# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_BGO1702
_database_code_depnum_ccdc_archive 'CCDC 1914363'
loop_
_audit_author_name
_audit_author_address
'Irina Kaurova'
;Moscow Technological University
Russia
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;

_chemical_name_systematic        'bismuth germanate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi15.81 Dy0.19 Ge12 O48'
_chemical_formula_sum            'Bi15.81 Dy0.19 Ge12 O48'
_chemical_formula_weight         4973.74
_chemical_absolute_configuration ad

_exptl_crystal_colour            colourless
_exptl_crystal_description       block
_exptl_crystal_preparation       Czochralsky
_exptl_crystal_density_diffrn    7.132

_cell_length_a                   10.5012(4)
_cell_length_b                   10.5012(4)
_cell_length_c                   10.5012(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1158.02(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)

_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'

loop_
_space_group_symop_operation_xyz
'x+, y+, z+'
'x+, -y+, -z+1/2'
'-x+, -y+1/2, z+'
'-x+, y+1/2, -z+1/2'
'y+1/4, -x+3/4, -z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'y+3/4, x+3/4, z+3/4'
'y+, z+, x+'
'-y+, -z+1/2, x+'
'y+, -z+, -x+1/2'
'-y+, z+1/2, -x+1/2'
'z+1/4, -y+3/4, -x+1/4'
'z+1/4, y+1/4, x+1/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+3/4, -y+1/4, x+1/4'
'z+, x+, y+'
'-z+1/2, x+, -y+'
'-z+, -x+1/2, y+'
'z+1/2, -x+1/2, -y+'
'x+3/4, z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1'
'y+3/4, -x+5/4, -z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'y+5/4, x+5/4, z+5/4'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+1/2, z+1, -x+1'
'z+3/4, -y+5/4, -x+3/4'
'z+3/4, y+3/4, x+3/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+5/4, -y+3/4, x+3/4'
'z+1/2, x+1/2, y+1/2'
'-z+1, x+1/2, -y+1/2'
'-z+1/2, -x+1, y+1/2'
'z+1, -x+1, -y+1/2'
'x+5/4, z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'

_diffrn_ambient_temperature      295(2)

_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0595

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
BI Bi 0.08739(4) 0.08739(4) 0.08739(4) 0.0205(2) Uani 0.9879 3 d S T P . .
DY Dy 0.08739(4) 0.08739(4) 0.08739(4) 0.0205(2) Uani 0.012 3 d S T P . .
GE Ge 0.0000 0.2500 0.3750 0.0186(5) Uani 1 4 d S T P . .
O O 0.0721(11) 0.1260(10) 0.2905(9) 0.026(2) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
BI 0.0205(2) 0.0205(2) 0.0205(2) -0.00005(15) -0.00005(15) -0.00005(15)
DY 0.0205(2) 0.0205(2) 0.0205(2) -0.00005(15) -0.00005(15) -0.00005(15)
GE 0.0189(7) 0.0189(7) 0.0182(11) 0.000 0.000 0.000
O 0.035(6) 0.018(4) 0.023(4) -0.005(3) -0.003(4) 0.003(4)


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
BI O 2.177(10) . ?
BI O 2.177(10) 17 ?
BI O 2.177(10) 9 ?
BI O 2.587(10) 18 ?
BI O 2.587(10) 10 ?
BI O 2.587(10) 2 ?
GE O 1.748(10) 3 ?
GE O 1.748(10) . ?
GE O 1.748(10) 31_445 ?
GE O 1.748(10) 29_445 ?
O DY 2.587(10) 2 ?
O BI 2.587(10) 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
O BI O 84.5(4) . 17 ?
O BI O 84.5(4) . 9 ?
O BI O 84.5(4) 17 9 ?
O BI O 153.7(4) . 18 ?
O BI O 70.8(4) 17 18 ?
O BI O 84.52(15) 9 18 ?
O BI O 84.52(15) . 10 ?
O BI O 153.7(4) 17 10 ?
O BI O 70.8(4) 9 10 ?
O BI O 113.98(19) 18 10 ?
O BI O 70.8(4) . 2 ?
O BI O 84.52(15) 17 2 ?
O BI O 153.7(4) 9 2 ?
O BI O 113.98(19) 18 2 ?
O BI O 113.98(19) 10 2 ?
O GE O 119.0(6) 3 . ?
O GE O 104.9(3) 3 31_445 ?
O GE O 104.9(3) . 31_445 ?
O GE O 104.9(3) 3 29_445 ?
O GE O 104.9(3) . 29_445 ?
O GE O 119.0(6) 31_445 29_445 ?
GE O BI 131.9(5) . . ?
GE O DY 114.9(5) . 2 ?
BI O DY 108.6 . 2 ?
GE O BI 114.9(5) . 2 ?
BI O BI 108.6(4) . 2 ?
DY O BI 0.0 2 2 ?

_refine_ls_abs_structure_details 
;
 Flack x determined using 125 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.048(15)
#########################################################################

_audit_creation_method           SHELXL-2015/1
_shelx_SHELXL_version_number     2015/1

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;

_cell_measurement_reflns_used    18349
_cell_measurement_theta_min      4.755
_cell_measurement_theta_max      31.027

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2092.6
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    67.872
_shelx_estimated_absorpt_T_min   0.026
_shelx_estimated_absorpt_T_max   0.026
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_factor_muR        6.787
_exptl_absorpt_process_details   
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_correction_T_min  0.0009
_exptl_absorpt_correction_T_max  0.0011

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'LFF Sealed Tube'
_diffrn_detector                 'Hybride pixel array detector'
_diffrn_detector_type            'DECTRIS Pilatus--100K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source                   'SEIFERT Iso--Debyeflex 3003'
_diffrn_measurement_device       'Four cyrcle diffractometer'
_diffrn_measurement_device_type  STADI--VARY
_diffrn_radiation_monochromator  'Plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_measurement_method       'Rotation method'
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            313
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0318 # before absorption correction
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.755
_diffrn_reflns_theta_max         31.027
_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             313
_reflns_number_gt                292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.749
_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       'X--AREA (STOE & CIE, 2012)'
_computing_cell_refinement       'X--AREA (STOE & CIE, 2012)'
_computing_data_reduction        'X--RED  (STOE & CIE, 2012)'
_computing_structure_solution    'SHELXS97       (Sheldrick,  2008)'
_computing_structure_refinement  'SHELXL-2015/1  (Sheldrick,  2015)'
_computing_molecular_graphics    'Ortep--3       (Farrugia,   1997)'
_computing_publication_material  'WinGX          (Farrugia,   1999)'

_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)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         313
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_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.
;

_refine_diff_density_max         1.375
_refine_diff_density_min         -2.675
_refine_diff_density_rms         0.350

_shelx_res_file                  
;
TITL bgo1702 in I -4 3 d
 BGO1702.res created by SHELXL-2015/1 at 15:09:56 on 15-Apr-2019
CELL   0.71073  10.5012  10.5012  10.5012  90.000  90.000  90.000
ZERR   1         0.0004   0.0004   0.0004   0.000   0.000   0.000
LATT   -2
SYMM   +X,-Y,1/2-Z
SYMM   -X,1/2-Y,+Z
SYMM   -X,1/2+Y,1/2-Z
SYMM   1/4+Y,3/4-X,1/4-Z
SYMM   1/4-Y,3/4-X,3/4+Z
SYMM   3/4-Y,3/4+X,1/4-Z
SYMM   3/4+Y,3/4+X,3/4+Z
SYMM   +Y,+Z,+X
SYMM   -Y,1/2-Z,+X
SYMM   +Y,-Z,1/2-X
SYMM   -Y,1/2+Z,1/2-X
SYMM   1/4+Z,3/4-Y,1/4-X
SYMM   1/4+Z,1/4+Y,1/4+X
SYMM   3/4-Z,3/4+Y,1/4-X
SYMM   3/4-Z,1/4-Y,1/4+X
SYMM   +Z,+X,+Y
SYMM   1/2-Z,+X,-Y
SYMM   -Z,1/2-X,+Y
SYMM   1/2+Z,1/2-X,-Y
SYMM   3/4+X,3/4+Z,3/4+Y
SYMM   3/4+X,1/4-Z,3/4-Y
SYMM   3/4-X,3/4+Z,1/4-Y
SYMM   1/4-X,3/4-Z,3/4+Y

SFAC  Bi    Ge  O   DY
UNIT  15.81 12  48  0.19
TEMP    22
SIZE  0.2 0.2 0.2
L.S.   10
FMAP 2
PLAN 5
EXYZ BI DY
EADP BI DY
ACTA
WGHT    0.043700
FVAR       1.01767
BI    1    0.087389    0.087389    0.087389    10.32930    0.02053    0.02053 =
         0.02053   -0.00005   -0.00005   -0.00005
DY    4    0.087389    0.087389    0.087389    10.00400    0.02053    0.02053 =
         0.02053   -0.00005   -0.00005   -0.00005
GE    2   10.000000   10.250000   10.374990    10.25000    0.01886    0.01886 =
         0.01823    0.00000    0.00000    0.00000
O     3    0.072093    0.126008    0.290472    11.00000    0.03529    0.01823 =
         0.02342   -0.00506   -0.00306    0.00306
HKLF  4

REM  bgo1702 in I -4 3 d
REM R1 =  0.0252 for     292 Fo > 4sig(Fo)  and  0.0280 for all     313 data
REM     15 parameters refined using      0 restraints

END

WGHT      0.0437      0.0000

REM Highest difference peak  1.375,  deepest hole -2.675,  1-sigma level  0.350
Q1    1  -0.0015 -0.0015 -0.0015  10.33333  0.05    1.37
Q2    1  -0.1250  0.0000  0.2500  10.25000  0.05    1.15
Q3    1   0.1616  0.0910  0.3496  11.00000  0.05    1.13
Q4    1  -0.0393  0.3217  0.4811  11.00000  0.05    1.08
Q5    1   0.0969  0.0874 -0.0479  11.00000  0.05    0.86
;
_shelx_res_checksum              59069

_exptl_crystal_recrystallization_method 'From the Melt'
