# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528693'
_audit_update_record             
;
2017-01-20 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca O3 Rb'
_chemical_formula_weight         184.36

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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P2(1)3

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

_cell_length_a                   7.430(6)
_cell_length_b                   7.430(6)
_cell_length_c                   7.430(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     410.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    389
_cell_measurement_theta_min      4.75
_cell_measurement_theta_max      21.96

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_absorpt_coefficient_mu    13.162
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5553
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2507
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.88
_diffrn_reflns_theta_max         27.47
_reflns_number_total             322
_reflns_number_gt                281
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0177P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         322
_refine_ls_number_parameters     19
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0479
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Rb1 Rb 0.62104(6) 0.87896(6) 0.12104(6) 0.0255(2) Uani 1 3 d S . .
Ca1 Ca 1.10070(11) 1.10070(11) 0.10070(11) 0.0136(3) Uani 1 3 d S . .
B1 B 1.1705(7) 0.8295(7) 0.3295(7) 0.0174(19) Uani 1 3 d S . .
O1 O 1.0280(4) 0.8160(4) 0.2094(4) 0.0179(7) 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
Rb1 O1 2.933(4) 9_564 ?
Rb1 O1 2.933(4) 4_465 ?
Rb1 O1 2.933(4) 7_574 ?
Rb1 O1 3.129(4) 12_664 ?
Rb1 O1 3.129(4) . ?
Rb1 O1 3.129(4) 6_566 ?
Rb1 Ca1 3.581(3) 3_745 ?
Rb1 B1 3.706(7) 3_755 ?
Rb1 B1 3.706(7) 4_465 ?
Rb1 B1 3.706(7) 1_455 ?
Rb1 B1 3.752(10) 2_674 ?
Rb1 Ca1 3.929(3) . ?
Ca1 O1 2.327(3) . ?
Ca1 O1 2.327(4) 9_564 ?
Ca1 O1 2.327(3) 5_654 ?
Ca1 O1 2.338(4) 7_674 ?
Ca1 O1 2.338(4) 3_755 ?
Ca1 O1 2.338(4) 11_566 ?
Ca1 B1 2.687(3) 3_755 ?
Ca1 B1 2.687(3) . ?
Ca1 B1 2.687(3) 2_774 ?
Ca1 Rb1 3.581(3) 3_755 ?
Ca1 Rb1 3.929(3) 2_674 ?
B1 O1 1.388(3) 7_674 ?
B1 O1 1.388(3) . ?
B1 O1 1.388(3) 10_756 ?
B1 Ca1 2.687(3) 2_775 ?
B1 Ca1 2.687(3) 3_745 ?
B1 Rb1 3.706(7) 4_565 ?
B1 Rb1 3.706(7) 3_745 ?
B1 Rb1 3.706(7) 1_655 ?
B1 Rb1 3.752(10) 2_675 ?
O1 Ca1 2.338(4) 3_745 ?
O1 Rb1 2.933(4) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Rb1 O1 109.42(6) 9_564 4_465 ?
O1 Rb1 O1 109.42(6) 9_564 7_574 ?
O1 Rb1 O1 109.42(6) 4_465 7_574 ?
O1 Rb1 O1 109.24(7) 9_564 12_664 ?
O1 Rb1 O1 137.76(6) 4_465 12_664 ?
O1 Rb1 O1 72.38(11) 7_574 12_664 ?
O1 Rb1 O1 72.38(11) 9_564 . ?
O1 Rb1 O1 109.24(7) 4_465 . ?
O1 Rb1 O1 137.76(6) 7_574 . ?
O1 Rb1 O1 67.76(9) 12_664 . ?
O1 Rb1 O1 137.76(6) 9_564 6_566 ?
O1 Rb1 O1 72.38(11) 4_465 6_566 ?
O1 Rb1 O1 109.24(7) 7_574 6_566 ?
O1 Rb1 O1 67.76(9) 12_664 6_566 ?
O1 Rb1 O1 67.76(9) . 6_566 ?
O1 Rb1 Ca1 109.52(6) 9_564 3_745 ?
O1 Rb1 Ca1 109.52(6) 4_465 3_745 ?
O1 Rb1 Ca1 109.52(6) 7_574 3_745 ?
O1 Rb1 Ca1 40.07(6) 12_664 3_745 ?
O1 Rb1 Ca1 40.07(6) . 3_745 ?
O1 Rb1 Ca1 40.07(6) 6_566 3_745 ?
O1 Rb1 B1 20.14(12) 9_564 3_755 ?
O1 Rb1 B1 128.87(12) 4_465 3_755 ?
O1 Rb1 B1 95.04(10) 7_574 3_755 ?
O1 Rb1 B1 91.79(10) 12_664 3_755 ?
O1 Rb1 B1 73.16(6) . 3_755 ?
O1 Rb1 B1 140.37(6) 6_566 3_755 ?
Ca1 Rb1 B1 102.88(3) 3_745 3_755 ?
O1 Rb1 B1 95.04(10) 9_564 4_465 ?
O1 Rb1 B1 20.14(12) 4_465 4_465 ?
O1 Rb1 B1 128.87(12) 7_574 4_465 ?
O1 Rb1 B1 140.37(6) 12_664 4_465 ?
O1 Rb1 B1 91.79(10) . 4_465 ?
O1 Rb1 B1 73.16(6) 6_566 4_465 ?
Ca1 Rb1 B1 102.88(3) 3_745 4_465 ?
B1 Rb1 B1 115.18(2) 3_755 4_465 ?
O1 Rb1 B1 128.87(12) 9_564 1_455 ?
O1 Rb1 B1 95.04(11) 4_465 1_455 ?
O1 Rb1 B1 20.14(12) 7_574 1_455 ?
O1 Rb1 B1 73.16(6) 12_664 1_455 ?
O1 Rb1 B1 140.37(6) . 1_455 ?
O1 Rb1 B1 91.79(10) 6_566 1_455 ?
Ca1 Rb1 B1 102.88(3) 3_745 1_455 ?
B1 Rb1 B1 115.18(2) 3_755 1_455 ?
B1 Rb1 B1 115.18(2) 4_465 1_455 ?
O1 Rb1 B1 70.48(6) 9_564 2_674 ?
O1 Rb1 B1 70.48(6) 4_465 2_674 ?
O1 Rb1 B1 70.48(6) 7_574 2_674 ?
O1 Rb1 B1 139.93(6) 12_664 2_674 ?
O1 Rb1 B1 139.93(6) . 2_674 ?
O1 Rb1 B1 139.93(6) 6_566 2_674 ?
Ca1 Rb1 B1 180.00(7) 3_745 2_674 ?
B1 Rb1 B1 77.12(3) 3_755 2_674 ?
B1 Rb1 B1 77.12(3) 4_465 2_674 ?
B1 Rb1 B1 77.12(3) 1_455 2_674 ?
O1 Rb1 Ca1 36.10(6) 9_564 . ?
O1 Rb1 Ca1 112.87(6) 4_465 . ?
O1 Rb1 Ca1 132.79(6) 7_574 . ?
O1 Rb1 Ca1 89.41(5) 12_664 . ?
O1 Rb1 Ca1 36.32(6) . . ?
O1 Rb1 Ca1 102.74(5) 6_566 . ?
Ca1 Rb1 Ca1 74.967(12) 3_745 . ?
B1 Rb1 Ca1 41.07(6) 3_755 . ?
B1 Rb1 Ca1 92.90(10) 4_465 . ?
B1 Rb1 Ca1 151.26(9) 1_455 . ?
B1 Rb1 Ca1 105.033(12) 2_674 . ?
O1 Ca1 O1 100.66(10) . 9_564 ?
O1 Ca1 O1 100.66(10) . 5_654 ?
O1 Ca1 O1 100.66(10) 9_564 5_654 ?
O1 Ca1 O1 62.03(14) . 7_674 ?
O1 Ca1 O1 148.13(8) 9_564 7_674 ?
O1 Ca1 O1 108.51(3) 5_654 7_674 ?
O1 Ca1 O1 108.51(3) . 3_755 ?
O1 Ca1 O1 62.03(14) 9_564 3_755 ?
O1 Ca1 O1 148.13(8) 5_654 3_755 ?
O1 Ca1 O1 96.53(10) 7_674 3_755 ?
O1 Ca1 O1 148.13(8) . 11_566 ?
O1 Ca1 O1 108.51(3) 9_564 11_566 ?
O1 Ca1 O1 62.03(14) 5_654 11_566 ?
O1 Ca1 O1 96.53(10) 7_674 11_566 ?
O1 Ca1 O1 96.53(10) 3_755 11_566 ?
O1 Ca1 B1 109.5(2) . 3_755 ?
O1 Ca1 B1 31.11(7) 9_564 3_755 ?
O1 Ca1 B1 125.63(13) 5_654 3_755 ?
O1 Ca1 B1 125.40(11) 7_674 3_755 ?
O1 Ca1 B1 31.10(7) 3_755 3_755 ?
O1 Ca1 B1 102.1(2) 11_566 3_755 ?
O1 Ca1 B1 31.11(7) . . ?
O1 Ca1 B1 125.63(13) 9_564 . ?
O1 Ca1 B1 109.5(2) 5_654 . ?
O1 Ca1 B1 31.10(7) 7_674 . ?
O1 Ca1 B1 102.1(2) 3_755 . ?
O1 Ca1 B1 125.40(11) 11_566 . ?
B1 Ca1 B1 119.810(13) 3_755 . ?
O1 Ca1 B1 125.63(13) . 2_774 ?
O1 Ca1 B1 109.5(2) 9_564 2_774 ?
O1 Ca1 B1 31.11(7) 5_654 2_774 ?
O1 Ca1 B1 102.1(2) 7_674 2_774 ?
O1 Ca1 B1 125.40(11) 3_755 2_774 ?
O1 Ca1 B1 31.10(7) 11_566 2_774 ?
B1 Ca1 B1 119.810(12) 3_755 2_774 ?
B1 Ca1 B1 119.810(12) . 2_774 ?
O1 Ca1 Rb1 117.28(8) . 3_755 ?
O1 Ca1 Rb1 117.28(8) 9_564 3_755 ?
O1 Ca1 Rb1 117.28(8) 5_654 3_755 ?
O1 Ca1 Rb1 59.50(8) 7_674 3_755 ?
O1 Ca1 Rb1 59.50(8) 3_755 3_755 ?
O1 Ca1 Rb1 59.50(8) 11_566 3_755 ?
B1 Ca1 Rb1 87.49(8) 3_755 3_755 ?
B1 Ca1 Rb1 87.49(8) . 3_755 ?
B1 Ca1 Rb1 87.49(8) 2_774 3_755 ?
O1 Ca1 Rb1 52.78(7) . . ?
O1 Ca1 Rb1 47.95(7) 9_564 . ?
O1 Ca1 Rb1 104.62(9) 5_654 . ?
O1 Ca1 Rb1 110.46(7) 7_674 . ?
O1 Ca1 Rb1 83.85(7) 3_755 . ?
O1 Ca1 Rb1 152.83(7) 11_566 . ?
B1 Ca1 Rb1 65.02(16) 3_755 . ?
B1 Ca1 Rb1 80.58(7) . . ?
B1 Ca1 Rb1 133.13(12) 2_774 . ?
Rb1 Ca1 Rb1 138.035(14) 3_755 . ?
O1 Ca1 Rb1 104.62(9) . 2_674 ?
O1 Ca1 Rb1 52.78(7) 9_564 2_674 ?
O1 Ca1 Rb1 47.95(7) 5_654 2_674 ?
O1 Ca1 Rb1 152.83(7) 7_674 2_674 ?
O1 Ca1 Rb1 110.46(7) 3_755 2_674 ?
O1 Ca1 Rb1 83.85(7) 11_566 2_674 ?
B1 Ca1 Rb1 80.58(7) 3_755 2_674 ?
B1 Ca1 Rb1 133.13(12) . 2_674 ?
B1 Ca1 Rb1 65.02(16) 2_774 2_674 ?
Rb1 Ca1 Rb1 138.035(14) 3_755 2_674 ?
Rb1 Ca1 Rb1 70.77(2) . 2_674 ?
O1 B1 O1 119.92(4) 7_674 . ?
O1 B1 O1 119.92(4) 7_674 10_756 ?
O1 B1 O1 119.92(4) . 10_756 ?
O1 B1 Ca1 60.01(14) 7_674 2_775 ?
O1 B1 Ca1 168.1(6) . 2_775 ?
O1 B1 Ca1 60.43(14) 10_756 2_775 ?
O1 B1 Ca1 168.1(6) 7_674 3_745 ?
O1 B1 Ca1 60.43(14) . 3_745 ?
O1 B1 Ca1 60.01(14) 10_756 3_745 ?
Ca1 B1 Ca1 116.86(12) 2_775 3_745 ?
O1 B1 Ca1 60.43(13) 7_674 . ?
O1 B1 Ca1 60.01(14) . . ?
O1 B1 Ca1 168.1(6) 10_756 . ?
Ca1 B1 Ca1 116.86(12) 2_775 . ?
Ca1 B1 Ca1 116.86(12) 3_745 . ?
O1 B1 Rb1 108.5(3) 7_674 4_565 ?
O1 B1 Rb1 46.7(3) . 4_565 ?
O1 B1 Rb1 115.3(3) 10_756 4_565 ?
Ca1 B1 Rb1 145.2(3) 2_775 4_565 ?
Ca1 B1 Rb1 80.54(10) 3_745 4_565 ?
Ca1 B1 Rb1 73.91(11) . 4_565 ?
O1 B1 Rb1 115.3(3) 7_674 3_745 ?
O1 B1 Rb1 108.5(3) . 3_745 ?
O1 B1 Rb1 46.7(3) 10_756 3_745 ?
Ca1 B1 Rb1 80.54(10) 2_775 3_745 ?
Ca1 B1 Rb1 73.91(11) 3_745 3_745 ?
Ca1 B1 Rb1 145.2(3) . 3_745 ?
Rb1 B1 Rb1 75.74(16) 4_565 3_745 ?
O1 B1 Rb1 46.7(3) 7_674 1_655 ?
O1 B1 Rb1 115.3(3) . 1_655 ?
O1 B1 Rb1 108.5(3) 10_756 1_655 ?
Ca1 B1 Rb1 73.91(11) 2_775 1_655 ?
Ca1 B1 Rb1 145.2(3) 3_745 1_655 ?
Ca1 B1 Rb1 80.54(10) . 1_655 ?
Rb1 B1 Rb1 75.74(16) 4_565 1_655 ?
Rb1 B1 Rb1 75.74(16) 3_745 1_655 ?
O1 B1 Rb1 88.4(4) 7_674 2_675 ?
O1 B1 Rb1 88.4(4) . 2_675 ?
O1 B1 Rb1 88.4(4) 10_756 2_675 ?
Ca1 B1 Rb1 79.7(2) 2_775 2_675 ?
Ca1 B1 Rb1 79.7(2) 3_745 2_675 ?
Ca1 B1 Rb1 79.7(2) . 2_675 ?
Rb1 B1 Rb1 134.86(10) 4_565 2_675 ?
Rb1 B1 Rb1 134.86(10) 3_745 2_675 ?
Rb1 B1 Rb1 134.86(10) 1_655 2_675 ?
B1 O1 Ca1 88.88(15) . . ?
B1 O1 Ca1 88.48(16) . 3_745 ?
Ca1 O1 Ca1 157.87(13) . 3_745 ?
B1 O1 Rb1 113.2(4) . 4_565 ?
Ca1 O1 Rb1 95.95(10) . 4_565 ?
Ca1 O1 Rb1 105.28(10) 3_745 4_565 ?
B1 O1 Rb1 149.4(4) . . ?
Ca1 O1 Rb1 90.90(10) . . ?
Ca1 O1 Rb1 80.43(9) 3_745 . ?
Rb1 O1 Rb1 97.23(8) 4_565 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.088
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528692'
_audit_update_record             
;
2017-01-20 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca Cs O3'
_chemical_formula_weight         231.80

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P2(1)3

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

_cell_length_a                   7.572(3)
_cell_length_b                   7.572(3)
_cell_length_c                   7.572(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     434.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    617
_cell_measurement_theta_min      3.80
_cell_measurement_theta_max      25.64

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             416
_exptl_absorpt_coefficient_mu    9.560
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5718
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2594
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0413
_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       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.81
_diffrn_reflns_theta_max         27.53
_reflns_number_total             336
_reflns_number_gt                305
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0089P)²+1.8492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_number_reflns         336
_refine_ls_number_parameters     19
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0457
_refine_ls_wR_factor_gt          0.0438
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.900
_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
Cs1 Cs 0.63993(5) 0.36007(5) 0.86007(5) 0.02456(17) Uani 1 3 d S . .
Ca1 Ca 0.85682(13) 0.85682(13) 0.85682(13) 0.0147(3) Uani 1 3 d S . .
B1 B 1.0960(8) 0.5960(8) 0.9040(8) 0.017(2) Uani 1 3 d S . .
O1 O 1.0869(6) 0.7337(5) 1.0242(5) 0.0204(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O1 3.150(4) 2_664 ?
Cs1 O1 3.150(4) 8_746 ?
Cs1 O1 3.150(4) 9_545 ?
Cs1 O1 3.223(4) 4_467 ?
Cs1 O1 3.223(4) 6_467 ?
Cs1 O1 3.223(4) 11_467 ?
Cs1 B1 3.464(11) 3_746 ?
Cs1 O1 3.696(4) 12_664 ?
Cs1 O1 3.696(4) 3_746 ?
Cs1 O1 3.696(4) 5_545 ?
Cs1 Ca1 3.713(2) 4_467 ?
Cs1 B1 3.902(8) . ?
Ca1 O1 2.336(5) 12_674 ?
Ca1 O1 2.336(5) 8_746 ?
Ca1 O1 2.336(5) 4_467 ?
Ca1 O1 2.347(5) 5 ?
Ca1 O1 2.347(5) . ?
Ca1 O1 2.347(5) 9 ?
Ca1 B1 2.7032(17) 3_756 ?
Ca1 B1 2.7032(17) . ?
Ca1 B1 2.7032(17) 4_467 ?
Ca1 Cs1 3.713(2) 4_567 ?
Ca1 Cs1 4.104(2) 2_664 ?
Ca1 Cs1 4.104(2) 3_656 ?
B1 O1 1.386(4) 8_746 ?
B1 O1 1.386(4) . ?
B1 O1 1.386(4) 11_567 ?
B1 Ca1 2.7032(17) 3_746 ?
B1 Ca1 2.7032(17) 4_567 ?
B1 Cs1 3.464(11) 3_756 ?
B1 Cs1 3.902(8) 2_665 ?
B1 Cs1 3.902(8) 4_557 ?
O1 Ca1 2.336(5) 4_567 ?
O1 Cs1 3.150(4) 2_665 ?
O1 Cs1 3.223(4) 4_567 ?
O1 Cs1 3.696(4) 3_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cs1 O1 112.41(7) 2_664 8_746 ?
O1 Cs1 O1 112.41(7) 2_664 9_545 ?
O1 Cs1 O1 112.41(7) 8_746 9_545 ?
O1 Cs1 O1 111.51(10) 2_664 4_467 ?
O1 Cs1 O1 68.99(16) 8_746 4_467 ?
O1 Cs1 O1 130.56(8) 9_545 4_467 ?
O1 Cs1 O1 130.56(8) 2_664 6_467 ?
O1 Cs1 O1 111.51(10) 8_746 6_467 ?
O1 Cs1 O1 68.99(16) 9_545 6_467 ?
O1 Cs1 O1 65.66(12) 4_467 6_467 ?
O1 Cs1 O1 68.99(16) 2_664 11_467 ?
O1 Cs1 O1 130.56(8) 8_746 11_467 ?
O1 Cs1 O1 111.51(10) 9_545 11_467 ?
O1 Cs1 O1 65.66(12) 4_467 11_467 ?
O1 Cs1 O1 65.66(12) 6_467 11_467 ?
O1 Cs1 B1 73.65(8) 2_664 3_746 ?
O1 Cs1 B1 73.65(8) 8_746 3_746 ?
O1 Cs1 B1 73.65(8) 9_545 3_746 ?
O1 Cs1 B1 141.24(8) 4_467 3_746 ?
O1 Cs1 B1 141.24(8) 6_467 3_746 ?
O1 Cs1 B1 141.24(8) 11_467 3_746 ?
O1 Cs1 O1 60.79(15) 2_664 12_664 ?
O1 Cs1 O1 95.40(9) 8_746 12_664 ?
O1 Cs1 O1 67.118(15) 9_545 12_664 ?
O1 Cs1 O1 159.33(5) 4_467 12_664 ?
O1 Cs1 O1 134.62(14) 6_467 12_664 ?
O1 Cs1 O1 122.06(8) 11_467 12_664 ?
B1 Cs1 O1 22.01(6) 3_746 12_664 ?
O1 Cs1 O1 67.118(16) 2_664 3_746 ?
O1 Cs1 O1 60.79(15) 8_746 3_746 ?
O1 Cs1 O1 95.40(9) 9_545 3_746 ?
O1 Cs1 O1 122.06(8) 4_467 3_746 ?
O1 Cs1 O1 159.33(5) 6_467 3_746 ?
O1 Cs1 O1 134.62(14) 11_467 3_746 ?
B1 Cs1 O1 22.01(6) 3_746 3_746 ?
O1 Cs1 O1 37.88(11) 12_664 3_746 ?
O1 Cs1 O1 95.40(9) 2_664 5_545 ?
O1 Cs1 O1 67.118(15) 8_746 5_545 ?
O1 Cs1 O1 60.79(15) 9_545 5_545 ?
O1 Cs1 O1 134.62(14) 4_467 5_545 ?
O1 Cs1 O1 122.06(8) 6_467 5_545 ?
O1 Cs1 O1 159.33(5) 11_467 5_545 ?
B1 Cs1 O1 22.01(6) 3_746 5_545 ?
O1 Cs1 O1 37.88(11) 12_664 5_545 ?
O1 Cs1 O1 37.88(11) 3_746 5_545 ?
O1 Cs1 Ca1 106.35(8) 2_664 4_467 ?
O1 Cs1 Ca1 106.35(8) 8_746 4_467 ?
O1 Cs1 Ca1 106.35(8) 9_545 4_467 ?
O1 Cs1 Ca1 38.76(8) 4_467 4_467 ?
O1 Cs1 Ca1 38.76(8) 6_467 4_467 ?
O1 Cs1 Ca1 38.76(8) 11_467 4_467 ?
B1 Cs1 Ca1 180.00(9) 3_746 4_467 ?
O1 Cs1 Ca1 157.99(6) 12_664 4_467 ?
O1 Cs1 Ca1 157.99(6) 3_746 4_467 ?
O1 Cs1 Ca1 157.99(6) 5_545 4_467 ?
O1 Cs1 B1 130.89(13) 2_664 . ?
O1 Cs1 B1 19.11(14) 8_746 . ?
O1 Cs1 B1 97.10(12) 9_545 . ?
O1 Cs1 B1 69.52(8) 4_467 . ?
O1 Cs1 B1 95.87(12) 6_467 . ?
O1 Cs1 B1 135.19(7) 11_467 . ?
B1 Cs1 B1 78.61(3) 3_746 . ?
O1 Cs1 B1 100.31(7) 12_664 . ?
O1 Cs1 B1 71.97(10) 3_746 . ?
O1 Cs1 B1 65.26(6) 5_545 . ?
Ca1 Cs1 B1 101.39(3) 4_467 . ?
O1 Ca1 O1 101.18(13) 12_674 8_746 ?
O1 Ca1 O1 101.18(13) 12_674 4_467 ?
O1 Ca1 O1 101.18(13) 8_746 4_467 ?
O1 Ca1 O1 61.62(19) 12_674 5 ?
O1 Ca1 O1 108.94(2) 8_746 5 ?
O1 Ca1 O1 147.47(11) 4_467 5 ?
O1 Ca1 O1 147.47(11) 12_674 . ?
O1 Ca1 O1 61.62(19) 8_746 . ?
O1 Ca1 O1 108.94(2) 4_467 . ?
O1 Ca1 O1 96.23(14) 5 . ?
O1 Ca1 O1 108.94(2) 12_674 9 ?
O1 Ca1 O1 147.47(11) 8_746 9 ?
O1 Ca1 O1 61.62(19) 4_467 9 ?
O1 Ca1 O1 96.23(14) 5 9 ?
O1 Ca1 O1 96.23(14) . 9 ?
O1 Ca1 B1 30.83(10) 12_674 3_756 ?
O1 Ca1 B1 108.7(3) 8_746 3_756 ?
O1 Ca1 B1 126.44(17) 4_467 3_756 ?
O1 Ca1 B1 30.83(10) 5 3_756 ?
O1 Ca1 B1 124.21(15) . 3_756 ?
O1 Ca1 B1 103.5(2) 9 3_756 ?
O1 Ca1 B1 126.44(17) 12_674 . ?
O1 Ca1 B1 30.83(10) 8_746 . ?
O1 Ca1 B1 108.7(3) 4_467 . ?
O1 Ca1 B1 103.5(2) 5 . ?
O1 Ca1 B1 30.83(10) . . ?
O1 Ca1 B1 124.21(15) 9 . ?
B1 Ca1 B1 119.831(14) 3_756 . ?
O1 Ca1 B1 108.7(3) 12_674 4_467 ?
O1 Ca1 B1 126.44(17) 8_746 4_467 ?
O1 Ca1 B1 30.83(10) 4_467 4_467 ?
O1 Ca1 B1 124.21(15) 5 4_467 ?
O1 Ca1 B1 103.5(2) . 4_467 ?
O1 Ca1 B1 30.83(10) 9 4_467 ?
B1 Ca1 B1 119.831(13) 3_756 4_467 ?
B1 Ca1 B1 119.831(13) . 4_467 ?
O1 Ca1 Cs1 116.85(10) 12_674 4_567 ?
O1 Ca1 Cs1 116.85(10) 8_746 4_567 ?
O1 Ca1 Cs1 116.85(10) 4_467 4_567 ?
O1 Ca1 Cs1 59.28(10) 5 4_567 ?
O1 Ca1 Cs1 59.28(10) . 4_567 ?
O1 Ca1 Cs1 59.28(10) 9 4_567 ?
B1 Ca1 Cs1 87.64(9) 3_756 4_567 ?
B1 Ca1 Cs1 87.64(9) . 4_567 ?
B1 Ca1 Cs1 87.64(9) 4_467 4_567 ?
O1 Ca1 Cs1 49.79(10) 12_674 2_664 ?
O1 Ca1 Cs1 51.60(10) 8_746 2_664 ?
O1 Ca1 Cs1 103.97(11) 4_467 2_664 ?
O1 Ca1 Cs1 85.97(10) 5 2_664 ?
O1 Ca1 Cs1 109.35(10) . 2_664 ?
O1 Ca1 Cs1 153.97(10) 9 2_664 ?
B1 Ca1 Cs1 66.28(18) 3_756 2_664 ?
B1 Ca1 Cs1 79.91(8) . 2_664 ?
B1 Ca1 Cs1 132.16(13) 4_467 2_664 ?
Cs1 Ca1 Cs1 139.170(16) 4_567 2_664 ?
O1 Ca1 Cs1 51.60(10) 12_674 3_656 ?
O1 Ca1 Cs1 103.97(11) 8_746 3_656 ?
O1 Ca1 Cs1 49.79(10) 4_467 3_656 ?
O1 Ca1 Cs1 109.35(10) 5 3_656 ?
O1 Ca1 Cs1 153.97(10) . 3_656 ?
O1 Ca1 Cs1 85.97(10) 9 3_656 ?
B1 Ca1 Cs1 79.91(8) 3_756 3_656 ?
B1 Ca1 Cs1 132.16(13) . 3_656 ?
B1 Ca1 Cs1 66.28(18) 4_467 3_656 ?
Cs1 Ca1 Cs1 139.170(16) 4_567 3_656 ?
Cs1 Ca1 Cs1 68.97(3) 2_664 3_656 ?
O1 B1 O1 119.93(4) 8_746 . ?
O1 B1 O1 119.93(4) 8_746 11_567 ?
O1 B1 O1 119.93(4) . 11_567 ?
O1 B1 Ca1 60.25(18) 8_746 3_746 ?
O1 B1 Ca1 172.1(7) . 3_746 ?
O1 B1 Ca1 59.78(19) 11_567 3_746 ?
O1 B1 Ca1 172.1(7) 8_746 4_567 ?
O1 B1 Ca1 59.78(19) . 4_567 ?
O1 B1 Ca1 60.25(19) 11_567 4_567 ?
Ca1 B1 Ca1 118.78(9) 3_746 4_567 ?
O1 B1 Ca1 59.78(19) 8_746 . ?
O1 B1 Ca1 60.25(19) . . ?
O1 B1 Ca1 172.1(7) 11_567 . ?
Ca1 B1 Ca1 118.78(9) 3_746 . ?
Ca1 B1 Ca1 118.78(9) 4_567 . ?
O1 B1 Cs1 88.5(5) 8_746 3_756 ?
O1 B1 Cs1 88.5(5) . 3_756 ?
O1 B1 Cs1 88.5(5) 11_567 3_756 ?
Ca1 B1 Cs1 83.6(2) 3_746 3_756 ?
Ca1 B1 Cs1 83.6(2) 4_567 3_756 ?
Ca1 B1 Cs1 83.6(2) . 3_756 ?
O1 B1 Cs1 48.1(4) 8_746 . ?
O1 B1 Cs1 110.9(4) . . ?
O1 B1 Cs1 111.7(4) 11_567 . ?
Ca1 B1 Cs1 75.41(13) 3_746 . ?
Ca1 B1 Cs1 139.8(3) 4_567 . ?
Ca1 B1 Cs1 74.36(13) . . ?
Cs1 B1 Cs1 136.55(11) 3_756 . ?
O1 B1 Cs1 111.7(4) 8_746 2_665 ?
O1 B1 Cs1 48.1(4) . 2_665 ?
O1 B1 Cs1 110.9(4) 11_567 2_665 ?
Ca1 B1 Cs1 139.8(3) 3_746 2_665 ?
Ca1 B1 Cs1 74.36(13) 4_567 2_665 ?
Ca1 B1 Cs1 75.41(13) . 2_665 ?
Cs1 B1 Cs1 136.55(11) 3_756 2_665 ?
Cs1 B1 Cs1 73.11(17) . 2_665 ?
O1 B1 Cs1 110.9(4) 8_746 4_557 ?
O1 B1 Cs1 111.7(4) . 4_557 ?
O1 B1 Cs1 48.1(4) 11_567 4_557 ?
Ca1 B1 Cs1 74.36(13) 3_746 4_557 ?
Ca1 B1 Cs1 75.41(13) 4_567 4_557 ?
Ca1 B1 Cs1 139.8(3) . 4_557 ?
Cs1 B1 Cs1 136.55(11) 3_756 4_557 ?
Cs1 B1 Cs1 73.11(17) . 4_557 ?
Cs1 B1 Cs1 73.11(17) 2_665 4_557 ?
B1 O1 Ca1 89.4(2) . 4_567 ?
B1 O1 Ca1 88.9(2) . . ?
Ca1 O1 Ca1 166.89(19) 4_567 . ?
B1 O1 Cs1 112.8(5) . 2_665 ?
Ca1 O1 Cs1 95.71(13) 4_567 2_665 ?
Ca1 O1 Cs1 96.93(13) . 2_665 ?
B1 O1 Cs1 152.9(5) . 4_567 ?
Ca1 O1 Cs1 93.79(13) 4_567 4_567 ?
Ca1 O1 Cs1 81.96(12) . 4_567 ?
Cs1 O1 Cs1 93.64(10) 2_665 4_567 ?
B1 O1 Cs1 69.5(5) . 3_756 ?
Ca1 O1 Cs1 83.69(11) 4_567 3_756 ?
Ca1 O1 Cs1 83.54(11) . 3_756 ?
Cs1 O1 Cs1 177.61(13) 2_665 3_756 ?
Cs1 O1 Cs1 84.10(9) 4_567 3_756 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.110
