# 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 1563594'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-08-28 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 Cs Na4 O13 P3'
_chemical_formula_weight         547.40

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'
Cs Cs -0.3680 2.1192 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   24.5034(9)
_cell_length_b                   6.7673(2)
_cell_length_c                   14.7803(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2450.90(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8301
_cell_measurement_theta_min      3.0102
_cell_measurement_theta_max      27.0836

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   sadabs

_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  bruker-CCD
_diffrn_measurement_method       'w scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14138
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.08
_reflns_number_total             4997
_reflns_number_gt                4568
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0282P)²+3.1907P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_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   0.00
_refine_ls_number_reflns         4997
_refine_ls_number_parameters     415
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.78140(8) -0.7231(2) 0.27336(13) 0.0121(4) Uani 1 1 d . . .
P2 P -0.82696(8) -0.72625(19) 0.02830(13) 0.0077(4) Uani 1 1 d . . .
P3 P -0.68233(7) -1.20610(19) 0.13424(12) 0.0092(3) Uani 1 1 d . . .
O1 O -0.6653(2) -1.2099(6) 0.2304(4) 0.0170(12) Uani 1 1 d . . .
O2 O -0.79896(15) -0.5225(5) 0.0500(3) 0.0090(8) Uani 1 1 d . . .
O3 O -0.71716(14) -0.6520(5) 0.1152(3) 0.0085(8) Uani 1 1 d . . .
O4 O -0.78020(14) -0.8824(5) 0.0475(3) 0.0094(8) Uani 1 1 d . . .
O5 O -0.7383(2) -0.6862(7) 0.3444(4) 0.0355(14) Uani 1 1 d . . .
O7 O -0.8406(2) -0.7306(6) -0.0705(4) 0.0160(12) Uani 1 1 d . . .
O8 O -0.76234(16) -0.8919(5) 0.2086(3) 0.0145(9) Uani 1 1 d . . .
O9 O -0.64228(15) -1.3007(5) 0.0717(3) 0.0139(9) Uani 1 1 d . . .
O10 O -0.74029(15) -1.3022(5) 0.1210(3) 0.0120(8) Uani 1 1 d . . .
O11 O -0.69249(14) -0.9890(5) 0.1010(3) 0.0115(8) Uani 1 1 d . . .
O12 O -0.78820(15) -0.5339(5) 0.2134(3) 0.0121(8) Uani 1 1 d . . .
O13 O -0.8369(2) -0.7763(6) 0.3085(4) 0.0247(12) Uani 1 1 d . . .
O14 O -0.8736(2) -0.7571(5) 0.0927(4) 0.0126(10) Uani 1 1 d . . .
B1 B -0.7366(2) -0.8507(9) 0.1185(4) 0.0080(12) Uani 1 1 d . . .
B4 B -0.7580(3) -0.5053(8) 0.1255(4) 0.0099(12) Uani 1 1 d U . .
P4 P -0.52960(8) -0.73340(19) 0.24824(14) 0.0124(4) Uani 1 1 d . . .
P5 P -0.57718(8) -0.73205(19) 0.49338(14) 0.0089(4) Uani 1 1 d . . .
P6 P -0.43200(8) -0.25415(18) 0.38909(13) 0.0111(4) Uani 1 1 d . . .
O15 O -0.4866(2) -0.7688(6) 0.1796(4) 0.0286(13) Uani 1 1 d . . .
O16 O -0.5849(2) -0.6777(6) 0.2123(3) 0.0266(11) Uani 1 1 d . . .
O17 O -0.53770(14) -0.9233(5) 0.3094(3) 0.0098(8) Uani 1 1 d . . .
O18 O -0.51095(17) -0.5644(5) 0.3140(3) 0.0166(9) Uani 1 1 d . . .
O19 O -0.62431(18) -0.7024(5) 0.4301(3) 0.0106(9) Uani 1 1 d . . .
O20 O -0.5918(2) -0.7246(5) 0.5916(4) 0.0174(12) Uani 1 1 d . . .
O21 O -0.53070(14) -0.5764(5) 0.4747(3) 0.0114(8) Uani 1 1 d . . .
O22 O -0.54940(15) -0.9354(5) 0.4720(3) 0.0088(8) Uani 1 1 d . . .
O23 O -0.4165(2) -0.2499(5) 0.2916(4) 0.0149(12) Uani 1 1 d . . .
O24 O -0.44212(14) -0.4701(5) 0.4240(2) 0.0092(7) Uani 1 1 d . . .
O25 O -0.48917(14) -0.1562(5) 0.4031(3) 0.0109(7) Uani 1 1 d . . .
O26 O -0.39054(16) -0.1648(6) 0.4508(3) 0.0162(9) Uani 1 1 d . . .
O27 O -0.46644(14) -0.8059(5) 0.4084(3) 0.0092(8) Uani 1 1 d . . .
B2 B -0.4867(3) -0.6062(8) 0.4035(4) 0.0091(12) Uani 1 1 d U . .
B3 B -0.5076(2) -0.9508(8) 0.3975(4) 0.0074(11) Uani 1 1 d . . .
Cs1 Cs -0.779993(18) -1.21037(5) 0.36211(2) 0.02011(10) Uani 1 1 d . . .
Cs2 Cs -0.529711(18) -1.23628(5) 0.15879(3) 0.02040(11) Uani 1 1 d . . .
Na1 Na -0.70853(11) -0.6991(3) 0.49212(19) 0.0146(5) Uani 1 1 d . . .
Na2 Na -0.63840(12) -0.9663(4) 0.3295(2) 0.0297(7) Uani 1 1 d . . .
Na3 Na -0.61020(12) -0.9917(4) 0.6903(2) 0.0271(7) Uani 1 1 d . . .
Na4 Na -0.62758(9) -0.6536(4) 0.07823(15) 0.0189(5) Uani 1 1 d . . .
Na5 Na -0.89655(13) -0.9737(4) 0.2050(2) 0.0312(7) Uani 1 1 d . . .
Na6 Na -0.64481(14) -1.4809(4) 0.3196(2) 0.0325(7) Uani 1 1 d . . .
Na7 Na -0.87682(9) -0.6753(3) 0.43700(15) 0.0166(5) Uani 1 1 d . . .
Na8 Na -0.54166(11) -1.2579(3) 0.5292(2) 0.0144(6) 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
P1 O13 1.500(5) . ?
P1 O5 1.510(5) . ?
P1 O8 1.562(4) . ?
P1 O12 1.566(4) . ?
P2 O7 1.498(6) . ?
P2 O14 1.502(6) . ?
P2 O2 1.573(4) . ?
P2 O4 1.584(4) . ?
P3 O1 1.481(6) . ?
P3 O9 1.493(4) . ?
P3 O11 1.569(4) . ?
P3 O10 1.574(4) . ?
O2 B4 1.506(7) . ?
O3 B4 1.418(7) . ?
O3 B1 1.428(7) . ?
O4 B1 1.513(7) . ?
O8 B1 1.499(7) . ?
O10 B4 1.443(6) 1_545 ?
O11 B1 1.454(7) . ?
O12 B4 1.508(7) . ?
B4 O10 1.443(6) 1_565 ?
P4 O15 1.482(6) . ?
P4 O16 1.503(5) . ?
P4 O18 1.569(4) . ?
P4 O17 1.584(4) . ?
P5 O20 1.496(6) . ?
P5 O19 1.499(5) . ?
P5 O22 1.567(4) . ?
P5 O21 1.576(4) . ?
P6 O23 1.490(6) . ?
P6 O26 1.493(4) . ?
P6 O25 1.564(4) . ?
P6 O24 1.570(3) . ?
O17 B3 1.507(7) . ?
O18 B2 1.478(7) . ?
O21 B2 1.520(7) . ?
O22 B3 1.508(7) . ?
O24 B2 1.461(7) . ?
O25 B3 1.464(6) 1_565 ?
O27 B3 1.416(6) . ?
O27 B2 1.441(6) . ?
B3 O25 1.464(6) 1_545 ?

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
O13 P1 O5 115.6(3) . . ?
O13 P1 O8 108.0(2) . . ?
O5 P1 O8 109.8(3) . . ?
O13 P1 O12 107.2(2) . . ?
O5 P1 O12 109.4(2) . . ?
O8 P1 O12 106.4(2) . . ?
O7 P2 O14 116.4(4) . . ?
O7 P2 O2 108.2(2) . . ?
O14 P2 O2 109.0(2) . . ?
O7 P2 O4 108.9(3) . . ?
O14 P2 O4 110.2(2) . . ?
O2 P2 O4 103.5(2) . . ?
O1 P3 O9 113.7(3) . . ?
O1 P3 O11 111.2(2) . . ?
O9 P3 O11 108.2(2) . . ?
O1 P3 O10 111.5(3) . . ?
O9 P3 O10 109.8(2) . . ?
O11 P3 O10 101.8(2) . . ?
B4 O2 P2 120.6(3) . . ?
B4 O3 B1 114.8(4) . . ?
B1 O4 P2 122.7(3) . . ?
B1 O8 P1 122.3(3) . . ?
B4 O10 P3 131.2(3) 1_545 . ?
B1 O11 P3 131.7(4) . . ?
B4 O12 P1 122.7(3) . . ?
O3 B1 O11 110.6(5) . . ?
O3 B1 O8 110.3(4) . . ?
O11 B1 O8 110.6(4) . . ?
O3 B1 O4 110.2(4) . . ?
O11 B1 O4 108.0(4) . . ?
O8 B1 O4 107.1(4) . . ?
O3 B4 O10 116.7(5) . 1_565 ?
O3 B4 O2 109.7(4) . . ?
O10 B4 O2 103.9(4) 1_565 . ?
O3 B4 O12 110.4(4) . . ?
O10 B4 O12 108.0(4) 1_565 . ?
O2 B4 O12 107.5(4) . . ?
O15 P4 O16 116.0(3) . . ?
O15 P4 O18 109.6(3) . . ?
O16 P4 O18 107.4(2) . . ?
O15 P4 O17 110.4(2) . . ?
O16 P4 O17 107.0(3) . . ?
O18 P4 O17 105.9(2) . . ?
O20 P5 O19 114.6(3) . . ?
O20 P5 O22 109.2(2) . . ?
O19 P5 O22 109.1(2) . . ?
O20 P5 O21 108.7(3) . . ?
O19 P5 O21 111.0(2) . . ?
O22 P5 O21 103.8(2) . . ?
O23 P6 O26 114.2(3) . . ?
O23 P6 O25 110.3(3) . . ?
O26 P6 O25 110.9(2) . . ?
O23 P6 O24 112.1(2) . . ?
O26 P6 O24 106.5(2) . . ?
O25 P6 O24 102.1(2) . . ?
B3 O17 P4 122.1(3) . . ?
B2 O18 P4 122.2(3) . . ?
B2 O21 P5 123.0(3) . . ?
B3 O22 P5 120.2(3) . . ?
B2 O24 P6 129.6(3) . . ?
B3 O25 P6 132.2(3) 1_565 . ?
B3 O27 B2 113.5(4) . . ?
O27 B2 O24 108.9(5) . . ?
O27 B2 O18 111.2(4) . . ?
O24 B2 O18 111.4(4) . . ?
O27 B2 O21 109.6(4) . . ?
O24 B2 O21 107.6(4) . . ?
O18 B2 O21 108.0(4) . . ?
O27 B3 O25 115.5(4) . 1_545 ?
O27 B3 O17 111.2(4) . . ?
O25 B3 O17 108.5(4) 1_545 . ?
O27 B3 O22 110.7(4) . . ?
O25 B3 O22 103.5(4) 1_545 . ?
O17 B3 O22 106.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 P2 O2 B4 -150.8(4) . . . . ?
O14 P2 O2 B4 81.7(4) . . . . ?
O4 P2 O2 B4 -35.4(5) . . . . ?
O7 P2 O4 B1 146.3(4) . . . . ?
O14 P2 O4 B1 -85.0(4) . . . . ?
O2 P2 O4 B1 31.4(5) . . . . ?
O13 P1 O8 B1 135.0(4) . . . . ?
O5 P1 O8 B1 -98.1(4) . . . . ?
O12 P1 O8 B1 20.2(4) . . . . ?
O1 P3 O10 B4 -71.9(5) . . . 1_545 ?
O9 P3 O10 B4 55.0(5) . . . 1_545 ?
O11 P3 O10 B4 169.4(5) . . . 1_545 ?
O1 P3 O11 B1 -74.1(5) . . . . ?
O9 P3 O11 B1 160.4(5) . . . . ?
O10 P3 O11 B1 44.8(5) . . . . ?
O13 P1 O12 B4 -139.9(4) . . . . ?
O5 P1 O12 B4 94.0(4) . . . . ?
O8 P1 O12 B4 -24.6(4) . . . . ?
B4 O3 B1 O11 175.9(5) . . . . ?
B4 O3 B1 O8 -61.5(6) . . . . ?
B4 O3 B1 O4 56.5(6) . . . . ?
P3 O11 B1 O3 150.0(4) . . . . ?
P3 O11 B1 O8 27.6(7) . . . . ?
P3 O11 B1 O4 -89.3(5) . . . . ?
P1 O8 B1 O3 18.4(6) . . . . ?
P1 O8 B1 O11 141.0(4) . . . . ?
P1 O8 B1 O4 -101.5(4) . . . . ?
P2 O4 B1 O3 -42.8(6) . . . . ?
P2 O4 B1 O11 -163.8(3) . . . . ?
P2 O4 B1 O8 77.1(5) . . . . ?
B1 O3 B4 O10 -179.0(4) . . . 1_565 ?
B1 O3 B4 O2 -61.2(6) . . . . ?
B1 O3 B4 O12 57.2(5) . . . . ?
P2 O2 B4 O3 51.9(6) . . . . ?
P2 O2 B4 O10 177.5(3) . . . 1_565 ?
P2 O2 B4 O12 -68.2(5) . . . . ?
P1 O12 B4 O3 -10.4(6) . . . . ?
P1 O12 B4 O10 -139.2(4) . . . 1_565 ?
P1 O12 B4 O2 109.2(4) . . . . ?
O15 P4 O17 B3 92.8(4) . . . . ?
O16 P4 O17 B3 -140.1(4) . . . . ?
O18 P4 O17 B3 -25.8(4) . . . . ?
O15 P4 O18 B2 -98.5(5) . . . . ?
O16 P4 O18 B2 134.6(4) . . . . ?
O17 P4 O18 B2 20.6(5) . . . . ?
O20 P5 O21 B2 147.7(4) . . . . ?
O19 P5 O21 B2 -85.4(4) . . . . ?
O22 P5 O21 B2 31.6(5) . . . . ?
O20 P5 O22 B3 -150.3(4) . . . . ?
O19 P5 O22 B3 83.8(4) . . . . ?
O21 P5 O22 B3 -34.5(5) . . . . ?
O23 P6 O24 B2 -70.5(5) . . . . ?
O26 P6 O24 B2 163.9(4) . . . . ?
O25 P6 O24 B2 47.6(5) . . . . ?
O23 P6 O25 B3 -70.8(5) . . . 1_565 ?
O26 P6 O25 B3 56.8(5) . . . 1_565 ?
O24 P6 O25 B3 169.8(5) . . . 1_565 ?
B3 O27 B2 O24 174.7(5) . . . . ?
B3 O27 B2 O18 -62.1(6) . . . . ?
B3 O27 B2 O21 57.2(6) . . . . ?
P6 O24 B2 O27 149.5(4) . . . . ?
P6 O24 B2 O18 26.5(7) . . . . ?
P6 O24 B2 O21 -91.8(5) . . . . ?
P4 O18 B2 O27 19.2(6) . . . . ?
P4 O18 B2 O24 140.9(4) . . . . ?
P4 O18 B2 O21 -101.1(4) . . . . ?
P5 O21 B2 O27 -44.0(6) . . . . ?
P5 O21 B2 O24 -162.2(3) . . . . ?
P5 O21 B2 O18 77.4(5) . . . . ?
B2 O27 B3 O25 -179.2(4) . . . 1_545 ?
B2 O27 B3 O17 56.6(6) . . . . ?
B2 O27 B3 O22 -62.0(6) . . . . ?
P4 O17 B3 O27 -9.8(6) . . . . ?
P4 O17 B3 O25 -137.8(3) . . . 1_545 ?
P4 O17 B3 O22 111.1(4) . . . . ?
P5 O22 B3 O27 51.9(6) . . . . ?
P5 O22 B3 O25 176.3(3) . . . 1_545 ?
P5 O22 B3 O17 -69.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.143
####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1563595'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-08-28 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 Na4 O13 P3 Rb'
_chemical_formula_weight         499.96

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   24.0348(9)
_cell_length_b                   6.7464(2)
_cell_length_c                   14.9206(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2419.35(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8386
_cell_measurement_theta_min      3.2142
_cell_measurement_theta_max      26.3664

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1919
_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   sadabs

_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  bruker-CCD
_diffrn_measurement_method       'w scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13216
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4830
_reflns_number_gt                4278
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0544P)²+13.3308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0125(6)
_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   0.00
_refine_ls_number_reflns         4830
_refine_ls_number_parameters     416
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1113
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.82341(10) -0.7257(2) 0.37929(15) 0.0071(5) Uani 1 1 d . . .
P2 P -0.77972(10) -0.7249(3) 0.62551(16) 0.0101(5) Uani 1 1 d . . .
P3 P -0.67740(9) -0.2059(2) 0.48967(14) 0.0049(4) Uani 1 1 d . . .
O2 O -0.79629(19) -0.5212(7) 0.4039(3) 0.0085(10) Uani 1 1 d . . .
O3 O -0.6350(2) -0.2973(7) 0.4293(4) 0.0136(11) Uani 1 1 d U . .
O4 O -0.7353(3) -0.6901(10) 0.6944(6) 0.0335(16) Uani 1 1 d . . .
O5 O -0.8348(3) -0.7284(8) 0.2816(5) 0.0168(15) Uani 1 1 d . . .
O6 O -0.6621(3) -0.2090(8) 0.5890(5) 0.0186(15) Uani 1 1 d . . .
O7 O -0.7133(2) -0.6520(7) 0.4714(4) 0.0093(10) Uani 1 1 d . . .
O8 O -0.7606(2) -0.8946(7) 0.5609(4) 0.0159(12) Uani 1 1 d . . .
O9 O -0.7367(2) -0.3022(7) 0.4746(4) 0.0124(10) Uani 1 1 d U . .
O10 O -0.68715(19) 0.0123(6) 0.4566(3) 0.0085(9) Uani 1 1 d U . .
O11 O -0.7866(2) -0.5325(7) 0.5668(3) 0.0136(11) Uani 1 1 d . . .
O14 O -0.8728(3) -0.7615(7) 0.4387(4) 0.0128(13) Uani 1 1 d . . .
O15 O -0.7760(2) -0.8816(7) 0.3995(3) 0.0094(10) Uani 1 1 d U . .
O16 O -0.8362(3) -0.7815(8) 0.6602(4) 0.0256(15) Uani 1 1 d . . .
B3 B -0.7549(3) -0.5047(10) 0.4788(5) 0.0083(14) Uani 1 1 d . . .
B4 B -0.7334(3) -0.8500(11) 0.4729(6) 0.0097(16) Uani 1 1 d . . .
P4 P -0.52839(10) -0.7408(3) 0.59881(16) 0.0098(5) Uani 1 1 d . . .
P5 P -0.57403(10) -0.7346(2) 0.84506(15) 0.0060(5) Uani 1 1 d . . .
P6 P -0.42740(10) -1.2586(2) 0.73544(15) 0.0066(4) Uani 1 1 d . . .
O12 O -0.5845(3) -0.6835(9) 0.5639(4) 0.0260(14) Uani 1 1 d . . .
O13 O -0.5468(2) -0.9391(7) 0.8207(3) 0.0094(10) Uani 1 1 d . . .
O17 O -0.5857(3) -0.7287(7) 0.9447(5) 0.0163(16) Uani 1 1 d . . .
O18 O -0.46291(19) -0.8129(6) 0.7562(3) 0.0073(10) Uani 1 1 d . . .
O19 O -0.5356(2) -0.9312(6) 0.6591(3) 0.0104(10) Uani 1 1 d . . .
O20 O -0.4855(2) -1.1624(7) 0.7548(3) 0.0107(10) Uani 1 1 d U . .
O21 O -0.5088(2) -0.5701(7) 0.6635(4) 0.0167(12) Uani 1 1 d . . .
O22 O -0.3832(2) -1.1712(7) 0.7944(4) 0.0152(11) Uani 1 1 d . . .
O23 O -0.6230(2) -0.7010(7) 0.7850(4) 0.0103(11) Uani 1 1 d . . .
O24 O -0.5260(2) -0.5796(7) 0.8236(4) 0.0122(11) Uani 1 1 d . . .
O25 O -0.43691(18) -1.4759(6) 0.7702(3) 0.0077(9) Uani 1 1 d U . .
O26 O -0.4837(3) -0.7790(9) 0.5300(6) 0.0321(17) Uani 1 1 d . . .
O27 O -0.4146(3) -1.2516(7) 0.6385(5) 0.0141(14) Uani 1 1 d . . .
B1 B -0.5046(3) -0.9585(10) 0.7472(6) 0.0094(15) Uani 1 1 d . . .
B2 B -0.4825(3) -0.6126(10) 0.7523(6) 0.0082(15) Uani 1 1 d . . .
Rb1 Rb -0.72264(4) -0.71653(13) 0.20235(8) 0.0300(3) Uani 1 1 d . . .
Rb2 Rb -0.52750(5) -1.24614(12) 0.52271(9) 0.0306(3) Uani 1 1 d . . .
Na1 Na -0.79004(14) -1.1999(4) 0.3448(2) 0.0128(7) Uani 1 1 d . . .
Na2 Na -0.62402(12) -0.6513(4) 0.4268(2) 0.0160(6) Uani 1 1 d . . .
Na3 Na -0.86045(15) -1.4617(5) 0.1829(3) 0.0250(8) Uani 1 1 d . . .
Na4 Na -0.85516(17) -0.9849(5) 0.1726(3) 0.0251(8) Uani 1 1 d . . .
Na5 Na -0.60847(15) -0.9986(4) 0.0394(3) 0.0217(8) Uani 1 1 d . . .
Na6 Na -0.96032(16) -0.7598(4) 0.3804(3) 0.0132(7) Uani 1 1 d . . .
Na7 Na -0.60571(17) -1.4739(5) 0.0529(3) 0.0283(9) Uani 1 1 d . . .
Na8 Na -0.62700(12) -1.1719(4) 0.2910(2) 0.0148(6) 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
P1 O5 1.483(8) . ?
P1 O14 1.501(7) . ?
P1 O2 1.570(5) . ?
P1 O15 1.580(5) . ?
P2 O4 1.500(7) . ?
P2 O16 1.503(7) . ?
P2 O8 1.566(5) . ?
P2 O11 1.575(5) . ?
P3 O3 1.494(6) . ?
P3 O6 1.527(7) . ?
P3 O10 1.570(5) . ?
P3 O9 1.583(5) . ?
O2 B3 1.501(9) . ?
O7 B3 1.413(8) . ?
O7 B4 1.421(9) . ?
O8 B4 1.497(10) . ?
O9 B3 1.435(8) . ?
O10 B4 1.470(9) 1_565 ?
O11 B3 1.530(9) . ?
O15 B4 1.514(10) . ?
B4 O10 1.470(9) 1_545 ?
P4 O12 1.497(7) . ?
P4 O26 1.508(8) . ?
P4 O21 1.575(5) . ?
P4 O19 1.578(5) . ?
P5 O23 1.497(6) . ?
P5 O17 1.514(8) . ?
P5 O13 1.570(5) . ?
P5 O24 1.590(5) . ?
P6 O27 1.480(7) . ?
P6 O22 1.500(5) . ?
P6 O20 1.567(5) . ?
P6 O25 1.572(5) . ?
O13 B1 1.501(9) . ?
O18 B1 1.409(8) . ?
O18 B2 1.432(8) . ?
O19 B1 1.521(10) . ?
O20 B1 1.454(8) . ?
O21 B2 1.496(10) . ?
O24 B2 1.507(10) . ?
O25 B2 1.458(9) 1_545 ?
B2 O25 1.458(9) 1_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
O5 P1 O14 115.6(4) . . ?
O5 P1 O2 108.5(3) . . ?
O14 P1 O2 109.4(3) . . ?
O5 P1 O15 108.2(3) . . ?
O14 P1 O15 110.5(3) . . ?
O2 P1 O15 104.0(3) . . ?
O4 P2 O16 116.5(5) . . ?
O4 P2 O8 109.1(4) . . ?
O16 P2 O8 107.0(3) . . ?
O4 P2 O11 109.1(3) . . ?
O16 P2 O11 107.8(3) . . ?
O8 P2 O11 106.9(3) . . ?
O3 P3 O6 114.6(4) . . ?
O3 P3 O10 107.4(3) . . ?
O6 P3 O10 110.7(3) . . ?
O3 P3 O9 111.1(3) . . ?
O6 P3 O9 110.4(4) . . ?
O10 P3 O9 101.9(3) . . ?
B3 O2 P1 121.0(4) . . ?
B3 O7 B4 114.8(6) . . ?
B4 O8 P2 121.4(4) . . ?
B3 O9 P3 131.1(5) . . ?
B4 O10 P3 130.8(5) 1_565 . ?
B3 O11 P2 121.7(4) . . ?
B4 O15 P1 122.1(4) . . ?
O7 B3 O9 116.9(6) . . ?
O7 B3 O2 111.0(6) . . ?
O9 B3 O2 103.8(5) . . ?
O7 B3 O11 109.5(6) . . ?
O9 B3 O11 107.8(5) . . ?
O2 B3 O11 107.4(5) . . ?
O7 B4 O10 109.5(6) . 1_545 ?
O7 B4 O8 110.5(6) . . ?
O10 B4 O8 110.3(6) 1_545 . ?
O7 B4 O15 110.6(6) . . ?
O10 B4 O15 107.6(6) 1_545 . ?
O8 B4 O15 108.2(6) . . ?
O12 P4 O26 116.7(5) . . ?
O12 P4 O21 107.1(3) . . ?
O26 P4 O21 109.2(4) . . ?
O12 P4 O19 108.1(3) . . ?
O26 P4 O19 109.1(3) . . ?
O21 P4 O19 106.1(3) . . ?
O23 P5 O17 116.0(4) . . ?
O23 P5 O13 108.8(3) . . ?
O17 P5 O13 109.1(3) . . ?
O23 P5 O24 110.6(3) . . ?
O17 P5 O24 108.3(4) . . ?
O13 P5 O24 103.2(3) . . ?
O27 P6 O22 114.4(4) . . ?
O27 P6 O20 110.7(4) . . ?
O22 P6 O20 111.1(3) . . ?
O27 P6 O25 112.5(3) . . ?
O22 P6 O25 106.0(3) . . ?
O20 P6 O25 101.3(3) . . ?
B1 O13 P5 121.9(4) . . ?
B1 O18 B2 114.8(6) . . ?
B1 O19 P4 122.5(4) . . ?
B1 O20 P6 131.2(5) . . ?
B2 O21 P4 121.9(4) . . ?
B2 O24 P5 123.2(4) . . ?
B2 O25 P6 129.7(4) 1_545 . ?
O18 B1 O20 115.4(6) . . ?
O18 B1 O13 110.5(6) . . ?
O20 B1 O13 103.8(5) . . ?
O18 B1 O19 110.2(6) . . ?
O20 B1 O19 109.6(5) . . ?
O13 B1 O19 106.8(5) . . ?
O18 B2 O25 110.0(6) . 1_565 ?
O18 B2 O21 110.8(6) . . ?
O25 B2 O21 111.0(6) 1_565 . ?
O18 B2 O24 109.8(6) . . ?
O25 B2 O24 107.4(6) 1_565 . ?
O21 B2 O24 107.7(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 P1 O2 B3 -148.3(5) . . . . ?
O14 P1 O2 B3 84.7(6) . . . . ?
O15 P1 O2 B3 -33.3(6) . . . . ?
O4 P2 O8 B4 -96.4(6) . . . . ?
O16 P2 O8 B4 136.7(6) . . . . ?
O11 P2 O8 B4 21.5(6) . . . . ?
O3 P3 O9 B3 55.7(7) . . . . ?
O6 P3 O9 B3 -72.5(7) . . . . ?
O10 P3 O9 B3 169.8(6) . . . . ?
O3 P3 O10 B4 160.7(6) . . . 1_565 ?
O6 P3 O10 B4 -73.5(7) . . . 1_565 ?
O9 P3 O10 B4 43.9(7) . . . 1_565 ?
O4 P2 O11 B3 92.9(6) . . . . ?
O16 P2 O11 B3 -139.7(5) . . . . ?
O8 P2 O11 B3 -24.9(6) . . . . ?
O5 P1 O15 B4 146.6(5) . . . . ?
O14 P1 O15 B4 -85.9(6) . . . . ?
O2 P1 O15 B4 31.4(6) . . . . ?
B4 O7 B3 O9 -178.0(6) . . . . ?
B4 O7 B3 O2 -59.2(7) . . . . ?
B4 O7 B3 O11 59.2(7) . . . . ?
P3 O9 B3 O7 -19.4(10) . . . . ?
P3 O9 B3 O2 -142.0(5) . . . . ?
P3 O9 B3 O11 104.3(6) . . . . ?
P1 O2 B3 O7 48.8(7) . . . . ?
P1 O2 B3 O9 175.1(4) . . . . ?
P1 O2 B3 O11 -70.9(6) . . . . ?
P2 O11 B3 O7 -11.4(8) . . . . ?
P2 O11 B3 O9 -139.5(5) . . . . ?
P2 O11 B3 O2 109.2(5) . . . . ?
B3 O7 B4 O10 175.0(6) . . . 1_545 ?
B3 O7 B4 O8 -63.3(8) . . . . ?
B3 O7 B4 O15 56.5(8) . . . . ?
P2 O8 B4 O7 17.9(8) . . . . ?
P2 O8 B4 O10 139.2(5) . . . 1_545 ?
P2 O8 B4 O15 -103.3(6) . . . . ?
P1 O15 B4 O7 -44.1(8) . . . . ?
P1 O15 B4 O10 -163.6(4) . . . 1_545 ?
P1 O15 B4 O8 77.1(6) . . . . ?
O23 P5 O13 B1 85.6(6) . . . . ?
O17 P5 O13 B1 -146.9(6) . . . . ?
O24 P5 O13 B1 -31.9(6) . . . . ?
O12 P4 O19 B1 -139.2(5) . . . . ?
O26 P4 O19 B1 93.0(6) . . . . ?
O21 P4 O19 B1 -24.6(6) . . . . ?
O27 P6 O20 B1 -67.2(7) . . . . ?
O22 P6 O20 B1 61.0(7) . . . . ?
O25 P6 O20 B1 173.3(6) . . . . ?
O12 P4 O21 B2 136.0(6) . . . . ?
O26 P4 O21 B2 -96.8(6) . . . . ?
O19 P4 O21 B2 20.7(6) . . . . ?
O23 P5 O24 B2 -86.6(6) . . . . ?
O17 P5 O24 B2 145.3(6) . . . . ?
O13 P5 O24 B2 29.7(6) . . . . ?
O27 P6 O25 B2 -69.7(7) . . . 1_545 ?
O22 P6 O25 B2 164.6(6) . . . 1_545 ?
O20 P6 O25 B2 48.5(6) . . . 1_545 ?
B2 O18 B1 O20 -177.5(6) . . . . ?
B2 O18 B1 O13 -60.2(8) . . . . ?
B2 O18 B1 O19 57.6(7) . . . . ?
P6 O20 B1 O18 -26.5(10) . . . . ?
P6 O20 B1 O13 -147.5(5) . . . . ?
P6 O20 B1 O19 98.6(7) . . . . ?
P5 O13 B1 O18 48.8(8) . . . . ?
P5 O13 B1 O20 173.0(4) . . . . ?
P5 O13 B1 O19 -71.1(6) . . . . ?
P4 O19 B1 O18 -11.0(8) . . . . ?
P4 O19 B1 O20 -139.0(5) . . . . ?
P4 O19 B1 O13 109.1(5) . . . . ?
B1 O18 B2 O25 175.0(6) . . . 1_565 ?
B1 O18 B2 O21 -61.8(8) . . . . ?
B1 O18 B2 O24 57.1(8) . . . . ?
P4 O21 B2 O18 17.8(9) . . . . ?
P4 O21 B2 O25 140.4(5) . . . 1_565 ?
P4 O21 B2 O24 -102.4(6) . . . . ?
P5 O24 B2 O18 -43.0(8) . . . . ?
P5 O24 B2 O25 -162.6(4) . . . 1_565 ?
P5 O24 B2 O21 77.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.826
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.146
