####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1545209'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-08-11 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         (NH4)2[GeF2(HPO4)2]
_chemical_formula_sum            'F2 Ge H10 N2 O8 P2'
_chemical_formula_weight         338.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.353(5)
_cell_length_b                   7.058(5)
_cell_length_c                   8.804(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.104(7)
_cell_angle_gamma                90
_cell_volume                     429.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2600
_cell_measurement_theta_min      2.950
_cell_measurement_theta_max      28.813

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_F_000             336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.013
_shelx_estimated_absorpt_T_min   0.532
_shelx_estimated_absorpt_T_max   0.766
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_process_details   'SMART (Bruker, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SMART (Bruker, 2001)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2600
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.950
_diffrn_reflns_theta_max         28.814
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1046
_reflns_number_gt                990
_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_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005) '
_computing_publication_material  
'SHELXL-2014/7 (Sheldrick, 2014) and WinGX (Farrugia, 2014)'
_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)+(0.0298P)²+0.5617P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1046
_refine_ls_number_parameters     90
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.096
_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
Ge1 Ge 0.0000 0.5000 0.0000 0.00822(13) Uani 1 2 d S . P . .
P1 P 0.15640(9) 0.64970(9) 0.35782(8) 0.01023(16) Uani 1 1 d . . . . .
F1 F -0.2515(2) 0.5517(2) -0.07761(19) 0.0135(3) Uani 1 1 d . . . . .
O2 O 0.0024(3) 0.5855(3) 0.1998(2) 0.0150(4) Uani 1 1 d . . . . .
O3 O -0.0442(3) 0.2500(3) 0.0476(2) 0.0157(4) Uani 1 1 d . . . . .
O4 O 0.3246(3) 0.7552(3) 0.3448(2) 0.0166(4) Uani 1 1 d . . . . .
O5 O 0.2373(3) 0.4664(3) 0.4581(3) 0.0168(4) Uani 1 1 d D . . . .
H5 H 0.155(6) 0.392(6) 0.455(7) 0.069(18) Uiso 1 1 d D . . . .
N1 N 0.4094(4) 0.1513(4) 0.3168(3) 0.0146(5) Uani 1 1 d D . . . .
H1 H 0.485(5) 0.164(6) 0.271(4) 0.032(11) Uiso 1 1 d D . . . .
H2 H 0.454(5) 0.189(5) 0.409(3) 0.029(10) Uiso 1 1 d D . . . .
H3 H 0.379(6) 0.041(3) 0.318(5) 0.034(11) Uiso 1 1 d D . . . .
H4 H 0.323(4) 0.221(5) 0.281(5) 0.032(11) Uiso 1 1 d 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
Ge1 F1 1.7749(19) 3_565 ?
Ge1 F1 1.7749(19) . ?
Ge1 O2 1.854(2) 3_565 ?
Ge1 O2 1.854(2) . ?
Ge1 O3 1.868(2) 3_565 ?
Ge1 O3 1.868(2) . ?
P1 O4 1.482(2) . ?
P1 O2 1.529(2) . ?
P1 O3 1.532(2) 2 ?
P1 O5 1.564(2) . ?
O3 P1 1.532(2) 2_545 ?
O5 H5 0.79(2) . ?
N1 H1 0.791(19) . ?
N1 H2 0.809(19) . ?
N1 H3 0.809(19) . ?
N1 H4 0.777(19) . ?

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
F1 Ge1 F1 180.0 3_565 . ?
F1 Ge1 O2 88.13(8) 3_565 3_565 ?
F1 Ge1 O2 91.87(8) . 3_565 ?
F1 Ge1 O2 91.87(8) 3_565 . ?
F1 Ge1 O2 88.13(8) . . ?
O2 Ge1 O2 180.0 3_565 . ?
F1 Ge1 O3 92.41(9) 3_565 3_565 ?
F1 Ge1 O3 87.59(9) . 3_565 ?
O2 Ge1 O3 92.30(9) 3_565 3_565 ?
O2 Ge1 O3 87.70(9) . 3_565 ?
F1 Ge1 O3 87.59(9) 3_565 . ?
F1 Ge1 O3 92.41(9) . . ?
O2 Ge1 O3 87.70(9) 3_565 . ?
O2 Ge1 O3 92.30(9) . . ?
O3 Ge1 O3 180.0 3_565 . ?
O4 P1 O2 117.08(12) . . ?
O4 P1 O3 115.47(12) . 2 ?
O2 P1 O3 105.21(12) . 2 ?
O4 P1 O5 107.07(13) . . ?
O2 P1 O5 106.70(13) . . ?
O3 P1 O5 104.29(12) 2 . ?
P1 O2 Ge1 136.22(13) . . ?
P1 O3 Ge1 136.56(12) 2_545 . ?
P1 O5 H5 113(4) . . ?
H1 N1 H2 111(4) . . ?
H1 N1 H3 111(4) . . ?
H2 N1 H3 109(4) . . ?
H1 N1 H4 110(4) . . ?
H2 N1 H4 101(4) . . ?
H3 N1 H4 115(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 F1 0.79(2) 2.63(5) 3.100(3) 120(4) 2_545
O5 H5 O2 0.79(2) 2.61(4) 3.253(3) 140(5) 2_545
O5 H5 O3 0.79(2) 2.16(3) 2.891(3) 155(5) 4_566
N1 H1 O4 0.791(19) 2.10(2) 2.881(3) 169(4) 2_645
N1 H2 O4 0.809(19) 2.25(2) 3.022(4) 159(4) 3_666
N1 H4 O5 0.777(19) 2.55(4) 3.030(3) 121(4) .
N1 H3 O4 0.809(19) 2.09(2) 2.893(4) 174(4) 1_545
N1 H4 F1 0.777(19) 2.33(3) 2.915(3) 133(4) 3_565
N1 H4 O2 0.777(19) 2.64(4) 3.017(4) 112(3) 2_545
N1 H4 O5 0.777(19) 2.55(4) 3.030(3) 121(4) .

_refine_diff_density_max         0.435
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1545206'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-08-11 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         Na2[GeF2(HPO4)2]
_chemical_formula_sum            'F2 Ge H2 Na2 O8 P2'
_chemical_formula_weight         348.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   10.372(8)
_cell_length_b                   8.562(7)
_cell_length_c                   4.483(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.939(10)
_cell_angle_gamma                90
_cell_volume                     398.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    919
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      28.30

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_F_000             336
_exptl_transmission_factor_min   0.73
_exptl_transmission_factor_max   0.80
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.420
_shelx_estimated_absorpt_T_min   0.538
_shelx_estimated_absorpt_T_max   0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SMART (Bruker, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1212
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         3.085
_diffrn_reflns_theta_max         28.651
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             507
_reflns_number_gt                497
_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  
'SHELXL-2014/7 (Sheldrick, 2014) and WinGX (Farrugia, 2014)'
_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)+(0.0201P)²+1.2084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         507
_refine_ls_number_parameters     44
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0552
_refine_ls_wR_factor_gt          0.0548
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.156
_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
Ge1 Ge 0.0000 0.5000 0.5000 0.00738(15) Uani 1 4 d S T P . .
P1 P 0.0000 0.24379(10) 0.0000 0.0082(2) Uani 1 2 d S T P . .
F1 F -0.15878(19) 0.5000 0.6563(4) 0.0112(4) Uani 1 2 d S T P . .
O1 O 0.06104(16) 0.3458(2) 0.7588(4) 0.0108(4) Uani 1 1 d . . . . .
O2 O 0.10877(18) 0.1451(2) 0.1350(4) 0.0147(4) Uani 1 1 d D . . . .
H2 H 0.108(6) 0.053(2) 0.125(14) 0.020(18) Uiso 0.5 1 d D . P . .
Na1 Na 0.2500 0.2500 0.5000 0.0188(4) Uani 1 2 d S . 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
Ge1 F1 1.800(2) . ?
Ge1 F1 1.800(2) 5_566 ?
Ge1 O1 1.8616(19) 6_565 ?
Ge1 O1 1.8616(19) 2_556 ?
Ge1 O1 1.8616(19) 5_566 ?
Ge1 O1 1.8616(19) . ?
Ge1 Na1 3.3623(19) 4_556 ?
Ge1 Na1 3.3623(19) 2_556 ?
Ge1 Na1 3.3623(19) . ?
Ge1 Na1 3.3623(19) 3_455 ?
P1 O2 1.5265(19) 2 ?
P1 O2 1.527(2) . ?
P1 O1 1.5348(19) 2_556 ?
P1 O1 1.5348(19) 1_554 ?
P1 Na1 3.4000(18) 2 ?
P1 Na1 3.4000(18) . ?
P1 Na1 3.4556(18) 2_556 ?
P1 Na1 3.4556(18) 1_554 ?
F1 Na1 2.4385(18) 2_556 ?
F1 Na1 2.4385(18) 3_455 ?
O1 P1 1.5347(19) 1_556 ?
O1 Na1 2.436(2) . ?
O2 Na1 2.356(2) . ?
O2 H2 0.79(2) . ?
Na1 O2 2.356(2) 7_556 ?
Na1 O1 2.436(2) 7_556 ?
Na1 F1 2.4385(18) 5_566 ?
Na1 F1 2.4385(18) 3_545 ?
Na1 Ge1 3.3623(19) 3_545 ?
Na1 P1 3.4000(18) 7_556 ?
Na1 P1 3.4556(18) 1_556 ?
Na1 P1 3.4556(18) 7 ?

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
F1 Ge1 F1 180.0 . 5_566 ?
F1 Ge1 O1 93.51(8) . 6_565 ?
F1 Ge1 O1 86.49(8) 5_566 6_565 ?
F1 Ge1 O1 86.49(8) . 2_556 ?
F1 Ge1 O1 93.51(8) 5_566 2_556 ?
O1 Ge1 O1 180.00(7) 6_565 2_556 ?
F1 Ge1 O1 86.49(8) . 5_566 ?
F1 Ge1 O1 93.51(8) 5_566 5_566 ?
O1 Ge1 O1 89.67(12) 6_565 5_566 ?
O1 Ge1 O1 90.33(12) 2_556 5_566 ?
F1 Ge1 O1 93.51(8) . . ?
F1 Ge1 O1 86.48(8) 5_566 . ?
O1 Ge1 O1 90.33(12) 6_565 . ?
O1 Ge1 O1 89.67(12) 2_556 . ?
O1 Ge1 O1 180.0 5_566 . ?
F1 Ge1 Na1 135.27(4) . 4_556 ?
F1 Ge1 Na1 44.73(4) 5_566 4_556 ?
O1 Ge1 Na1 45.10(6) 6_565 4_556 ?
O1 Ge1 Na1 134.90(6) 2_556 4_556 ?
O1 Ge1 Na1 78.63(7) 5_566 4_556 ?
O1 Ge1 Na1 101.37(7) . 4_556 ?
F1 Ge1 Na1 44.73(4) . 2_556 ?
F1 Ge1 Na1 135.27(4) 5_566 2_556 ?
O1 Ge1 Na1 134.90(6) 6_565 2_556 ?
O1 Ge1 Na1 45.10(6) 2_556 2_556 ?
O1 Ge1 Na1 101.37(7) 5_566 2_556 ?
O1 Ge1 Na1 78.63(7) . 2_556 ?
Na1 Ge1 Na1 180.0 4_556 2_556 ?
F1 Ge1 Na1 135.27(4) . . ?
F1 Ge1 Na1 44.73(4) 5_566 . ?
O1 Ge1 Na1 101.37(7) 6_565 . ?
O1 Ge1 Na1 78.63(7) 2_556 . ?
O1 Ge1 Na1 134.90(6) 5_566 . ?
O1 Ge1 Na1 45.10(6) . . ?
Na1 Ge1 Na1 79.08(6) 4_556 . ?
Na1 Ge1 Na1 100.92(6) 2_556 . ?
F1 Ge1 Na1 44.73(4) . 3_455 ?
F1 Ge1 Na1 135.27(4) 5_566 3_455 ?
O1 Ge1 Na1 78.63(7) 6_565 3_455 ?
O1 Ge1 Na1 101.37(7) 2_556 3_455 ?
O1 Ge1 Na1 45.10(6) 5_566 3_455 ?
O1 Ge1 Na1 134.90(6) . 3_455 ?
Na1 Ge1 Na1 100.92(6) 4_556 3_455 ?
Na1 Ge1 Na1 79.08(6) 2_556 3_455 ?
Na1 Ge1 Na1 180.0 . 3_455 ?
O2 P1 O2 112.81(15) 2 . ?
O2 P1 O1 106.47(11) 2 2_556 ?
O2 P1 O1 110.26(11) . 2_556 ?
O2 P1 O1 110.26(11) 2 1_554 ?
O2 P1 O1 106.47(11) . 1_554 ?
O1 P1 O1 110.62(15) 2_556 1_554 ?
O2 P1 Na1 36.54(7) 2 2 ?
O2 P1 Na1 145.16(8) . 2 ?
O1 P1 Na1 97.85(8) 2_556 2 ?
O1 P1 Na1 81.12(8) 1_554 2 ?
O2 P1 Na1 145.16(8) 2 . ?
O2 P1 Na1 36.54(7) . . ?
O1 P1 Na1 81.12(8) 2_556 . ?
O1 P1 Na1 97.85(8) 1_554 . ?
Na1 P1 Na1 178.21(3) 2 . ?
O2 P1 Na1 73.03(9) 2 2_556 ?
O2 P1 Na1 107.99(9) . 2_556 ?
O1 P1 Na1 37.97(7) 2_556 2_556 ?
O1 P1 Na1 140.43(8) 1_554 2_556 ?
Na1 P1 Na1 81.67(6) 2 2_556 ?
Na1 P1 Na1 98.30(6) . 2_556 ?
O2 P1 Na1 107.99(9) 2 1_554 ?
O2 P1 Na1 73.03(9) . 1_554 ?
O1 P1 Na1 140.43(8) 2_556 1_554 ?
O1 P1 Na1 37.97(7) 1_554 1_554 ?
Na1 P1 Na1 98.30(6) 2 1_554 ?
Na1 P1 Na1 81.67(6) . 1_554 ?
Na1 P1 Na1 178.24(3) 2_556 1_554 ?
Ge1 F1 Na1 103.96(6) . 2_556 ?
Ge1 F1 Na1 103.96(6) . 3_455 ?
Na1 F1 Na1 122.75(9) 2_556 3_455 ?
P1 O1 Ge1 134.64(11) 1_556 . ?
P1 O1 Na1 119.23(10) 1_556 . ?
Ge1 O1 Na1 102.12(8) . . ?
P1 O2 Na1 120.77(11) . . ?
P1 O2 H2 122(4) . . ?
Na1 O2 H2 115(4) . . ?
O2 Na1 O2 180.0 . 7_556 ?
O2 Na1 O1 87.89(8) . . ?
O2 Na1 O1 92.11(8) 7_556 . ?
O2 Na1 O1 92.11(8) . 7_556 ?
O2 Na1 O1 87.89(8) 7_556 7_556 ?
O1 Na1 O1 180.0 . 7_556 ?
O2 Na1 F1 84.32(7) . 5_566 ?
O2 Na1 F1 95.68(7) 7_556 5_566 ?
O1 Na1 F1 61.96(7) . 5_566 ?
O1 Na1 F1 118.04(6) 7_556 5_566 ?
O2 Na1 F1 95.68(7) . 3_545 ?
O2 Na1 F1 84.32(7) 7_556 3_545 ?
O1 Na1 F1 118.04(7) . 3_545 ?
O1 Na1 F1 61.96(6) 7_556 3_545 ?
F1 Na1 F1 180.0 5_566 3_545 ?
O2 Na1 Ge1 76.81(6) . . ?
O2 Na1 Ge1 103.19(6) 7_556 . ?
O1 Na1 Ge1 32.77(4) . . ?
O1 Na1 Ge1 147.23(4) 7_556 . ?
F1 Na1 Ge1 31.31(5) 5_566 . ?
F1 Na1 Ge1 148.69(5) 3_545 . ?
O2 Na1 Ge1 103.19(6) . 3_545 ?
O2 Na1 Ge1 76.81(6) 7_556 3_545 ?
O1 Na1 Ge1 147.23(4) . 3_545 ?
O1 Na1 Ge1 32.77(4) 7_556 3_545 ?
F1 Na1 Ge1 148.69(5) 5_566 3_545 ?
F1 Na1 Ge1 31.31(5) 3_545 3_545 ?
Ge1 Na1 Ge1 180.0 . 3_545 ?
O2 Na1 P1 157.31(5) . 7_556 ?
O2 Na1 P1 22.69(5) 7_556 7_556 ?
O1 Na1 P1 106.95(7) . 7_556 ?
O1 Na1 P1 73.05(7) 7_556 7_556 ?
F1 Na1 P1 117.64(5) 5_566 7_556 ?
F1 Na1 P1 62.36(5) 3_545 7_556 ?
Ge1 Na1 P1 124.74(3) . 7_556 ?
Ge1 Na1 P1 55.26(3) 3_545 7_556 ?
O2 Na1 P1 22.69(5) . . ?
O2 Na1 P1 157.31(5) 7_556 . ?
O1 Na1 P1 73.05(7) . . ?
O1 Na1 P1 106.95(7) 7_556 . ?
F1 Na1 P1 62.36(5) 5_566 . ?
F1 Na1 P1 117.64(5) 3_545 . ?
Ge1 Na1 P1 55.26(4) . . ?
Ge1 Na1 P1 124.74(4) 3_545 . ?
P1 Na1 P1 180.0 7_556 . ?
O2 Na1 P1 88.86(7) . 1_556 ?
O2 Na1 P1 91.14(7) 7_556 1_556 ?
O1 Na1 P1 22.80(4) . 1_556 ?
O1 Na1 P1 157.19(4) 7_556 1_556 ?
F1 Na1 P1 84.73(5) 5_566 1_556 ?
F1 Na1 P1 95.27(5) 3_545 1_556 ?
Ge1 Na1 P1 54.75(3) . 1_556 ?
Ge1 Na1 P1 125.25(3) 3_545 1_556 ?
P1 Na1 P1 98.33(6) 7_556 1_556 ?
P1 Na1 P1 81.67(6) . 1_556 ?
O2 Na1 P1 91.14(7) . 7 ?
O2 Na1 P1 88.86(7) 7_556 7 ?
O1 Na1 P1 157.20(4) . 7 ?
O1 Na1 P1 22.81(4) 7_556 7 ?
F1 Na1 P1 95.27(5) 5_566 7 ?
F1 Na1 P1 84.73(5) 3_545 7 ?
Ge1 Na1 P1 125.25(3) . 7 ?
Ge1 Na1 P1 54.75(3) 3_545 7 ?
P1 Na1 P1 81.67(6) 7_556 7 ?
P1 Na1 P1 98.33(6) . 7 ?
P1 Na1 P1 180.0 1_556 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O2 0.79(2) 1.70(2) 2.485(4) 175(7) 6

_refine_diff_density_max         0.512
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1545661'
_audit_update_record             
;
2017-04-24 deposited with the CCDC.
2017-08-11 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 F2 Ge H2 O8 P2'
_chemical_formula_weight         568.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           127
_space_group_name_H-M_alt        'P 4/m b m'
_space_group_name_Hall           '-P 4 2ab'

_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, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x-1/2, y-1/2, z'
'-y-1/2, -x-1/2, z'
'x-1/2, -y-1/2, z'
'y-1/2, x-1/2, z'

_cell_length_a                   8.567(8)
_cell_length_b                   8.567(8)
_cell_length_c                   6.389(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     468.9(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2609
_cell_measurement_theta_min      3.189
_cell_measurement_theta_max      28.601

_exptl_crystal_description       'Tetragonal bipyramid'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    4.025
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    11.313
_shelx_estimated_absorpt_T_min   0.235
_shelx_estimated_absorpt_T_max   0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SMART (Bruker, 2001)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2609
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.189
_diffrn_reflns_theta_max         28.601
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             353
_reflns_number_gt                319
_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       'SAINT (Bruker, 2001)'
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005) '
_computing_publication_material  
'SHELXL-2014/7 (Sheldrick, 2014) and WinGX (Farrugia, 2014)'
_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)+6.7140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         353
_refine_ls_number_parameters     28
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.223
_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
Ge1 Ge 0.0000 0.0000 0.0000 0.0081(4) Uani 1 8 d S T P . .
P1 P 0.1740(3) 0.3260(3) 0.0000 0.0102(6) Uani 1 4 d S T P . .
Cs1 Cs 0.30960(8) 0.19040(8) 0.5000 0.0346(3) Uani 1 4 d S T P . .
F1 F 0.0000 0.0000 0.2769(13) 0.0257(18) Uani 1 4 d S T P . .
O1 O 0.1576(7) 0.1490(7) 0.0000 0.0158(13) Uani 1 2 d S TU P . .
O2 O 0.1030(5) 0.3970(5) 0.1968(10) 0.0167(13) Uani 1 2 d DS T P . .
H2 H 0.038(5) 0.462(5) 0.16(3) 0.050 Uiso 0.5 2 d DS 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
Ge1 F1 1.769(8) . ?
Ge1 F1 1.769(8) 9 ?
Ge1 O1 1.858(6) . ?
Ge1 O1 1.858(6) 9 ?
Ge1 O1 1.858(6) 10 ?
Ge1 O1 1.858(6) 2 ?
P1 O2 1.523(7) 11 ?
P1 O2 1.523(7) . ?
P1 O1 1.523(6) 14_665 ?
P1 O1 1.523(6) . ?
P1 Cs1 3.592(3) . ?
P1 Cs1 3.592(3) 1_554 ?
Cs1 O2 3.165(6) 11_556 ?
Cs1 O2 3.165(6) . ?
Cs1 O2 3.261(5) 12_656 ?
Cs1 O2 3.261(5) 4 ?
Cs1 O2 3.261(5) 2_655 ?
Cs1 O2 3.261(5) 10_556 ?
Cs1 F1 3.424(4) 5_556 ?
Cs1 F1 3.424(4) 13_665 ?
Cs1 F1 3.424(4) 9_556 ?
Cs1 F1 3.424(4) . ?
Cs1 O1 3.468(4) 14_666 ?
Cs1 O1 3.468(4) 14_665 ?
F1 Cs1 3.424(4) 9_556 ?
F1 Cs1 3.424(4) 2 ?
F1 Cs1 3.424(4) 10_556 ?
O1 Cs1 3.468(4) 1_554 ?
O2 Cs1 3.261(5) 10_566 ?
O2 Cs1 3.261(5) 2 ?
O2 H2 0.82(2) . ?

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
F1 Ge1 F1 180.0 . 9 ?
F1 Ge1 O1 90.0 . . ?
F1 Ge1 O1 90.0 9 . ?
F1 Ge1 O1 90.0 . 9 ?
F1 Ge1 O1 90.0 9 9 ?
O1 Ge1 O1 180.0 . 9 ?
F1 Ge1 O1 90.0 . 10 ?
F1 Ge1 O1 90.0 9 10 ?
O1 Ge1 O1 90.0 . 10 ?
O1 Ge1 O1 90.0 9 10 ?
F1 Ge1 O1 90.0 . 2 ?
F1 Ge1 O1 90.0 9 2 ?
O1 Ge1 O1 90.0 . 2 ?
O1 Ge1 O1 90.0 9 2 ?
O1 Ge1 O1 180.0(3) 10 2 ?
O2 P1 O2 111.3(5) 11 . ?
O2 P1 O1 111.15(16) 11 14_665 ?
O2 P1 O1 111.15(16) . 14_665 ?
O2 P1 O1 111.15(16) 11 . ?
O2 P1 O1 111.15(16) . . ?
O1 P1 O1 100.5(5) 14_665 . ?
O2 P1 Cs1 172.9(3) 11 . ?
O2 P1 Cs1 61.6(2) . . ?
O1 P1 Cs1 73.00(10) 14_665 . ?
O1 P1 Cs1 73.00(10) . . ?
O2 P1 Cs1 61.6(2) 11 1_554 ?
O2 P1 Cs1 172.9(3) . 1_554 ?
O1 P1 Cs1 73.00(10) 14_665 1_554 ?
O1 P1 Cs1 73.00(10) . 1_554 ?
Cs1 P1 Cs1 125.56(11) . 1_554 ?
O2 Cs1 O2 75.5(2) 11_556 . ?
O2 Cs1 O2 101.3(2) 11_556 12_656 ?
O2 Cs1 O2 157.39(9) . 12_656 ?
O2 Cs1 O2 157.39(9) 11_556 4 ?
O2 Cs1 O2 101.3(2) . 4 ?
O2 Cs1 O2 89.94(17) 12_656 4 ?
O2 Cs1 O2 157.39(9) 11_556 2_655 ?
O2 Cs1 O2 101.3(2) . 2_655 ?
O2 Cs1 O2 72.9(2) 12_656 2_655 ?
O2 Cs1 O2 45.0(2) 4 2_655 ?
O2 Cs1 O2 101.3(2) 11_556 10_556 ?
O2 Cs1 O2 157.39(9) . 10_556 ?
O2 Cs1 O2 45.0(2) 12_656 10_556 ?
O2 Cs1 O2 72.9(2) 4 10_556 ?
O2 Cs1 O2 89.94(17) 2_655 10_556 ?
O2 Cs1 F1 65.07(7) 11_556 5_556 ?
O2 Cs1 F1 95.05(10) . 5_556 ?
O2 Cs1 F1 64.11(11) 12_656 5_556 ?
O2 Cs1 F1 137.30(12) 4 5_556 ?
O2 Cs1 F1 93.32(13) 2_655 5_556 ?
O2 Cs1 F1 103.91(15) 10_556 5_556 ?
O2 Cs1 F1 95.05(10) 11_556 13_665 ?
O2 Cs1 F1 65.07(7) . 13_665 ?
O2 Cs1 F1 93.32(13) 12_656 13_665 ?
O2 Cs1 F1 103.91(15) 4 13_665 ?
O2 Cs1 F1 64.11(11) 2_655 13_665 ?
O2 Cs1 F1 137.30(12) 10_556 13_665 ?
F1 Cs1 F1 49.2(3) 5_556 13_665 ?
O2 Cs1 F1 65.07(7) 11_556 9_556 ?
O2 Cs1 F1 95.05(10) . 9_556 ?
O2 Cs1 F1 103.91(15) 12_656 9_556 ?
O2 Cs1 F1 93.32(13) 4 9_556 ?
O2 Cs1 F1 137.30(11) 2_655 9_556 ?
O2 Cs1 F1 64.11(11) 10_556 9_556 ?
F1 Cs1 F1 124.4(2) 5_556 9_556 ?
F1 Cs1 F1 155.66(4) 13_665 9_556 ?
O2 Cs1 F1 95.05(10) 11_556 . ?
O2 Cs1 F1 65.07(7) . . ?
O2 Cs1 F1 137.30(12) 12_656 . ?
O2 Cs1 F1 64.11(11) 4 . ?
O2 Cs1 F1 103.91(15) 2_655 . ?
O2 Cs1 F1 93.32(13) 10_556 . ?
F1 Cs1 F1 155.66(4) 5_556 . ?
F1 Cs1 F1 124.4(2) 13_665 . ?
F1 Cs1 F1 49.2(3) 9_556 . ?
O2 Cs1 O1 44.23(15) 11_556 14_666 ?
O2 Cs1 O1 114.28(16) . 14_666 ?
O2 Cs1 O1 57.32(14) 12_656 14_666 ?
O2 Cs1 O1 144.41(13) 4 14_666 ?
O2 Cs1 O1 123.68(15) 2_655 14_666 ?
O2 Cs1 O1 73.66(15) 10_556 14_666 ?
F1 Cs1 O1 43.71(14) 5_556 14_666 ?
F1 Cs1 O1 92.51(16) 13_665 14_666 ?
F1 Cs1 O1 82.80(16) 9_556 14_666 ?
F1 Cs1 O1 129.90(15) . 14_666 ?
O2 Cs1 O1 114.28(16) 11_556 14_665 ?
O2 Cs1 O1 44.23(15) . 14_665 ?
O2 Cs1 O1 123.68(15) 12_656 14_665 ?
O2 Cs1 O1 73.66(15) 4 14_665 ?
O2 Cs1 O1 57.32(14) 2_655 14_665 ?
O2 Cs1 O1 144.41(13) 10_556 14_665 ?
F1 Cs1 O1 92.51(16) 5_556 14_665 ?
F1 Cs1 O1 43.71(14) 13_665 14_665 ?
F1 Cs1 O1 129.90(15) 9_556 14_665 ?
F1 Cs1 O1 82.80(16) . 14_665 ?
O1 Cs1 O1 134.20(18) 14_666 14_665 ?
Ge1 F1 Cs1 114.59(13) . . ?
Ge1 F1 Cs1 114.59(13) . 9_556 ?
Cs1 F1 Cs1 130.8(3) . 9_556 ?
Ge1 F1 Cs1 114.59(13) . 2 ?
Cs1 F1 Cs1 80.03(10) . 2 ?
Cs1 F1 Cs1 80.03(10) 9_556 2 ?
Ge1 F1 Cs1 114.59(13) . 10_556 ?
Cs1 F1 Cs1 80.03(10) . 10_556 ?
Cs1 F1 Cs1 80.03(10) 9_556 10_556 ?
Cs1 F1 Cs1 130.8(3) 2 10_556 ?
P1 O1 Ge1 138.7(4) . . ?
P1 O1 Cs1 82.16(12) . . ?
Ge1 O1 Cs1 110.07(10) . . ?
P1 O1 Cs1 82.16(12) . 1_554 ?
Ge1 O1 Cs1 110.07(10) . 1_554 ?
Cs1 O1 Cs1 134.20(18) . 1_554 ?
P1 O2 Cs1 93.4(3) . . ?
P1 O2 Cs1 134.95(8) . 10_566 ?
Cs1 O2 Cs1 86.50(14) . 10_566 ?
P1 O2 Cs1 134.95(8) . 2 ?
Cs1 O2 Cs1 86.50(14) . 2 ?
Cs1 O2 Cs1 90.06(17) 10_566 2 ?
P1 O2 H2 109(10) . . ?
Cs1 O2 H2 158(10) . . ?
Cs1 O2 H2 78(10) 10_566 . ?
Cs1 O2 H2 78(10) 2 . ?

_refine_diff_density_max         0.942
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.248

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1545208'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-08-11 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         Rb2[GeF2(HPO4)2]
_chemical_formula_sum            'F2 Ge H2 O8 P2 Rb2'
_chemical_formula_weight         473.49

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.927(8)
_cell_length_b                   4.631(3)
_cell_length_c                   16.057(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.979(9)
_cell_angle_gamma                90
_cell_volume                     919.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2548
_cell_measurement_theta_min      2.646
_cell_measurement_theta_max      28.805

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.421
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   0.26
_exptl_transmission_factor_max   0.43
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    14.254
_shelx_estimated_absorpt_T_min   0.209
_shelx_estimated_absorpt_T_max   0.482
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SMART (Bruker, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SMART (Bruker, 2001)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1115
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.653
_diffrn_reflns_theta_max         28.742
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1115
_reflns_number_gt                971
_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_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005) '
_computing_publication_material  
'SHELXL-2014/7 (Sheldrick, 2014) and WinGX (Farrugia, 2014)'
_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)+(0.0393P)²+9.3368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1115
_refine_ls_number_parameters     74
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1040
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.104
_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
Ge1 Ge 0.2500 0.2500 0.5000 0.0052(2) Uani 1 2 d S . P . .
P1 P 0.25258(14) 0.7401(4) 0.36609(11) 0.0063(4) Uani 1 1 d . . . . .
Rb1 Rb 0.48613(6) 0.16546(16) 0.38604(4) 0.0161(2) Uani 1 1 d . . . . .
F1 F 0.1145(3) 0.1148(9) 0.4723(2) 0.0108(8) Uani 1 1 d . . . . .
O1 O 0.2066(4) 0.4762(10) 0.4002(3) 0.0099(10) Uani 1 1 d . U . . .
O2 O 0.2974(4) 0.9607(10) 0.4383(3) 0.0091(10) Uani 1 1 d . . . . .
O3 O 0.3405(4) 0.6754(11) 0.3262(3) 0.0109(10) Uani 1 1 d . . . . .
O4 O 0.1493(4) 0.8616(11) 0.2991(3) 0.0097(10) Uani 1 1 d D . . . .
H4 H 0.152(10) 0.96(2) 0.259(5) 0.07(4) Uiso 1 1 d 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
Ge1 F1 1.790(4) . ?
Ge1 F1 1.790(4) 7_556 ?
Ge1 O1 1.859(4) . ?
Ge1 O1 1.859(4) 7_556 ?
Ge1 O2 1.872(5) 7_566 ?
Ge1 O2 1.872(5) 1_545 ?
Ge1 Rb1 3.8782(19) 5_656 ?
Ge1 Rb1 3.8782(19) 3_455 ?
Ge1 Rb1 4.010(2) 7_556 ?
Ge1 Rb1 4.010(2) . ?
P1 O3 1.489(5) . ?
P1 O2 1.528(5) . ?
P1 O1 1.529(5) . ?
P1 O4 1.555(5) . ?
P1 Rb1 3.540(3) 1_565 ?
P1 Rb1 3.568(3) 3_455 ?
P1 Rb1 3.967(3) . ?
Rb1 F1 2.767(4) 3 ?
Rb1 O3 2.926(5) 1_545 ?
Rb1 O1 2.926(5) 3_545 ?
Rb1 O2 2.958(5) 1_545 ?
Rb1 O4 2.990(5) 3_545 ?
Rb1 O3 2.998(5) . ?
Rb1 F1 3.103(4) 7_556 ?
Rb1 O4 3.113(5) 4_545 ?
Rb1 F1 3.135(4) 3_545 ?
Rb1 O2 3.393(5) 5_666 ?
Rb1 P1 3.540(3) 1_545 ?
Rb1 P1 3.568(3) 3_545 ?
F1 Rb1 2.767(4) 3_445 ?
F1 Rb1 3.103(4) 7_556 ?
F1 Rb1 3.135(4) 3_455 ?
O1 Rb1 2.926(5) 3_455 ?
O2 Ge1 1.872(5) 1_565 ?
O2 Rb1 2.958(5) 1_565 ?
O2 Rb1 3.393(5) 5_666 ?
O3 Rb1 2.926(5) 1_565 ?
O4 Rb1 2.990(5) 3_455 ?
O4 Rb1 3.113(5) 4 ?
O4 H4 0.81(2) . ?

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
F1 Ge1 F1 180.0 . 7_556 ?
F1 Ge1 O1 87.46(19) . . ?
F1 Ge1 O1 92.54(19) 7_556 . ?
F1 Ge1 O1 92.54(19) . 7_556 ?
F1 Ge1 O1 87.46(19) 7_556 7_556 ?
O1 Ge1 O1 180.0 . 7_556 ?
F1 Ge1 O2 86.21(19) . 7_566 ?
F1 Ge1 O2 93.80(19) 7_556 7_566 ?
O1 Ge1 O2 89.4(2) . 7_566 ?
O1 Ge1 O2 90.6(2) 7_556 7_566 ?
F1 Ge1 O2 93.79(19) . 1_545 ?
F1 Ge1 O2 86.20(19) 7_556 1_545 ?
O1 Ge1 O2 90.6(2) . 1_545 ?
O1 Ge1 O2 89.4(2) 7_556 1_545 ?
O2 Ge1 O2 180.0 7_566 1_545 ?
F1 Ge1 Rb1 127.30(14) . 5_656 ?
F1 Ge1 Rb1 52.70(14) 7_556 5_656 ?
O1 Ge1 Rb1 133.54(15) . 5_656 ?
O1 Ge1 Rb1 46.46(15) 7_556 5_656 ?
O2 Ge1 Rb1 118.96(14) 7_566 5_656 ?
O2 Ge1 Rb1 61.04(14) 1_545 5_656 ?
F1 Ge1 Rb1 52.70(14) . 3_455 ?
F1 Ge1 Rb1 127.30(14) 7_556 3_455 ?
O1 Ge1 Rb1 46.46(15) . 3_455 ?
O1 Ge1 Rb1 133.54(15) 7_556 3_455 ?
O2 Ge1 Rb1 61.04(14) 7_566 3_455 ?
O2 Ge1 Rb1 118.96(14) 1_545 3_455 ?
Rb1 Ge1 Rb1 180.0 5_656 3_455 ?
F1 Ge1 Rb1 47.73(13) . 7_556 ?
F1 Ge1 Rb1 132.27(13) 7_556 7_556 ?
O1 Ge1 Rb1 105.06(15) . 7_556 ?
O1 Ge1 Rb1 74.93(15) 7_556 7_556 ?
O2 Ge1 Rb1 43.81(15) 7_566 7_556 ?
O2 Ge1 Rb1 136.19(15) 1_545 7_556 ?
Rb1 Ge1 Rb1 121.00(4) 5_656 7_556 ?
Rb1 Ge1 Rb1 59.00(4) 3_455 7_556 ?
F1 Ge1 Rb1 132.27(13) . . ?
F1 Ge1 Rb1 47.73(13) 7_556 . ?
O1 Ge1 Rb1 74.93(15) . . ?
O1 Ge1 Rb1 105.07(15) 7_556 . ?
O2 Ge1 Rb1 136.19(15) 7_566 . ?
O2 Ge1 Rb1 43.81(15) 1_545 . ?
Rb1 Ge1 Rb1 59.01(4) 5_656 . ?
Rb1 Ge1 Rb1 120.99(4) 3_455 . ?
Rb1 Ge1 Rb1 180.00(2) 7_556 . ?
O3 P1 O2 107.0(3) . . ?
O3 P1 O1 114.8(3) . . ?
O2 P1 O1 111.3(3) . . ?
O3 P1 O4 112.6(3) . . ?
O2 P1 O4 110.0(3) . . ?
O1 P1 O4 101.1(3) . . ?
O3 P1 Rb1 54.0(2) . 1_565 ?
O2 P1 Rb1 55.55(18) . 1_565 ?
O1 P1 Rb1 145.39(19) . 1_565 ?
O4 P1 Rb1 113.5(2) . 1_565 ?
O3 P1 Rb1 153.8(2) . 3_455 ?
O2 P1 Rb1 99.14(19) . 3_455 ?
O1 P1 Rb1 53.40(19) . 3_455 ?
O4 P1 Rb1 55.98(19) . 3_455 ?
Rb1 P1 Rb1 149.98(6) 1_565 3_455 ?
O3 P1 Rb1 40.6(2) . . ?
O2 P1 Rb1 106.04(19) . . ?
O1 P1 Rb1 78.5(2) . . ?
O4 P1 Rb1 141.1(2) . . ?
Rb1 P1 Rb1 75.95(6) 1_565 . ?
Rb1 P1 Rb1 131.28(6) 3_455 . ?
F1 Rb1 O3 169.03(12) 3 1_545 ?
F1 Rb1 O1 76.02(13) 3 3_545 ?
O3 Rb1 O1 108.16(14) 1_545 3_545 ?
F1 Rb1 O2 121.50(12) 3 1_545 ?
O3 Rb1 O2 48.69(13) 1_545 1_545 ?
O1 Rb1 O2 138.34(13) 3_545 1_545 ?
F1 Rb1 O4 66.66(13) 3 3_545 ?
O3 Rb1 O4 123.79(13) 1_545 3_545 ?
O1 Rb1 O4 47.43(13) 3_545 3_545 ?
O2 Rb1 O4 169.23(13) 1_545 3_545 ?
F1 Rb1 O3 78.26(13) 3 . ?
O3 Rb1 O3 102.85(16) 1_545 . ?
O1 Rb1 O3 140.08(13) 3_545 . ?
O2 Rb1 O3 81.42(14) 1_545 . ?
O4 Rb1 O3 94.22(14) 3_545 . ?
F1 Rb1 F1 72.83(13) 3 7_556 ?
O3 Rb1 F1 97.35(12) 1_545 7_556 ?
O1 Rb1 F1 130.42(11) 3_545 7_556 ?
O2 Rb1 F1 48.72(12) 1_545 7_556 ?
O4 Rb1 F1 138.27(13) 3_545 7_556 ?
O3 Rb1 F1 67.56(12) . 7_556 ?
F1 Rb1 O4 110.26(13) 3 4_545 ?
O3 Rb1 O4 77.55(14) 1_545 4_545 ?
O1 Rb1 O4 115.14(13) 3_545 4_545 ?
O2 Rb1 O4 94.84(13) 1_545 4_545 ?
O4 Rb1 O4 75.05(16) 3_545 4_545 ?
O3 Rb1 O4 48.61(13) . 4_545 ?
F1 Rb1 O4 111.43(12) 7_556 4_545 ?
F1 Rb1 F1 103.19(12) 3 3_545 ?
O3 Rb1 F1 73.78(13) 1_545 3_545 ?
O1 Rb1 F1 49.04(11) 3_545 3_545 ?
O2 Rb1 F1 89.30(12) 1_545 3_545 ?
O4 Rb1 F1 95.68(12) 3_545 3_545 ?
O3 Rb1 F1 169.72(11) . 3_545 ?
F1 Rb1 F1 102.94(10) 7_556 3_545 ?
O4 Rb1 F1 137.44(12) 4_545 3_545 ?
F1 Rb1 O2 59.03(12) 3 5_666 ?
O3 Rb1 O2 115.75(13) 1_545 5_666 ?
O1 Rb1 O2 48.39(12) 3_545 5_666 ?
O2 Rb1 O2 104.89(11) 1_545 5_666 ?
O4 Rb1 O2 85.27(13) 3_545 5_666 ?
O3 Rb1 O2 133.64(12) . 5_666 ?
F1 Rb1 O2 82.39(12) 7_556 5_666 ?
O4 Rb1 O2 160.27(12) 4_545 5_666 ?
F1 Rb1 O2 44.88(11) 3_545 5_666 ?
F1 Rb1 P1 146.56(9) 3 1_545 ?
O3 Rb1 P1 24.33(9) 1_545 1_545 ?
O1 Rb1 P1 128.74(11) 3_545 1_545 ?
O2 Rb1 P1 25.21(9) 1_545 1_545 ?
O4 Rb1 P1 145.68(10) 3_545 1_545 ?
O3 Rb1 P1 88.30(11) . 1_545 ?
F1 Rb1 P1 73.74(8) 7_556 1_545 ?
O4 Rb1 P1 81.32(10) 4_545 1_545 ?
F1 Rb1 P1 85.10(9) 3_545 1_545 ?
O2 Rb1 P1 116.98(9) 5_666 1_545 ?
F1 Rb1 P1 61.24(9) 3 3_545 ?
O3 Rb1 P1 126.22(10) 1_545 3_545 ?
O1 Rb1 P1 24.79(10) 3_545 3_545 ?
O2 Rb1 P1 162.60(10) 1_545 3_545 ?
O4 Rb1 P1 25.53(9) 3_545 3_545 ?
O3 Rb1 P1 115.29(10) . 3_545 ?
F1 Rb1 P1 131.01(8) 7_556 3_545 ?
O4 Rb1 P1 100.04(10) 4_545 3_545 ?
F1 Rb1 P1 73.64(8) 3_545 3_545 ?
O2 Rb1 P1 60.53(9) 5_666 3_545 ?
P1 Rb1 P1 149.98(6) 1_545 3_545 ?
Ge1 F1 Rb1 142.0(2) . 3_445 ?
Ge1 F1 Rb1 106.99(16) . 7_556 ?
Rb1 F1 Rb1 107.17(13) 3_445 7_556 ?
Ge1 F1 Rb1 100.28(16) . 3_455 ?
Rb1 F1 Rb1 103.19(12) 3_445 3_455 ?
Rb1 F1 Rb1 77.06(10) 7_556 3_455 ?
P1 O1 Ge1 135.1(3) . . ?
P1 O1 Rb1 101.8(2) . 3_455 ?
Ge1 O1 Rb1 106.13(19) . 3_455 ?
P1 O2 Ge1 140.4(3) . 1_565 ?
P1 O2 Rb1 99.2(2) . 1_565 ?
Ge1 O2 Rb1 110.2(2) 1_565 1_565 ?
P1 O2 Rb1 123.6(2) . 5_666 ?
Ge1 O2 Rb1 90.09(16) 1_565 5_666 ?
Rb1 O2 Rb1 75.10(11) 1_565 5_666 ?
P1 O3 Rb1 101.6(2) . 1_565 ?
P1 O3 Rb1 120.5(3) . . ?
Rb1 O3 Rb1 102.85(16) 1_565 . ?
P1 O4 Rb1 98.5(2) . 3_455 ?
P1 O4 Rb1 133.2(3) . 4 ?
Rb1 O4 Rb1 94.63(14) 3_455 4 ?
P1 O4 H4 122(9) . . ?
Rb1 O4 H4 139(9) 3_455 . ?
Rb1 O4 H4 63(9) 4 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O3 0.81(2) 1.70(2) 2.517(7) 179(14) 4

_refine_diff_density_max         0.990
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.296

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1545207'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-08-11 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         K2[GeF2(HPO4)2]
_chemical_formula_sum            'F2 Ge H2 K2 O8 P2'
_chemical_formula_weight         380.75

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.361(8)
_cell_length_b                   4.602(3)
_cell_length_c                   16.119(11)
_cell_angle_alpha                90
_cell_angle_beta                 107.203(8)
_cell_angle_gamma                90
_cell_volume                     875.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2548
_cell_measurement_theta_min      2.646
_cell_measurement_theta_max      28.805

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.888
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   0.75
_exptl_transmission_factor_max   0.79
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.871
_shelx_estimated_absorpt_T_min   0.323
_shelx_estimated_absorpt_T_max   0.793
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SMART (Bruker, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SMART (Bruker, 2001)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2548
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.646
_diffrn_reflns_theta_max         28.805
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1046
_reflns_number_gt                1028
_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_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005) '
_computing_publication_material  
'SHELXL-2014/7 (Sheldrick, 2014) and WinGX (Farrugia, 2014)'
_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)+(0.0345P)²+0.8746P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1046
_refine_ls_number_parameters     74
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_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
Ge1 Ge 0.2500 0.2500 0.5000 0.00620(12) Uani 1 2 d S . P . .
P1 P 0.25231(5) 0.74373(9) 0.36602(4) 0.00745(15) Uani 1 1 d . . . . .
K1 K 0.48482(4) 0.17367(11) 0.38620(3) 0.01808(14) Uani 1 1 d . . . . .
F1 F 0.10950(10) 0.1069(2) 0.47166(7) 0.0122(2) Uani 1 1 d . . . . .
O1 O 0.20285(12) 0.4849(3) 0.40241(9) 0.0116(3) Uani 1 1 d . . . . .
O2 O 0.30121(12) 0.9717(3) 0.43679(9) 0.0113(3) Uani 1 1 d . . . . .
O3 O 0.34459(13) 0.6693(3) 0.32691(10) 0.0139(3) Uani 1 1 d . . . . .
O4 O 0.14440(12) 0.8641(3) 0.29817(9) 0.0134(3) Uani 1 1 d D . . . .
H4 H 0.157(3) 0.965(7) 0.2615(18) 0.042(10) Uiso 1 1 d 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
Ge1 F1 1.7858(15) 7_556 ?
Ge1 F1 1.7858(15) . ?
Ge1 O1 1.8546(16) 7_556 ?
Ge1 O1 1.8546(16) . ?
Ge1 O2 1.8601(15) 7_566 ?
Ge1 O2 1.8601(15) 1_545 ?
Ge1 K1 3.7886(18) 5_656 ?
Ge1 K1 3.7886(18) 3_455 ?
Ge1 K1 3.8810(19) 7_556 ?
Ge1 K1 3.8811(19) . ?
P1 O3 1.4971(17) . ?
P1 O1 1.5326(16) . ?
P1 O2 1.5361(16) . ?
P1 O4 1.5553(17) . ?
P1 K1 3.4245(18) 1_565 ?
P1 K1 3.432(2) 3_455 ?
P1 K1 3.8333(19) . ?
K1 F1 2.6439(16) 3 ?
K1 O1 2.769(2) 3_545 ?
K1 O2 2.788(2) 1_545 ?
K1 O3 2.853(2) . ?
K1 O3 2.885(2) 1_545 ?
K1 O4 2.886(2) 3_545 ?
K1 F1 3.0346(19) 7_556 ?
K1 O4 3.057(2) 4_545 ?
K1 F1 3.1336(19) 3_545 ?
K1 O2 3.335(2) 5_666 ?
K1 P1 3.4245(18) 1_545 ?
K1 P1 3.432(2) 3_545 ?
F1 K1 2.6440(16) 3_445 ?
F1 K1 3.0346(19) 7_556 ?
F1 K1 3.1336(19) 3_455 ?
O1 K1 2.769(2) 3_455 ?
O2 Ge1 1.8601(15) 1_565 ?
O2 K1 2.788(2) 1_565 ?
O2 K1 3.335(2) 5_666 ?
O3 K1 2.885(2) 1_565 ?
O4 K1 2.886(2) 3_455 ?
O4 K1 3.057(2) 4 ?
O4 H4 0.799(18) . ?

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
F1 Ge1 F1 180.0 7_556 . ?
F1 Ge1 O1 87.71(6) 7_556 7_556 ?
F1 Ge1 O1 92.29(6) . 7_556 ?
F1 Ge1 O1 92.29(6) 7_556 . ?
F1 Ge1 O1 87.71(6) . . ?
O1 Ge1 O1 180.00(5) 7_556 . ?
F1 Ge1 O2 93.94(7) 7_556 7_566 ?
F1 Ge1 O2 86.06(7) . 7_566 ?
O1 Ge1 O2 90.52(8) 7_556 7_566 ?
O1 Ge1 O2 89.48(8) . 7_566 ?
F1 Ge1 O2 86.06(7) 7_556 1_545 ?
F1 Ge1 O2 93.94(7) . 1_545 ?
O1 Ge1 O2 89.48(8) 7_556 1_545 ?
O1 Ge1 O2 90.52(8) . 1_545 ?
O2 Ge1 O2 180.0 7_566 1_545 ?
F1 Ge1 K1 55.20(5) 7_556 5_656 ?
F1 Ge1 K1 124.80(5) . 5_656 ?
O1 Ge1 K1 43.92(5) 7_556 5_656 ?
O1 Ge1 K1 136.08(5) . 5_656 ?
O2 Ge1 K1 118.36(6) 7_566 5_656 ?
O2 Ge1 K1 61.64(6) 1_545 5_656 ?
F1 Ge1 K1 124.80(5) 7_556 3_455 ?
F1 Ge1 K1 55.20(5) . 3_455 ?
O1 Ge1 K1 136.08(5) 7_556 3_455 ?
O1 Ge1 K1 43.92(5) . 3_455 ?
O2 Ge1 K1 61.64(6) 7_566 3_455 ?
O2 Ge1 K1 118.36(6) 1_545 3_455 ?
K1 Ge1 K1 180.0 5_656 3_455 ?
F1 Ge1 K1 130.72(5) 7_556 7_556 ?
F1 Ge1 K1 49.28(5) . 7_556 ?
O1 Ge1 K1 75.12(6) 7_556 7_556 ?
O1 Ge1 K1 104.88(6) . 7_556 ?
O2 Ge1 K1 41.89(5) 7_566 7_556 ?
O2 Ge1 K1 138.11(5) 1_545 7_556 ?
K1 Ge1 K1 118.60(4) 5_656 7_556 ?
K1 Ge1 K1 61.40(4) 3_455 7_556 ?
F1 Ge1 K1 49.28(5) 7_556 . ?
F1 Ge1 K1 130.72(5) . . ?
O1 Ge1 K1 104.88(6) 7_556 . ?
O1 Ge1 K1 75.12(6) . . ?
O2 Ge1 K1 138.11(5) 7_566 . ?
O2 Ge1 K1 41.89(5) 1_545 . ?
K1 Ge1 K1 61.40(4) 5_656 . ?
K1 Ge1 K1 118.60(4) 3_455 . ?
K1 Ge1 K1 180.0 7_556 . ?
O3 P1 O1 115.04(9) . . ?
O3 P1 O2 106.70(9) . . ?
O1 P1 O2 111.13(9) . . ?
O3 P1 O4 112.77(10) . . ?
O1 P1 O4 100.93(9) . . ?
O2 P1 O4 110.27(9) . . ?
O3 P1 K1 56.60(7) . 1_565 ?
O1 P1 K1 146.23(6) . 1_565 ?
O2 P1 K1 53.13(6) . 1_565 ?
O4 P1 K1 112.47(7) . 1_565 ?
O3 P1 K1 153.36(7) . 3_455 ?
O1 P1 K1 52.13(6) . 3_455 ?
O2 P1 K1 99.92(6) . 3_455 ?
O4 P1 K1 56.65(7) . 3_455 ?
K1 P1 K1 148.24(3) 1_565 3_455 ?
O3 P1 K1 39.98(7) . . ?
O1 P1 K1 79.02(7) . . ?
O2 P1 K1 106.49(7) . . ?
O4 P1 K1 140.25(7) . . ?
K1 P1 K1 78.47(5) 1_565 . ?
K1 P1 K1 130.31(4) 3_455 . ?
F1 K1 O1 77.66(5) 3 3_545 ?
F1 K1 O2 119.89(5) 3 1_545 ?
O1 K1 O2 136.17(6) 3_545 1_545 ?
F1 K1 O3 76.97(6) 3 . ?
O1 K1 O3 139.49(5) 3_545 . ?
O2 K1 O3 84.14(6) 1_545 . ?
F1 K1 O3 168.40(4) 3 1_545 ?
O1 K1 O3 104.56(6) 3_545 1_545 ?
O2 K1 O3 50.77(5) 1_545 1_545 ?
O3 K1 O3 106.62(7) . 1_545 ?
F1 K1 O4 69.48(5) 3 3_545 ?
O1 K1 O4 49.76(5) 3_545 3_545 ?
O2 K1 O4 168.21(4) 1_545 3_545 ?
O3 K1 O4 91.63(6) . 3_545 ?
O3 K1 O4 120.82(5) 1_545 3_545 ?
F1 K1 F1 69.56(5) 3 7_556 ?
O1 K1 F1 127.85(4) 3_545 7_556 ?
O2 K1 F1 50.38(4) 1_545 7_556 ?
O3 K1 F1 69.87(5) . 7_556 ?
O3 K1 F1 100.98(5) 1_545 7_556 ?
O4 K1 F1 137.85(5) 3_545 7_556 ?
F1 K1 O4 110.30(5) 3 4_545 ?
O1 K1 O4 113.31(5) 3_545 4_545 ?
O2 K1 O4 98.24(6) 1_545 4_545 ?
O3 K1 O4 49.77(4) . 4_545 ?
O3 K1 O4 79.54(5) 1_545 4_545 ?
O4 K1 O4 70.83(7) 3_545 4_545 ?
F1 K1 O4 115.57(6) 7_556 4_545 ?
F1 K1 F1 105.27(6) 3 3_545 ?
O1 K1 F1 50.14(4) 3_545 3_545 ?
O2 K1 F1 86.05(5) 1_545 3_545 ?
O3 K1 F1 169.65(4) . 3_545 ?
O3 K1 F1 69.23(6) 1_545 3_545 ?
O4 K1 F1 98.63(5) 3_545 3_545 ?
F1 K1 F1 101.18(5) 7_556 3_545 ?
O4 K1 F1 135.53(4) 4_545 3_545 ?
F1 K1 O2 60.85(5) 3 5_666 ?
O1 K1 O2 49.67(5) 3_545 5_666 ?
O2 K1 O2 101.02(6) 1_545 5_666 ?
O3 K1 O2 134.15(4) . 5_666 ?
O3 K1 O2 111.65(5) 1_545 5_666 ?
O4 K1 O2 89.83(6) 3_545 5_666 ?
F1 K1 O2 78.78(6) 7_556 5_666 ?
O4 K1 O2 160.66(4) 4_545 5_666 ?
F1 K1 O2 45.12(3) 3_545 5_666 ?
F1 K1 P1 145.95(4) 3 1_545 ?
O1 K1 P1 126.42(5) 3_545 1_545 ?
O2 K1 P1 26.15(3) 1_545 1_545 ?
O3 K1 P1 91.16(6) . 1_545 ?
O3 K1 P1 25.67(3) 1_545 1_545 ?
O4 K1 P1 143.63(4) 3_545 1_545 ?
F1 K1 P1 76.40(4) 7_556 1_545 ?
O4 K1 P1 83.72(4) 4_545 1_545 ?
F1 K1 P1 81.42(5) 3_545 1_545 ?
O2 K1 P1 113.35(4) 5_666 1_545 ?
F1 K1 P1 63.20(4) 3 3_545 ?
O1 K1 P1 25.90(4) 3_545 3_545 ?
O2 K1 P1 161.69(4) 1_545 3_545 ?
O3 K1 P1 113.58(5) . 3_545 ?
O3 K1 P1 123.05(4) 1_545 3_545 ?
O4 K1 P1 26.76(3) 3_545 3_545 ?
F1 K1 P1 129.52(3) 7_556 3_545 ?
O4 K1 P1 97.01(5) 4_545 3_545 ?
F1 K1 P1 75.96(4) 3_545 3_545 ?
O2 K1 P1 63.73(5) 5_666 3_545 ?
P1 K1 P1 148.24(3) 1_545 3_545 ?
Ge1 F1 K1 141.65(6) . 3_445 ?
Ge1 F1 K1 104.23(6) . 7_556 ?
K1 F1 K1 110.45(5) 3_445 7_556 ?
Ge1 F1 K1 96.90(6) . 3_455 ?
K1 F1 K1 105.27(6) 3_445 3_455 ?
K1 F1 K1 78.82(5) 7_556 3_455 ?
P1 O1 Ge1 135.78(9) . . ?
P1 O1 K1 101.96(8) . 3_455 ?
Ge1 O1 K1 108.41(6) . 3_455 ?
P1 O2 Ge1 138.94(10) . 1_565 ?
P1 O2 K1 100.72(7) . 1_565 ?
Ge1 O2 K1 111.66(7) 1_565 1_565 ?
P1 O2 K1 122.46(8) . 5_666 ?
Ge1 O2 K1 88.96(6) 1_565 5_666 ?
K1 O2 K1 78.98(6) 1_565 5_666 ?
P1 O3 K1 120.32(9) . . ?
P1 O3 K1 97.73(8) . 1_565 ?
K1 O3 K1 106.62(7) . 1_565 ?
P1 O4 K1 96.60(8) . 3_455 ?
P1 O4 K1 132.42(9) . 4 ?
K1 O4 K1 98.88(6) 3_455 4 ?
P1 O4 H4 115(3) . . ?
K1 O4 H4 148(3) 3_455 . ?
K1 O4 H4 67(3) 4 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O3 0.799(18) 1.705(19) 2.494(2) 169(4) 4

_refine_diff_density_max         0.423
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.174

