# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_170508lym_0m
_database_code_depnum_ccdc_archive 'CCDC 1817602'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Li2Ge(IO3)6
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge I6 Li2 O18'
_chemical_formula_weight         1135.87

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 0.0060 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   9.1879(12)
_cell_length_b                   9.1879(12)
_cell_length_c                   5.2332(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     382.59(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2274
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      30.52

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.930
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    14.206
_shelx_estimated_absorpt_T_min   0.331
_shelx_estimated_absorpt_T_max   0.600
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2208
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.560
_diffrn_reflns_theta_max         24.917
_diffrn_reflns_theta_full        24.917
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             453
_reflns_number_gt                452
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+5.2181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 192 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         453
_refine_ls_number_parameters     45
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0556
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.6667 0.3333 0.215(5) 0.001(7) Uani 1 3 d S TU P . .
I1 I 0.31672(9) 0.35025(9) 0.2821(5) 0.0153(4) Uani 1 1 d . . . . .
Ge1 Ge 0.0000 0.0000 0.1468(12) 0.0103(10) Uani 0.5 3 d S T P . .
O1 O 0.1864(13) 0.1310(14) 0.398(3) 0.033(3) Uani 1 1 d . . . . .
O2 O 0.2372(14) 0.4468(13) 0.491(2) 0.015(2) Uani 1 1 d . . . . .
O3 O 0.4998(13) 0.3874(14) 0.4509(19) 0.014(2) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Li1 O2 2.111(19) 6_654 ?
Li1 O2 2.111(19) 5_554 ?
Li1 O2 2.111(19) 2_664 ?
Li1 O3 2.208(19) . ?
Li1 O3 2.208(19) 4_665 ?
Li1 O3 2.208(19) 3_655 ?
Li1 I1 3.314(3) 3_655 ?
Li1 I1 3.314(3) 4_665 ?
I1 O3 1.776(10) . ?
I1 O2 1.778(10) . ?
I1 O1 1.857(12) . ?
Ge1 O1 2.003(13) 5_554 ?
Ge1 O1 2.003(13) 2_554 ?
Ge1 O1 2.003(13) 6_554 ?
Ge1 O1 2.012(14) 3 ?
Ge1 O1 2.012(14) . ?
Ge1 O1 2.012(14) 4 ?
Ge1 Ge1 2.6166(4) 2 ?
Ge1 Ge1 2.6166(4) 2_554 ?
O1 Ge1 2.003(13) 2 ?
O2 Li1 2.111(19) 2_665 ?

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 Li1 O2 92.0(10) 6_654 5_554 ?
O2 Li1 O2 92.0(10) 6_654 2_664 ?
O2 Li1 O2 92.0(10) 5_554 2_664 ?
O2 Li1 O3 169.8(4) 6_654 . ?
O2 Li1 O3 81.2(4) 5_554 . ?
O2 Li1 O3 95.8(4) 2_664 . ?
O2 Li1 O3 95.8(4) 6_654 4_665 ?
O2 Li1 O3 169.8(4) 5_554 4_665 ?
O2 Li1 O3 81.2(4) 2_664 4_665 ?
O3 Li1 O3 91.9(9) . 4_665 ?
O2 Li1 O3 81.2(4) 6_654 3_655 ?
O2 Li1 O3 95.8(4) 5_554 3_655 ?
O2 Li1 O3 169.8(4) 2_664 3_655 ?
O3 Li1 O3 91.9(9) . 3_655 ?
O3 Li1 O3 91.9(9) 4_665 3_655 ?
O2 Li1 I1 52.7(3) 6_654 3_655 ?
O2 Li1 I1 88.0(3) 5_554 3_655 ?
O2 Li1 I1 144.7(9) 2_664 3_655 ?
O3 Li1 I1 119.0(7) . 3_655 ?
O3 Li1 I1 101.9(5) 4_665 3_655 ?
O3 Li1 I1 29.8(3) 3_655 3_655 ?
O2 Li1 I1 88.0(3) 6_654 4_665 ?
O2 Li1 I1 144.7(9) 5_554 4_665 ?
O2 Li1 I1 52.7(3) 2_664 4_665 ?
O3 Li1 I1 101.9(5) . 4_665 ?
O3 Li1 I1 29.8(3) 4_665 4_665 ?
O3 Li1 I1 119.0(7) 3_655 4_665 ?
I1 Li1 I1 118.90(17) 3_655 4_665 ?
O3 I1 O2 100.7(5) . . ?
O3 I1 O1 94.6(5) . . ?
O2 I1 O1 97.9(5) . . ?
O1 Ge1 O1 82.3(6) 5_554 2_554 ?
O1 Ge1 O1 82.3(6) 5_554 6_554 ?
O1 Ge1 O1 82.3(6) 2_554 6_554 ?
O1 Ge1 O1 179.7(7) 5_554 3 ?
O1 Ge1 O1 97.9(3) 2_554 3 ?
O1 Ge1 O1 97.9(3) 6_554 3 ?
O1 Ge1 O1 97.9(3) 5_554 . ?
O1 Ge1 O1 179.7(7) 2_554 . ?
O1 Ge1 O1 97.9(3) 6_554 . ?
O1 Ge1 O1 81.9(6) 3 . ?
O1 Ge1 O1 97.9(3) 5_554 4 ?
O1 Ge1 O1 97.9(3) 2_554 4 ?
O1 Ge1 O1 179.7(7) 6_554 4 ?
O1 Ge1 O1 81.9(6) 3 4 ?
O1 Ge1 O1 81.9(6) . 4 ?
O1 Ge1 Ge1 130.5(4) 5_554 2 ?
O1 Ge1 Ge1 130.5(4) 2_554 2 ?
O1 Ge1 Ge1 130.5(4) 6_554 2 ?
O1 Ge1 Ge1 49.2(4) 3 2 ?
O1 Ge1 Ge1 49.2(4) . 2 ?
O1 Ge1 Ge1 49.2(4) 4 2 ?
O1 Ge1 Ge1 49.5(4) 5_554 2_554 ?
O1 Ge1 Ge1 49.5(4) 2_554 2_554 ?
O1 Ge1 Ge1 49.5(4) 6_554 2_554 ?
O1 Ge1 Ge1 130.8(4) 3 2_554 ?
O1 Ge1 Ge1 130.8(4) . 2_554 ?
O1 Ge1 Ge1 130.8(4) 4 2_554 ?
Ge1 Ge1 Ge1 180.0 2 2_554 ?
I1 O1 Ge1 139.3(7) . 2 ?
I1 O1 Ge1 109.2(7) . . ?
Ge1 O1 Ge1 81.3(4) 2 . ?
I1 O2 Li1 137.7(6) . 2_665 ?
I1 O3 Li1 112.1(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 I1 O1 Ge1 105.5(11) . . . 2 ?
O2 I1 O1 Ge1 4.1(12) . . . 2 ?
O3 I1 O1 Ge1 -155.2(6) . . . . ?
O2 I1 O1 Ge1 103.3(6) . . . . ?
O3 I1 O2 Li1 40.9(13) . . . 2_665 ?
O1 I1 O2 Li1 137.1(12) . . . 2_665 ?
O2 I1 O3 Li1 -167.8(6) . . . . ?
O1 I1 O3 Li1 93.2(7) . . . . ?

_refine_diff_density_max         2.164
_refine_diff_density_min         -2.121
_refine_diff_density_rms         0.347



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_171120b_0m
_database_code_depnum_ccdc_archive 'CCDC 1817627'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge I6 O18 Rb2'
_chemical_formula_weight         1292.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   11.3325(11)
_cell_length_b                   11.3325(11)
_cell_length_c                   11.4291(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1271.1(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2492
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      31.67

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.067
_exptl_crystal_F_000             1704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    18.537
_shelx_estimated_absorpt_T_min   0.259
_shelx_estimated_absorpt_T_max   0.259
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4659
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.736
_diffrn_reflns_theta_max         32.170
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             952
_reflns_number_gt                899
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0194P)²+6.7631P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00155(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         952
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_restrained_S_all      1.232
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.64123(2) 0.91888(2) 0.06057(2) 0.00823(9) Uani 1 1 d . . . . .
Rb1 Rb 1.0000 1.0000 0.16574(6) 0.01605(14) Uani 1 3 d S T P . .
Ge1 Ge 1.0000 1.0000 0.5000 0.00769(18) Uani 1 6 d S T P . .
O3 O 0.7250(3) 0.8663(3) -0.0420(3) 0.0168(6) Uani 1 1 d . . . . .
O1 O 0.7119(3) 0.9024(3) 0.1964(2) 0.0168(5) Uani 1 1 d . . . . .
O4 O 0.4855(3) 0.7457(3) 0.0655(2) 0.0120(5) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
I1 O3 1.788(3) . ?
I1 O1 1.799(3) . ?
I1 O4 1.872(3) . ?
I1 Rb1 4.1439(5) 7_444 ?
Rb1 O1 2.898(3) 3_675 ?
Rb1 O1 2.898(3) 2_765 ?
Rb1 O1 2.898(3) . ?
Rb1 O3 3.048(3) 12_655 ?
Rb1 O3 3.048(3) 10_775 ?
Rb1 O3 3.048(3) 11_565 ?
Rb1 O4 3.054(3) 4 ?
Rb1 O4 3.054(3) 6_565 ?
Rb1 O4 3.054(3) 5_665 ?
Rb1 O3 3.595(3) 2_765 ?
Rb1 O3 3.595(3) 3_675 ?
Rb1 O3 3.595(3) . ?
Ge1 O4 1.889(3) 18_655 ?
Ge1 O4 1.889(3) 6_565 ?
Ge1 O4 1.889(3) 16_665 ?
Ge1 O4 1.889(3) 4 ?
Ge1 O4 1.889(3) 17 ?
Ge1 O4 1.889(2) 5_665 ?
Ge1 Rb1 3.8203(8) 10_776 ?
O3 Rb1 3.048(3) 10_775 ?
O4 Ge1 1.889(2) 7_444 ?
O4 Rb1 3.054(3) 7_444 ?

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
O3 I1 O1 101.15(14) . . ?
O3 I1 O4 92.82(12) . . ?
O1 I1 O4 95.78(13) . . ?
O3 I1 Rb1 76.20(10) . 7_444 ?
O1 I1 Rb1 137.45(9) . 7_444 ?
O4 I1 Rb1 42.99(8) . 7_444 ?
O1 Rb1 O1 118.56(2) 3_675 2_765 ?
O1 Rb1 O1 118.56(2) 3_675 . ?
O1 Rb1 O1 118.56(2) 2_765 . ?
O1 Rb1 O3 157.37(8) 3_675 12_655 ?
O1 Rb1 O3 59.68(8) 2_765 12_655 ?
O1 Rb1 O3 75.54(8) . 12_655 ?
O1 Rb1 O3 59.68(8) 3_675 10_775 ?
O1 Rb1 O3 75.54(8) 2_765 10_775 ?
O1 Rb1 O3 157.37(8) . 10_775 ?
O3 Rb1 O3 100.19(7) 12_655 10_775 ?
O1 Rb1 O3 75.54(8) 3_675 11_565 ?
O1 Rb1 O3 157.37(8) 2_765 11_565 ?
O1 Rb1 O3 59.68(8) . 11_565 ?
O3 Rb1 O3 100.19(7) 12_655 11_565 ?
O3 Rb1 O3 100.19(7) 10_775 11_565 ?
O1 Rb1 O4 64.57(8) 3_675 4 ?
O1 Rb1 O4 75.11(7) 2_765 4 ?
O1 Rb1 O4 111.69(7) . 4 ?
O3 Rb1 O4 129.46(7) 12_655 4 ?
O3 Rb1 O4 88.38(8) 10_775 4 ?
O3 Rb1 O4 127.36(8) 11_565 4 ?
O1 Rb1 O4 111.69(7) 3_675 6_565 ?
O1 Rb1 O4 64.57(8) 2_765 6_565 ?
O1 Rb1 O4 75.11(7) . 6_565 ?
O3 Rb1 O4 88.38(8) 12_655 6_565 ?
O3 Rb1 O4 127.37(8) 10_775 6_565 ?
O3 Rb1 O4 129.46(7) 11_565 6_565 ?
O4 Rb1 O4 50.13(8) 4 6_565 ?
O1 Rb1 O4 75.11(7) 3_675 5_665 ?
O1 Rb1 O4 111.70(7) 2_765 5_665 ?
O1 Rb1 O4 64.57(8) . 5_665 ?
O3 Rb1 O4 127.37(8) 12_655 5_665 ?
O3 Rb1 O4 129.46(7) 10_775 5_665 ?
O3 Rb1 O4 88.38(8) 11_565 5_665 ?
O4 Rb1 O4 50.12(8) 4 5_665 ?
O4 Rb1 O4 50.12(8) 6_565 5_665 ?
O1 Rb1 O3 109.83(7) 3_675 2_765 ?
O1 Rb1 O3 49.09(7) 2_765 2_765 ?
O1 Rb1 O3 123.75(8) . 2_765 ?
O3 Rb1 O3 50.28(3) 12_655 2_765 ?
O3 Rb1 O3 50.28(3) 10_775 2_765 ?
O3 Rb1 O3 111.02(6) 11_565 2_765 ?
O4 Rb1 O3 113.87(7) 4 2_765 ?
O4 Rb1 O3 112.35(6) 6_565 2_765 ?
O4 Rb1 O3 160.57(6) 5_665 2_765 ?
O1 Rb1 O3 49.09(7) 3_675 3_675 ?
O1 Rb1 O3 123.75(8) 2_765 3_675 ?
O1 Rb1 O3 109.83(7) . 3_675 ?
O3 Rb1 O3 111.02(6) 12_655 3_675 ?
O3 Rb1 O3 50.28(3) 10_775 3_675 ?
O3 Rb1 O3 50.28(3) 11_565 3_675 ?
O4 Rb1 O3 112.35(7) 4 3_675 ?
O4 Rb1 O3 160.57(6) 6_565 3_675 ?
O4 Rb1 O3 113.87(7) 5_665 3_675 ?
O3 Rb1 O3 81.13(7) 2_765 3_675 ?
O1 Rb1 O3 123.75(8) 3_675 . ?
O1 Rb1 O3 109.83(7) 2_765 . ?
O1 Rb1 O3 49.09(7) . . ?
O3 Rb1 O3 50.28(3) 12_655 . ?
O3 Rb1 O3 111.02(6) 10_775 . ?
O3 Rb1 O3 50.28(3) 11_565 . ?
O4 Rb1 O3 160.57(6) 4 . ?
O4 Rb1 O3 113.87(7) 6_565 . ?
O4 Rb1 O3 112.35(7) 5_665 . ?
O3 Rb1 O3 81.13(7) 2_765 . ?
O3 Rb1 O3 81.13(7) 3_675 . ?
O4 Ge1 O4 180.0 18_655 6_565 ?
O4 Ge1 O4 86.44(12) 18_655 16_665 ?
O4 Ge1 O4 93.56(12) 6_565 16_665 ?
O4 Ge1 O4 93.56(12) 18_655 4 ?
O4 Ge1 O4 86.44(12) 6_565 4 ?
O4 Ge1 O4 180.0 16_665 4 ?
O4 Ge1 O4 86.43(12) 18_655 17 ?
O4 Ge1 O4 93.57(12) 6_565 17 ?
O4 Ge1 O4 86.43(12) 16_665 17 ?
O4 Ge1 O4 93.57(12) 4 17 ?
O4 Ge1 O4 93.57(12) 18_655 5_665 ?
O4 Ge1 O4 86.43(12) 6_565 5_665 ?
O4 Ge1 O4 93.57(12) 16_665 5_665 ?
O4 Ge1 O4 86.43(12) 4 5_665 ?
O4 Ge1 O4 180.0 17 5_665 ?
O4 Ge1 Rb1 52.25(8) 18_655 10_776 ?
O4 Ge1 Rb1 127.75(8) 6_565 10_776 ?
O4 Ge1 Rb1 52.25(8) 16_665 10_776 ?
O4 Ge1 Rb1 127.75(8) 4 10_776 ?
O4 Ge1 Rb1 52.25(8) 17 10_776 ?
O4 Ge1 Rb1 127.75(8) 5_665 10_776 ?
O4 Ge1 Rb1 127.75(8) 18_655 . ?
O4 Ge1 Rb1 52.25(8) 6_565 . ?
O4 Ge1 Rb1 127.75(8) 16_665 . ?
O4 Ge1 Rb1 52.25(8) 4 . ?
O4 Ge1 Rb1 127.75(8) 17 . ?
O4 Ge1 Rb1 52.25(8) 5_665 . ?
Rb1 Ge1 Rb1 180.0 10_776 . ?
I1 O3 Rb1 136.04(14) . 10_775 ?
I1 O3 Rb1 85.37(10) . . ?
Rb1 O3 Rb1 68.98(6) 10_775 . ?
I1 O1 Rb1 109.33(12) . . ?
I1 O4 Ge1 132.36(14) . 7_444 ?
I1 O4 Rb1 112.30(11) . 7_444 ?
Ge1 O4 Rb1 98.46(10) 7_444 7_444 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 I1 O3 Rb1 -82.9(2) . . . 10_775 ?
O4 I1 O3 Rb1 -179.3(2) . . . 10_775 ?
Rb1 I1 O3 Rb1 140.7(2) 7_444 . . 10_775 ?
O1 I1 O3 Rb1 -29.90(11) . . . . ?
O4 I1 O3 Rb1 -126.36(9) . . . . ?
Rb1 I1 O3 Rb1 -166.35(6) 7_444 . . . ?
O3 I1 O1 Rb1 40.80(15) . . . . ?
O4 I1 O1 Rb1 134.83(12) . . . . ?
Rb1 I1 O1 Rb1 122.48(9) 7_444 . . . ?
O3 I1 O4 Ge1 167.7(2) . . . 7_444 ?
O1 I1 O4 Ge1 66.2(2) . . . 7_444 ?
Rb1 I1 O4 Ge1 -126.1(3) 7_444 . . 7_444 ?
O3 I1 O4 Rb1 -66.24(13) . . . 7_444 ?
O1 I1 O4 Rb1 -167.75(13) . . . 7_444 ?

_refine_diff_density_max         1.083
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.230



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_170508LYM22_0m
_database_code_depnum_ccdc_archive 'CCDC 1817626'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge I6 K2 O18'
_chemical_formula_weight         1200.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 '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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   11.1450(17)
_cell_length_b                   11.1450(17)
_cell_length_c                   11.3101(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1216.6(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2320
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.914
_exptl_crystal_F_000             1596
_exptl_transmission_factor_min   0.3111
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    13.918
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2979
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.774
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             668
_reflns_number_gt                659
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+13.7134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0047(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         668
_refine_ls_number_parameters     43
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0258
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_restrained_S_all      1.329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.07806(3) 0.72321(3) 0.05989(3) 0.00486(17) Uani 1 1 d . . . . .
Ge1 Ge 0.3333 0.6667 0.1667 0.0039(3) Uani 1 6 d S T P . .
K1 K 0.3333 0.6667 -0.1614(2) 0.0155(4) Uani 1 3 d S T P . .
O2 O 0.0970(4) 0.8153(4) 0.1957(4) 0.0127(8) Uani 1 1 d . U . . .
O1 O 0.1293(4) 0.8596(4) -0.0464(4) 0.0116(8) Uani 1 1 d . U . . .
O3 O 0.1785(4) 0.5898(4) 0.2677(3) 0.0091(7) Uani 1 1 d . U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
I1 O1 1.793(4) . ?
I1 O2 1.800(4) . ?
I1 O3 1.881(4) 14_455 ?
I1 O1 2.480(4) 11_455 ?
I1 K1 3.8161(10) 4_455 ?
I1 K1 4.0679(15) . ?
Ge1 O3 1.881(4) 15 ?
Ge1 O3 1.881(4) 13_565 ?
Ge1 O3 1.881(4) 3_565 ?
Ge1 O3 1.881(4) 2_665 ?
Ge1 O3 1.882(4) 14_455 ?
Ge1 O3 1.882(4) . ?
Ge1 K1 3.710(2) . ?
Ge1 K1 3.710(2) 13_565 ?
K1 O2 2.776(4) 9_454 ?
K1 O2 2.776(4) 8_664 ?
K1 O2 2.776(4) 7_544 ?
K1 O1 2.966(4) 16_564 ?
K1 O1 2.966(4) 17_444 ?
K1 O1 2.966(4) 18_654 ?
K1 O3 2.971(4) 13_565 ?
K1 O3 2.971(4) 15 ?
K1 O3 2.971(4) 14_455 ?
K1 I1 3.8161(10) 9_454 ?
K1 I1 3.8161(10) 8_664 ?
O2 K1 2.776(4) 4_455 ?
O1 I1 2.480(4) 12_665 ?
O1 K1 2.966(4) 16_564 ?
O3 I1 1.881(4) 15 ?
O3 K1 2.971(4) 13_565 ?

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
O1 I1 O2 101.07(19) . . ?
O1 I1 O3 92.71(17) . 14_455 ?
O2 I1 O3 94.76(17) . 14_455 ?
O1 I1 O1 80.39(19) . 11_455 ?
O2 I1 O1 82.63(15) . 11_455 ?
O3 I1 O1 171.96(14) 14_455 11_455 ?
O1 I1 K1 69.01(13) . 4_455 ?
O2 I1 K1 42.70(13) . 4_455 ?
O3 I1 K1 122.66(11) 14_455 4_455 ?
O1 I1 K1 50.98(9) 11_455 4_455 ?
O1 I1 K1 76.59(13) . . ?
O2 I1 K1 136.18(12) . . ?
O3 I1 K1 42.62(12) 14_455 . ?
O1 I1 K1 137.81(10) 11_455 . ?
K1 I1 K1 142.12(3) 4_455 . ?
O3 Ge1 O3 86.93(17) 15 13_565 ?
O3 Ge1 O3 180.00(19) 15 3_565 ?
O3 Ge1 O3 93.07(17) 13_565 3_565 ?
O3 Ge1 O3 93.08(17) 15 2_665 ?
O3 Ge1 O3 93.08(17) 13_565 2_665 ?
O3 Ge1 O3 86.93(17) 3_565 2_665 ?
O3 Ge1 O3 86.93(17) 15 14_455 ?
O3 Ge1 O3 86.93(17) 13_565 14_455 ?
O3 Ge1 O3 93.07(17) 3_565 14_455 ?
O3 Ge1 O3 180.0 2_665 14_455 ?
O3 Ge1 O3 93.07(17) 15 . ?
O3 Ge1 O3 180.0 13_565 . ?
O3 Ge1 O3 86.93(17) 3_565 . ?
O3 Ge1 O3 86.93(17) 2_665 . ?
O3 Ge1 O3 93.07(17) 14_455 . ?
O3 Ge1 K1 52.59(12) 15 . ?
O3 Ge1 K1 52.59(12) 13_565 . ?
O3 Ge1 K1 127.41(12) 3_565 . ?
O3 Ge1 K1 127.41(12) 2_665 . ?
O3 Ge1 K1 52.59(12) 14_455 . ?
O3 Ge1 K1 127.41(12) . . ?
O3 Ge1 K1 127.41(12) 15 13_565 ?
O3 Ge1 K1 127.41(12) 13_565 13_565 ?
O3 Ge1 K1 52.59(12) 3_565 13_565 ?
O3 Ge1 K1 52.59(12) 2_665 13_565 ?
O3 Ge1 K1 127.41(12) 14_455 13_565 ?
O3 Ge1 K1 52.59(12) . 13_565 ?
K1 Ge1 K1 180.0 . 13_565 ?
O2 K1 O2 119.07(3) 9_454 8_664 ?
O2 K1 O2 119.07(3) 9_454 7_544 ?
O2 K1 O2 119.07(3) 8_664 7_544 ?
O2 K1 O1 59.91(11) 9_454 16_564 ?
O2 K1 O1 74.39(11) 8_664 16_564 ?
O2 K1 O1 155.48(14) 7_544 16_564 ?
O2 K1 O1 74.39(11) 9_454 17_444 ?
O2 K1 O1 155.48(14) 8_664 17_444 ?
O2 K1 O1 59.91(11) 7_544 17_444 ?
O1 K1 O1 98.98(12) 16_564 17_444 ?
O2 K1 O1 155.48(14) 9_454 18_654 ?
O2 K1 O1 59.91(11) 8_664 18_654 ?
O2 K1 O1 74.39(11) 7_544 18_654 ?
O1 K1 O1 98.98(12) 16_564 18_654 ?
O1 K1 O1 98.98(12) 17_444 18_654 ?
O2 K1 O3 114.16(13) 9_454 13_565 ?
O2 K1 O3 66.08(11) 8_664 13_565 ?
O2 K1 O3 75.21(11) 7_544 13_565 ?
O1 K1 O3 128.83(11) 16_564 13_565 ?
O1 K1 O3 129.96(11) 17_444 13_565 ?
O1 K1 O3 88.41(11) 18_654 13_565 ?
O2 K1 O3 75.20(11) 9_454 15 ?
O2 K1 O3 114.16(13) 8_664 15 ?
O2 K1 O3 66.08(11) 7_544 15 ?
O1 K1 O3 129.96(11) 16_564 15 ?
O1 K1 O3 88.41(11) 17_444 15 ?
O1 K1 O3 128.83(11) 18_654 15 ?
O3 K1 O3 51.66(12) 13_565 15 ?
O2 K1 O3 66.08(11) 9_454 14_455 ?
O2 K1 O3 75.20(11) 8_664 14_455 ?
O2 K1 O3 114.16(13) 7_544 14_455 ?
O1 K1 O3 88.41(11) 16_564 14_455 ?
O1 K1 O3 128.83(11) 17_444 14_455 ?
O1 K1 O3 129.96(11) 18_654 14_455 ?
O3 K1 O3 51.66(12) 13_565 14_455 ?
O3 K1 O3 51.66(12) 15 14_455 ?
O2 K1 Ge1 84.43(10) 9_454 . ?
O2 K1 Ge1 84.43(10) 8_664 . ?
O2 K1 Ge1 84.43(10) 7_544 . ?
O1 K1 Ge1 118.61(9) 16_564 . ?
O1 K1 Ge1 118.61(9) 17_444 . ?
O1 K1 Ge1 118.61(9) 18_654 . ?
O3 K1 Ge1 30.20(7) 13_565 . ?
O3 K1 Ge1 30.20(7) 15 . ?
O3 K1 Ge1 30.20(7) 14_455 . ?
O2 K1 I1 26.10(8) 9_454 9_454 ?
O2 K1 I1 112.83(8) 8_664 9_454 ?
O2 K1 I1 127.35(8) 7_544 9_454 ?
O1 K1 I1 40.51(7) 16_564 9_454 ?
O1 K1 I1 69.42(8) 17_444 9_454 ?
O1 K1 I1 129.40(11) 18_654 9_454 ?
O3 K1 I1 137.65(9) 13_565 9_454 ?
O3 K1 I1 100.71(7) 15 9_454 ?
O3 K1 I1 86.34(7) 14_455 9_454 ?
Ge1 K1 I1 109.40(3) . 9_454 ?
O2 K1 I1 127.35(8) 9_454 8_664 ?
O2 K1 I1 26.10(8) 8_664 8_664 ?
O2 K1 I1 112.83(8) 7_544 8_664 ?
O1 K1 I1 69.42(8) 16_564 8_664 ?
O1 K1 I1 129.40(11) 17_444 8_664 ?
O1 K1 I1 40.51(7) 18_654 8_664 ?
O3 K1 I1 86.33(7) 13_565 8_664 ?
O3 K1 I1 137.65(9) 15 8_664 ?
O3 K1 I1 100.71(7) 14_455 8_664 ?
Ge1 K1 I1 109.40(3) . 8_664 ?
I1 K1 I1 109.55(3) 9_454 8_664 ?
I1 O2 K1 111.20(18) . 4_455 ?
I1 O1 I1 127.63(19) . 12_665 ?
I1 O1 K1 137.37(18) . 16_564 ?
I1 O1 K1 88.51(11) 12_665 16_564 ?
I1 O3 Ge1 131.2(2) 15 . ?
I1 O3 K1 111.98(16) 15 13_565 ?
Ge1 O3 K1 97.21(14) . 13_565 ?

_refine_diff_density_max         1.507
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.256



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_171019c_0m
_database_code_depnum_ccdc_archive 'CCDC 1817628'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cs2 Ge I6 O18'
_chemical_formula_weight         1387.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   11.562(3)
_cell_length_b                   11.562(3)
_cell_length_c                   11.640(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1347.6(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    2195
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      25.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.130
_exptl_crystal_F_000             1812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    16.096
_shelx_estimated_absorpt_T_min   0.296
_shelx_estimated_absorpt_T_max   0.325
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2760
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.683
_diffrn_reflns_theta_max         24.975
_diffrn_reflns_theta_full        24.975
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             522
_reflns_number_gt                508
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+0.4563P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00177(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         522
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0664
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_restrained_S_all      1.220
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.0000 0.0000 0.16158(6) 0.0178(3) Uani 1 3 d S T P . .
Ge1 Ge 0.3333 0.6667 0.1667 0.0110(4) Uani 1 6 d S T P . .
I2 I 0.27865(3) 0.36367(3) 0.06197(3) 0.0118(3) Uani 1 1 d . . . . .
O1 O 0.1980(4) 0.2971(4) 0.1967(4) 0.0217(10) Uani 1 1 d . . . . .
O2 O 0.2645(4) 0.5177(4) 0.0677(4) 0.0176(9) Uani 1 1 d . . . . .
O3 O 0.1421(4) 0.2808(4) -0.0358(4) 0.0224(10) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Cs1 O1 3.057(4) . ?
Cs1 O1 3.057(4) 2 ?
Cs1 O1 3.057(4) 3 ?
Cs1 O2 3.162(4) 5 ?
Cs1 O2 3.162(4) 4_445 ?
Cs1 O2 3.162(4) 6_455 ?
Cs1 O3 3.170(4) 12 ?
Cs1 O3 3.170(4) 10 ?
Cs1 O3 3.170(4) 11 ?
Cs1 O3 3.630(4) 3 ?
Cs1 O3 3.630(4) 2 ?
Cs1 Cs1 3.7614(16) 10 ?
Ge1 O2 1.886(4) 15 ?
Ge1 O2 1.886(4) . ?
Ge1 O2 1.886(4) 3_565 ?
Ge1 O2 1.886(4) 2_665 ?
Ge1 O2 1.886(4) 14_455 ?
Ge1 O2 1.886(4) 13_565 ?
Ge1 Cs1 3.9392(12) 16 ?
Ge1 Cs1 3.9392(12) 7_554 ?
I2 O3 1.787(4) . ?
I2 O1 1.790(4) . ?
I2 O2 1.869(4) . ?
I2 Cs1 4.2261(9) 7_554 ?
O2 Cs1 3.162(4) 7_554 ?
O3 Cs1 3.170(4) 10 ?

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
O1 Cs1 O1 118.24(4) . 2 ?
O1 Cs1 O1 118.24(4) . 3 ?
O1 Cs1 O1 118.24(4) 2 3 ?
O1 Cs1 O2 63.93(11) . 5 ?
O1 Cs1 O2 109.72(11) 2 5 ?
O1 Cs1 O2 75.44(11) 3 5 ?
O1 Cs1 O2 109.72(11) . 4_445 ?
O1 Cs1 O2 75.44(11) 2 4_445 ?
O1 Cs1 O2 63.93(11) 3 4_445 ?
O2 Cs1 O2 48.28(12) 5 4_445 ?
O1 Cs1 O2 75.44(11) . 6_455 ?
O1 Cs1 O2 63.93(11) 2 6_455 ?
O1 Cs1 O2 109.72(11) 3 6_455 ?
O2 Cs1 O2 48.28(12) 5 6_455 ?
O2 Cs1 O2 48.28(12) 4_445 6_455 ?
O1 Cs1 O3 76.60(11) . 12 ?
O1 Cs1 O3 59.41(10) 2 12 ?
O1 Cs1 O3 157.82(12) 3 12 ?
O2 Cs1 O3 126.71(11) 5 12 ?
O2 Cs1 O3 129.41(10) 4_445 12 ?
O2 Cs1 O3 89.36(11) 6_455 12 ?
O1 Cs1 O3 157.82(12) . 10 ?
O1 Cs1 O3 76.60(11) 2 10 ?
O1 Cs1 O3 59.41(10) 3 10 ?
O2 Cs1 O3 129.41(10) 5 10 ?
O2 Cs1 O3 89.37(11) 4_445 10 ?
O2 Cs1 O3 126.71(11) 6_455 10 ?
O3 Cs1 O3 100.36(11) 12 10 ?
O1 Cs1 O3 59.41(10) . 11 ?
O1 Cs1 O3 157.82(12) 2 11 ?
O1 Cs1 O3 76.59(11) 3 11 ?
O2 Cs1 O3 89.37(11) 5 11 ?
O2 Cs1 O3 126.71(11) 4_445 11 ?
O2 Cs1 O3 129.41(10) 6_455 11 ?
O3 Cs1 O3 100.36(11) 12 11 ?
O3 Cs1 O3 100.36(11) 10 11 ?
O1 Cs1 O3 109.93(10) . 3 ?
O1 Cs1 O3 125.65(11) 2 3 ?
O1 Cs1 O3 47.93(11) 3 3 ?
O2 Cs1 O3 113.03(10) 5 3 ?
O2 Cs1 O3 111.03(10) 4_445 3 ?
O2 Cs1 O3 157.36(9) 6_455 3 ?
O3 Cs1 O3 113.24(8) 12 3 ?
O3 Cs1 O3 50.53(4) 10 3 ?
O3 Cs1 O3 50.53(4) 11 3 ?
O1 Cs1 O3 125.65(11) . 2 ?
O1 Cs1 O3 47.93(11) 2 2 ?
O1 Cs1 O3 109.93(10) 3 2 ?
O2 Cs1 O3 157.36(9) 5 2 ?
O2 Cs1 O3 113.03(10) 4_445 2 ?
O2 Cs1 O3 111.03(10) 6_455 2 ?
O3 Cs1 O3 50.53(4) 12 2 ?
O3 Cs1 O3 50.53(4) 10 2 ?
O3 Cs1 O3 113.24(8) 11 2 ?
O3 Cs1 O3 84.23(10) 3 2 ?
O1 Cs1 Cs1 97.68(8) . 10 ?
O1 Cs1 Cs1 97.68(8) 2 10 ?
O1 Cs1 Cs1 97.68(8) 3 10 ?
O2 Cs1 Cs1 151.82(7) 5 10 ?
O2 Cs1 Cs1 151.82(7) 4_445 10 ?
O2 Cs1 Cs1 151.82(7) 6_455 10 ?
O3 Cs1 Cs1 62.49(9) 12 10 ?
O3 Cs1 Cs1 62.49(9) 10 10 ?
O3 Cs1 Cs1 62.49(9) 11 10 ?
O3 Cs1 Cs1 50.75(7) 3 10 ?
O3 Cs1 Cs1 50.75(7) 2 10 ?
O2 Ge1 O2 93.43(18) 15 . ?
O2 Ge1 O2 180.0 15 3_565 ?
O2 Ge1 O2 86.58(18) . 3_565 ?
O2 Ge1 O2 93.43(18) 15 2_665 ?
O2 Ge1 O2 86.58(18) . 2_665 ?
O2 Ge1 O2 86.58(18) 3_565 2_665 ?
O2 Ge1 O2 86.58(18) 15 14_455 ?
O2 Ge1 O2 93.43(18) . 14_455 ?
O2 Ge1 O2 93.42(18) 3_565 14_455 ?
O2 Ge1 O2 180.0 2_665 14_455 ?
O2 Ge1 O2 86.58(18) 15 13_565 ?
O2 Ge1 O2 180.0 . 13_565 ?
O2 Ge1 O2 93.42(18) 3_565 13_565 ?
O2 Ge1 O2 93.43(18) 2_665 13_565 ?
O2 Ge1 O2 86.57(18) 14_455 13_565 ?
O2 Ge1 Cs1 52.35(13) 15 16 ?
O2 Ge1 Cs1 127.65(13) . 16 ?
O2 Ge1 Cs1 127.65(13) 3_565 16 ?
O2 Ge1 Cs1 127.65(13) 2_665 16 ?
O2 Ge1 Cs1 52.35(13) 14_455 16 ?
O2 Ge1 Cs1 52.35(13) 13_565 16 ?
O2 Ge1 Cs1 127.65(13) 15 7_554 ?
O2 Ge1 Cs1 52.35(13) . 7_554 ?
O2 Ge1 Cs1 52.35(13) 3_565 7_554 ?
O2 Ge1 Cs1 52.35(13) 2_665 7_554 ?
O2 Ge1 Cs1 127.65(13) 14_455 7_554 ?
O2 Ge1 Cs1 127.65(13) 13_565 7_554 ?
Cs1 Ge1 Cs1 180.0 16 7_554 ?
O3 I2 O1 101.3(2) . . ?
O3 I2 O2 93.39(16) . . ?
O1 I2 O2 95.95(19) . . ?
O3 I2 Cs1 76.15(14) . 7_554 ?
O1 I2 Cs1 138.63(13) . 7_554 ?
O2 I2 Cs1 44.04(13) . 7_554 ?
I2 O1 Cs1 107.61(18) . . ?
I2 O2 Ge1 134.0(2) . . ?
I2 O2 Cs1 111.70(17) . 7_554 ?
Ge1 O2 Cs1 99.47(15) . 7_554 ?
I2 O3 Cs1 135.23(18) . 10 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 I2 O1 Cs1 40.38(18) . . . . ?
O2 I2 O1 Cs1 135.05(16) . . . . ?
Cs1 I2 O1 Cs1 122.24(13) 7_554 . . . ?
O3 I2 O2 Ge1 164.9(3) . . . . ?
O1 I2 O2 Ge1 63.1(3) . . . . ?
Cs1 I2 O2 Ge1 -129.0(4) 7_554 . . . ?
O3 I2 O2 Cs1 -66.0(2) . . . 7_554 ?
O1 I2 O2 Cs1 -167.82(17) . . . 7_554 ?
O2 Ge1 O2 I2 -3.7(3) 15 . . . ?
O2 Ge1 O2 I2 176.4(3) 3_565 . . . ?
O2 Ge1 O2 I2 89.6(4) 2_665 . . . ?
O2 Ge1 O2 I2 -90.4(4) 14_455 . . . ?
Cs1 Ge1 O2 I2 -47.0(4) 16 . . . ?
Cs1 Ge1 O2 I2 133.0(4) 7_554 . . . ?
O2 Ge1 O2 Cs1 -136.62(8) 15 . . 7_554 ?
O2 Ge1 O2 Cs1 43.39(8) 3_565 . . 7_554 ?
O2 Ge1 O2 Cs1 -43.38(8) 2_665 . . 7_554 ?
O2 Ge1 O2 Cs1 136.62(8) 14_455 . . 7_554 ?
Cs1 Ge1 O2 Cs1 180.002(0) 16 . . 7_554 ?
O1 I2 O3 Cs1 -84.4(3) . . . 10 ?
O2 I2 O3 Cs1 178.8(3) . . . 10 ?
Cs1 I2 O3 Cs1 137.9(3) 7_554 . . 10 ?

_refine_diff_density_max         0.705
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.249



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_170719a_0m
_database_code_depnum_ccdc_archive 'CCDC 1817629'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ge I6 O18, H2 O, Ba'
_chemical_formula_sum            'Ba Ge H2 I6 O19'
_chemical_formula_weight         1277.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   11.3784(14)
_cell_length_b                   11.3784(14)
_cell_length_c                   11.3287(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1270.2(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4459
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      32.11

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.010
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    15.122
_shelx_estimated_absorpt_T_min   0.313
_shelx_estimated_absorpt_T_max   0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4437
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.740
_diffrn_reflns_theta_max         30.468
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1705
_reflns_number_gt                1703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0292P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0106(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.40(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1705
_refine_ls_number_parameters     84
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0531
_refine_ls_wR_factor_gt          0.0531
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.6667 0.3333 0.28637(6) 0.00974(18) Uani 1 3 d S T P . .
Ge1 Ge 0.6667 0.3333 0.71246(11) 0.0056(2) Uani 1 3 d S T P . .
I1 I 0.63852(5) 0.05777(5) 0.56050(3) 0.00622(13) Uani 1 1 d . . . . .
I2 I 0.36186(5) 0.08270(4) 0.80177(4) 0.00627(14) Uani 1 1 d . . . . .
O1 O 0.7279(7) 0.1503(7) 0.4312(5) 0.0157(12) Uani 1 1 d . . . . .
O2 O 0.5852(5) 0.1779(6) 0.6158(5) 0.0119(10) Uani 1 1 d . . . . .
O3 O 0.4742(6) -0.0581(6) 0.5041(6) 0.0150(11) Uani 1 1 d . . . . .
O4 O 0.5123(6) 0.2577(6) 0.8088(5) 0.0130(10) Uani 1 1 d . . . . .
O5 O 0.2966(6) 0.1027(6) 0.6648(5) 0.0161(11) Uani 1 1 d . . . . .
O6 O 0.2741(6) 0.1275(6) 0.9069(5) 0.0153(11) Uani 1 1 d . . . . .
O8 O 0.6667 0.3333 0.0559(9) 0.017(2) Uani 1 3 d S T P . .
H8 H 0.6478 0.3898 0.0318 0.026 Uiso 0.6667 1 d R U P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Ba1 O8 2.611(11) . ?
Ba1 O6 2.753(6) 4_554 ?
Ba1 O6 2.753(6) 6_554 ?
Ba1 O6 2.753(6) 5_554 ?
Ba1 O1 2.994(6) . ?
Ba1 O1 2.994(6) 2_655 ?
Ba1 O1 2.994(6) 3_665 ?
Ba1 O3 3.012(6) 8_544 ?
Ba1 O3 3.012(6) 7_554 ?
Ba1 O3 3.012(6) 9_654 ?
Ba1 H8 2.9863 . ?
Ge1 O4 1.872(6) . ?
Ge1 O4 1.872(6) 2_655 ?
Ge1 O4 1.872(6) 3_665 ?
Ge1 O2 1.884(6) 2_655 ?
Ge1 O2 1.884(6) . ?
Ge1 O2 1.884(5) 3_665 ?
I1 O3 1.783(6) . ?
I1 O1 1.794(5) . ?
I1 O2 1.860(5) . ?
I2 O5 1.784(6) . ?
I2 O6 1.784(6) . ?
I2 O4 1.869(6) . ?
O3 Ba1 3.012(6) 4_445 ?
O6 Ba1 2.753(6) 7_445 ?
O8 H8 0.8200 . ?

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
O8 Ba1 O6 79.05(13) . 4_554 ?
O8 Ba1 O6 79.05(13) . 6_554 ?
O6 Ba1 O6 116.48(8) 4_554 6_554 ?
O8 Ba1 O6 79.05(13) . 5_554 ?
O6 Ba1 O6 116.48(8) 4_554 5_554 ?
O6 Ba1 O6 116.48(8) 6_554 5_554 ?
O8 Ba1 O1 123.22(12) . . ?
O6 Ba1 O1 82.80(18) 4_554 . ?
O6 Ba1 O1 62.35(18) 6_554 . ?
O6 Ba1 O1 154.39(16) 5_554 . ?
O8 Ba1 O1 123.23(12) . 2_655 ?
O6 Ba1 O1 62.35(18) 4_554 2_655 ?
O6 Ba1 O1 154.39(16) 6_554 2_655 ?
O6 Ba1 O1 82.80(18) 5_554 2_655 ?
O1 Ba1 O1 92.85(16) . 2_655 ?
O8 Ba1 O1 123.23(12) . 3_665 ?
O6 Ba1 O1 154.39(16) 4_554 3_665 ?
O6 Ba1 O1 82.80(18) 6_554 3_665 ?
O6 Ba1 O1 62.35(18) 5_554 3_665 ?
O1 Ba1 O1 92.85(16) . 3_665 ?
O1 Ba1 O1 92.85(16) 2_655 3_665 ?
O8 Ba1 O3 64.22(12) . 8_544 ?
O6 Ba1 O3 143.24(17) 4_554 8_544 ?
O6 Ba1 O3 57.00(17) 6_554 8_544 ?
O6 Ba1 O3 59.71(18) 5_554 8_544 ?
O1 Ba1 O3 115.45(17) . 8_544 ?
O1 Ba1 O3 140.67(16) 2_655 8_544 ?
O1 Ba1 O3 60.77(16) 3_665 8_544 ?
O8 Ba1 O3 64.22(12) . 7_554 ?
O6 Ba1 O3 59.71(18) 4_554 7_554 ?
O6 Ba1 O3 143.24(17) 6_554 7_554 ?
O6 Ba1 O3 57.00(17) 5_554 7_554 ?
O1 Ba1 O3 140.67(16) . 7_554 ?
O1 Ba1 O3 60.77(16) 2_655 7_554 ?
O1 Ba1 O3 115.45(17) 3_665 7_554 ?
O3 Ba1 O3 102.50(15) 8_544 7_554 ?
O8 Ba1 O3 64.22(12) . 9_654 ?
O6 Ba1 O3 57.00(17) 4_554 9_654 ?
O6 Ba1 O3 59.71(18) 6_554 9_654 ?
O6 Ba1 O3 143.24(17) 5_554 9_654 ?
O1 Ba1 O3 60.76(16) . 9_654 ?
O1 Ba1 O3 115.45(17) 2_655 9_654 ?
O1 Ba1 O3 140.67(16) 3_665 9_654 ?
O3 Ba1 O3 102.49(15) 8_544 9_654 ?
O3 Ba1 O3 102.49(15) 7_554 9_654 ?
O8 Ba1 H8 15.0 . . ?
O6 Ba1 H8 83.5 4_554 . ?
O6 Ba1 H8 89.6 6_554 . ?
O6 Ba1 H8 64.5 5_554 . ?
O1 Ba1 H8 138.2 . . ?
O1 Ba1 H8 114.9 2_655 . ?
O1 Ba1 H8 114.9 3_665 . ?
O3 Ba1 H8 61.4 8_544 . ?
O3 Ba1 H8 54.2 7_554 . ?
O3 Ba1 H8 78.7 9_654 . ?
O4 Ge1 O4 89.4(3) . 2_655 ?
O4 Ge1 O4 89.4(3) . 3_665 ?
O4 Ge1 O4 89.4(3) 2_655 3_665 ?
O4 Ge1 O2 179.2(2) . 2_655 ?
O4 Ge1 O2 89.9(2) 2_655 2_655 ?
O4 Ge1 O2 91.0(3) 3_665 2_655 ?
O4 Ge1 O2 89.9(2) . . ?
O4 Ge1 O2 91.0(3) 2_655 . ?
O4 Ge1 O2 179.2(2) 3_665 . ?
O2 Ge1 O2 89.6(3) 2_655 . ?
O4 Ge1 O2 91.0(3) . 3_665 ?
O4 Ge1 O2 179.2(3) 2_655 3_665 ?
O4 Ge1 O2 89.9(2) 3_665 3_665 ?
O2 Ge1 O2 89.6(3) 2_655 3_665 ?
O2 Ge1 O2 89.6(3) . 3_665 ?
O3 I1 O1 102.6(3) . . ?
O3 I1 O2 93.3(3) . . ?
O1 I1 O2 98.1(3) . . ?
O5 I2 O6 102.5(3) . . ?
O5 I2 O4 96.9(3) . . ?
O6 I2 O4 90.7(3) . . ?
I1 O1 Ba1 126.5(3) . . ?
I1 O2 Ge1 134.2(3) . . ?
I1 O3 Ba1 115.4(3) . 4_445 ?
I2 O4 Ge1 127.9(3) . . ?
I2 O6 Ba1 128.7(3) . 7_445 ?
Ba1 O8 H8 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 I1 O1 Ba1 64.8(4) . . . . ?
O2 I1 O1 Ba1 -30.5(4) . . . . ?
O3 I1 O2 Ge1 170.2(5) . . . . ?
O1 I1 O2 Ge1 -86.5(5) . . . . ?
O4 Ge1 O2 I1 -127.4(5) . . . . ?
O4 Ge1 O2 I1 -37.9(5) 2_655 . . . ?
O2 Ge1 O2 I1 52.0(6) 2_655 . . . ?
O2 Ge1 O2 I1 141.6(3) 3_665 . . . ?
O1 I1 O3 Ba1 145.0(3) . . . 4_445 ?
O2 I1 O3 Ba1 -115.9(3) . . . 4_445 ?
O5 I2 O4 Ge1 -68.7(5) . . . . ?
O6 I2 O4 Ge1 -171.4(4) . . . . ?
O4 Ge1 O4 I2 -83.9(6) 2_655 . . . ?
O4 Ge1 O4 I2 -173.4(4) 3_665 . . . ?
O2 Ge1 O4 I2 7.1(4) . . . . ?
O2 Ge1 O4 I2 96.7(4) 3_665 . . . ?
O5 I2 O6 Ba1 63.8(4) . . . 7_445 ?
O4 I2 O6 Ba1 161.0(4) . . . 7_445 ?

_refine_diff_density_max         1.859
_refine_diff_density_min         -3.018
_refine_diff_density_rms         0.275



# start Validation Reply Form
_vrf_PLAT430_mo_170719a_0m       
;
PROBLEM: Short Inter D...A Contact  O3     ..  O6      ..       2.76 Ang.  
RESPONSE: A carefull check shows that the iner D...A contact
can be omitted.
;
# end Validation Reply Form




