redhammer, Günther J.'
'Tippelt, Gerold'
_publ_section_title
;
 The polar phase of Li₂Ge₄O₉ at 298, 150 and 90K
;
_journal_coeditor_code           KU3106
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1091
_journal_page_last               1095
_journal_paper_doi               10.1107/S0108270113025110
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Li2 Ge4 O9'
_chemical_formula_moiety         'Ge4 O9, 2(Li)'
_chemical_formula_sum            'Ge4 Li2 O9'
_chemical_formula_weight         448.24
_chemical_name_systematic
;
Dilithium tetragermanate
;
_space_group_IT_number           29
_space_group_name_Hall           'P -2ac 2a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2ac 2a'
_symmetry_space_group_name_H-M   'P 21 c a'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3044(5)
_cell_length_b                   4.6253(2)
_cell_length_c                   15.8331(8)
_cell_measurement_temperature    90.0(10)
_cell_volume                     681.39(6)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(10)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method
'rotation, ω scans at four different φ positions'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9727
_diffrn_reflns_theta_full        28.8
_diffrn_reflns_theta_max         28.8
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    17.504
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.738
_refine_ls_abs_structure_details
'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.623(14)
_refine_ls_extinction_coef       0.00155(15)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1705
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0151
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0179P)²+0.3290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0379
_reflns_number_gt                1664
_reflns_number_total             1705
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ku3106.cif
_cod_data_source_block           laz1_90k_tr
_cod_database_code               2019178
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, y, -z+1/2'
'x+1/2, -y, -z'
'x, -y, z+1/2'
loop_
_atom_site_type_symbol
_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_occupancy
Li Li1 0.4675(6) 0.4497(10) 0.2646(3) 0.0109(11) Uani d 1
Li Li2 0.2706(6) 0.5814(13) 0.4764(4) 0.0197(12) Uani d 1
Ge Ge1 0.23525(8) 0.48544(5) 0.155922(15) 0.00427(7) Uani d 1
Ge Ge2 0.23398(8) 0.99032(5) 0.295855(15) 0.00452(7) Uani d 1
Ge Ge3 0.52529(4) 1.00110(5) 0.40166(2) 0.00486(10) Uani d 1
Ge Ge4 0.44493(3) 1.02143(6) 0.59436(2) 0.00451(9) Uani d 1
O O1 0.0719(3) 0.7104(4) 0.16149(12) 0.0061(4) Uani d 1
O O2 0.1534(3) 0.2577(4) 0.06946(13) 0.0069(4) Uani d 1
O O3 0.3236(3) 0.7020(4) 0.07130(13) 0.0060(4) Uani d 1
O O4 0.3967(3) 0.2460(4) 0.16485(14) 0.0066(4) Uani d 1
O O5 0.3172(3) 0.7106(4) 0.24166(14) 0.0066(4) Uani d 1
O O6 0.1444(3) 0.2480(4) 0.23671(13) 0.0069(4) Uani d 1
O O7 0.3712(3) 1.1678(4) 0.35565(12) 0.0062(4) Uani d 1
O O8 0.1164(3) 0.8445(4) 0.37343(13) 0.0077(4) Uani d 1
O O9 0.4611(2) 0.8423(3) 0.49598(13) 0.0077(4) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O5 Li1 O6 . 2 163.8(3)
O5 Li1 O1 . 2 95.2(2)
O6 Li1 O1 2 2 83.0(3)
O5 Li1 O4 . . 84.4(3)
O6 Li1 O4 2 . 92.7(2)
O1 Li1 O4 2 . 162.9(3)
O5 Li1 O7 . 1_545 102.1(2)
O6 Li1 O7 2 1_545 94.1(2)
O1 Li1 O7 2 1_545 100.5(3)
O4 Li1 O7 . 1_545 96.3(2)
O2 Li2 O3 4_565 4_565 80.1(2)
O2 Li2 O9 4_565 . 97.7(3)
O3 Li2 O9 4_565 . 93.1(2)
O2 Li2 O8 4_565 . 89.2(2)
O3 Li2 O8 4_565 . 158.4(3)
O9 Li2 O8 . . 107.0(2)
O1 Ge1 O3 . . 95.44(9)
O1 Ge1 O4 . . 172.65(8)
O3 Ge1 O4 . . 91.04(11)
O1 Ge1 O5 . . 89.27(9)
O3 Ge1 O5 . . 92.44(10)
O4 Ge1 O5 . . 86.99(11)
O1 Ge1 O6 . . 85.81(11)
O3 Ge1 O6 . . 176.51(9)
O4 Ge1 O6 . . 87.92(10)
O5 Ge1 O6 . . 90.83(8)
O1 Ge1 O2 . . 90.98(11)
O3 Ge1 O2 . . 87.51(7)
O4 Ge1 O2 . . 92.76(9)
O5 Ge1 O2 . . 179.75(13)
O6 Ge1 O2 . . 89.21(10)
O6 Ge2 O5 1_565 . 117.45(8)
O6 Ge2 O8 1_565 . 109.83(13)
O5 Ge2 O8 . . 109.47(9)
O6 Ge2 O7 1_565 . 108.31(9)
O5 Ge2 O7 . . 106.58(12)
O8 Ge2 O7 . . 104.33(10)
O1 Ge3 O2 2 2_565 120.61(14)
O1 Ge3 O9 2 . 104.46(9)
O2 Ge3 O9 2_565 . 107.00(9)
O1 Ge3 O7 2 . 107.53(10)
O2 Ge3 O7 2_565 . 111.27(9)
O9 Ge3 O7 . . 104.65(11)
O4 Ge4 O3 4_565 4_575 119.52(13)
O4 Ge4 O9 4_565 . 104.82(9)
O3 Ge4 O9 4_575 . 102.35(9)
O4 Ge4 O8 4_565 3_576 107.24(11)
O3 Ge4 O8 4_575 3_576 112.54(9)
O9 Ge4 O8 . 3_576 109.74(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Li1 O5 . 1.883(6)
Li1 O6 2 1.892(6)
Li1 O1 2 1.941(6)
Li1 O4 . 1.954(6)
Li1 O7 1_545 2.140(5)
Li2 O2 4_565 1.978(6)
Li2 O3 4_565 2.054(6)
Li2 O9 . 2.166(6)
Li2 O8 . 2.490(6)
Ge1 O1 . 1.844(3)
Ge1 O3 . 1.864(2)
Ge1 O4 . 1.872(2)
Ge1 O5 . 1.873(2)
Ge1 O6 . 1.886(2)
Ge1 O2 . 1.888(2)
Ge2 O6 1_565 1.729(2)
Ge2 O5 . 1.735(2)
Ge2 O8 . 1.777(2)
Ge2 O7 . 1.789(2)
Ge3 O1 2 1.731(2)
Ge3 O2 2_565 1.743(2)
Ge3 O9 . 1.768(2)
Ge3 O7 . 1.783(2)
Ge4 O4 4_565 1.725(2)
Ge4 O3 4_575 1.744(2)
Ge4 O9 . 1.771(2)
Ge4 O8 3_576 1.786(2)
