# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# 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_A
_database_code_depnum_ccdc_archive 'CCDC 1909492'
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 Ca2 Ge O7'
_chemical_formula_weight         286.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Ca Ca 0.2262 0.3064 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_H-M_alt        'P -4 21 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'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   7.2548(2)
_cell_length_b                   7.2548(2)
_cell_length_c                   4.8248(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     253.94(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.745
_exptl_crystal_F_000             276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    8.034
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1807
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.972
_diffrn_reflns_theta_max         29.692
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             369
_reflns_number_gt                332
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.624
_reflns_Friedel_fraction_max     0.954
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0405P)²+0.6408P] 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
_refine_ls_extinction_coef       0.033(11)
_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   0.02(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         369
_refine_ls_number_parameters     36
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0900
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_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
Ca1 Ca -0.33941(17) -0.16059(17) 0.5085(4) 0.0088(5) Uani 1 2 d S T P . .
Ge1 Ge 0.0000 0.0000 0.0000 0.0086(5) Uani 1 4 d S T P . .
B1 B 0.3697(11) -0.1303(11) 0.045(2) 0.011(2) Uani 1 2 d S T P . .
O1 O -0.5000 0.0000 0.162(2) 0.010(2) Uani 1 4 d S T P . .
O2 O -0.1449(7) -0.3551(7) 0.2415(14) 0.0127(15) Uani 1 2 d S T P . .
O3 O 0.1844(7) -0.0784(7) 0.2014(11) 0.0111(11) 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
Ca1 O1 2.349(7) . ?
Ca1 O3 2.361(5) 3_556 ?
Ca1 O3 2.361(5) 6_446 ?
Ca1 O2 2.376(7) . ?
Ca1 O2 2.525(5) 3_556 ?
Ca1 O2 2.525(5) 4_456 ?
Ca1 O3 2.543(5) 8_445 ?
Ca1 O3 2.543(5) 2 ?
Ca1 B1 3.039(11) 3_556 ?
Ca1 B1 3.082(10) 1_455 ?
Ca1 B1 3.082(10) 2 ?
Ca1 Ca1 3.295(4) 2_455 ?
Ge1 O3 1.748(5) . ?
Ge1 O3 1.748(5) 3 ?
Ge1 O3 1.748(5) 4 ?
Ge1 O3 1.748(5) 2 ?
Ge1 Ca1 3.6115(15) 1_554 ?
Ge1 Ca1 3.6115(15) 3_556 ?
Ge1 Ca1 3.6115(15) 2_554 ?
Ge1 Ca1 3.6115(15) 4_556 ?
Ge1 Ca1 3.6661(15) 2 ?
Ge1 Ca1 3.6661(15) 4 ?
Ge1 Ca1 3.6661(15) 3 ?
B1 O2 1.391(13) 4 ?
B1 O1 1.450(12) 1_655 ?
B1 O3 1.586(8) 8_545 ?
B1 O3 1.586(8) . ?
B1 Ca1 3.039(11) 4_556 ?
B1 Ca1 3.082(10) 2 ?
B1 Ca1 3.082(10) 1_655 ?
O1 B1 1.450(12) 1_455 ?
O1 B1 1.450(12) 2 ?
O1 Ca1 2.349(7) 2_455 ?
O2 B1 1.391(13) 3 ?
O2 Ca1 2.525(5) 4_556 ?
O2 Ca1 2.525(5) 3_546 ?
O3 Ca1 2.361(5) 4_556 ?
O3 Ca1 2.543(5) 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
O1 Ca1 O3 148.94(13) . 3_556 ?
O1 Ca1 O3 148.94(13) . 6_446 ?
O3 Ca1 O3 62.0(3) 3_556 6_446 ?
O1 Ca1 O2 101.7(2) . . ?
O3 Ca1 O2 78.55(19) 3_556 . ?
O3 Ca1 O2 78.55(19) 6_446 . ?
O1 Ca1 O2 83.26(19) . 3_556 ?
O3 Ca1 O2 79.48(16) 3_556 3_556 ?
O3 Ca1 O2 115.08(19) 6_446 3_556 ?
O2 Ca1 O2 143.82(13) . 3_556 ?
O1 Ca1 O2 83.26(19) . 4_456 ?
O3 Ca1 O2 115.08(19) 3_556 4_456 ?
O3 Ca1 O2 79.48(16) 6_446 4_456 ?
O2 Ca1 O2 143.82(13) . 4_456 ?
O2 Ca1 O2 72.1(3) 3_556 4_456 ?
O1 Ca1 O3 57.71(13) . 8_445 ?
O3 Ca1 O3 149.31(10) 3_556 8_445 ?
O3 Ca1 O3 92.3(2) 6_446 8_445 ?
O2 Ca1 O3 80.00(16) . 8_445 ?
O2 Ca1 O3 129.45(17) 3_556 8_445 ?
O2 Ca1 O3 72.55(18) 4_456 8_445 ?
O1 Ca1 O3 57.71(13) . 2 ?
O3 Ca1 O3 92.3(2) 3_556 2 ?
O3 Ca1 O3 149.31(10) 6_446 2 ?
O2 Ca1 O3 80.00(16) . 2 ?
O2 Ca1 O3 72.55(18) 3_556 2 ?
O2 Ca1 O3 129.45(17) 4_456 2 ?
O3 Ca1 O3 105.3(2) 8_445 2 ?
O1 Ca1 B1 179.7(3) . 3_556 ?
O3 Ca1 B1 31.05(13) 3_556 3_556 ?
O3 Ca1 B1 31.05(13) 6_446 3_556 ?
O2 Ca1 B1 77.9(3) . 3_556 ?
O2 Ca1 B1 97.0(2) 3_556 3_556 ?
O2 Ca1 B1 97.0(2) 4_456 3_556 ?
O3 Ca1 B1 122.17(15) 8_445 3_556 ?
O3 Ca1 B1 122.17(15) 2 3_556 ?
O1 Ca1 B1 26.89(18) . 1_455 ?
O3 Ca1 B1 169.8(2) 3_556 1_455 ?
O3 Ca1 B1 122.5(2) 6_446 1_455 ?
O2 Ca1 B1 93.2(2) . 1_455 ?
O2 Ca1 B1 104.65(17) 3_556 1_455 ?
O2 Ca1 B1 75.1(2) 4_456 1_455 ?
O3 Ca1 B1 30.9(2) 8_445 1_455 ?
O3 Ca1 B1 80.3(2) 2 1_455 ?
B1 Ca1 B1 153.01(14) 3_556 1_455 ?
O1 Ca1 B1 26.89(18) . 2 ?
O3 Ca1 B1 122.5(2) 3_556 2 ?
O3 Ca1 B1 169.8(2) 6_446 2 ?
O2 Ca1 B1 93.2(2) . 2 ?
O2 Ca1 B1 75.1(2) 3_556 2 ?
O2 Ca1 B1 104.65(17) 4_456 2 ?
O3 Ca1 B1 80.3(2) 8_445 2 ?
O3 Ca1 B1 30.9(2) 2 2 ?
B1 Ca1 B1 153.01(14) 3_556 2 ?
B1 Ca1 B1 51.4(4) 1_455 2 ?
O1 Ca1 Ca1 45.45(17) . 2_455 ?
O3 Ca1 Ca1 128.23(13) 3_556 2_455 ?
O3 Ca1 Ca1 128.23(13) 6_446 2_455 ?
O2 Ca1 Ca1 147.16(18) . 2_455 ?
O2 Ca1 Ca1 49.28(11) 3_556 2_455 ?
O2 Ca1 Ca1 49.28(11) 4_456 2_455 ?
O3 Ca1 Ca1 80.25(12) 8_445 2_455 ?
O3 Ca1 Ca1 80.25(12) 2 2_455 ?
B1 Ca1 Ca1 134.9(2) 3_556 2_455 ?
B1 Ca1 Ca1 57.68(12) 1_455 2_455 ?
B1 Ca1 Ca1 57.68(12) 2 2_455 ?
O3 Ge1 O3 107.98(16) . 3 ?
O3 Ge1 O3 107.98(16) . 4 ?
O3 Ge1 O3 112.5(3) 3 4 ?
O3 Ge1 O3 112.5(3) . 2 ?
O3 Ge1 O3 107.98(16) 3 2 ?
O3 Ge1 O3 107.98(16) 4 2 ?
O3 Ge1 Ca1 141.40(17) . 1_554 ?
O3 Ge1 Ca1 33.55(17) 3 1_554 ?
O3 Ge1 Ca1 95.96(17) 4 1_554 ?
O3 Ge1 Ca1 87.02(17) 2 1_554 ?
O3 Ge1 Ca1 95.96(17) . 3_556 ?
O3 Ge1 Ca1 141.40(17) 3 3_556 ?
O3 Ge1 Ca1 87.02(17) 4 3_556 ?
O3 Ge1 Ca1 33.55(17) 2 3_556 ?
Ca1 Ge1 Ca1 115.54(3) 1_554 3_556 ?
O3 Ge1 Ca1 87.02(17) . 2_554 ?
O3 Ge1 Ca1 95.96(17) 3 2_554 ?
O3 Ge1 Ca1 33.55(17) 4 2_554 ?
O3 Ge1 Ca1 141.40(17) 2 2_554 ?
Ca1 Ge1 Ca1 97.92(5) 1_554 2_554 ?
Ca1 Ge1 Ca1 115.54(3) 3_556 2_554 ?
O3 Ge1 Ca1 33.55(17) . 4_556 ?
O3 Ge1 Ca1 87.02(17) 3 4_556 ?
O3 Ge1 Ca1 141.40(17) 4 4_556 ?
O3 Ge1 Ca1 95.96(17) 2 4_556 ?
Ca1 Ge1 Ca1 115.54(3) 1_554 4_556 ?
Ca1 Ge1 Ca1 97.92(5) 3_556 4_556 ?
Ca1 Ge1 Ca1 115.54(3) 2_554 4_556 ?
O3 Ge1 Ca1 38.52(17) . 2 ?
O3 Ge1 Ca1 146.46(17) 3 2 ?
O3 Ge1 Ca1 84.85(17) 4 2 ?
O3 Ge1 Ca1 92.22(17) 2 2 ?
Ca1 Ge1 Ca1 179.03(5) 1_554 2 ?
Ca1 Ge1 Ca1 63.934(7) 3_556 2 ?
Ca1 Ge1 Ca1 83.048(13) 2_554 2 ?
Ca1 Ge1 Ca1 63.934(7) 4_556 2 ?
O3 Ge1 Ca1 84.85(17) . 4 ?
O3 Ge1 Ca1 38.52(17) 3 4 ?
O3 Ge1 Ca1 92.22(17) 4 4 ?
O3 Ge1 Ca1 146.46(17) 2 4 ?
Ca1 Ge1 Ca1 63.934(7) 1_554 4 ?
Ca1 Ge1 Ca1 179.03(5) 3_556 4 ?
Ca1 Ge1 Ca1 63.934(7) 2_554 4 ?
Ca1 Ge1 Ca1 83.048(13) 4_556 4 ?
Ca1 Ge1 Ca1 116.61(3) 2 4 ?
O3 Ge1 Ca1 146.46(17) . 3 ?
O3 Ge1 Ca1 92.22(17) 3 3 ?
O3 Ge1 Ca1 38.52(17) 4 3 ?
O3 Ge1 Ca1 84.85(17) 2 3 ?
Ca1 Ge1 Ca1 63.934(7) 1_554 3 ?
Ca1 Ge1 Ca1 83.048(13) 3_556 3 ?
Ca1 Ge1 Ca1 63.934(7) 2_554 3 ?
Ca1 Ge1 Ca1 179.03(5) 4_556 3 ?
Ca1 Ge1 Ca1 116.61(3) 2 3 ?
Ca1 Ge1 Ca1 95.98(5) 4 3 ?
O3 Ge1 Ca1 92.22(17) . . ?
O3 Ge1 Ca1 84.85(17) 3 . ?
O3 Ge1 Ca1 146.46(17) 4 . ?
O3 Ge1 Ca1 38.52(17) 2 . ?
Ca1 Ge1 Ca1 83.049(13) 1_554 . ?
Ca1 Ge1 Ca1 63.934(7) 3_556 . ?
Ca1 Ge1 Ca1 179.03(5) 2_554 . ?
Ca1 Ge1 Ca1 63.933(7) 4_556 . ?
Ca1 Ge1 Ca1 95.98(5) 2 . ?
Ca1 Ge1 Ca1 116.61(3) 4 . ?
Ca1 Ge1 Ca1 116.61(3) 3 . ?
O2 B1 O1 118.9(9) 4 1_655 ?
O2 B1 O3 115.2(6) 4 8_545 ?
O1 B1 O3 102.3(6) 1_655 8_545 ?
O2 B1 O3 115.2(6) 4 . ?
O1 B1 O3 102.3(6) 1_655 . ?
O3 B1 O3 100.2(7) 8_545 . ?
O2 B1 Ca1 128.9(7) 4 4_556 ?
O1 B1 Ca1 112.1(6) 1_655 4_556 ?
O3 B1 Ca1 50.1(3) 8_545 4_556 ?
O3 B1 Ca1 50.1(3) . 4_556 ?
O2 B1 Ca1 140.1(4) 4 2 ?
O1 B1 Ca1 47.1(3) 1_655 2 ?
O3 B1 Ca1 104.6(5) 8_545 2 ?
O3 B1 Ca1 55.4(3) . 2 ?
Ca1 B1 Ca1 78.0(2) 4_556 2 ?
O2 B1 Ca1 140.1(4) 4 1_655 ?
O1 B1 Ca1 47.1(3) 1_655 1_655 ?
O3 B1 Ca1 55.4(3) 8_545 1_655 ?
O3 B1 Ca1 104.6(5) . 1_655 ?
Ca1 B1 Ca1 78.0(2) 4_556 1_655 ?
Ca1 B1 Ca1 64.6(2) 2 1_655 ?
B1 O1 B1 134.4(11) 1_455 2 ?
B1 O1 Ca1 106.0(3) 1_455 2_455 ?
B1 O1 Ca1 106.0(3) 2 2_455 ?
B1 O1 Ca1 106.0(3) 1_455 . ?
B1 O1 Ca1 106.0(3) 2 . ?
Ca1 O1 Ca1 89.1(3) 2_455 . ?
B1 O2 Ca1 129.0(6) 3 . ?
B1 O2 Ca1 114.3(4) 3 4_556 ?
Ca1 O2 Ca1 103.6(2) . 4_556 ?
B1 O2 Ca1 114.3(4) 3 3_546 ?
Ca1 O2 Ca1 103.6(2) . 3_546 ?
Ca1 O2 Ca1 81.4(2) 4_556 3_546 ?
B1 O3 Ge1 117.5(4) . . ?
B1 O3 Ca1 98.8(4) . 4_556 ?
Ge1 O3 Ca1 122.3(3) . 4_556 ?
B1 O3 Ca1 93.7(5) . 2 ?
Ge1 O3 Ca1 116.1(2) . 2 ?
Ca1 O3 Ca1 103.51(19) 4_556 2 ?

_refine_diff_density_max         0.830
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.194

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1909493'
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 Ca1.78 Cd0.22 Ge O7'
_chemical_formula_weight         302.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Ca Ca 0.2262 0.3064 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.2300(2)
_cell_length_b                   7.2300(2)
_cell_length_c                   4.8066(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     251.25(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.996
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             288
_exptl_absorpt_coefficient_mu    8.801
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3348
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         5.09
_diffrn_reflns_theta_max         29.63
_reflns_number_total             373
_reflns_number_gt                368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0178P)²+0.1435P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.350(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(19)
_refine_ls_number_reflns         373
_refine_ls_number_parameters     36
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0406
_refine_ls_wR_factor_gt          0.0398
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.103
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.34062(4) 0.15938(4) -0.01011(11) 0.0024(2) Uani 0.889(2) 2 d SP . .
Cd1 Cd 0.34062(4) 0.15938(4) -0.01011(11) 0.0024(2) Uani 0.111(2) 2 d SP . .
Ge1 Ge 0.0000 0.0000 0.5000 0.00122(18) Uani 1 4 d S . .
B1 B -0.3682(3) 0.1318(3) 0.4555(7) 0.0008(6) Uani 1 2 d SU . .
O1 O 0.5000 0.0000 0.3373(6) 0.0031(6) Uani 1 4 d S . .
O2 O 0.1449(2) 0.3551(2) 0.2588(5) 0.0036(5) Uani 1 2 d S . .
O3 O -0.1844(2) 0.0798(2) 0.2977(3) 0.0028(3) 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
Ca1 O1 2.333(2) . ?
Ca1 O3 2.3453(16) 3 ?
Ca1 O3 2.3453(16) 6 ?
Ca1 O2 2.382(2) . ?
Ca1 O2 2.5061(17) 3 ?
Ca1 O2 2.5061(17) 4_655 ?
Ca1 O3 2.5405(16) 8 ?
Ca1 O3 2.5405(16) 2 ?
Ca1 B1 3.024(3) 3 ?
Ca1 B1 3.079(3) 1_655 ?
Ca1 B1 3.079(3) 2 ?
Ca1 Ca1 3.2592(9) 2_655 ?
Ge1 O3 1.7482(16) 3_556 ?
Ge1 O3 1.7482(16) 4_556 ?
Ge1 O3 1.7482(16) 2 ?
Ge1 O3 1.7482(16) . ?
Ge1 Ca1 3.5968(4) 1_556 ?
Ge1 Ca1 3.5968(4) 3 ?
Ge1 Ca1 3.5968(4) 2_556 ?
Ge1 Ca1 3.5968(4) 4 ?
Ge1 Ca1 3.6612(4) 2 ?
Ge1 Ca1 3.6612(4) 4_556 ?
Ge1 Ca1 3.6612(4) 3_556 ?
B1 O2 1.380(4) 4_556 ?
B1 O1 1.462(3) 1_455 ?
B1 O3 1.576(3) 8_455 ?
B1 O3 1.576(3) . ?
B1 Ca1 3.024(3) 4 ?
B1 Ca1 3.079(3) 2 ?
B1 Ca1 3.079(3) 1_455 ?
O1 B1 1.462(3) 1_655 ?
O1 B1 1.462(3) 2 ?
O1 Cd1 2.333(2) 2_655 ?
O1 Ca1 2.333(2) 2_655 ?
O2 B1 1.380(4) 3_556 ?
O2 Cd1 2.5061(17) 4 ?
O2 Ca1 2.5061(17) 4 ?
O2 Ca1 2.5061(17) 3_565 ?
O2 Cd1 2.5061(17) 3_565 ?
O3 Cd1 2.3453(16) 4 ?
O3 Ca1 2.3453(16) 4 ?
O3 Ca1 2.5405(16) 2 ?
O3 Cd1 2.5405(16) 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
O1 Ca1 O3 148.99(4) . 3 ?
O1 Ca1 O3 148.99(4) . 6 ?
O3 Ca1 O3 61.86(8) 3 6 ?
O1 Ca1 O2 101.44(8) . . ?
O3 Ca1 O2 78.25(6) 3 . ?
O3 Ca1 O2 78.25(6) 6 . ?
O1 Ca1 O2 83.52(6) . 3 ?
O3 Ca1 O2 79.64(5) 3 3 ?
O3 Ca1 O2 115.35(6) 6 3 ?
O2 Ca1 O2 143.61(4) . 3 ?
O1 Ca1 O2 83.52(6) . 4_655 ?
O3 Ca1 O2 115.35(6) 3 4_655 ?
O3 Ca1 O2 79.64(5) 6 4_655 ?
O2 Ca1 O2 143.61(4) . 4_655 ?
O2 Ca1 O2 72.51(9) 3 4_655 ?
O1 Ca1 O3 57.76(4) . 8 ?
O3 Ca1 O3 148.90(3) 3 8 ?
O3 Ca1 O3 92.20(7) 6 8 ?
O2 Ca1 O3 79.88(5) . 8 ?
O2 Ca1 O3 129.77(5) 3 8 ?
O2 Ca1 O3 72.47(6) 4_655 8 ?
O1 Ca1 O3 57.76(4) . 2 ?
O3 Ca1 O3 92.20(7) 3 2 ?
O3 Ca1 O3 148.90(3) 6 2 ?
O2 Ca1 O3 79.88(5) . 2 ?
O2 Ca1 O3 72.47(6) 3 2 ?
O2 Ca1 O3 129.77(5) 4_655 2 ?
O3 Ca1 O3 105.42(7) 8 2 ?
O1 Ca1 B1 179.37(9) . 3 ?
O3 Ca1 B1 30.97(4) 3 3 ?
O3 Ca1 B1 30.97(4) 6 3 ?
O2 Ca1 B1 77.93(8) . 3 ?
O2 Ca1 B1 96.99(7) 3 3 ?
O2 Ca1 B1 96.99(7) 4_655 3 ?
O3 Ca1 B1 122.02(4) 8 3 ?
O3 Ca1 B1 122.02(4) 2 3 ?
O1 Ca1 B1 27.14(5) . 1_655 ?
O3 Ca1 B1 169.49(6) 3 1_655 ?
O3 Ca1 B1 122.24(7) 6 1_655 ?
O2 Ca1 B1 92.88(6) . 1_655 ?
O2 Ca1 B1 105.14(5) 3 1_655 ?
O2 Ca1 B1 75.15(7) 4_655 1_655 ?
O3 Ca1 B1 30.70(6) 8 1_655 ?
O3 Ca1 B1 80.58(7) 2 1_655 ?
B1 Ca1 B1 152.68(4) 3 1_655 ?
O1 Ca1 B1 27.14(5) . 2 ?
O3 Ca1 B1 122.24(7) 3 2 ?
O3 Ca1 B1 169.49(6) 6 2 ?
O2 Ca1 B1 92.88(6) . 2 ?
O2 Ca1 B1 75.15(7) 3 2 ?
O2 Ca1 B1 105.14(5) 4_655 2 ?
O3 Ca1 B1 80.58(7) 8 2 ?
O3 Ca1 B1 30.70(6) 2 2 ?
B1 Ca1 B1 152.68(4) 3 2 ?
B1 Ca1 B1 51.90(11) 1_655 2 ?
O1 Ca1 Ca1 45.70(5) . 2_655 ?
O3 Ca1 Ca1 128.55(4) 3 2_655 ?
O3 Ca1 Ca1 128.55(4) 6 2_655 ?
O2 Ca1 Ca1 147.14(5) . 2_655 ?
O2 Ca1 Ca1 49.44(3) 3 2_655 ?
O2 Ca1 Ca1 49.44(3) 4_655 2_655 ?
O3 Ca1 Ca1 80.39(4) 8 2_655 ?
O3 Ca1 Ca1 80.39(4) 2 2_655 ?
B1 Ca1 Ca1 134.93(7) 3 2_655 ?
B1 Ca1 Ca1 58.04(3) 1_655 2_655 ?
B1 Ca1 Ca1 58.04(3) 2 2_655 ?
O3 Ge1 O3 112.42(10) 3_556 4_556 ?
O3 Ge1 O3 108.02(5) 3_556 2 ?
O3 Ge1 O3 108.02(5) 4_556 2 ?
O3 Ge1 O3 108.02(5) 3_556 . ?
O3 Ge1 O3 108.02(5) 4_556 . ?
O3 Ge1 O3 112.42(10) 2 . ?
O3 Ge1 Ca1 33.45(5) 3_556 1_556 ?
O3 Ge1 Ca1 96.09(5) 4_556 1_556 ?
O3 Ge1 Ca1 86.99(5) 2 1_556 ?
O3 Ge1 Ca1 141.32(5) . 1_556 ?
O3 Ge1 Ca1 141.32(5) 3_556 3 ?
O3 Ge1 Ca1 86.99(5) 4_556 3 ?
O3 Ge1 Ca1 33.45(5) 2 3 ?
O3 Ge1 Ca1 96.09(5) . 3 ?
Ca1 Ge1 Ca1 115.377(8) 1_556 3 ?
O3 Ge1 Ca1 96.09(5) 3_556 2_556 ?
O3 Ge1 Ca1 33.45(5) 4_556 2_556 ?
O3 Ge1 Ca1 141.32(5) 2 2_556 ?
O3 Ge1 Ca1 86.99(5) . 2_556 ?
Ca1 Ge1 Ca1 98.213(14) 1_556 2_556 ?
Ca1 Ge1 Ca1 115.377(8) 3 2_556 ?
O3 Ge1 Ca1 86.99(5) 3_556 4 ?
O3 Ge1 Ca1 141.32(5) 4_556 4 ?
O3 Ge1 Ca1 96.09(5) 2 4 ?
O3 Ge1 Ca1 33.45(5) . 4 ?
Ca1 Ge1 Ca1 115.377(8) 1_556 4 ?
Ca1 Ge1 Ca1 98.213(14) 3 4 ?
Ca1 Ge1 Ca1 115.377(8) 2_556 4 ?
O3 Ge1 Ca1 84.86(5) 3_556 . ?
O3 Ge1 Ca1 146.56(5) 4_556 . ?
O3 Ge1 Ca1 38.58(5) 2 . ?
O3 Ge1 Ca1 92.11(5) . . ?
Ca1 Ge1 Ca1 82.937(6) 1_556 . ?
Ca1 Ge1 Ca1 63.997(3) 3 . ?
Ca1 Ge1 Ca1 178.850(13) 2_556 . ?
Ca1 Ge1 Ca1 63.997(3) 4 . ?
O3 Ge1 Ca1 146.56(5) 3_556 2 ?
O3 Ge1 Ca1 84.86(5) 4_556 2 ?
O3 Ge1 Ca1 92.11(5) 2 2 ?
O3 Ge1 Ca1 38.58(5) . 2 ?
Ca1 Ge1 Ca1 178.849(13) 1_556 2 ?
Ca1 Ge1 Ca1 63.997(3) 3 2 ?
Ca1 Ge1 Ca1 82.937(6) 2_556 2 ?
Ca1 Ge1 Ca1 63.997(3) 4 2 ?
Ca1 Ge1 Ca1 95.912(14) . 2 ?
O3 Ge1 Ca1 38.58(5) 3_556 4_556 ?
O3 Ge1 Ca1 92.11(5) 4_556 4_556 ?
O3 Ge1 Ca1 146.56(5) 2 4_556 ?
O3 Ge1 Ca1 84.86(5) . 4_556 ?
Ca1 Ge1 Ca1 63.997(3) 1_556 4_556 ?
Ca1 Ge1 Ca1 178.849(13) 3 4_556 ?
Ca1 Ge1 Ca1 63.997(3) 2_556 4_556 ?
Ca1 Ge1 Ca1 82.937(6) 4 4_556 ?
Ca1 Ge1 Ca1 116.647(8) . 4_556 ?
Ca1 Ge1 Ca1 116.647(8) 2 4_556 ?
O3 Ge1 Ca1 92.11(5) 3_556 3_556 ?
O3 Ge1 Ca1 38.58(5) 4_556 3_556 ?
O3 Ge1 Ca1 84.86(5) 2 3_556 ?
O3 Ge1 Ca1 146.56(5) . 3_556 ?
Ca1 Ge1 Ca1 63.997(3) 1_556 3_556 ?
Ca1 Ge1 Ca1 82.937(6) 3 3_556 ?
Ca1 Ge1 Ca1 63.997(3) 2_556 3_556 ?
Ca1 Ge1 Ca1 178.849(13) 4 3_556 ?
Ca1 Ge1 Ca1 116.648(8) . 3_556 ?
Ca1 Ge1 Ca1 116.647(8) 2 3_556 ?
Ca1 Ge1 Ca1 95.912(14) 4_556 3_556 ?
O2 B1 O1 118.5(3) 4_556 1_455 ?
O2 B1 O3 115.92(17) 4_556 8_455 ?
O1 B1 O3 101.95(17) 1_455 8_455 ?
O2 B1 O3 115.92(17) 4_556 . ?
O1 B1 O3 101.95(17) 1_455 . ?
O3 B1 O3 99.8(2) 8_455 . ?
O2 B1 Ca1 129.5(2) 4_556 4 ?
O1 B1 Ca1 112.1(2) 1_455 4 ?
O3 B1 Ca1 49.99(11) 8_455 4 ?
O3 B1 Ca1 49.99(11) . 4 ?
O2 B1 Ca1 140.02(12) 4_556 2 ?
O1 B1 Ca1 46.71(11) 1_455 2 ?
O3 B1 Ca1 104.02(16) 8_455 2 ?
O3 B1 Ca1 55.41(10) . 2 ?
Ca1 B1 Ca1 78.14(7) 4 2 ?
O2 B1 Ca1 140.02(12) 4_556 1_455 ?
O1 B1 Ca1 46.71(11) 1_455 1_455 ?
O3 B1 Ca1 55.41(10) 8_455 1_455 ?
O3 B1 Ca1 104.02(16) . 1_455 ?
Ca1 B1 Ca1 78.14(8) 4 1_455 ?
Ca1 B1 Ca1 63.92(7) 2 1_455 ?
B1 O1 B1 134.3(3) 1_655 2 ?
B1 O1 Cd1 106.15(11) 1_655 2_655 ?
B1 O1 Cd1 106.15(11) 2 2_655 ?
B1 O1 Ca1 106.15(11) 1_655 2_655 ?
B1 O1 Ca1 106.15(11) 2 2_655 ?
Cd1 O1 Ca1 0.00(3) 2_655 2_655 ?
B1 O1 Ca1 106.15(11) 1_655 . ?
B1 O1 Ca1 106.15(11) 2 . ?
Cd1 O1 Ca1 88.60(11) 2_655 . ?
Ca1 O1 Ca1 88.60(11) 2_655 . ?
B1 O2 Ca1 128.47(19) 3_556 . ?
B1 O2 Cd1 114.63(13) 3_556 4 ?
Ca1 O2 Cd1 103.77(7) . 4 ?
B1 O2 Ca1 114.63(13) 3_556 4 ?
Ca1 O2 Ca1 103.77(7) . 4 ?
Cd1 O2 Ca1 0.000(8) 4 4 ?
B1 O2 Ca1 114.63(13) 3_556 3_565 ?
Ca1 O2 Ca1 103.77(7) . 3_565 ?
Cd1 O2 Ca1 81.12(7) 4 3_565 ?
Ca1 O2 Ca1 81.12(7) 4 3_565 ?
B1 O2 Cd1 114.63(13) 3_556 3_565 ?
Ca1 O2 Cd1 103.77(7) . 3_565 ?
Cd1 O2 Cd1 81.12(7) 4 3_565 ?
Ca1 O2 Cd1 81.12(7) 4 3_565 ?
Ca1 O2 Cd1 0.00(2) 3_565 3_565 ?
B1 O3 Ge1 117.02(14) . . ?
B1 O3 Cd1 99.04(12) . 4 ?
Ge1 O3 Cd1 122.29(8) . 4 ?
B1 O3 Ca1 99.04(12) . 4 ?
Ge1 O3 Ca1 122.29(8) . 4 ?
Cd1 O3 Ca1 0.00(2) 4 4 ?
B1 O3 Ca1 93.88(14) . 2 ?
Ge1 O3 Ca1 116.00(7) . 2 ?
Cd1 O3 Ca1 103.79(6) 4 2 ?
Ca1 O3 Ca1 103.79(6) 4 2 ?
B1 O3 Cd1 93.88(14) . 2 ?
Ge1 O3 Cd1 116.00(7) . 2 ?
Cd1 O3 Cd1 103.79(6) 4 2 ?
Ca1 O3 Cd1 103.79(6) 4 2 ?
Ca1 O3 Cd1 0.00(2) 2 2 ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.63
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.130
