#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324111.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_4324111
loop_
_publ_author_name
'Bing Guo'
'Andrew K. Inge'
'Charlotte Bonneau'
'Junliang Sun'
'Kirsten E. Christensen'
'Zhong-Yong Yuan'
'Xiaodong Zou'
_publ_section_title
;
 Investigation of the GeO2-1,6-Diaminohexane-Water-Pyridine-HF Phase
 Diagram Leading to the Discovery of Two Novel Layered Germanates with
 Extra-Large Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              201
_journal_page_last               207
_journal_paper_doi               10.1021/ic1017505
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Ge21 O51'
_chemical_formula_weight         2340.39
_chemical_name_common            SU-63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           185
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2'
_symmetry_space_group_name_H-M   'P 63 c m'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   28.794(2)
_cell_length_b                   28.794(2)
_cell_length_c                   20.603(4)
_cell_measurement_reflns_used    4988
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.58
_cell_volume                     14793(3)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_molecular_graphics    CrystalMake
_computing_publication_material  CrystalMake
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      106(2)
_diffrn_detector_area_resol_mean 12.613
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'MARCCD, MARDTB Phi-Axis Goniometer'
_diffrn_measurement_device_type  MarDTB
_diffrn_measurement_method       'profile data'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_orient_matrix_type
;  x  =  h UB
   coordinate system: 
     x from crystal towards source
     z vertical, towards goniometer base
     y so that x,y,z is right-handed
;
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_polarisn_norm  0.00
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90800
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51182
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        33.84
_diffrn_reflns_theta_max         33.84
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.353
_exptl_absorpt_correction_T_max  0.8835
_exptl_absorpt_correction_T_min  0.4491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
   Shape function based on spherical harmonics.
   Highest even and odd order for spherical harmonics:  8  and  1
   Point group:  622
   Friedel opposites are not equivalent.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       0.00314(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1507P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2422
_reflns_number_gt                5624
_reflns_number_total             8692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1017505_si_002_1.cif
_cod_data_source_block           SU-63
_cod_database_code               4324111
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.32589(7) 0.14236(7) 0.09572(13) 0.0721(6) Uani 1 1 d . . .
Ge2 Ge 0.27135(7) 0.20827(7) 0.13111(12) 0.0700(6) Uani 1 1 d . . .
Ge3 Ge 0.39000(7) 0.26538(7) 0.09720(14) 0.0773(7) Uani 1 1 d . . .
Ge4 Ge 0.41542(10) 0.23141(9) 0.23116(16) 0.0949(9) Uani 1 1 d . . .
Ge5 Ge 0.30078(10) 0.17279(9) 0.25938(14) 0.0857(7) Uani 1 1 d . . .
Ge6 Ge 0.28599(7) 0.06381(7) 0.21342(12) 0.0686(6) Uani 1 1 d D . .
Ge7 Ge 0.40521(7) 0.12431(7) 0.18191(15) 0.0852(8) Uani 1 1 d D . .
Ge8 Ge 0.46375(6) 0.06055(6) 0.13502(14) 0.0763(7) Uani 1 1 d . . .
Ge9 Ge 0.51158(9) 0.05822(13) 0.00080(16) 0.1067(10) Uani 1 1 d . . .
Ge10 Ge 0.61414(6) 0.06111(7) 0.04910(13) 0.0722(6) Uani 1 1 d . . .
Ge11 Ge 0.52619(8) 0.0000 0.15067(16) 0.0620(7) Uani 1 2 d S . .
O1 O 0.3123(4) 0.1118(3) 0.0162(6) 0.060(3) Uani 1 1 d . . .
O2 O 0.3432(3) 0.1802(3) 0.1693(6) 0.053(3) Uani 1 1 d . . .
O3 O 0.2682(5) 0.1562(5) 0.0874(7) 0.079(4) Uani 1 1 d . . .
O4 O 0.3739(5) 0.2070(5) 0.0595(7) 0.074(4) Uani 1 1 d . . .
O5 O 0.3864(4) 0.1246(4) 0.1050(4) 0.066(3) Uani 1 1 d D . .
O6 O 0.2797(5) 0.0745(4) 0.1344(5) 0.089(5) Uani 1 1 d D . .
O7 O 0.2208(6) 0.2208(6) 0.1092(10) 0.080(5) Uani 1 2 d S . .
O8 O 0.2630(5) 0.1941(5) 0.2157(7) 0.072(3) Uani 1 1 d . . .
O9 O 0.3306(5) 0.2693(5) 0.1225(7) 0.074(3) Uani 1 1 d . . .
O10 O 0.4270(5) 0.3211(6) 0.0393(9) 0.092(5) Uani 1 1 d . . .
O11 O 0.4311(4) 0.2779(4) 0.1607(6) 0.064(3) Uani 1 1 d . . .
O12 O 0.4655(7) 0.2743(7) 0.2820(10) 0.114(6) Uani 1 1 d . . .
O13 O 0.3653(5) 0.2184(5) 0.2830(8) 0.080(4) Uani 1 1 d . . .
O14 O 0.4386(5) 0.1845(5) 0.2234(7) 0.080(4) Uani 1 1 d . . .
O15 O 0.2742(6) 0.1749(6) 0.3363(7) 0.088(4) Uani 1 1 d . . .
O16 O 0.2708(5) 0.1020(5) 0.2643(7) 0.070(3) Uani 1 1 d . . .
O17 O 0.2421(5) 0.0000 0.2372(9) 0.067(5) Uani 1 2 d S . .
O18 O 0.3530(4) 0.0779(4) 0.2274(7) 0.068(3) Uani 1 1 d . . .
O19 O 0.4539(4) 0.1060(5) 0.1813(8) 0.084(4) Uani 1 1 d . . .
O20 O 0.4021(5) 0.0000 0.1247(11) 0.078(6) Uani 1 2 d S . .
O21 O 0.4852(4) 0.0869(5) 0.0511(8) 0.076(4) Uani 1 1 d . . .
O22 O 0.5122(4) 0.0537(5) 0.1746(9) 0.084(4) Uani 1 1 d . . .
O23 O 0.4710(9) 0.0000 -0.0471(13) 0.124(10) Uani 1 2 d S . .
O24 O 0.5112(6) 0.0981(8) -0.0643(9) 0.109(6) Uani 1 1 d . . .
O25 O 0.5808(6) 0.0892(7) 0.0070(10) 0.109(6) Uani 1 1 d . . .
O26 O 0.5016(5) 0.0000 0.0642(9) 0.062(4) Uani 1 2 d S . .
O27 O 0.6040(4) 0.0000 0.0184(8) 0.056(4) Uani 1 2 d S . .
O28 O 0.5984(4) 0.0545(4) 0.1269(7) 0.063(3) Uani 1 1 d . . .
O29 O 0.5484(5) 0.0000 0.2303(8) 0.061(4) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ge1 O1 173.1(5) . . ?
O2 Ge1 O4 83.5(6) . . ?
O1 Ge1 O4 89.8(6) . . ?
O2 Ge1 O3 87.4(5) . . ?
O1 Ge1 O3 91.3(6) . . ?
O4 Ge1 O3 92.6(6) . . ?
O2 Ge1 O6 96.3(5) . . ?
O1 Ge1 O6 90.5(4) . . ?
O4 Ge1 O6 176.4(5) . . ?
O3 Ge1 O6 91.0(6) . . ?
O2 Ge1 O5 93.4(4) . . ?
O1 Ge1 O5 88.1(4) . . ?
O4 Ge1 O5 89.3(4) . . ?
O3 Ge1 O5 178.0(5) . . ?
O6 Ge1 O5 87.2(4) . . ?
O3 Ge2 O7 111.3(7) . . ?
O3 Ge2 O9 115.2(6) . . ?
O7 Ge2 O9 105.5(7) . . ?
O3 Ge2 O8 111.9(6) . . ?
O7 Ge2 O8 105.8(8) . . ?
O9 Ge2 O8 106.4(6) . . ?
O11 Ge3 O4 112.6(6) . . ?
O11 Ge3 O9 110.0(6) . . ?
O4 Ge3 O9 112.8(6) . . ?
O11 Ge3 O10 106.1(6) . . ?
O4 Ge3 O10 108.6(7) . . ?
O9 Ge3 O10 106.2(6) . . ?
O13 Ge4 O12 95.3(9) . . ?
O13 Ge4 O14 119.5(7) . . ?
O12 Ge4 O14 95.9(7) . . ?
O13 Ge4 O11 121.7(6) . . ?
O12 Ge4 O11 98.2(8) . . ?
O14 Ge4 O11 115.1(6) . . ?
O13 Ge4 O2 78.7(6) . . ?
O12 Ge4 O2 172.2(6) . . ?
O14 Ge4 O2 91.5(4) . . ?
O11 Ge4 O2 81.0(4) . . ?
O13 Ge4 Ge5 31.5(5) . . ?
O12 Ge4 Ge5 126.7(7) . . ?
O14 Ge4 Ge5 108.8(4) . . ?
O11 Ge4 Ge5 111.5(3) . . ?
O2 Ge4 Ge5 47.6(3) . . ?
O13 Ge5 O8 120.1(6) . . ?
O13 Ge5 O15 92.3(7) . . ?
O8 Ge5 O15 95.3(7) . . ?
O13 Ge5 O16 125.4(6) . . ?
O8 Ge5 O16 113.8(6) . . ?
O15 Ge5 O16 91.1(7) . . ?
O13 Ge5 O2 80.1(5) . . ?
O8 Ge5 O2 86.8(6) . . ?
O15 Ge5 O2 172.1(6) . . ?
O16 Ge5 O2 95.0(5) . . ?
O13 Ge5 Ge4 30.6(5) . . ?
O8 Ge5 Ge4 114.7(5) . . ?
O15 Ge5 Ge4 122.7(5) . . ?
O16 Ge5 Ge4 115.8(4) . . ?
O2 Ge5 Ge4 49.8(2) . . ?
O6 Ge6 O17 112.8(7) . . ?
O6 Ge6 O16 112.7(6) . . ?
O17 Ge6 O16 103.0(7) . . ?
O6 Ge6 O18 108.5(6) . . ?
O17 Ge6 O18 109.6(6) . . ?
O16 Ge6 O18 110.3(6) . . ?
O5 Ge7 O18 111.3(6) . . ?
O5 Ge7 O19 108.0(7) . . ?
O18 Ge7 O19 107.2(6) . . ?
O5 Ge7 O14 118.7(6) . . ?
O18 Ge7 O14 110.1(7) . . ?
O19 Ge7 O14 100.4(6) . . ?
O22 Ge8 O19 105.8(7) . . ?
O22 Ge8 O20 114.7(6) . . ?
O19 Ge8 O20 110.1(6) . . ?
O22 Ge8 O21 111.4(6) . . ?
O19 Ge8 O21 110.2(6) . . ?
O20 Ge8 O21 104.7(8) . . ?
O21 Ge9 O25 112.2(7) . . ?
O21 Ge9 O24 89.8(7) . . ?
O25 Ge9 O24 95.8(8) . . ?
O21 Ge9 O23 123.1(9) . . ?
O25 Ge9 O23 124.5(10) . . ?
O24 Ge9 O23 88.7(10) . . ?
O21 Ge9 O26 95.4(6) . . ?
O25 Ge9 O26 91.7(7) . . ?
O24 Ge9 O26 168.5(8) . . ?
O23 Ge9 O26 79.9(8) . . ?
O21 Ge9 Ge9 114.6(4) . 11 ?
O25 Ge9 Ge9 116.4(6) . 11 ?
O24 Ge9 Ge9 124.2(7) . 11 ?
O23 Ge9 Ge9 35.6(7) . 11 ?
O26 Ge9 Ge9 44.3(4) . 11 ?
O28 Ge10 O10 110.0(7) . 2_655 ?
O28 Ge10 O27 109.7(6) . . ?
O10 Ge10 O27 107.1(6) 2_655 . ?
O28 Ge10 O25 110.5(7) . . ?
O10 Ge10 O25 104.0(7) 2_655 . ?
O27 Ge10 O25 115.3(8) . . ?
O29 Ge11 O22 89.0(7) . 11 ?
O29 Ge11 O22 89.0(7) . . ?
O22 Ge11 O22 92.9(7) 11 . ?
O29 Ge11 O26 179.6(7) . . ?
O22 Ge11 O26 90.7(7) 11 . ?
O22 Ge11 O26 90.7(7) . . ?
O29 Ge11 O28 89.6(5) . . ?
O22 Ge11 O28 177.6(5) 11 . ?
O22 Ge11 O28 89.1(5) . . ?
O26 Ge11 O28 90.7(5) . . ?
O29 Ge11 O28 89.6(5) . 11 ?
O22 Ge11 O28 89.1(5) 11 11 ?
O22 Ge11 O28 177.6(5) . 11 ?
O26 Ge11 O28 90.7(5) . 11 ?
O28 Ge11 O28 89.0(6) . 11 ?
Ge1 O2 Ge5 133.9(4) . . ?
Ge1 O2 Ge4 140.0(5) . . ?
Ge5 O2 Ge4 82.6(4) . . ?
Ge2 O3 Ge1 117.8(7) . . ?
Ge3 O4 Ge1 121.0(8) . . ?
Ge7 O5 Ge1 113.9(6) . . ?
Ge6 O6 Ge1 120.6(6) . . ?
Ge2 O7 Ge2 131.4(12) 10 . ?
Ge5 O8 Ge2 123.4(7) . . ?
Ge2 O9 Ge3 116.0(7) . . ?
Ge10 O10 Ge3 128.3(9) 3_665 . ?
Ge3 O11 Ge4 124.0(6) . . ?
Ge4 O13 Ge5 117.9(9) . . ?
Ge7 O14 Ge4 124.8(6) . . ?
Ge6 O16 Ge5 124.4(7) . . ?
Ge6 O17 Ge6 138.7(11) 11 . ?
Ge7 O18 Ge6 121.2(7) . . ?
Ge7 O19 Ge8 133.6(8) . . ?
Ge8 O20 Ge8 116.9(8) . 11 ?
Ge9 O21 Ge8 119.9(6) . . ?
Ge8 O22 Ge11 120.0(9) . . ?
Ge9 O23 Ge9 108.8(14) . 11 ?
Ge9 O25 Ge10 123.4(11) . . ?
Ge11 O26 Ge9 134.3(4) . 11 ?
Ge11 O26 Ge9 134.3(4) . . ?
Ge9 O26 Ge9 91.3(8) 11 . ?
Ge10 O27 Ge10 120.9(8) 11 . ?
Ge10 O28 Ge11 117.3(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O2 1.787(11) . ?
Ge1 O1 1.807(11) . ?
Ge1 O4 1.832(13) . ?
Ge1 O3 1.900(13) . ?
Ge1 O6 1.903(11) . ?
Ge1 O5 2.055(12) . ?
Ge2 O3 1.712(14) . ?
Ge2 O7 1.726(8) . ?
Ge2 O9 1.741(13) . ?
Ge2 O8 1.778(15) . ?
Ge3 O11 1.679(12) . ?
Ge3 O4 1.693(12) . ?
Ge3 O9 1.843(13) . ?
Ge3 O10 1.849(17) . ?
Ge4 O13 1.681(13) . ?
Ge4 O12 1.710(17) . ?
Ge4 O14 1.788(13) . ?
Ge4 O11 1.870(13) . ?
Ge4 O2 2.248(10) . ?
Ge4 Ge5 2.917(3) . ?
Ge5 O13 1.724(14) . ?
Ge5 O8 1.744(13) . ?
Ge5 O15 1.774(15) . ?
Ge5 O16 1.774(12) . ?
Ge5 O2 2.172(12) . ?
Ge6 O6 1.683(9) . ?
Ge6 O17 1.701(7) . ?
Ge6 O16 1.727(12) . ?
Ge6 O18 1.785(10) . ?
Ge7 O5 1.676(8) . ?
Ge7 O18 1.706(12) . ?
Ge7 O19 1.728(12) . ?
Ge7 O14 1.730(13) . ?
Ge8 O22 1.711(14) . ?
Ge8 O19 1.753(14) . ?
Ge8 O20 1.772(8) . ?
Ge8 O21 1.865(15) . ?
Ge9 O21 1.721(13) . ?
Ge9 O25 1.733(14) . ?
Ge9 O24 1.770(15) . ?
Ge9 O23 1.786(16) . ?
Ge9 O26 2.029(13) . ?
Ge9 Ge9 2.904(7) 11 ?
Ge10 O28 1.651(15) . ?
Ge10 O10 1.667(14) 2_655 ?
Ge10 O27 1.752(7) . ?
Ge10 O25 1.762(17) . ?
Ge11 O29 1.762(16) . ?
Ge11 O22 1.849(12) 11 ?
Ge11 O22 1.849(12) . ?
Ge11 O26 1.917(19) . ?
Ge11 O28 1.941(11) . ?
Ge11 O28 1.941(11) 11 ?
O7 Ge2 1.726(8) 10 ?
O10 Ge10 1.667(14) 3_665 ?
O17 Ge6 1.701(7) 11 ?
O20 Ge8 1.772(8) 11 ?
O23 Ge9 1.786(16) 11 ?
O26 Ge9 2.029(13) 11 ?
O27 Ge10 1.752(7) 11 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.015 -0.011 0.070 9390 563 ' '
