# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc2b5z8s
_database_code_depnum_ccdc_archive 'CCDC 2150695'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.802(4)
_cell_length_b                   7.196(4)
_cell_length_c                   7.435(4)
_cell_angle_alpha                115.306(10)
_cell_angle_beta                 100.789(12)
_cell_angle_gamma                106.907(11)
_cell_volume                     293.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1891
_cell_measurement_theta_min      3.249
_cell_measurement_theta_max      31.184

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.783
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.894
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX DUO CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5554
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.249
_diffrn_reflns_theta_max         31.184
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1891
_reflns_number_gt                1433
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0319P)²+0.3003P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1891
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0783
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Na1 Na 1.13320(19) 0.7659(2) 0.75065(19) 0.0215(3) Uani 1 1 d . . . . .
B1 B 0.2222(4) -0.3262(5) 0.3503(4) 0.0087(5) Uani 1 1 d . . . . .
Si1 Si 0.35432(11) 0.04915(12) 0.32016(11) 0.00735(16) Uani 1 1 d . . . . .
Si2 Si 0.20977(11) 0.31545(12) 0.69623(11) 0.00734(16) Uani 1 1 d . . . . .
Si3 Si 0.67976(11) 0.69546(12) 0.89924(11) 0.00746(16) Uani 1 1 d . . . . .
O1 O -0.0033(3) 0.3568(3) 0.6292(3) 0.0102(4) Uani 1 1 d . . . . .
O2 O 0.2064(3) 0.2090(3) 0.8493(3) 0.0111(4) Uani 1 1 d . . . . .
O3 O 0.4171(3) 0.5600(3) 0.8240(3) 0.0116(4) Uani 1 1 d . . . . .
O4 O 0.2761(3) 0.0744(3) 0.1118(3) 0.0090(4) Uani 1 1 d . . . . .
O5 O 0.2738(3) -0.2167(3) 0.2307(3) 0.0103(4) Uani 1 1 d . . . . .
O6 O 0.2337(3) 0.1507(3) 0.4810(3) 0.0124(4) Uani 1 1 d . . . . .
O7 O 0.7884(3) 0.5563(3) 0.7542(3) 0.0121(4) Uani 1 1 d . . . . .
O8 O 0.6173(3) 0.1915(3) 0.4282(3) 0.0117(4) 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
Na1 O8 2.373(2) 2_766 ?
Na1 O4 2.399(2) 1_666 ?
Na1 O7 2.403(2) . ?
Na1 O1 2.453(3) 2_666 ?
Na1 O1 2.484(3) 1_655 ?
Na1 O2 2.809(3) 1_665 ?
Na1 O3 2.861(3) 1_655 ?
Na1 B1 2.981(3) 1_665 ?
Na1 B1 3.043(3) 2_656 ?
Na1 Si3 3.268(2) 2_777 ?
Na1 Si2 3.299(2) 1_655 ?
Na1 Si2 3.386(2) 2_666 ?
B1 O5 1.446(3) . ?
B1 O7 1.470(3) 2_656 ?
B1 O8 1.480(3) 2_656 ?
B1 O1 1.488(3) 2_556 ?
Si1 O5 1.603(2) . ?
Si1 O8 1.609(2) . ?
Si1 O6 1.6144(19) . ?
Si1 O4 1.644(2) . ?
Si2 O1 1.595(2) . ?
Si2 O6 1.606(2) . ?
Si2 O3 1.617(2) . ?
Si2 O2 1.621(2) . ?
Si3 O7 1.5868(19) . ?
Si3 O3 1.613(2) . ?
Si3 O2 1.618(2) 2_667 ?
Si3 O4 1.636(2) 2_666 ?

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
O8 Na1 O4 111.91(8) 2_766 1_666 ?
O8 Na1 O7 150.75(8) 2_766 . ?
O4 Na1 O7 97.33(8) 1_666 . ?
O8 Na1 O1 58.46(7) 2_766 2_666 ?
O4 Na1 O1 146.94(9) 1_666 2_666 ?
O7 Na1 O1 96.88(8) . 2_666 ?
O8 Na1 O1 102.15(7) 2_766 1_655 ?
O4 Na1 O1 126.74(8) 1_666 1_655 ?
O7 Na1 O1 57.15(6) . 1_655 ?
O1 Na1 O1 85.85(7) 2_666 1_655 ?
O8 Na1 O2 82.80(7) 2_766 1_665 ?
O4 Na1 O2 58.03(7) 1_666 1_665 ?
O7 Na1 O2 114.57(7) . 1_665 ?
O1 Na1 O2 88.91(7) 2_666 1_665 ?
O1 Na1 O2 169.42(8) 1_655 1_665 ?
O8 Na1 O3 72.41(7) 2_766 1_655 ?
O4 Na1 O3 95.54(8) 1_666 1_655 ?
O7 Na1 O3 105.57(8) . 1_655 ?
O1 Na1 O3 109.08(7) 2_666 1_655 ?
O1 Na1 O3 57.04(7) 1_655 1_655 ?
O2 Na1 O3 133.52(7) 1_665 1_655 ?
O8 Na1 B1 29.38(7) 2_766 1_665 ?
O4 Na1 B1 137.32(9) 1_666 1_665 ?
O7 Na1 B1 123.04(8) . 1_665 ?
O1 Na1 B1 29.79(7) 2_666 1_665 ?
O1 Na1 B1 89.99(8) 1_655 1_665 ?
O2 Na1 B1 90.02(8) 1_665 1_665 ?
O3 Na1 B1 87.00(8) 1_655 1_665 ?
O8 Na1 B1 127.14(8) 2_766 2_656 ?
O4 Na1 B1 116.32(8) 1_666 2_656 ?
O7 Na1 B1 28.32(7) . 2_656 ?
O1 Na1 B1 89.15(8) 2_666 2_656 ?
O1 Na1 B1 29.03(7) 1_655 2_656 ?
O2 Na1 B1 141.88(8) 1_665 2_656 ?
O3 Na1 B1 82.57(9) 1_655 2_656 ?
B1 Na1 B1 106.27(7) 1_665 2_656 ?
O8 Na1 Si3 95.84(6) 2_766 2_777 ?
O4 Na1 Si3 28.65(5) 1_666 2_777 ?
O7 Na1 Si3 110.80(6) . 2_777 ?
O1 Na1 Si3 118.39(7) 2_666 2_777 ?
O1 Na1 Si3 155.17(7) 1_655 2_777 ?
O2 Na1 Si3 29.66(5) 1_665 2_777 ?
O3 Na1 Si3 114.12(6) 1_655 2_777 ?
B1 Na1 Si3 113.61(7) 1_665 2_777 ?
B1 Na1 Si3 137.01(7) 2_656 2_777 ?
O8 Na1 Si2 86.70(6) 2_766 1_655 ?
O4 Na1 Si2 114.47(7) 1_666 1_655 ?
O7 Na1 Si2 80.78(6) . 1_655 ?
O1 Na1 Si2 97.18(6) 2_666 1_655 ?
O1 Na1 Si2 27.72(5) 1_655 1_655 ?
O2 Na1 Si2 162.79(6) 1_665 1_655 ?
O3 Na1 Si2 29.35(4) 1_655 1_655 ?
B1 Na1 Si2 87.45(7) 1_665 1_655 ?
B1 Na1 Si2 54.68(7) 2_656 1_655 ?
Si3 Na1 Si2 139.69(5) 2_777 1_655 ?
O8 Na1 Si2 80.30(7) 2_766 2_666 ?
O4 Na1 Si2 129.96(7) 1_666 2_666 ?
O7 Na1 Si2 81.08(7) . 2_666 ?
O1 Na1 Si2 25.94(5) 2_666 2_666 ?
O1 Na1 Si2 94.39(6) 1_655 2_666 ?
O2 Na1 Si2 77.10(5) 1_665 2_666 ?
O3 Na1 Si2 133.39(6) 1_655 2_666 ?
B1 Na1 Si2 54.17(7) 1_665 2_666 ?
B1 Na1 Si2 84.91(7) 2_656 2_666 ?
Si3 Na1 Si2 105.50(5) 2_777 2_666 ?
Si2 Na1 Si2 114.55(4) 1_655 2_666 ?
O5 B1 O7 111.6(2) . 2_656 ?
O5 B1 O8 111.4(2) . 2_656 ?
O7 B1 O8 110.1(2) 2_656 2_656 ?
O5 B1 O1 113.6(2) . 2_556 ?
O7 B1 O1 104.50(19) 2_656 2_556 ?
O8 B1 O1 105.20(19) 2_656 2_556 ?
O5 B1 Na1 140.24(18) . 1_445 ?
O7 B1 Na1 108.14(16) 2_656 1_445 ?
O8 B1 Na1 51.88(11) 2_656 1_445 ?
O1 B1 Na1 55.01(12) 2_556 1_445 ?
O5 B1 Na1 134.79(17) . 2_656 ?
O7 B1 Na1 50.86(11) 2_656 2_656 ?
O8 B1 Na1 113.81(16) 2_656 2_656 ?
O1 B1 Na1 54.13(12) 2_556 2_656 ?
Na1 B1 Na1 73.73(7) 1_445 2_656 ?
O5 Si1 O8 114.33(10) . . ?
O5 Si1 O6 109.85(10) . . ?
O8 Si1 O6 111.38(10) . . ?
O5 Si1 O4 106.14(10) . . ?
O8 Si1 O4 106.05(10) . . ?
O6 Si1 O4 108.76(10) . . ?
O1 Si2 O6 107.52(10) . . ?
O1 Si2 O3 106.47(11) . . ?
O6 Si2 O3 110.15(10) . . ?
O1 Si2 O2 114.78(10) . . ?
O6 Si2 O2 109.72(11) . . ?
O3 Si2 O2 108.12(11) . . ?
O1 Si2 Na1 46.40(7) . 1_455 ?
O6 Si2 Na1 120.04(8) . 1_455 ?
O3 Si2 Na1 60.13(8) . 1_455 ?
O2 Si2 Na1 129.99(8) . 1_455 ?
O1 Si2 Na1 42.26(7) . 2_666 ?
O6 Si2 Na1 66.43(8) . 2_666 ?
O3 Si2 Na1 111.58(8) . 2_666 ?
O2 Si2 Na1 138.69(8) . 2_666 ?
Na1 Si2 Na1 65.45(4) 1_455 2_666 ?
O7 Si3 O3 113.57(11) . . ?
O7 Si3 O2 113.89(11) . 2_667 ?
O3 Si3 O2 109.57(10) . 2_667 ?
O7 Si3 O4 108.31(10) . 2_666 ?
O3 Si3 O4 107.51(10) . 2_666 ?
O2 Si3 O4 103.29(10) 2_667 2_666 ?
O7 Si3 Na1 131.15(8) . 2_777 ?
O3 Si3 Na1 113.69(8) . 2_777 ?
O2 Si3 Na1 59.24(8) 2_667 2_777 ?
O4 Si3 Na1 44.68(8) 2_666 2_777 ?
O7 Si3 Na1 38.21(7) . . ?
O3 Si3 Na1 146.62(8) . . ?
O2 Si3 Na1 100.96(8) 2_667 . ?
O4 Si3 Na1 77.30(7) 2_666 . ?
Na1 Si3 Na1 93.18(4) 2_777 . ?
B1 O1 Si2 142.75(17) 2_556 . ?
B1 O1 Na1 95.19(14) 2_556 2_666 ?
Si2 O1 Na1 111.80(9) . 2_666 ?
B1 O1 Na1 96.84(14) 2_556 1_455 ?
Si2 O1 Na1 105.89(9) . 1_455 ?
Na1 O1 Na1 94.15(7) 2_666 1_455 ?
Si3 O2 Si2 135.84(13) 2_667 . ?
Si3 O2 Na1 91.10(9) 2_667 1_445 ?
Si2 O2 Na1 129.56(10) . 1_445 ?
Si3 O3 Si2 146.34(13) . . ?
Si3 O3 Na1 119.55(10) . 1_455 ?
Si2 O3 Na1 90.52(9) . 1_455 ?
Si3 O4 Si1 128.94(11) 2_666 . ?
Si3 O4 Na1 106.67(10) 2_666 1_444 ?
Si1 O4 Na1 123.39(11) . 1_444 ?
B1 O5 Si1 125.25(17) . . ?
Si2 O6 Si1 158.15(13) . . ?
B1 O7 Si3 139.52(16) 2_656 . ?
B1 O7 Na1 100.83(14) 2_656 . ?
Si3 O7 Na1 117.68(11) . . ?
B1 O8 Si1 134.50(16) 2_656 . ?
B1 O8 Na1 98.74(14) 2_656 2_766 ?
Si1 O8 Na1 126.75(11) . 2_766 ?

_refine_diff_density_max         0.576
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.130

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zgz
_database_code_depnum_ccdc_archive 'CCDC 2150701'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.3777(14)
_cell_length_b                   6.4083(13)
_cell_length_c                   6.6321(6)
_cell_angle_alpha                103.787(12)
_cell_angle_beta                 115.708(15)
_cell_angle_gamma                102.068(18)
_cell_volume                     221.55(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    528
_cell_measurement_theta_min      2.424
_cell_measurement_theta_max      17.204

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.689
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.124
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            766
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.424
_diffrn_reflns_theta_max         17.204
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.133
_diffrn_measured_fraction_theta_full 0.246
_diffrn_reflns_Laue_measured_fraction_max 0.133
_diffrn_reflns_Laue_measured_fraction_full 0.246
_diffrn_reflns_point_group_measured_fraction_max 0.133
_diffrn_reflns_point_group_measured_fraction_full 0.246
_reflns_number_total             528
_reflns_number_gt                504
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)²] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         528
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_ref         0.3070
_refine_ls_wR_factor_gt          0.2650
_refine_ls_goodness_of_fit_ref   2.691
_refine_ls_restrained_S_all      2.691
_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
Si1 Si 0.7946(11) 0.7377(6) 0.6515(5) 0.033(5) Uani 1 1 d . . . . .
Si3 Si 0.4359(11) 0.8375(7) 0.3101(4) 0.030(5) Uani 1 1 d . . . . .
Si2 Si 0.7557(10) 0.8357(6) 1.1103(4) 0.012(5) Uani 1 1 d . . . . .
Na1 Na 0.7180(17) 0.2888(10) 1.3034(8) 0.0122(7) Uiso 1 1 d . . . . .
O1 O 0.788(3) 0.6176(18) 1.1621(13) 0.0121(10) Uiso 1 1 d . . . . .
O2 O 0.720(3) 0.8291(17) 0.8515(11) 0.0092(9) Uiso 1 1 d . . . . .
O3 O 0.131(3) 0.6749(15) 0.0866(10) 0.0076(9) Uiso 1 1 d . . . . .
O4 O 0.513(3) 0.8366(16) 1.0966(10) 0.0075(9) Uiso 1 1 d . . . . .
O5 O 1.024(3) 0.9301(19) 0.6895(11) 0.0082(9) Uiso 1 1 d . . . . .
O6 O 0.554(3) 0.6463(16) 0.3960(10) 0.0094(9) Uiso 1 1 d . . . . .
O7 O 0.320(3) 0.9179(17) 0.4866(12) 0.0106(9) Uiso 1 1 d . . . . .
O8 O 1.096(3) 0.4677(17) 1.3389(11) 0.0086(9) Uiso 1 1 d . . . . .
B1 B 0.983(5) 0.525(2) 1.1514(18) 0.0087(12) Uiso 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
Si1 O6 1.570(13) . ?
Si1 O5 1.581(7) . ?
Si1 O8 1.62(2) 2_767 ?
Si1 O2 1.619(12) . ?
Si1 Si3 2.753(10) . ?
Si1 Na1 3.018(8) 1_554 ?
Si1 Na1 3.037(13) 2_767 ?
Si1 Na1 3.383(12) 2_667 ?
Si3 O6 1.655(19) . ?
Si3 O7 1.675(13) . ?
Si3 O4 1.686(7) 1_554 ?
Si3 O7 1.688(6) 2_676 ?
Si3 O3 1.726(12) . ?
Si3 Si3 2.520(6) 2_676 ?
Si3 Na1 3.091(5) 1_564 ?
Si3 Na1 3.321(3) 2_667 ?
Si2 O4 1.515(19) . ?
Si2 O1 1.549(18) . ?
Si2 O5 1.594(6) 2_777 ?
Si2 O2 1.620(5) . ?
Si2 Na1 2.837(11) 2_667 ?
Si2 Na1 2.986(11) 1_565 ?
Na1 O8 2.119(6) 2_768 ?
Na1 O7 2.189(10) 2_667 ?
Na1 O4 2.225(9) 2_667 ?
Na1 O8 2.325(14) . ?
Na1 O5 2.37(3) 2_767 ?
Na1 O2 2.386(18) 2_667 ?
Na1 O1 2.535(13) . ?
Na1 O4 2.637(10) 1_545 ?
Na1 B1 2.704(9) . ?
Na1 O6 2.76(2) 1_556 ?
O1 B1 1.51(4) . ?
O3 B1 1.471(9) 1_454 ?
O3 B1 1.521(11) 2_666 ?
O8 B1 1.32(2) . ?
B1 B1 2.067(18) 2_767 ?

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
O6 Si1 O5 114.8(5) . . ?
O6 Si1 O8 106.3(7) . 2_767 ?
O5 Si1 O8 99.5(9) . 2_767 ?
O6 Si1 O2 107.8(9) . . ?
O5 Si1 O2 110.8(4) . . ?
O8 Si1 O2 117.7(6) 2_767 . ?
O6 Si1 Si3 32.3(6) . . ?
O5 Si1 Si3 95.5(7) . . ?
O8 Si1 Si3 137.5(3) 2_767 . ?
O2 Si1 Si3 93.0(7) . . ?
O6 Si1 Na1 65.3(7) . 1_554 ?
O5 Si1 Na1 107.9(6) . 1_554 ?
O8 Si1 Na1 42.1(3) 2_767 1_554 ?
O2 Si1 Na1 139.3(3) . 1_554 ?
Si3 Si1 Na1 95.4(2) . 1_554 ?
O6 Si1 Na1 120.2(6) . 2_767 ?
O5 Si1 Na1 50.5(8) . 2_767 ?
O8 Si1 Na1 49.1(4) 2_767 2_767 ?
O2 Si1 Na1 132.0(6) . 2_767 ?
Si3 Si1 Na1 128.30(15) . 2_767 ?
Na1 Si1 Na1 68.1(2) 1_554 2_767 ?
O6 Si1 Na1 68.8(5) . 2_667 ?
O5 Si1 Na1 137.2(8) . 2_667 ?
O8 Si1 Na1 121.0(3) 2_767 2_667 ?
O2 Si1 Na1 40.1(5) . 2_667 ?
Si3 Si1 Na1 64.6(2) . 2_667 ?
Na1 Si1 Na1 111.2(2) 1_554 2_667 ?
Na1 Si1 Na1 166.9(3) 2_767 2_667 ?
O6 Si3 O7 105.0(6) . . ?
O6 Si3 O4 97.8(7) . 1_554 ?
O7 Si3 O4 157.2(9) . 1_554 ?
O6 Si3 O7 99.7(8) . 2_676 ?
O7 Si3 O7 82.9(6) . 2_676 ?
O4 Si3 O7 92.3(3) 1_554 2_676 ?
O6 Si3 O3 104.0(6) . . ?
O7 Si3 O3 86.1(6) . . ?
O4 Si3 O3 89.5(4) 1_554 . ?
O7 Si3 O3 155.7(11) 2_676 . ?
O6 Si3 Si3 106.6(4) . 2_676 ?
O7 Si3 Si3 41.6(3) . 2_676 ?
O4 Si3 Si3 129.8(2) 1_554 2_676 ?
O7 Si3 Si3 41.3(4) 2_676 2_676 ?
O3 Si3 Si3 124.4(7) . 2_676 ?
O6 Si3 Si1 30.5(2) . . ?
O7 Si3 Si1 93.1(6) . . ?
O4 Si3 Si1 106.3(7) 1_554 . ?
O7 Si3 Si1 70.3(7) 2_676 . ?
O3 Si3 Si1 132.0(5) . . ?
Si3 Si3 Si1 79.1(3) 2_676 . ?
O6 Si3 Na1 126.5(5) . 1_564 ?
O7 Si3 Na1 105.3(4) . 1_564 ?
O4 Si3 Na1 58.5(3) 1_554 1_564 ?
O7 Si3 Na1 43.1(3) 2_676 1_564 ?
O3 Si3 Na1 121.0(5) . 1_564 ?
Si3 Si3 Na1 71.75(14) 2_676 1_564 ?
Si1 Si3 Na1 105.5(2) . 1_564 ?
O6 Si3 Na1 70.3(4) . 2_667 ?
O7 Si3 Na1 35.6(5) . 2_667 ?
O4 Si3 Na1 166.3(6) 1_554 2_667 ?
O7 Si3 Na1 96.23(18) 2_676 2_667 ?
O3 Si3 Na1 87.1(2) . 2_667 ?
Si3 Si3 Na1 62.13(11) 2_676 2_667 ?
Si1 Si3 Na1 66.9(2) . 2_667 ?
Na1 Si3 Na1 133.88(10) 1_564 2_667 ?
O4 Si2 O1 104.8(7) . . ?
O4 Si2 O5 110.1(8) . 2_777 ?
O1 Si2 O5 114.3(9) . 2_777 ?
O4 Si2 O2 105.8(8) . . ?
O1 Si2 O2 114.1(7) . . ?
O5 Si2 O2 107.4(3) 2_777 . ?
O4 Si2 Na1 51.1(3) . 2_667 ?
O1 Si2 Na1 109.2(5) . 2_667 ?
O5 Si2 Na1 136.1(8) 2_777 2_667 ?
O2 Si2 Na1 57.2(6) . 2_667 ?
O4 Si2 Na1 61.9(4) . 1_565 ?
O1 Si2 Na1 144.2(3) . 1_565 ?
O5 Si2 Na1 52.1(8) 2_777 1_565 ?
O2 Si2 Na1 101.7(6) . 1_565 ?
Na1 Si2 Na1 88.5(2) 2_667 1_565 ?
O8 Na1 O7 76.0(3) 2_768 2_667 ?
O8 Na1 O4 155.6(9) 2_768 2_667 ?
O7 Na1 O4 123.4(3) 2_667 2_667 ?
O8 Na1 O8 80.7(5) 2_768 . ?
O7 Na1 O8 123.2(7) 2_667 . ?
O4 Na1 O8 97.1(3) 2_667 . ?
O8 Na1 O5 104.5(8) 2_768 2_767 ?
O7 Na1 O5 74.3(6) 2_667 2_767 ?
O4 Na1 O5 95.7(6) 2_667 2_767 ?
O8 Na1 O5 62.6(5) . 2_767 ?
O8 Na1 O2 108.7(7) 2_768 2_667 ?
O7 Na1 O2 79.6(5) 2_667 2_667 ?
O4 Na1 O2 65.6(4) 2_667 2_667 ?
O8 Na1 O2 157.2(5) . 2_667 ?
O5 Na1 O2 130.8(4) 2_767 2_667 ?
O8 Na1 O1 88.9(4) 2_768 . ?
O7 Na1 O1 164.1(4) 2_667 . ?
O4 Na1 O1 70.0(3) 2_667 . ?
O8 Na1 O1 57.4(8) . . ?
O5 Na1 O1 115.0(6) 2_767 . ?
O2 Na1 O1 101.1(7) 2_667 . ?
O8 Na1 O4 135.4(4) 2_768 1_545 ?
O7 Na1 O4 59.7(2) 2_667 1_545 ?
O4 Na1 O4 66.8(5) 2_667 1_545 ?
O8 Na1 O4 118.5(7) . 1_545 ?
O5 Na1 O4 60.9(5) 2_767 1_545 ?
O2 Na1 O4 70.0(5) 2_667 1_545 ?
O1 Na1 O4 135.7(2) . 1_545 ?
O8 Na1 B1 96.5(2) 2_768 . ?
O7 Na1 B1 152.0(10) 2_667 . ?
O4 Na1 B1 72.7(4) 2_667 . ?
O8 Na1 B1 29.3(6) . . ?
O5 Na1 B1 81.7(7) 2_767 . ?
O2 Na1 B1 127.9(8) 2_667 . ?
O1 Na1 B1 33.3(10) . . ?
O4 Na1 B1 119.9(5) 1_545 . ?
O8 Na1 O6 61.4(7) 2_768 1_556 ?
O7 Na1 O6 109.0(5) 2_667 1_556 ?
O4 Na1 O6 96.1(7) 2_667 1_556 ?
O8 Na1 O6 103.4(5) . 1_556 ?
O5 Na1 O6 162.7(4) 2_767 1_556 ?
O2 Na1 O6 65.9(5) 2_667 1_556 ?
O1 Na1 O6 58.1(5) . 1_556 ?
O4 Na1 O6 135.8(6) 1_545 1_556 ?
B1 Na1 O6 89.8(7) . 1_556 ?
O8 Na1 Si2 133.8(8) 2_768 2_667 ?
O7 Na1 Si2 108.5(4) 2_667 2_667 ?
O4 Na1 Si2 32.0(5) 2_667 2_667 ?
O8 Na1 Si2 124.6(3) . 2_667 ?
O5 Na1 Si2 121.2(2) 2_767 2_667 ?
O2 Na1 Si2 34.79(18) 2_667 2_667 ?
O1 Na1 Si2 78.4(4) . 2_667 ?
O4 Na1 Si2 70.7(4) 1_545 2_667 ?
B1 Na1 Si2 96.2(5) . 2_667 ?
O6 Na1 Si2 74.5(4) 1_556 2_667 ?
O8 Na1 Si2 130.5(8) 2_768 1_545 ?
O7 Na1 Si2 70.3(4) 2_667 1_545 ?
O4 Na1 Si2 73.3(5) 2_667 1_545 ?
O8 Na1 Si2 88.5(5) . 1_545 ?
O5 Na1 Si2 32.1(2) 2_767 1_545 ?
O2 Na1 Si2 99.8(4) 2_667 1_545 ?
O1 Na1 Si2 124.7(4) . 1_545 ?
O4 Na1 Si2 30.4(4) 1_545 1_545 ?
B1 Na1 Si2 96.7(6) . 1_545 ?
O6 Na1 Si2 165.2(4) 1_556 1_545 ?
Si2 Na1 Si2 91.5(2) 2_667 1_545 ?
B1 O1 Si2 123.5(6) . . ?
B1 O1 Na1 79.5(10) . . ?
Si2 O1 Na1 156.6(10) . . ?
Si1 O2 Si2 144.7(14) . . ?
Si1 O2 Na1 113.9(4) . 2_667 ?
Si2 O2 Na1 88.0(6) . 2_667 ?
B1 O3 B1 87.4(5) 1_454 2_666 ?
B1 O3 Si3 116.3(9) 1_454 . ?
B1 O3 Si3 132.4(15) 2_666 . ?
Si2 O4 Si3 127.7(9) . 1_556 ?
Si2 O4 Na1 96.9(4) . 2_667 ?
Si3 O4 Na1 131.9(8) 1_556 2_667 ?
Si2 O4 Na1 87.6(3) . 1_565 ?
Si3 O4 Na1 88.5(4) 1_556 1_565 ?
Na1 O4 Na1 113.2(5) 2_667 1_565 ?
Si1 O5 Si2 140.5(4) . 2_777 ?
Si1 O5 Na1 98.5(8) . 2_767 ?
Si2 O5 Na1 95.8(9) 2_777 2_767 ?
Si1 O6 Si3 117.2(5) . . ?
Si1 O6 Na1 83.6(9) . 1_554 ?
Si3 O6 Na1 149.8(3) . 1_554 ?
Si3 O7 Si3 97.1(6) . 2_676 ?
Si3 O7 Na1 117.9(10) . 2_667 ?
Si3 O7 Na1 105.0(5) 2_676 2_667 ?
B1 O8 Si1 128.0(11) . 2_767 ?
B1 O8 Na1 121.1(11) . 2_768 ?
Si1 O8 Na1 107.1(9) 2_767 2_768 ?
B1 O8 Na1 91.5(11) . . ?
Si1 O8 Na1 99.2(4) 2_767 . ?
Na1 O8 Na1 99.3(5) 2_768 . ?
O8 B1 O3 120.2(19) . 1_656 ?
O8 B1 O1 111.4(11) . . ?
O3 B1 O1 109.1(18) 1_656 . ?
O8 B1 O3 111.9(17) . 2_666 ?
O3 B1 O3 92.6(5) 1_656 2_666 ?
O1 B1 O3 110.2(17) . 2_666 ?
O8 B1 B1 129(3) . 2_767 ?
O3 B1 B1 47.3(4) 1_656 2_767 ?
O1 B1 B1 119(2) . 2_767 ?
O3 B1 B1 45.3(4) 2_666 2_767 ?
O8 B1 Na1 59.2(6) . . ?
O3 B1 Na1 174.3(11) 1_656 . ?
O1 B1 Na1 67.2(6) . . ?
O3 B1 Na1 92.7(4) 2_666 . ?
B1 B1 Na1 138.0(5) 2_767 . ?
O8 B1 Na1 36.9(6) . 2_768 ?
O3 B1 Na1 103.8(6) 1_656 2_768 ?
O1 B1 Na1 89.7(5) . 2_768 ?
O3 B1 Na1 148.7(16) 2_666 2_768 ?
B1 B1 Na1 143.0(17) 2_767 2_768 ?
Na1 B1 Na1 72.3(2) . 2_768 ?

_refine_diff_density_max         1.256
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.267


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.246 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.76 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        596 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          6 Check 
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zfy
_database_code_depnum_ccdc_archive 'CCDC 2150700'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.7571(19)
_cell_length_b                   7.109(2)
_cell_length_c                   11.921(2)
_cell_angle_alpha                97.574(18)
_cell_angle_beta                 90.949(18)
_cell_angle_gamma                118.25(3)
_cell_volume                     498.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1276
_cell_measurement_theta_min      1.623
_cell_measurement_theta_max      17.958

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.120
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1824
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.623
_diffrn_reflns_theta_max         17.958
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.127
_diffrn_measured_fraction_theta_full 0.258
_diffrn_reflns_Laue_measured_fraction_max 0.127
_diffrn_reflns_Laue_measured_fraction_full 0.258
_diffrn_reflns_point_group_measured_fraction_max 0.127
_diffrn_reflns_point_group_measured_fraction_full 0.258
_reflns_number_total             1276
_reflns_number_gt                915
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1725P)²+4.0090P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1276
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.3088
_refine_ls_wR_factor_gt          0.2403
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Si1 Si 0.8183(7) 0.4421(7) 0.8463(3) 0.0098(4) Uiso 1 1 d . . . . .
Si2 Si 0.6188(7) 0.3904(7) 0.6021(3) 0.014(4) Uani 1 1 d . . . . .
Si3 Si 0.1807(7) 0.0575(7) 0.6666(3) 0.021(4) Uani 1 1 d . . . . .
Si4 Si 0.3860(7) 0.0940(7) 0.8962(3) 0.016(4) Uani 1 1 d . . . . .
Si5 Si 0.7103(7) 0.3885(7) 0.1804(3) 0.021(4) Uani 1 1 d . . . . .
Si6 Si 0.2924(7) 0.1292(7) 0.3292(3) 0.032(4) Uani 1 1 d . . . . .
Na1 Na 0.0564(11) 0.3178(11) 0.5410(4) 0.0125(6) Uiso 1 1 d . . . . .
Na2 Na 0.0132(11) -0.1602(12) 1.0721(5) 0.031(7) Uani 1 1 d . . . . .
O1 O 1.0519(19) 0.4479(19) 0.8643(7) 0.0128(10) Uiso 1 1 d . . . . .
O2 O 0.3552(18) 0.2199(18) 0.5883(7) 0.0112(9) Uiso 1 1 d . . . . .
O3 O 0.6517(19) 0.6344(18) 0.6025(7) 0.0134(10) Uiso 1 1 d . . . . .
O4 O 0.7350(18) 0.3760(18) 0.7144(7) 0.0129(10) Uiso 1 1 d . . . . .
O5 O -0.0515(18) 0.0482(18) 0.6313(7) 0.0125(10) Uiso 1 1 d . . . . .
O6 O 0.2638(17) 0.1413(17) 0.7965(7) 0.0105(9) Uiso 1 1 d . . . . .
O7 O 0.872(2) 0.673(2) 0.8960(8) 0.0174(12) Uiso 1 1 d . . . . .
O8 O 0.5170(19) 0.4391(18) 0.1328(8) 0.0126(9) Uiso 1 1 d . . . . .
O9 O 0.4815(18) 0.0729(18) 0.3635(7) 0.0123(9) Uiso 1 1 d . . . . .
O10 O 0.2461(18) 0.1150(18) 0.1972(7) 0.0123(9) Uiso 1 1 d . . . . .
O11 O 0.7514(19) 0.3550(19) 0.5046(8) 0.0138(10) Uiso 1 1 d . . . . .
O12 O 0.2699(19) 0.1069(18) 1.0023(7) 0.0118(9) Uiso 1 1 d . . . . .
O13 O 0.7416(19) 0.4188(19) 0.3145(8) 0.0140(10) Uiso 1 1 d . . . . .
O14 O 0.1210(19) -0.183(2) 0.6382(8) 0.0149(10) Uiso 1 1 d . . . . .
O15 O 0.6521(19) 0.2523(18) 0.9128(7) 0.0129(9) Uiso 1 1 d . . . . .
O16 O 0.3417(19) -0.1503(19) 0.8680(8) 0.0141(10) Uiso 1 1 d . . . . .
B1 B 0.699(3) 0.263(3) 0.3903(11) 0.0106(12) Uiso 1 1 d . . . . .
B2 B 0.297(3) 0.256(3) 0.1111(10) 0.0098(12) Uiso 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
Si1 O7 1.534(19) . ?
Si1 O1 1.569(18) . ?
Si1 O4 1.592(7) . ?
Si1 O15 1.609(6) . ?
Si1 Na2 2.983(12) 2_657 ?
Si1 Na2 3.366(9) 1_665 ?
Si2 O11 1.545(19) . ?
Si2 O4 1.580(7) . ?
Si2 O2 1.601(8) . ?
Si2 O3 1.640(17) . ?
Si2 Na1 2.962(5) 2_666 ?
Si2 Na1 3.310(13) 1_655 ?
Si3 O14 1.549(19) . ?
Si3 O6 1.575(8) . ?
Si3 O5 1.586(16) . ?
Si3 O2 1.621(7) . ?
Si3 Si6 2.826(7) 2_556 ?
Si3 Na1 2.921(9) . ?
Si3 Na1 3.145(7) 2_556 ?
Si3 Na2 3.520(11) 2_557 ?
Si4 O12 1.515(17) . ?
Si4 O6 1.595(9) . ?
Si4 O15 1.597(9) . ?
Si4 O16 1.603(18) . ?
Si4 Na2 2.971(14) 2_557 ?
Si4 Na2 3.298(7) . ?
Si5 O16 1.580(17) 2_656 ?
Si5 O13 1.581(8) . ?
Si5 O8 1.622(17) . ?
Si5 O1 1.626(10) 2_766 ?
Si5 Na2 3.334(5) 1_664 ?
Si6 O9 1.572(18) . ?
Si6 O10 1.580(6) . ?
Si6 O3 1.630(17) 2_666 ?
Si6 O5 1.643(9) 2_556 ?
Si6 Na2 3.414(6) 1_554 ?
Si6 Na1 3.461(13) . ?
Si6 Na1 3.517(4) 2_556 ?
Na1 O5 2.148(9) . ?
Na1 O11 2.212(9) 2_666 ?
Na1 O13 2.234(11) 2_666 ?
Na1 O11 2.24(2) 1_455 ?
Na1 O14 2.281(8) 2_556 ?
Na1 O2 2.505(19) . ?
Na1 O3 2.562(19) 2_666 ?
Na1 B1 2.634(18) 2_666 ?
Na1 B1 2.827(16) 1_455 ?
Na2 O1 2.126(14) 2_657 ?
Na2 O12 2.157(7) . ?
Na2 O10 2.183(10) 1_556 ?
Na2 O7 2.219(10) 1_445 ?
Na2 O12 2.304(18) 2_557 ?
Na2 O6 2.50(2) 2_557 ?
Na2 B2 2.621(14) 1_556 ?
Na2 O15 2.65(2) 2_657 ?
Na2 B2 2.780(10) 2_556 ?
Na2 Na2 3.095(14) 2_557 ?
O7 B2 1.46(4) 2_666 ?
O8 B2 1.430(9) . ?
O9 B1 1.442(9) . ?
O10 B2 1.459(11) . ?
O11 B1 1.393(19) . ?
O12 B2 1.51(3) 1_556 ?
O13 B1 1.448(14) . ?
O14 B1 1.59(4) 2_656 ?

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
O7 Si1 O1 102.7(7) . . ?
O7 Si1 O4 114.2(7) . . ?
O1 Si1 O4 109.1(9) . . ?
O7 Si1 O15 116.7(9) . . ?
O1 Si1 O15 104.0(7) . . ?
O4 Si1 O15 109.2(3) . . ?
O7 Si1 Na2 129.5(4) . 2_657 ?
O1 Si1 Na2 43.1(3) . 2_657 ?
O4 Si1 Na2 112.6(8) . 2_657 ?
O15 Si1 Na2 62.1(7) . 2_657 ?
O7 Si1 Na2 32.0(3) . 1_665 ?
O1 Si1 Na2 84.9(5) . 1_665 ?
O4 Si1 Na2 146.0(6) . 1_665 ?
O15 Si1 Na2 96.3(5) . 1_665 ?
Na2 Si1 Na2 98.9(3) 2_657 1_665 ?
O11 Si2 O4 105.8(9) . . ?
O11 Si2 O2 114.4(6) . . ?
O4 Si2 O2 110.3(4) . . ?
O11 Si2 O3 105.6(7) . . ?
O4 Si2 O3 111.3(6) . . ?
O2 Si2 O3 109.3(9) . . ?
O11 Si2 Na1 46.8(5) . 2_666 ?
O4 Si2 Na1 113.3(4) . 2_666 ?
O2 Si2 Na1 135.9(2) . 2_666 ?
O3 Si2 Na1 59.7(6) . 2_666 ?
O11 Si2 Na1 35.5(4) . 1_655 ?
O4 Si2 Na1 70.3(7) . 1_655 ?
O2 Si2 Na1 129.9(8) . 1_655 ?
O3 Si2 Na1 116.8(6) . 1_655 ?
Na1 Si2 Na1 62.8(3) 2_666 1_655 ?
O14 Si3 O6 109.5(6) . . ?
O14 Si3 O5 101.9(7) . . ?
O6 Si3 O5 114.1(9) . . ?
O14 Si3 O2 116.5(10) . . ?
O6 Si3 O2 111.1(3) . . ?
O5 Si3 O2 103.5(6) . . ?
O14 Si3 Si6 81.7(6) . 2_556 ?
O6 Si3 Si6 101.8(6) . 2_556 ?
O5 Si3 Si6 29.5(2) . 2_556 ?
O2 Si3 Si6 132.3(5) . 2_556 ?
O14 Si3 Na1 130.2(3) . . ?
O6 Si3 Na1 118.1(7) . . ?
O5 Si3 Na1 46.0(3) . . ?
O2 Si3 Na1 58.9(6) . . ?
Si6 Si3 Na1 75.4(2) 2_556 . ?
O14 Si3 Na1 43.4(3) . 2_556 ?
O6 Si3 Na1 151.6(4) . 2_556 ?
O5 Si3 Na1 73.1(6) . 2_556 ?
O2 Si3 Na1 92.5(4) . 2_556 ?
Si6 Si3 Na1 70.6(2) 2_556 2_556 ?
Na1 Si3 Na1 87.1(3) . 2_556 ?
O14 Si3 Na2 111.0(5) . 2_557 ?
O6 Si3 Na2 39.0(6) . 2_557 ?
O5 Si3 Na2 76.1(5) . 2_557 ?
O2 Si3 Na2 131.3(6) . 2_557 ?
Si6 Si3 Na2 64.00(17) 2_556 2_557 ?
Na1 Si3 Na2 97.7(3) . 2_557 ?
Na1 Si3 Na2 131.23(17) 2_556 2_557 ?
O12 Si4 O6 107.0(9) . . ?
O12 Si4 O15 112.9(6) . . ?
O6 Si4 O15 112.7(4) . . ?
O12 Si4 O16 106.4(7) . . ?
O6 Si4 O16 109.1(6) . . ?
O15 Si4 O16 108.6(9) . . ?
O12 Si4 Na2 49.8(5) . 2_557 ?
O6 Si4 Na2 57.3(6) . 2_557 ?
O15 Si4 Na2 133.7(8) . 2_557 ?
O16 Si4 Na2 117.4(5) . 2_557 ?
O12 Si4 Na2 31.5(4) . . ?
O6 Si4 Na2 109.1(5) . . ?
O15 Si4 Na2 132.9(3) . . ?
O16 Si4 Na2 76.2(5) . . ?
Na2 Si4 Na2 58.9(3) 2_557 . ?
O16 Si5 O13 108.0(7) 2_656 . ?
O16 Si5 O8 111.2(6) 2_656 . ?
O13 Si5 O8 113.7(10) . . ?
O16 Si5 O1 107.3(10) 2_656 2_766 ?
O13 Si5 O1 108.4(4) . 2_766 ?
O8 Si5 O1 108.0(6) . 2_766 ?
O16 Si5 Na2 128.3(5) 2_656 1_664 ?
O13 Si5 Na2 114.2(4) . 1_664 ?
O8 Si5 Na2 77.8(3) . 1_664 ?
O1 Si5 Na2 31.5(7) 2_766 1_664 ?
O9 Si6 O10 114.8(10) . . ?
O9 Si6 O3 109.8(6) . 2_666 ?
O10 Si6 O3 111.1(7) . 2_666 ?
O9 Si6 O5 108.9(6) . 2_556 ?
O10 Si6 O5 104.8(3) . 2_556 ?
O3 Si6 O5 107.0(9) 2_666 2_556 ?
O9 Si6 Si3 136.9(3) . 2_556 ?
O10 Si6 Si3 85.5(5) . 2_556 ?
O3 Si6 Si3 95.5(6) 2_666 2_556 ?
O5 Si6 Si3 28.4(5) 2_556 2_556 ?
O9 Si6 Na2 111.1(6) . 1_554 ?
O10 Si6 Na2 29.5(3) . 1_554 ?
O3 Si6 Na2 133.8(4) 2_666 1_554 ?
O5 Si6 Na2 79.1(3) 2_556 1_554 ?
Si3 Si6 Na2 67.93(19) 2_556 1_554 ?
O9 Si6 Na1 119.0(5) . . ?
O10 Si6 Na1 125.9(8) . . ?
O3 Si6 Na1 44.3(4) 2_666 . ?
O5 Si6 Na1 62.9(7) 2_556 . ?
Si3 Si6 Na1 58.99(19) 2_556 . ?
Na2 Si6 Na1 124.1(3) 1_554 . ?
O9 Si6 Na1 83.7(3) . 2_556 ?
O10 Si6 Na1 118.5(2) . 2_556 ?
O3 Si6 Na1 115.9(4) 2_666 2_556 ?
O5 Si6 Na1 25.2(6) 2_556 2_556 ?
Si3 Si6 Na1 53.50(18) 2_556 2_556 ?
Na2 Si6 Na1 89.18(11) 1_554 2_556 ?
Na1 Si6 Na1 73.7(3) . 2_556 ?
O5 Na1 O11 161.6(2) . 2_666 ?
O5 Na1 O13 98.1(3) . 2_666 ?
O11 Na1 O13 64.6(3) 2_666 2_666 ?
O5 Na1 O11 106.5(5) . 1_455 ?
O11 Na1 O11 85.1(5) 2_666 1_455 ?
O13 Na1 O11 105.0(8) 2_666 1_455 ?
O5 Na1 O14 106.9(4) . 2_556 ?
O11 Na1 O14 91.0(3) 2_666 2_556 ?
O13 Na1 O14 154.5(5) 2_666 2_556 ?
O11 Na1 O14 63.3(7) 1_455 2_556 ?
O5 Na1 O2 65.0(5) . . ?
O11 Na1 O2 103.7(5) 2_666 . ?
O13 Na1 O2 79.4(6) 2_666 . ?
O11 Na1 O2 171.2(3) 1_455 . ?
O14 Na1 O2 115.8(8) 2_556 . ?
O5 Na1 O3 117.7(8) . 2_666 ?
O11 Na1 O3 63.8(6) 2_666 2_666 ?
O13 Na1 O3 102.7(4) 2_666 2_666 ?
O11 Na1 O3 122.9(4) 1_455 2_666 ?
O14 Na1 O3 70.3(5) 2_556 2_666 ?
O2 Na1 O3 62.5(4) . 2_666 ?
O5 Na1 B1 131.4(3) . 2_666 ?
O11 Na1 B1 31.9(4) 2_666 2_666 ?
O13 Na1 B1 33.4(3) 2_666 2_666 ?
O11 Na1 B1 90.9(7) 1_455 2_666 ?
O14 Na1 B1 121.3(4) 2_556 2_666 ?
O2 Na1 B1 96.7(6) . 2_666 ?
O3 Na1 B1 85.9(6) 2_666 2_666 ?
O5 Na1 B1 110.5(3) . 1_455 ?
O11 Na1 B1 86.6(4) 2_666 1_455 ?
O13 Na1 B1 130.4(9) 2_666 1_455 ?
O11 Na1 B1 29.1(7) 1_455 1_455 ?
O14 Na1 B1 34.2(9) 2_556 1_455 ?
O2 Na1 B1 149.4(8) . 1_455 ?
O3 Na1 B1 98.6(5) 2_666 1_455 ?
B1 Na1 B1 106.3(3) 2_666 1_455 ?
O5 Na1 Si3 32.1(4) . . ?
O11 Na1 Si3 133.3(4) 2_666 . ?
O13 Na1 Si3 83.8(4) 2_666 . ?
O11 Na1 Si3 138.2(3) 1_455 . ?
O14 Na1 Si3 120.5(6) 2_556 . ?
O2 Na1 Si3 33.7(2) . . ?
O3 Na1 Si3 93.5(5) 2_666 . ?
B1 Na1 Si3 113.6(4) 2_666 . ?
B1 Na1 Si3 139.0(4) 1_455 . ?
O5 Na1 Si2 149.7(7) . 2_666 ?
O11 Na1 Si2 30.6(5) 2_666 2_666 ?
O13 Na1 Si2 85.0(2) 2_666 2_666 ?
O11 Na1 Si2 101.8(3) 1_455 2_666 ?
O14 Na1 Si2 76.2(2) 2_556 2_666 ?
O2 Na1 Si2 86.2(3) . 2_666 ?
O3 Na1 Si2 33.6(4) 2_666 2_666 ?
B1 Na1 Si2 57.8(4) 2_666 2_666 ?
B1 Na1 Si2 89.1(2) 1_455 2_666 ?
Si3 Na1 Si2 119.9(4) . 2_666 ?
O5 Na1 Si3 81.5(3) . 2_556 ?
O11 Na1 Si3 114.9(3) 2_666 2_556 ?
O13 Na1 Si3 173.8(7) 2_666 2_556 ?
O11 Na1 Si3 81.0(4) 1_455 2_556 ?
O14 Na1 Si3 27.8(4) 2_556 2_556 ?
O2 Na1 Si3 95.0(4) . 2_556 ?
O3 Na1 Si3 72.2(3) 2_666 2_556 ?
B1 Na1 Si3 146.8(2) 2_666 2_556 ?
B1 Na1 Si3 55.0(6) 1_455 2_556 ?
Si3 Na1 Si3 92.9(3) . 2_556 ?
Si2 Na1 Si3 92.2(2) 2_666 2_556 ?
O1 Na2 O12 142.6(9) 2_657 . ?
O1 Na2 O10 108.0(3) 2_657 1_556 ?
O12 Na2 O10 64.8(3) . 1_556 ?
O1 Na2 O7 94.5(5) 2_657 1_445 ?
O12 Na2 O7 88.6(3) . 1_445 ?
O10 Na2 O7 153.3(3) 1_556 1_445 ?
O1 Na2 O12 122.6(4) 2_657 2_557 ?
O12 Na2 O12 92.2(5) . 2_557 ?
O10 Na2 O12 111.9(8) 1_556 2_557 ?
O7 Na2 O12 64.3(7) 1_445 2_557 ?
O1 Na2 O6 85.7(6) 2_657 2_557 ?
O12 Na2 O6 126.0(8) . 2_557 ?
O10 Na2 O6 80.9(6) 1_556 2_557 ?
O7 Na2 O6 115.8(6) 1_445 2_557 ?
O12 Na2 O6 62.5(5) 2_557 2_557 ?
O1 Na2 B2 139.8(4) 2_657 1_556 ?
O12 Na2 B2 35.2(6) . 1_556 ?
O10 Na2 B2 33.8(2) 1_556 1_556 ?
O7 Na2 B2 120.2(3) 1_445 1_556 ?
O12 Na2 B2 92.5(6) 2_557 1_556 ?
O6 Na2 B2 95.4(7) 2_557 1_556 ?
O1 Na2 O15 62.2(6) 2_657 2_657 ?
O12 Na2 O15 80.5(6) . 2_657 ?
O10 Na2 O15 80.4(6) 1_556 2_657 ?
O7 Na2 O15 98.3(8) 1_445 2_657 ?
O12 Na2 O15 161.5(5) 2_557 2_657 ?
O6 Na2 O15 135.1(3) 2_557 2_657 ?
B2 Na2 O15 91.2(6) 1_556 2_657 ?
O1 Na2 B2 110.1(4) 2_657 2_556 ?
O12 Na2 B2 91.5(3) . 2_556 ?
O10 Na2 B2 139.7(8) 1_556 2_556 ?
O7 Na2 B2 31.4(9) 1_445 2_556 ?
O12 Na2 B2 32.9(7) 2_557 2_556 ?
O6 Na2 B2 89.1(6) 2_557 2_556 ?
B2 Na2 B2 110.1(3) 1_556 2_556 ?
O15 Na2 B2 129.6(8) 2_657 2_556 ?
O1 Na2 Si4 107.6(6) 2_657 2_557 ?
O12 Na2 Si4 109.6(7) . 2_557 ?
O10 Na2 Si4 96.6(7) 1_556 2_557 ?
O7 Na2 Si4 89.9(6) 1_445 2_557 ?
O12 Na2 Si4 30.1(4) 2_557 2_557 ?
O6 Na2 Si4 32.5(3) 2_557 2_557 ?
B2 Na2 Si4 93.1(7) 1_556 2_557 ?
O15 Na2 Si4 167.3(2) 2_657 2_557 ?
B2 Na2 Si4 59.5(6) 2_556 2_557 ?
O1 Na2 Si1 30.3(4) 2_657 2_657 ?
O12 Na2 Si1 112.8(6) . 2_657 ?
O10 Na2 Si1 91.3(5) 1_556 2_657 ?
O7 Na2 Si1 101.9(7) 1_445 2_657 ?
O12 Na2 Si1 151.8(2) 2_557 2_657 ?
O6 Na2 Si1 108.2(3) 2_557 2_657 ?
B2 Na2 Si1 115.5(5) 1_556 2_657 ?
O15 Na2 Si1 32.52(19) 2_657 2_657 ?
B2 Na2 Si1 128.7(6) 2_556 2_657 ?
Si4 Na2 Si1 136.07(18) 2_557 2_657 ?
O1 Na2 Na2 162.7(2) 2_657 2_557 ?
O12 Na2 Na2 48.1(4) . 2_557 ?
O10 Na2 Na2 89.0(5) 1_556 2_557 ?
O7 Na2 Na2 70.1(4) 1_445 2_557 ?
O12 Na2 Na2 44.1(3) 2_557 2_557 ?
O6 Na2 Na2 93.8(6) 2_557 2_557 ?
B2 Na2 Na2 57.5(3) 1_556 2_557 ?
O15 Na2 Na2 126.2(4) 2_657 2_557 ?
B2 Na2 Na2 52.7(3) 2_556 2_557 ?
Si4 Na2 Na2 65.8(4) 2_557 2_557 ?
Si1 Na2 Na2 157.8(6) 2_657 2_557 ?
Si1 O1 Si5 127.4(8) . 2_766 ?
Si1 O1 Na2 106.6(4) . 2_657 ?
Si5 O1 Na2 124.9(12) 2_766 2_657 ?
Si2 O2 Si3 135.3(4) . . ?
Si2 O2 Na1 122.9(7) . . ?
Si3 O2 Na1 87.4(7) . . ?
Si6 O3 Si2 150.4(4) 2_666 . ?
Si6 O3 Na1 109.3(3) 2_666 2_666 ?
Si2 O3 Na1 86.7(9) . 2_666 ?
Si2 O4 Si1 153.8(15) . . ?
Si3 O5 Si6 122.1(7) . 2_556 ?
Si3 O5 Na1 101.9(4) . . ?
Si6 O5 Na1 135.8(10) 2_556 . ?
Si3 O6 Si4 139.3(13) . . ?
Si3 O6 Na2 117.7(7) . 2_557 ?
Si4 O6 Na2 90.2(5) . 2_557 ?
B2 O7 Si1 121.1(6) 2_666 . ?
B2 O7 Na2 96.0(12) 2_666 1_665 ?
Si1 O7 Na2 126.5(7) . 1_665 ?
B2 O8 Si5 114.6(13) . . ?
B1 O9 Si6 112.2(14) . . ?
B2 O10 Si6 140.1(10) . . ?
B2 O10 Na2 89.8(5) . 1_554 ?
Si6 O10 Na2 129.6(4) . 1_554 ?
B1 O11 Si2 135.5(13) . . ?
B1 O11 Na1 91.0(6) . 2_666 ?
Si2 O11 Na1 102.7(10) . 2_666 ?
B1 O11 Na1 99.5(16) . 1_655 ?
Si2 O11 Na1 120.8(4) . 1_655 ?
Na1 O11 Na1 94.9(5) 2_666 1_655 ?
B2 O12 Si4 141.9(6) 1_556 . ?
B2 O12 Na2 89.4(7) 1_556 . ?
Si4 O12 Na2 126.9(9) . . ?
B2 O12 Na2 91.1(13) 1_556 2_557 ?
Si4 O12 Na2 100.1(4) . 2_557 ?
Na2 O12 Na2 87.8(5) . 2_557 ?
B1 O13 Si5 130.8(13) . . ?
B1 O13 Na1 88.7(6) . 2_666 ?
Si5 O13 Na1 138.2(4) . 2_666 ?
Si3 O14 B1 123.9(6) . 2_656 ?
Si3 O14 Na1 108.9(6) . 2_556 ?
B1 O14 Na1 92.0(10) 2_656 2_556 ?
Si4 O15 Si1 132.5(6) . . ?
Si4 O15 Na2 129.6(9) . 2_657 ?
Si1 O15 Na2 85.4(7) . 2_657 ?
Si5 O16 Si4 170.7(4) 2_656 . ?
O11 B1 O9 115.1(12) . . ?
O11 B1 O13 113.4(16) . . ?
O9 B1 O13 112.9(8) . . ?
O11 B1 O14 105.2(13) . 2_656 ?
O9 B1 O14 105.6(19) . 2_656 ?
O13 B1 O14 103.3(14) . 2_656 ?
O11 B1 Na1 57.1(7) . 2_666 ?
O9 B1 Na1 150(2) . 2_666 ?
O13 B1 Na1 58.0(7) . 2_666 ?
O14 B1 Na1 104.4(6) 2_656 2_666 ?
O11 B1 Na1 51.4(10) . 1_655 ?
O9 B1 Na1 126.8(10) . 1_655 ?
O13 B1 Na1 119.3(6) . 1_655 ?
O14 B1 Na1 53.8(5) 2_656 1_655 ?
Na1 B1 Na1 73.7(3) 2_666 1_655 ?
O8 B2 O7 109.9(17) . 2_666 ?
O8 B2 O10 112.5(7) . . ?
O7 B2 O10 109.9(15) 2_666 . ?
O8 B2 O12 112.7(16) . 1_554 ?
O7 B2 O12 108.4(9) 2_666 1_554 ?
O10 B2 O12 103.2(15) . 1_554 ?
O8 B2 Na2 153.8(19) . 1_554 ?
O7 B2 Na2 96.3(6) 2_666 1_554 ?
O10 B2 Na2 56.4(5) . 1_554 ?
O12 B2 Na2 55.4(5) 1_554 1_554 ?
O8 B2 Na2 126.0(6) . 2_556 ?
O7 B2 Na2 52.6(5) 2_666 2_556 ?
O10 B2 Na2 121.5(5) . 2_556 ?
O12 B2 Na2 56.0(7) 1_554 2_556 ?
Na2 B2 Na2 69.9(3) 1_554 2_556 ?

_refine_diff_density_max         0.887
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.187


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.258 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1328 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zbv
_database_code_depnum_ccdc_archive 'CCDC 2150697'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.7152(8)
_cell_length_b                   7.0429(17)
_cell_length_c                   7.3048(15)
_cell_angle_alpha                116.50(2)
_cell_angle_beta                 100.246(13)
_cell_angle_gamma                106.716(15)
_cell_volume                     276.56(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    689
_cell_measurement_theta_min      1.554
_cell_measurement_theta_max      17.461

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.955
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.111
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1000
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         17.461
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.134
_diffrn_measured_fraction_theta_full 0.251
_diffrn_reflns_Laue_measured_fraction_max 0.134
_diffrn_reflns_Laue_measured_fraction_full 0.251
_diffrn_reflns_point_group_measured_fraction_max 0.134
_diffrn_reflns_point_group_measured_fraction_full 0.251
_reflns_number_total             689
_reflns_number_gt                607
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0493P)²+1.1436P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       1.19(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         689
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1374
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_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
Na1 Na 0.8710(4) 0.7362(7) 0.2573(6) 0.0125(4) Uiso 1 1 d . . . . .
B1 B 0.2225(10) 0.1680(15) 0.3540(13) 0.0073(7) Uiso 1 1 d . . . . .
Si1 Si 0.3523(3) 0.5301(4) 0.3099(4) 0.014(3) Uani 1 1 d . . . . .
Si2 Si 0.2085(2) 0.8150(4) -0.3043(4) 0.009(3) Uani 1 1 d . . . . .
Si3 Si 0.3198(3) 0.7953(4) 0.1003(4) 0.007(3) Uani 1 1 d . . . . .
O1 O -0.0022(7) 0.8599(11) -0.3724(10) 0.0088(5) Uiso 1 1 d . . . . .
O2 O 0.1944(8) 0.7071(12) -0.1544(11) 0.0120(6) Uiso 1 1 d . . . . .
O3 O 0.4158(7) 1.0683(12) -0.1735(10) 0.0105(5) Uiso 1 1 d . . . . .
O4 O 0.2756(7) 0.5542(12) 0.0989(10) 0.0101(6) Uiso 1 1 d . . . . .
O5 O 0.2678(7) 0.2584(11) 0.2153(10) 0.0099(5) Uiso 1 1 d . . . . .
O6 O 0.2317(7) 0.6439(11) 0.4749(10) 0.0103(5) Uiso 1 1 d . . . . .
O7 O 0.2166(7) 0.9372(11) 0.2644(10) 0.0107(6) Uiso 1 1 d . . . . .
O8 O 0.6137(7) 0.6770(11) 0.4172(10) 0.0098(5) Uiso 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
Na1 O4 2.259(5) 2_665 ?
Na1 O8 2.293(5) . ?
Na1 O7 2.323(4) 1_655 ?
Na1 O1 2.335(9) 1_656 ?
Na1 O1 2.394(10) 2_675 ?
Na1 O2 2.740(12) 2_665 ?
Na1 O3 2.799(13) 2_675 ?
Na1 B1 2.842(9) 2_666 ?
Na1 B1 2.946(10) 1_665 ?
Na1 Si3 3.131(4) 2_665 ?
Na1 Si2 3.234(8) 2_675 ?
Na1 Si2 3.288(7) 1_656 ?
B1 O7 1.441(14) 1_545 ?
B1 O5 1.449(17) . ?
B1 O1 1.474(6) 2_565 ?
B1 O8 1.490(10) 2_666 ?
Si1 O8 1.584(4) . ?
Si1 O5 1.586(9) . ?
Si1 O6 1.616(3) . ?
Si1 O4 1.635(12) . ?
Si2 O1 1.580(10) . ?
Si2 O2 1.589(14) . ?
Si2 O6 1.594(3) 1_554 ?
Si2 O3 1.616(5) . ?
Si3 O7 1.594(3) . ?
Si3 O3 1.607(4) 2_675 ?
Si3 O4 1.632(12) . ?
Si3 O2 1.633(10) . ?

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
O4 Na1 O8 108.37(16) 2_665 . ?
O4 Na1 O7 98.49(17) 2_665 1_655 ?
O8 Na1 O7 153.13(18) . 1_655 ?
O4 Na1 O1 149.9(5) 2_665 1_656 ?
O8 Na1 O1 61.4(2) . 1_656 ?
O7 Na1 O1 94.6(2) 1_655 1_656 ?
O4 Na1 O1 122.7(5) 2_665 2_675 ?
O8 Na1 O1 105.4(3) . 2_675 ?
O7 Na1 O1 58.5(3) 1_655 2_675 ?
O1 Na1 O1 87.2(4) 1_656 2_675 ?
O4 Na1 O2 61.1(4) 2_665 2_665 ?
O8 Na1 O2 81.5(3) . 2_665 ?
O7 Na1 O2 111.7(3) 1_655 2_665 ?
O1 Na1 O2 88.8(4) 1_656 2_665 ?
O1 Na1 O2 169.0(3) 2_675 2_665 ?
O4 Na1 O3 90.3(3) 2_665 2_675 ?
O8 Na1 O3 73.0(4) . 2_675 ?
O7 Na1 O3 108.5(4) 1_655 2_675 ?
O1 Na1 O3 111.1(2) 1_656 2_675 ?
O1 Na1 O3 57.8(2) 2_675 2_675 ?
O2 Na1 O3 133.14(19) 2_665 2_675 ?
O4 Na1 B1 137.7(2) 2_665 2_666 ?
O8 Na1 B1 31.49(19) . 2_666 ?
O7 Na1 B1 122.3(2) 1_655 2_666 ?
O1 Na1 B1 31.2(2) 1_656 2_666 ?
O1 Na1 B1 90.9(3) 2_675 2_666 ?
O2 Na1 B1 90.9(4) 2_665 2_666 ?
O3 Na1 B1 87.4(3) 2_675 2_666 ?
O4 Na1 B1 114.3(3) 2_665 1_665 ?
O8 Na1 B1 131.23(19) . 1_665 ?
O7 Na1 B1 28.8(3) 1_655 1_665 ?
O1 Na1 B1 89.6(3) 1_656 1_665 ?
O1 Na1 B1 29.8(2) 2_675 1_665 ?
O2 Na1 B1 140.0(3) 2_665 1_665 ?
O3 Na1 B1 84.1(3) 2_675 1_665 ?
B1 Na1 B1 107.5(2) 2_666 1_665 ?
O4 Na1 Si3 30.1(3) 2_665 2_665 ?
O8 Na1 Si3 92.89(18) . 2_665 ?
O7 Na1 Si3 110.61(13) 1_655 2_665 ?
O1 Na1 Si3 119.8(4) 1_656 2_665 ?
O1 Na1 Si3 152.6(3) 2_675 2_665 ?
O2 Na1 Si3 31.4(2) 2_665 2_665 ?
O3 Na1 Si3 110.76(16) 2_675 2_665 ?
B1 Na1 Si3 114.4(3) 2_666 2_665 ?
B1 Na1 Si3 135.77(11) 1_665 2_665 ?
O4 Na1 Si2 109.7(4) 2_665 2_675 ?
O8 Na1 Si2 88.9(3) . 2_675 ?
O7 Na1 Si2 82.9(3) 1_655 2_675 ?
O1 Na1 Si2 98.8(3) 1_656 2_675 ?
O1 Na1 Si2 27.8(2) 2_675 2_675 ?
O2 Na1 Si2 163.11(19) 2_665 2_675 ?
O3 Na1 Si2 29.97(12) 2_675 2_675 ?
B1 Na1 Si2 88.0(3) 2_666 2_675 ?
B1 Na1 Si2 55.7(3) 1_665 2_675 ?
Si3 Na1 Si2 136.7(2) 2_665 2_675 ?
O4 Na1 Si2 132.6(4) 2_665 1_656 ?
O8 Na1 Si2 82.7(3) . 1_656 ?
O7 Na1 Si2 78.4(3) 1_655 1_656 ?
O1 Na1 Si2 26.30(18) 1_656 1_656 ?
O1 Na1 Si2 96.1(2) 2_675 1_656 ?
O2 Na1 Si2 76.0(3) 2_665 1_656 ?
O3 Na1 Si2 136.02(12) 2_675 1_656 ?
B1 Na1 Si2 55.8(3) 2_666 1_656 ?
B1 Na1 Si2 85.3(3) 1_665 1_656 ?
Si3 Na1 Si2 106.5(2) 2_665 1_656 ?
Si2 Na1 Si2 116.64(10) 2_675 1_656 ?
O7 B1 O5 111.2(5) 1_545 . ?
O7 B1 O1 104.6(6) 1_545 2_565 ?
O5 B1 O1 112.7(11) . 2_565 ?
O7 B1 O8 109.4(12) 1_545 2_666 ?
O5 B1 O8 112.8(6) . 2_666 ?
O1 B1 O8 105.7(4) 2_565 2_666 ?
O7 B1 Na1 104.3(8) 1_545 2_666 ?
O5 B1 Na1 144.5(6) . 2_666 ?
O1 B1 Na1 55.0(4) 2_565 2_666 ?
O8 B1 Na1 53.5(3) 2_666 2_666 ?
O7 B1 Na1 50.8(3) 1_545 1_445 ?
O5 B1 Na1 131.0(4) . 1_445 ?
O1 B1 Na1 53.9(5) 2_565 1_445 ?
O8 B1 Na1 116.2(8) 2_666 1_445 ?
Na1 B1 Na1 72.5(2) 2_666 1_445 ?
O8 Si1 O5 116.0(5) . . ?
O8 Si1 O6 110.87(18) . . ?
O5 Si1 O6 111.1(4) . . ?
O8 Si1 O4 104.9(4) . . ?
O5 Si1 O4 105.8(4) . . ?
O6 Si1 O4 107.6(5) . . ?
O8 Si1 Na1 115.2(3) . 2_665 ?
O5 Si1 Na1 74.8(4) . 2_665 ?
O6 Si1 Na1 124.1(4) . 2_665 ?
O4 Si1 Na1 31.4(2) . 2_665 ?
O8 Si1 Na1 29.8(3) . . ?
O5 Si1 Na1 109.05(17) . . ?
O6 Si1 Na1 135.00(17) . . ?
O4 Si1 Na1 79.66(17) . . ?
Na1 Si1 Na1 85.45(9) 2_665 . ?
O1 Si2 O2 113.7(4) . . ?
O1 Si2 O6 107.0(4) . 1_554 ?
O2 Si2 O6 110.3(5) . 1_554 ?
O1 Si2 O3 104.9(5) . . ?
O2 Si2 O3 110.3(5) . . ?
O6 Si2 O3 110.5(2) 1_554 . ?
O1 Si2 Na1 45.0(3) . 2_675 ?
O2 Si2 Na1 130.3(2) . 2_675 ?
O6 Si2 Na1 118.7(5) 1_554 2_675 ?
O3 Si2 Na1 60.0(4) . 2_675 ?
O1 Si2 Na1 40.9(2) . 1_454 ?
O2 Si2 Na1 136.82(18) . 1_454 ?
O6 Si2 Na1 67.1(4) 1_554 1_454 ?
O3 Si2 Na1 110.4(5) . 1_454 ?
Na1 Si2 Na1 63.36(10) 2_675 1_454 ?
O7 Si3 O3 113.28(18) . 2_675 ?
O7 Si3 O4 107.5(4) . . ?
O3 Si3 O4 107.2(5) 2_675 . ?
O7 Si3 O2 113.5(5) . . ?
O3 Si3 O2 110.6(4) 2_675 . ?
O4 Si3 O2 104.2(4) . . ?
O7 Si3 Na1 130.55(18) . 2_665 ?
O3 Si3 Na1 113.9(2) 2_675 2_665 ?
O4 Si3 Na1 43.9(3) . 2_665 ?
O2 Si3 Na1 61.0(4) . 2_665 ?
O7 Si3 Na1 36.86(18) . 1_455 ?
O3 Si3 Na1 146.74(16) 2_675 1_455 ?
O4 Si3 Na1 79.55(17) . 1_455 ?
O2 Si3 Na1 98.63(17) . 1_455 ?
Na1 Si3 Na1 93.70(7) 2_665 1_455 ?
B1 O1 Si2 142.9(10) 2_565 . ?
B1 O1 Na1 93.8(6) 2_565 1_454 ?
Si2 O1 Na1 112.82(18) . 1_454 ?
B1 O1 Na1 96.3(6) 2_565 2_675 ?
Si2 O1 Na1 107.1(2) . 2_675 ?
Na1 O1 Na1 92.8(4) 1_454 2_675 ?
Si2 O2 Si3 136.5(4) . . ?
Si2 O2 Na1 129.26(19) . 2_665 ?
Si3 O2 Na1 87.6(6) . 2_665 ?
Si3 O3 Si2 145.2(6) 2_675 . ?
Si3 O3 Na1 120.5(6) 2_675 2_675 ?
Si2 O3 Na1 90.1(4) . 2_675 ?
Si3 O4 Si1 127.0(2) . . ?
Si3 O4 Na1 106.0(5) . 2_665 ?
Si1 O4 Na1 126.5(5) . 2_665 ?
B1 O5 Si1 120.1(4) . . ?
Si2 O6 Si1 158.4(3) 1_556 . ?
B1 O7 Si3 134.3(7) 1_565 . ?
B1 O7 Na1 100.4(3) 1_565 1_455 ?
Si3 O7 Na1 118.8(3) . 1_455 ?
B1 O8 Si1 134.8(4) 2_666 . ?
B1 O8 Na1 95.0(3) 2_666 . ?
Si1 O8 Na1 130.1(4) . . ?

_refine_diff_density_max         0.479
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.108


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.251 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        740 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zcw
_database_code_depnum_ccdc_archive 'CCDC 2150698'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.6565(9)
_cell_length_b                   6.944(2)
_cell_length_c                   7.234(2)
_cell_angle_alpha                117.19(3)
_cell_angle_beta                 99.971(17)
_cell_angle_gamma                106.418(18)
_cell_volume                     266.79(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    560
_cell_measurement_theta_min      1.573
_cell_measurement_theta_max      17.154

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.063
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.115
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            771
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.573
_diffrn_reflns_theta_max         17.154
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.119
_diffrn_measured_fraction_theta_full 0.218
_diffrn_reflns_Laue_measured_fraction_max 0.119
_diffrn_reflns_Laue_measured_fraction_full 0.218
_diffrn_reflns_point_group_measured_fraction_max 0.119
_diffrn_reflns_point_group_measured_fraction_full 0.218
_reflns_number_total             560
_reflns_number_gt                493
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0786P)²+3.9356P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.8(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         560
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.2510
_refine_ls_wR_factor_gt          0.2037
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.194
_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
Na1 Na 0.8747(9) 0.7361(14) 0.2609(14) 0.0160(9) Uiso 1 1 d . . . . .
B1 B 0.214(2) 0.177(3) 0.344(4) 0.0141(16) Uiso 1 1 d . . . . .
Si1 Si 0.3487(5) 0.5237(8) 0.3010(8) 0.0106(6) Uiso 1 1 d . . . . .
Si2 Si 0.2094(5) 0.8144(8) -0.3009(8) 0.0110(6) Uiso 1 1 d . . . . .
Si3 Si 0.3212(5) 0.7899(8) 0.1021(8) 0.0107(6) Uiso 1 1 d . . . . .
O1 O 0.0020(15) 0.856(2) -0.367(2) 0.0152(12) Uiso 1 1 d . . . . .
O2 O 0.1903(16) 0.703(3) -0.151(3) 0.0170(13) Uiso 1 1 d . . . . .
O3 O 0.4154(15) 1.074(2) -0.170(2) 0.0155(12) Uiso 1 1 d . . . . .
O4 O 0.2722(13) 0.540(2) 0.091(2) 0.0108(11) Uiso 1 1 d . . . . .
O5 O 0.2639(14) 0.242(2) 0.207(2) 0.0122(11) Uiso 1 1 d . . . . .
O6 O 0.2259(14) 0.642(2) 0.466(2) 0.0147(12) Uiso 1 1 d . . . . .
O7 O 0.2242(14) 0.937(2) 0.276(2) 0.0138(12) Uiso 1 1 d . . . . .
O8 O 0.6139(14) 0.665(2) 0.412(2) 0.0138(12) Uiso 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
Na1 O4 2.175(10) 2_665 ?
Na1 O8 2.261(12) . ?
Na1 O7 2.305(10) 1_655 ?
Na1 O1 2.33(2) 1_656 ?
Na1 O1 2.40(2) 2_675 ?
Na1 O2 2.65(2) 2_665 ?
Na1 O3 2.77(3) 2_675 ?
Na1 B1 2.85(3) 2_666 ?
Na1 O6 2.94(3) 1_655 ?
Na1 B1 2.96(2) 1_665 ?
Na1 Si3 3.049(7) 2_665 ?
Na1 Si2 3.218(16) 2_675 ?
B1 O5 1.32(4) . ?
B1 O1 1.441(11) 2_565 ?
B1 O7 1.53(3) 1_545 ?
B1 O8 1.57(3) 2_666 ?
Si1 O4 1.58(2) . ?
Si1 O8 1.591(8) . ?
Si1 O6 1.609(6) . ?
Si1 O5 1.623(18) . ?
Si1 Si3 2.837(12) . ?
Si2 O1 1.53(2) . ?
Si2 O2 1.60(3) . ?
Si2 O6 1.607(8) 1_554 ?
Si2 O3 1.617(11) . ?
Si3 O7 1.590(6) . ?
Si3 O3 1.596(7) 2_675 ?
Si3 O2 1.62(2) . ?
Si3 O4 1.64(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
O4 Na1 O8 106.7(4) 2_665 . ?
O4 Na1 O7 99.4(4) 2_665 1_655 ?
O8 Na1 O7 153.9(5) . 1_655 ?
O4 Na1 O1 151.1(10) 2_665 1_656 ?
O8 Na1 O1 62.6(5) . 1_656 ?
O7 Na1 O1 93.3(6) 1_655 1_656 ?
O4 Na1 O1 118.5(10) 2_665 2_675 ?
O8 Na1 O1 107.7(5) . 2_675 ?
O7 Na1 O1 59.5(5) 1_655 2_675 ?
O1 Na1 O1 90.3(9) 1_656 2_675 ?
O4 Na1 O2 62.7(7) 2_665 2_665 ?
O8 Na1 O2 80.2(6) . 2_665 ?
O7 Na1 O2 110.9(6) 1_655 2_665 ?
O1 Na1 O2 88.5(8) 1_656 2_665 ?
O1 Na1 O2 170.3(4) 2_675 2_665 ?
O4 Na1 O3 86.7(7) 2_665 2_675 ?
O8 Na1 O3 74.1(7) . 2_675 ?
O7 Na1 O3 109.9(9) 1_655 2_675 ?
O1 Na1 O3 113.2(5) 1_656 2_675 ?
O1 Na1 O3 57.0(5) 2_675 2_675 ?
O2 Na1 O3 132.0(4) 2_665 2_675 ?
O4 Na1 B1 137.8(5) 2_665 2_666 ?
O8 Na1 B1 33.4(4) . 2_666 ?
O7 Na1 B1 121.0(5) 1_655 2_666 ?
O1 Na1 B1 30.3(5) 1_656 2_666 ?
O1 Na1 B1 94.2(6) 2_675 2_666 ?
O2 Na1 B1 89.7(8) 2_665 2_666 ?
O3 Na1 B1 90.4(7) 2_675 2_666 ?
O4 Na1 O6 107.3(6) 2_665 1_655 ?
O8 Na1 O6 102.5(9) . 1_655 ?
O7 Na1 O6 67.1(7) 1_655 1_655 ?
O1 Na1 O6 54.5(5) 1_656 1_655 ?
O1 Na1 O6 112.8(5) 2_675 1_655 ?
O2 Na1 O6 59.1(5) 2_665 1_655 ?
O3 Na1 O6 165.9(3) 2_675 1_655 ?
B1 Na1 O6 80.3(8) 2_666 1_655 ?
O4 Na1 B1 111.3(8) 2_665 1_665 ?
O8 Na1 B1 133.4(4) . 1_665 ?
O7 Na1 B1 30.7(6) 1_655 1_665 ?
O1 Na1 B1 92.8(7) 1_656 1_665 ?
O1 Na1 B1 28.8(4) 2_675 1_665 ?
O2 Na1 B1 141.7(5) 2_665 1_665 ?
O3 Na1 B1 82.0(7) 2_675 1_665 ?
B1 Na1 B1 109.9(6) 2_666 1_665 ?
O6 Na1 B1 91.1(7) 1_655 1_665 ?
O4 Na1 Si3 31.1(7) 2_665 2_665 ?
O8 Na1 Si3 90.7(3) . 2_665 ?
O7 Na1 Si3 111.4(2) 1_655 2_665 ?
O1 Na1 Si3 119.9(7) 1_656 2_665 ?
O1 Na1 Si3 149.6(8) 2_675 2_665 ?
O2 Na1 Si3 32.0(5) 2_665 2_665 ?
O3 Na1 Si3 108.1(4) 2_675 2_665 ?
B1 Na1 Si3 113.4(6) 2_666 2_665 ?
O6 Na1 Si3 85.4(4) 1_655 2_665 ?
B1 Na1 Si3 135.2(3) 1_665 2_665 ?
O4 Na1 Si2 106.0(8) 2_665 2_675 ?
O8 Na1 Si2 90.8(6) . 2_675 ?
O7 Na1 Si2 83.7(7) 1_655 2_675 ?
O1 Na1 Si2 101.1(5) 1_656 2_675 ?
O1 Na1 Si2 26.9(4) 2_675 2_675 ?
O2 Na1 Si2 162.1(4) 2_665 2_675 ?
O3 Na1 Si2 30.2(3) 2_675 2_675 ?
B1 Na1 Si2 91.3(7) 2_666 2_675 ?
O6 Na1 Si2 138.6(3) 1_655 2_675 ?
B1 Na1 Si2 53.7(6) 1_665 2_675 ?
Si3 Na1 Si2 134.0(5) 2_665 2_675 ?
O5 B1 O1 120(3) . 2_565 ?
O5 B1 O7 110.5(10) . 1_545 ?
O1 B1 O7 103.5(17) 2_565 1_545 ?
O5 B1 O8 115.9(12) . 2_666 ?
O1 B1 O8 104.7(12) 2_565 2_666 ?
O7 B1 O8 100(2) 1_545 2_666 ?
O5 B1 Na1 152.6(14) . 2_666 ?
O1 B1 Na1 54.6(12) 2_565 2_666 ?
O7 B1 Na1 96.5(17) 1_545 2_666 ?
O8 B1 Na1 52.4(8) 2_666 2_666 ?
O5 B1 Na1 131.3(8) . 1_445 ?
O1 B1 Na1 53.4(11) 2_565 1_445 ?
O7 B1 Na1 50.1(6) 1_545 1_445 ?
O8 B1 Na1 111.7(18) 2_666 1_445 ?
Na1 B1 Na1 70.1(6) 2_666 1_445 ?
O4 Si1 O8 107.3(9) . . ?
O4 Si1 O6 107.5(10) . . ?
O8 Si1 O6 111.9(4) . . ?
O4 Si1 O5 105.6(8) . . ?
O8 Si1 O5 113.2(9) . . ?
O6 Si1 O5 111.0(8) . . ?
O4 Si1 Si3 28.6(4) . . ?
O8 Si1 Si3 91.3(10) . . ?
O6 Si1 Si3 92.8(10) . . ?
O5 Si1 Si3 134.2(8) . . ?
O4 Si1 Na1 29.1(5) . 2_665 ?
O8 Si1 Na1 116.3(6) . 2_665 ?
O6 Si1 Na1 122.5(8) . 2_665 ?
O5 Si1 Na1 76.8(8) . 2_665 ?
Si3 Si1 Na1 57.5(3) . 2_665 ?
O4 Si1 Na1 81.1(4) . . ?
O8 Si1 Na1 29.2(6) . . ?
O6 Si1 Na1 134.1(4) . . ?
O5 Si1 Na1 109.5(3) . . ?
Si3 Si1 Na1 73.5(3) . . ?
Na1 Si1 Na1 87.1(2) 2_665 . ?
O1 Si2 O2 112.0(9) . . ?
O1 Si2 O6 104.2(9) . 1_554 ?
O2 Si2 O6 112.8(11) . 1_554 ?
O1 Si2 O3 104.7(11) . . ?
O2 Si2 O3 112.1(10) . . ?
O6 Si2 O3 110.4(6) 1_554 . ?
O1 Si2 Na1 45.3(6) . 2_675 ?
O2 Si2 Na1 130.9(4) . 2_675 ?
O6 Si2 Na1 115.0(11) 1_554 2_675 ?
O3 Si2 Na1 59.6(8) . 2_675 ?
O1 Si2 Na1 41.0(6) . 1_454 ?
O2 Si2 Na1 136.1(4) . 1_454 ?
O6 Si2 Na1 64.3(9) 1_554 1_454 ?
O3 Si2 Na1 109.1(10) . 1_454 ?
Na1 Si2 Na1 62.1(2) 2_675 1_454 ?
O7 Si3 O3 112.7(4) . 2_675 ?
O7 Si3 O2 113.5(10) . . ?
O3 Si3 O2 110.7(9) 2_675 . ?
O7 Si3 O4 107.7(9) . . ?
O3 Si3 O4 108.5(10) 2_675 . ?
O2 Si3 O4 103.1(8) . . ?
O7 Si3 Si1 91.0(10) . . ?
O3 Si3 Si1 96.5(10) 2_675 . ?
O2 Si3 Si1 130.5(8) . . ?
O4 Si3 Si1 27.5(5) . . ?
O7 Si3 Na1 130.9(4) . 2_665 ?
O3 Si3 Na1 114.4(4) 2_675 2_665 ?
O2 Si3 Na1 60.5(8) . 2_665 ?
O4 Si3 Na1 43.5(6) . 2_665 ?
Si1 Si3 Na1 70.9(4) . 2_665 ?
O7 Si3 Na1 37.5(4) . 1_455 ?
O3 Si3 Na1 147.7(4) 2_675 1_455 ?
O2 Si3 Na1 96.8(3) . 1_455 ?
O4 Si3 Na1 79.9(3) . 1_455 ?
Si1 Si3 Na1 76.7(3) . 1_455 ?
Na1 Si3 Na1 93.39(13) 2_665 1_455 ?
B1 O1 Si2 141(3) 2_565 . ?
B1 O1 Na1 95.1(15) 2_565 1_454 ?
Si2 O1 Na1 113.5(4) . 1_454 ?
B1 O1 Na1 97.8(15) 2_565 2_675 ?
Si2 O1 Na1 107.8(5) . 2_675 ?
Na1 O1 Na1 89.7(9) 1_454 2_675 ?
Si2 O2 Si3 135.7(8) . . ?
Si2 O2 Na1 128.4(5) . 2_665 ?
Si3 O2 Na1 87.6(12) . 2_665 ?
Si3 O3 Si2 144.3(10) 2_675 . ?
Si3 O3 Na1 120.5(12) 2_675 2_675 ?
Si2 O3 Na1 90.3(7) . 2_675 ?
Si1 O4 Si3 123.9(5) . . ?
Si1 O4 Na1 130.3(11) . 2_665 ?
Si3 O4 Na1 105.4(11) . 2_665 ?
B1 O5 Si1 116.0(8) . . ?
Si2 O6 Si1 156.1(9) 1_556 . ?
Si2 O6 Na1 86.2(8) 1_556 1_455 ?
Si1 O6 Na1 112.9(11) . 1_455 ?
B1 O7 Si3 130.1(16) 1_565 . ?
B1 O7 Na1 99.1(7) 1_565 1_455 ?
Si3 O7 Na1 117.7(5) . 1_455 ?
B1 O8 Si1 134.7(9) 2_666 . ?
B1 O8 Na1 94.3(7) 2_666 . ?
Si1 O8 Na1 130.7(10) . . ?

_refine_diff_density_max         0.791
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.173


# start Validation Reply Form
_vrf_ATOM007_shelx               
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.218 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        745 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zh0
_database_code_depnum_ccdc_archive 'CCDC 2150702'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.350(2)
_cell_length_b                   6.351(2)
_cell_length_c                   6.5954(10)
_cell_angle_alpha                115.71(2)
_cell_angle_beta                 103.664(19)
_cell_angle_gamma                101.84(3)
_cell_volume                     218.04(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    521
_cell_measurement_theta_min      2.432
_cell_measurement_theta_max      17.250

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.748
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.126
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            761
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.432
_diffrn_reflns_theta_max         17.250
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.133
_diffrn_measured_fraction_theta_full 0.247
_diffrn_reflns_Laue_measured_fraction_max 0.133
_diffrn_reflns_Laue_measured_fraction_full 0.247
_diffrn_reflns_point_group_measured_fraction_max 0.133
_diffrn_reflns_point_group_measured_fraction_full 0.247
_reflns_number_total             521
_reflns_number_gt                448
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1049P)²+2.1408P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         521
_refine_ls_number_parameters     63
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0741
_refine_ls_wR_factor_ref         0.2268
_refine_ls_wR_factor_gt          0.2004
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_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
Si1 Si 0.7630(7) 1.2058(12) 0.8506(5) 0.0078(5) Uiso 1 1 d . . . . .
Si2 Si 0.3355(8) 0.7555(11) 0.6097(5) 0.017(5) Uani 1 1 d . . . . .
Si3 Si 0.3374(7) 0.4336(11) 0.8082(4) 0.010(5) Uani 1 1 d . . . . .
Na1 Na 0.7919(12) 0.7128(18) 0.8012(7) 0.0109(7) Uiso 1 1 d . . . . .
B1 B -0.029(3) 0.034(5) 0.3552(17) 0.0072(13) Uiso 1 1 d . . . . .
O2 O 0.332(2) 0.721(3) 0.3495(12) 0.0101(10) Uiso 1 1 d . . . . .
O3 O 0.1782(18) 0.122(3) 0.5814(11) 0.0071(9) Uiso 1 1 d . . . . .
O4 O 0.341(2) 0.503(3) 0.5918(11) 0.0074(9) Uiso 1 1 d . . . . .
O5 O 0.567(2) 0.976(3) 0.8125(12) 0.0083(9) Uiso 1 1 d . . . . .
O6 O 0.1379(19) 0.555(3) 0.8937(11) 0.0092(10) Uiso 1 1 d . . . . .
O7 O 0.5768(19) 0.682(3) 1.0146(11) 0.0080(9) Uiso 1 1 d . . . . .
O8 O 0.969(2) 1.096(3) 0.8412(12) 0.0084(9) Uiso 1 1 d . . . . .
O1 O -0.112(2) 0.208(4) 0.3378(14) 0.0107(10) Uiso 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
Si1 O6 1.560(13) 2_677 ?
Si1 O5 1.590(7) . ?
Si1 O8 1.61(2) . ?
Si1 O2 1.609(13) 2_676 ?
Si1 Si3 2.743(10) 2_677 ?
Si1 Na1 2.971(9) 2_777 ?
Si1 Na1 3.053(14) . ?
Si1 Na1 3.348(12) 1_565 ?
Si2 O4 1.56(2) . ?
Si2 O1 1.58(2) 2_566 ?
Si2 O5 1.586(6) . ?
Si2 O2 1.628(6) . ?
Si2 Na1 2.798(11) 2_666 ?
Si2 Na1 2.994(12) . ?
Si3 O4 1.672(7) . ?
Si3 O7 1.675(14) 2_667 ?
Si3 O7 1.681(7) . ?
Si3 O6 1.70(2) . ?
Si3 O3 1.752(13) . ?
Si3 Si3 2.518(6) 2_667 ?
Si3 Na1 3.084(5) . ?
Si3 Na1 3.308(4) 2_667 ?
Na1 O8 2.099(6) 2_777 ?
Na1 O4 2.173(8) 2_666 ?
Na1 O7 2.219(11) . ?
Na1 O8 2.333(15) . ?
Na1 O2 2.36(2) 2_666 ?
Na1 O5 2.40(3) . ?
Na1 O1 2.466(14) 2_666 ?
Na1 O4 2.617(11) . ?
Na1 O6 2.65(2) 1_655 ?
Na1 B1 2.661(9) 2_666 ?
B1 O1 1.35(5) . ?
B1 O8 1.39(3) 2_666 ?
B1 O3 1.492(10) 2_556 ?
B1 O3 1.520(15) . ?
B1 B1 2.10(2) 2_556 ?

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
O6 Si1 O5 115.9(5) 2_677 . ?
O6 Si1 O8 104.4(8) 2_677 . ?
O5 Si1 O8 99.9(10) . . ?
O6 Si1 O2 108.7(9) 2_677 2_676 ?
O5 Si1 O2 109.7(5) . 2_676 ?
O8 Si1 O2 118.4(7) . 2_676 ?
O6 Si1 Si3 34.2(7) 2_677 2_677 ?
O5 Si1 Si3 95.6(7) . 2_677 ?
O8 Si1 Si3 137.4(3) . 2_677 ?
O2 Si1 Si3 92.6(8) 2_676 2_677 ?
O6 Si1 Na1 62.7(8) 2_677 2_777 ?
O5 Si1 Na1 108.7(6) . 2_777 ?
O8 Si1 Na1 42.8(3) . 2_777 ?
O2 Si1 Na1 139.9(3) 2_676 2_777 ?
Si3 Si1 Na1 94.6(2) 2_677 2_777 ?
O6 Si1 Na1 119.8(6) 2_677 . ?
O5 Si1 Na1 51.2(8) . . ?
O8 Si1 Na1 48.8(4) . . ?
O2 Si1 Na1 131.4(6) 2_676 . ?
Si3 Si1 Na1 129.14(16) 2_677 . ?
Na1 Si1 Na1 69.0(2) 2_777 . ?
O6 Si1 Na1 69.5(6) 2_677 1_565 ?
O5 Si1 Na1 137.2(9) . 1_565 ?
O8 Si1 Na1 120.5(4) . 1_565 ?
O2 Si1 Na1 40.2(5) 2_676 1_565 ?
Si3 Si1 Na1 64.9(2) 2_677 1_565 ?
Na1 Si1 Na1 110.4(2) 2_777 1_565 ?
Na1 Si1 Na1 165.7(3) . 1_565 ?
O4 Si2 O1 107.0(7) . 2_566 ?
O4 Si2 O5 109.9(8) . . ?
O1 Si2 O5 113.1(9) 2_566 . ?
O4 Si2 O2 104.7(9) . . ?
O1 Si2 O2 114.0(8) 2_566 . ?
O5 Si2 O2 107.8(3) . . ?
O4 Si2 Na1 50.6(3) . 2_666 ?
O1 Si2 Na1 108.9(5) 2_566 2_666 ?
O5 Si2 Na1 137.7(9) . 2_666 ?
O2 Si2 Na1 57.4(6) . 2_666 ?
O4 Si2 Na1 60.9(4) . . ?
O1 Si2 Na1 144.8(3) 2_566 . ?
O5 Si2 Na1 53.0(9) . . ?
O2 Si2 Na1 101.2(7) . . ?
Na1 Si2 Na1 88.8(3) 2_666 . ?
O4 Si3 O7 154.5(10) . 2_667 ?
O4 Si3 O7 92.8(3) . . ?
O7 Si3 O7 82.7(7) 2_667 . ?
O4 Si3 O6 99.0(9) . . ?
O7 Si3 O6 106.5(7) 2_667 . ?
O7 Si3 O6 98.3(8) . . ?
O4 Si3 O3 88.7(5) . . ?
O7 Si3 O3 85.8(6) 2_667 . ?
O7 Si3 O3 156.2(11) . . ?
O6 Si3 O3 105.0(7) . . ?
O4 Si3 Si3 129.2(3) . 2_667 ?
O7 Si3 Si3 41.5(3) 2_667 2_667 ?
O7 Si3 Si3 41.3(5) . 2_667 ?
O6 Si3 Si3 106.5(4) . 2_667 ?
O3 Si3 Si3 124.2(7) . 2_667 ?
O4 Si3 Si1 107.9(8) . 2_677 ?
O7 Si3 Si1 93.8(6) 2_667 2_677 ?
O7 Si3 Si1 68.4(7) . 2_677 ?
O6 Si3 Si1 31.1(2) . 2_677 ?
O3 Si3 Si1 133.5(6) . 2_677 ?
Si3 Si3 Si1 78.4(3) 2_667 2_677 ?
O4 Si3 Na1 58.0(4) . . ?
O7 Si3 Na1 104.0(4) 2_667 . ?
O7 Si3 Na1 44.4(4) . . ?
O6 Si3 Na1 126.8(5) . . ?
O3 Si3 Na1 119.9(5) . . ?
Si3 Si3 Na1 71.57(15) 2_667 . ?
Si1 Si3 Na1 105.3(3) 2_677 . ?
O4 Si3 Na1 167.2(7) . 2_667 ?
O7 Si3 Na1 37.2(6) 2_667 2_667 ?
O7 Si3 Na1 95.42(19) . 2_667 ?
O6 Si3 Na1 70.1(4) . 2_667 ?
O3 Si3 Na1 87.8(2) . 2_667 ?
Si3 Si3 Na1 62.19(12) 2_667 2_667 ?
Si1 Si3 Na1 66.4(3) 2_677 2_667 ?
Na1 Si3 Na1 133.76(12) . 2_667 ?
O8 Na1 O4 158.9(9) 2_777 2_666 ?
O8 Na1 O7 76.0(3) 2_777 . ?
O4 Na1 O7 122.4(3) 2_666 . ?
O8 Na1 O8 79.5(5) 2_777 . ?
O4 Na1 O8 96.8(4) 2_666 . ?
O7 Na1 O8 121.1(8) . . ?
O8 Na1 O2 110.0(7) 2_777 2_666 ?
O4 Na1 O2 67.6(5) 2_666 2_666 ?
O7 Na1 O2 79.5(5) . 2_666 ?
O8 Na1 O2 159.3(6) . 2_666 ?
O8 Na1 O5 102.6(8) 2_777 . ?
O4 Na1 O5 93.6(7) 2_666 . ?
O7 Na1 O5 72.3(7) . . ?
O8 Na1 O5 62.3(6) . . ?
O2 Na1 O5 129.6(5) 2_666 . ?
O8 Na1 O1 89.7(4) 2_777 2_666 ?
O4 Na1 O1 71.4(3) 2_666 2_666 ?
O7 Na1 O1 165.5(4) . 2_666 ?
O8 Na1 O1 56.6(9) . 2_666 ?
O2 Na1 O1 104.1(8) 2_666 2_666 ?
O5 Na1 O1 113.7(7) . 2_666 ?
O8 Na1 O4 135.3(5) 2_777 . ?
O4 Na1 O4 64.6(6) 2_666 . ?
O7 Na1 O4 59.6(3) . . ?
O8 Na1 O4 118.8(7) . . ?
O2 Na1 O4 68.1(6) 2_666 . ?
O5 Na1 O4 61.7(5) . . ?
O1 Na1 O4 134.9(2) 2_666 . ?
O8 Na1 O6 62.4(7) 2_777 1_655 ?
O4 Na1 O6 99.1(8) 2_666 1_655 ?
O7 Na1 O6 109.9(6) . 1_655 ?
O8 Na1 O6 104.1(5) . 1_655 ?
O2 Na1 O6 67.0(6) 2_666 1_655 ?
O5 Na1 O6 162.5(4) . 1_655 ?
O1 Na1 O6 60.2(6) 2_666 1_655 ?
O4 Na1 O6 135.1(6) . 1_655 ?
O8 Na1 B1 96.7(3) 2_777 2_666 ?
O4 Na1 B1 71.8(3) 2_666 2_666 ?
O7 Na1 B1 152.0(11) . 2_666 ?
O8 Na1 B1 31.4(7) . 2_666 ?
O2 Na1 B1 127.9(8) 2_666 2_666 ?
O5 Na1 B1 83.3(8) . 2_666 ?
O1 Na1 B1 30.3(10) 2_666 2_666 ?
O4 Na1 B1 120.2(5) . 2_666 ?
O6 Na1 B1 89.3(7) 1_655 2_666 ?
O8 Na1 Si2 135.8(9) 2_777 2_666 ?
O4 Na1 Si2 33.8(5) 2_666 2_666 ?
O7 Na1 Si2 108.9(4) . 2_666 ?
O8 Na1 Si2 125.6(3) . 2_666 ?
O2 Na1 Si2 35.5(2) 2_666 2_666 ?
O5 Na1 Si2 120.9(3) . 2_666 ?
O1 Na1 Si2 79.9(5) 2_666 2_666 ?
O4 Na1 Si2 69.2(5) . 2_666 ?
O6 Na1 Si2 75.4(4) 1_655 2_666 ?
B1 Na1 Si2 95.3(5) 2_666 2_666 ?
O8 Na1 Si1 31.4(7) 2_777 2_777 ?
O4 Na1 Si1 128.6(7) 2_666 2_777 ?
O7 Na1 Si1 96.9(3) . 2_777 ?
O8 Na1 Si1 88.0(4) . 2_777 ?
O2 Na1 Si1 91.5(5) 2_666 2_777 ?
O5 Na1 Si1 132.0(4) . 2_777 ?
O1 Na1 Si1 69.2(4) 2_666 2_777 ?
O4 Na1 Si1 150.4(3) . 2_777 ?
O6 Na1 Si1 31.6(3) 1_655 2_777 ?
B1 Na1 Si1 89.1(5) 2_666 2_777 ?
Si2 Na1 Si1 106.9(5) 2_666 2_777 ?
O1 B1 O8 112.2(12) . 2_666 ?
O1 B1 O3 112(2) . 2_556 ?
O8 B1 O3 115.6(19) 2_666 2_556 ?
O1 B1 O3 117.5(16) . . ?
O8 B1 O3 106.6(19) 2_666 . ?
O3 B1 O3 91.4(7) 2_556 . ?
O1 B1 B1 127(2) . 2_556 ?
O8 B1 B1 121(3) 2_666 2_556 ?
O3 B1 B1 46.3(5) 2_556 2_556 ?
O3 B1 B1 45.2(5) . 2_556 ?
O1 B1 Na1 66.8(6) . 2_666 ?
O8 B1 Na1 61.1(6) 2_666 2_666 ?
O3 B1 Na1 174.5(5) 2_556 2_666 ?
O3 B1 Na1 93.9(4) . 2_666 ?
B1 B1 Na1 139.0(8) 2_556 2_666 ?
O1 B1 Na1 90.5(6) . 1_444 ?
O8 B1 Na1 35.4(6) 2_666 1_444 ?
O3 B1 Na1 102.1(7) 2_556 1_444 ?
O3 B1 Na1 141.8(17) . 1_444 ?
B1 B1 Na1 135.7(18) 2_556 1_444 ?
Na1 B1 Na1 72.7(3) 2_666 1_444 ?
Si1 O2 Si2 144.1(15) 2_676 . ?
Si1 O2 Na1 113.6(4) 2_676 2_666 ?
Si2 O2 Na1 87.1(6) . 2_666 ?
B1 O3 B1 88.6(7) 2_556 . ?
B1 O3 Si3 117.0(10) 2_556 . ?
B1 O3 Si3 125.7(16) . . ?
Si2 O4 Si3 124.8(10) . . ?
Si2 O4 Na1 95.6(5) . 2_666 ?
Si3 O4 Na1 134.2(8) . 2_666 ?
Si2 O4 Na1 87.7(4) . . ?
Si3 O4 Na1 89.1(5) . . ?
Na1 O4 Na1 115.4(6) 2_666 . ?
Si2 O5 Si1 140.0(4) . . ?
Si2 O5 Na1 95.2(9) . . ?
Si1 O5 Na1 97.8(9) . . ?
Si1 O6 Si3 114.7(7) 2_677 . ?
Si1 O6 Na1 85.7(10) 2_677 1_455 ?
Si3 O6 Na1 150.0(3) . 1_455 ?
Si3 O7 Si3 97.3(7) 2_667 . ?
Si3 O7 Na1 115.6(11) 2_667 . ?
Si3 O7 Na1 103.7(5) . . ?
B1 O8 Si1 129.4(11) 2_666 . ?
B1 O8 Na1 122.0(13) 2_666 2_777 ?
Si1 O8 Na1 105.8(9) . 2_777 ?
B1 O8 Na1 87.4(11) 2_666 . ?
Si1 O8 Na1 99.9(4) . . ?
Na1 O8 Na1 100.5(5) 2_777 . ?
B1 O1 Si2 123.0(7) . 2_566 ?
B1 O1 Na1 82.8(12) . 2_666 ?
Si2 O1 Na1 154.0(12) 2_566 2_666 ?

_refine_diff_density_max         0.874
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.176


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.247 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        589 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC6
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zj1
_database_code_depnum_ccdc_archive 'CCDC 2150703'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.245(7)
_cell_length_b                   6.324(8)
_cell_length_c                   6.544(7)
_cell_angle_alpha                116.01(13)
_cell_angle_beta                 103.12(11)
_cell_angle_gamma                101.56(11)
_cell_volume                     212.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    434
_cell_measurement_theta_min      2.442
_cell_measurement_theta_max      17.840

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.845
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.130
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            633
_diffrn_reflns_av_unetI/netI     0.1567
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.442
_diffrn_reflns_theta_max         17.840
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.103
_diffrn_measured_fraction_theta_full 0.241
_diffrn_reflns_Laue_measured_fraction_max 0.103
_diffrn_reflns_Laue_measured_fraction_full 0.241
_diffrn_reflns_point_group_measured_fraction_max 0.103
_diffrn_reflns_point_group_measured_fraction_full 0.241
_reflns_number_total             434
_reflns_number_gt                214
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1862P)²+4.8391P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         434
_refine_ls_number_parameters     63
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2070
_refine_ls_R_factor_gt           0.1374
_refine_ls_wR_factor_ref         0.3799
_refine_ls_wR_factor_gt          0.3223
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_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
Si1 Si 0.7583(16) 1.212(3) 0.8569(10) 0.0261(13) Uiso 1 1 d . . . . .
Si2 Si 0.3359(18) 0.750(3) 0.6065(13) 0.065(15) Uani 1 1 d . . . . .
Si3 Si 0.3372(18) 0.435(3) 0.8080(12) 0.046(14) Uani 1 1 d . . . . .
B1 B 0.994(9) 1.030(15) 0.671(6) 0.039(5) Uiso 1 1 d . . . . .
Na1 Na 0.798(3) 0.707(4) 0.7991(17) 0.031(2) Uiso 1 1 d . . . . .
O2 O 0.330(5) 0.729(8) 0.349(3) 0.034(3) Uiso 1 1 d . . . . .
O3 O 0.181(4) 0.112(7) 0.578(3) 0.030(3) Uiso 1 1 d . . . . .
O4 O 0.335(5) 0.519(7) 0.599(3) 0.031(3) Uiso 1 1 d . . . . .
O5 O 0.569(4) 0.983(7) 0.819(3) 0.029(3) Uiso 1 1 d . . . . .
O6 O 0.136(4) 0.562(7) 0.896(3) 0.030(3) Uiso 1 1 d . . . . .
O7 O 0.567(5) 0.691(7) 1.020(3) 0.033(3) Uiso 1 1 d . . . . .
O8 O 0.973(4) 1.100(7) 0.842(3) 0.024(3) Uiso 1 1 d . . . . .
O1 O -0.117(7) 0.231(10) 0.350(4) 0.042(4) Uiso 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
Si1 O6 1.48(3) 2_677 ?
Si1 O5 1.557(19) . ?
Si1 O2 1.56(3) 2_676 ?
Si1 O8 1.64(5) . ?
Si1 B1 2.29(10) . ?
Si1 Si3 2.64(2) 2_677 ?
Si1 Na1 2.93(2) 2_777 ?
Si1 Na1 3.12(3) . ?
Si1 Na1 3.28(3) 1_565 ?
Si2 O4 1.44(5) . ?
Si2 O1 1.47(6) 2_566 ?
Si2 O2 1.625(13) . ?
Si2 O5 1.628(17) . ?
Si2 Na1 2.72(3) 2_666 ?
Si2 Si3 2.827(18) . ?
Si2 Na1 2.99(3) . ?
Si3 O4 1.67(2) . ?
Si3 O7 1.67(2) . ?
Si3 O6 1.70(5) . ?
Si3 O7 1.72(4) 2_667 ?
Si3 O3 1.80(3) . ?
Si3 Si3 2.516(16) 2_667 ?
Si3 Na1 3.069(13) . ?
Si3 Na1 3.294(9) 2_667 ?
Si3 Na1 3.513(10) 2_666 ?
B1 O8 1.06(5) . ?
B1 O3 1.48(3) 2_666 ?
B1 O3 1.54(4) 1_665 ?
B1 O1 1.92(14) 2_666 ?
B1 B1 2.12(6) 2_776 ?
B1 Na1 2.71(5) . ?
B1 Na1 2.92(3) 2_777 ?
Na1 O8 2.077(14) 2_777 ?
Na1 O4 2.19(2) 2_666 ?
Na1 O7 2.28(3) . ?
Na1 O8 2.37(4) . ?
Na1 O2 2.36(5) 2_666 ?
Na1 O1 2.44(4) 2_666 ?
Na1 O5 2.45(5) . ?
Na1 O6 2.52(5) 1_655 ?
Na1 O4 2.65(3) . ?

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
O6 Si1 O5 117.5(10) 2_677 . ?
O6 Si1 O2 113(2) 2_677 2_676 ?
O5 Si1 O2 110.1(11) . 2_676 ?
O6 Si1 O8 102(2) 2_677 . ?
O5 Si1 O8 99(2) . . ?
O2 Si1 O8 114.4(17) 2_676 . ?
O6 Si1 B1 119.9(18) 2_677 . ?
O5 Si1 B1 102(2) . . ?
O2 Si1 B1 91(2) 2_676 . ?
O8 Si1 B1 24.9(12) . . ?
O6 Si1 Si3 36.5(17) 2_677 2_677 ?
O5 Si1 Si3 97.3(16) . 2_677 ?
O2 Si1 Si3 96.2(19) 2_676 2_677 ?
O8 Si1 Si3 137.3(7) . 2_677 ?
B1 Si1 Si3 155.8(9) . 2_677 ?
O6 Si1 Na1 59.5(19) 2_677 2_777 ?
O5 Si1 Na1 107.9(14) . 2_777 ?
O2 Si1 Na1 139.0(8) 2_676 2_777 ?
O8 Si1 Na1 43.6(7) . 2_777 ?
B1 Si1 Na1 66.6(10) . 2_777 ?
Si3 Si1 Na1 93.8(6) 2_677 2_777 ?
O6 Si1 Na1 118.3(17) 2_677 . ?
O5 Si1 Na1 50.8(18) . . ?
O2 Si1 Na1 127.9(17) 2_676 . ?
O8 Si1 Na1 48.3(10) . . ?
B1 Si1 Na1 57.7(16) . . ?
Si3 Si1 Na1 130.3(4) 2_677 . ?
Na1 Si1 Na1 68.8(6) 2_777 . ?
O6 Si1 Na1 71.8(14) 2_677 1_565 ?
O5 Si1 Na1 139.9(18) . 1_565 ?
O2 Si1 Na1 42.0(14) 2_676 1_565 ?
O8 Si1 Na1 117.9(9) . 1_565 ?
B1 Si1 Na1 105.3(16) . 1_565 ?
Si3 Si1 Na1 66.6(5) 2_677 1_565 ?
Na1 Si1 Na1 109.5(6) 2_777 1_565 ?
Na1 Si1 Na1 162.6(7) . 1_565 ?
O4 Si2 O1 101(2) . 2_566 ?
O4 Si2 O2 110(2) . . ?
O1 Si2 O2 112.1(19) 2_566 . ?
O4 Si2 O5 111.7(19) . . ?
O1 Si2 O5 114(2) 2_566 . ?
O2 Si2 O5 107.8(8) . . ?
O4 Si2 Na1 53.4(9) . 2_666 ?
O1 Si2 Na1 104.4(16) 2_566 2_666 ?
O2 Si2 Na1 59.8(16) . 2_666 ?
O5 Si2 Na1 141.5(19) . 2_666 ?
O4 Si2 Si3 26.4(9) . . ?
O1 Si2 Si3 88(2) 2_566 . ?
O2 Si2 Si3 137(2) . . ?
O5 Si2 Si3 97.3(12) . . ?
Na1 Si2 Si3 78.6(6) 2_666 . ?
O4 Si2 Na1 62.4(13) . . ?
O1 Si2 Na1 144.4(11) 2_566 . ?
O2 Si2 Na1 103.4(17) . . ?
O5 Si2 Na1 54.9(19) . . ?
Na1 Si2 Na1 90.6(7) 2_666 . ?
Si3 Si2 Na1 63.6(5) . . ?
O4 Si3 O7 92.3(10) . . ?
O4 Si3 O6 95(2) . . ?
O7 Si3 O6 94(2) . . ?
O4 Si3 O7 155(2) . 2_667 ?
O7 Si3 O7 84.2(19) . 2_667 ?
O6 Si3 O7 109.8(16) . 2_667 ?
O4 Si3 O3 91.9(13) . . ?
O7 Si3 O3 158(3) . . ?
O6 Si3 O3 107.0(15) . . ?
O7 Si3 O3 82.8(16) 2_667 . ?
O4 Si3 Si3 130.1(8) . 2_667 ?
O7 Si3 Si3 42.8(13) . 2_667 ?
O6 Si3 Si3 106.5(9) . 2_667 ?
O7 Si3 Si3 41.4(8) 2_667 2_667 ?
O3 Si3 Si3 122.0(18) . 2_667 ?
O4 Si3 Si1 104(2) . 2_677 ?
O7 Si3 Si1 64.5(18) . 2_677 ?
O6 Si3 Si1 31.4(6) . 2_677 ?
O7 Si3 Si1 96.4(14) 2_667 2_677 ?
O3 Si3 Si1 135.1(12) . 2_677 ?
Si3 Si3 Si1 77.9(8) 2_667 2_677 ?
O4 Si3 Si2 22.6(17) . . ?
O7 Si3 Si2 78.2(13) . . ?
O6 Si3 Si2 78.9(11) . . ?
O7 Si3 Si2 161.0(6) 2_667 . ?
O3 Si3 Si2 111.4(8) . . ?
Si3 Si3 Si2 120.6(6) 2_667 . ?
Si1 Si3 Si2 82.4(7) 2_677 . ?
O4 Si3 Na1 59.7(10) . . ?
O7 Si3 Na1 46.8(10) . . ?
O6 Si3 Na1 126.7(12) . . ?
O7 Si3 Na1 101.7(9) 2_667 . ?
O3 Si3 Na1 118.9(12) . . ?
Si3 Si3 Na1 71.5(4) 2_667 . ?
Si1 Si3 Na1 105.3(6) 2_677 . ?
Si2 Si3 Na1 60.8(5) . . ?
O4 Si3 Na1 164.2(18) . 2_667 ?
O7 Si3 Na1 94.4(5) . 2_667 ?
O6 Si3 Na1 70.1(9) . 2_667 ?
O7 Si3 Na1 40.4(13) 2_667 2_667 ?
O3 Si3 Na1 87.4(6) . 2_667 ?
Si3 Si3 Na1 62.1(3) 2_667 2_667 ?
Si1 Si3 Na1 66.1(6) 2_677 2_667 ?
Si2 Si3 Na1 147.4(9) . 2_667 ?
Na1 Si3 Na1 133.6(3) . 2_667 ?
O4 Si3 Na1 28.1(12) . 2_666 ?
O7 Si3 Na1 117.5(6) . 2_666 ?
O6 Si3 Na1 104.0(9) . 2_666 ?
O7 Si3 Na1 138.0(15) 2_667 2_666 ?
O3 Si3 Na1 63.8(6) . 2_666 ?
Si3 Si3 Na1 144.6(8) 2_667 2_666 ?
Si1 Si3 Na1 125.0(8) 2_677 2_666 ?
Si2 Si3 Na1 49.3(5) . 2_666 ?
Na1 Si3 Na1 76.0(3) . 2_666 ?
Na1 Si3 Na1 148.0(4) 2_667 2_666 ?
O8 B1 O3 131(5) . 2_666 ?
O8 B1 O3 135(3) . 1_665 ?
O3 B1 O3 90.5(18) 2_666 1_665 ?
O8 B1 O1 103(5) . 2_666 ?
O3 B1 O1 97(5) 2_666 2_666 ?
O3 B1 O1 87(5) 1_665 2_666 ?
O8 B1 B1 164(10) . 2_776 ?
O3 B1 B1 46.4(12) 2_666 2_776 ?
O3 B1 B1 44.1(15) 1_665 2_776 ?
O1 B1 B1 93(7) 2_666 2_776 ?
O8 B1 Si1 41(4) . . ?
O3 B1 Si1 96(4) 2_666 . ?
O3 B1 Si1 135(6) 1_665 . ?
O1 B1 Si1 136.2(18) 2_666 . ?
B1 B1 Si1 126(7) 2_776 . ?
O8 B1 Na1 60(3) . . ?
O3 B1 Na1 93(2) 2_666 . ?
O3 B1 Na1 148(7) 1_665 . ?
O1 B1 Na1 61.0(19) 2_666 . ?
B1 B1 Na1 131(5) 2_776 . ?
Si1 B1 Na1 76.6(13) . . ?
O8 B1 Na1 30.5(18) . 2_777 ?
O3 B1 Na1 161(4) 2_666 2_777 ?
O3 B1 Na1 107.3(14) 1_665 2_777 ?
O1 B1 Na1 90.1(19) 2_666 2_777 ?
B1 B1 Na1 151(2) 2_776 2_777 ?
Si1 B1 Na1 67.2(15) . 2_777 ?
Na1 B1 Na1 74.8(8) . 2_777 ?
O8 Na1 O4 160(2) 2_777 2_666 ?
O8 Na1 O7 75.0(8) 2_777 . ?
O4 Na1 O7 122.0(9) 2_666 . ?
O8 Na1 O8 79.5(12) 2_777 . ?
O4 Na1 O8 98.2(10) 2_666 . ?
O7 Na1 O8 117.7(19) . . ?
O8 Na1 O2 110.3(15) 2_777 2_666 ?
O4 Na1 O2 67.1(12) 2_666 2_666 ?
O7 Na1 O2 80.7(12) . 2_666 ?
O8 Na1 O2 161.3(14) . 2_666 ?
O8 Na1 O1 92.2(10) 2_777 2_666 ?
O4 Na1 O1 70.4(8) 2_666 2_666 ?
O7 Na1 O1 167.1(8) . 2_666 ?
O8 Na1 O1 60(2) . 2_666 ?
O2 Na1 O1 103(2) 2_666 2_666 ?
O8 Na1 O5 100.1(18) 2_777 . ?
O4 Na1 O5 95.5(16) 2_666 . ?
O7 Na1 O5 69.3(15) . . ?
O8 Na1 O5 60.7(13) . . ?
O2 Na1 O5 129.6(13) 2_666 . ?
O1 Na1 O5 115.0(18) 2_666 . ?
O8 Na1 O6 62.8(17) 2_777 1_655 ?
O4 Na1 O6 99.7(18) 2_666 1_655 ?
O7 Na1 O6 111.8(13) . 1_655 ?
O8 Na1 O6 104.6(12) . 1_655 ?
O2 Na1 O6 68.4(15) 2_666 1_655 ?
O1 Na1 O6 59.8(15) 2_666 1_655 ?
O5 Na1 O6 160.5(9) . 1_655 ?
O8 Na1 O4 132.4(12) 2_777 . ?
O4 Na1 O4 66.1(15) 2_666 . ?
O7 Na1 O4 57.9(7) . . ?
O8 Na1 O4 115.5(17) . . ?
O2 Na1 O4 70.3(15) 2_666 . ?
O1 Na1 O4 135.0(6) 2_666 . ?
O5 Na1 O4 59.5(13) . . ?
O6 Na1 O4 138.6(15) 1_655 . ?
O8 Na1 B1 96.6(9) 2_777 . ?
O4 Na1 B1 77.2(12) 2_666 . ?
O7 Na1 B1 138(3) . . ?
O8 Na1 B1 22.8(16) . . ?
O2 Na1 B1 139(2) 2_666 . ?
O1 Na1 B1 43(3) 2_666 . ?
O5 Na1 B1 72(2) . . ?
O6 Na1 B1 100(2) 1_655 . ?
O4 Na1 B1 113.4(16) . . ?
O8 Na1 Si2 139(2) 2_777 2_666 ?
O4 Na1 Si2 31.8(13) 2_666 2_666 ?
O7 Na1 Si2 109.6(9) . 2_666 ?
O8 Na1 Si2 126.5(7) . 2_666 ?
O2 Na1 Si2 36.5(5) 2_666 2_666 ?
O1 Na1 Si2 79.2(13) 2_666 2_666 ?
O5 Na1 Si2 120.4(7) . 2_666 ?
O6 Na1 Si2 78.3(11) 1_655 2_666 ?
O4 Na1 Si2 70.4(11) . 2_666 ?
B1 Na1 Si2 103.8(15) . 2_666 ?
O8 Na1 B1 15.0(13) 2_777 2_777 ?
O4 Na1 B1 174(3) 2_666 2_777 ?
O7 Na1 B1 60.3(11) . 2_777 ?
O8 Na1 B1 85.1(13) . 2_777 ?
O2 Na1 B1 108.5(17) 2_666 2_777 ?
O1 Na1 B1 106.9(11) 2_666 2_777 ?
O5 Na1 B1 91(2) . 2_777 ?
O6 Na1 B1 74(2) 1_655 2_777 ?
O4 Na1 B1 117.5(15) . 2_777 ?
B1 Na1 B1 105.2(8) . 2_777 ?
Si2 Na1 B1 143(2) 2_666 2_777 ?
Si1 O2 Si2 150(4) 2_676 . ?
Si1 O2 Na1 111.7(12) 2_676 2_666 ?
Si2 O2 Na1 83.7(15) . 2_666 ?
B1 O3 B1 89.5(18) 2_666 1_445 ?
B1 O3 Si3 137(4) 2_666 . ?
B1 O3 Si3 104(3) 1_445 . ?
Si2 O4 Si3 131(3) . . ?
Si2 O4 Na1 94.8(12) . 2_666 ?
Si3 O4 Na1 131(2) . 2_666 ?
Si2 O4 Na1 88.9(9) . . ?
Si3 O4 Na1 87.5(13) . . ?
Na1 O4 Na1 113.9(14) 2_666 . ?
Si1 O5 Si2 139.6(11) . . ?
Si1 O5 Na1 99.7(19) . . ?
Si2 O5 Na1 92(2) . . ?
Si1 O6 Si3 112.1(17) 2_677 . ?
Si1 O6 Na1 90(2) 2_677 1_455 ?
Si3 O6 Na1 149.1(7) . 1_455 ?
Si3 O7 Si3 95.8(19) . 2_667 ?
Si3 O7 Na1 100.8(14) . . ?
Si3 O7 Na1 110(2) 2_667 . ?
B1 O8 Si1 114(5) . . ?
B1 O8 Na1 135(3) . 2_777 ?
Si1 O8 Na1 103(2) . 2_777 ?
B1 O8 Na1 97(4) . . ?
Si1 O8 Na1 100.4(10) . . ?
Na1 O8 Na1 100.5(11) 2_777 . ?
Si2 O1 B1 125(2) 2_566 2_666 ?
Si2 O1 Na1 157(3) 2_566 2_666 ?
B1 O1 Na1 76(3) 2_666 2_666 ?

_refine_diff_density_max         0.557
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.164


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.241 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT084_shelx               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.89 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        582 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC7
_audit_block_doi                 10.5517/ccdc.csd.cc2b5zdx
_database_code_depnum_ccdc_archive 'CCDC 2150699'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.5869(15)
_cell_length_b                   6.8464(17)
_cell_length_c                   7.1774(8)
_cell_angle_alpha                117.906(17)
_cell_angle_beta                 99.654(13)
_cell_angle_gamma                106.06(2)
_cell_volume                     257.50(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    631
_cell_measurement_theta_min      2.057
_cell_measurement_theta_max      17.816

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    3.174
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.120
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            907
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.057
_diffrn_reflns_theta_max         17.816
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.124
_diffrn_measured_fraction_theta_full 0.252
_diffrn_reflns_Laue_measured_fraction_max 0.124
_diffrn_reflns_Laue_measured_fraction_full 0.252
_diffrn_reflns_point_group_measured_fraction_max 0.124
_diffrn_reflns_point_group_measured_fraction_full 0.252
_reflns_number_total             631
_reflns_number_gt                595
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1364P)²+1.8389P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       1.1(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         631
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.2266
_refine_ls_wR_factor_gt          0.2192
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
Na1 Na 0.8820(9) 0.7363(15) 0.2666(8) 0.029(7) Uani 1 1 d . . . . .
B1 B 0.2236(19) 0.161(4) 0.3590(19) 0.019(13) Uani 1 1 d . . . . .
Si1 Si 0.3506(5) 0.5143(8) 0.3007(4) 0.020(3) Uani 1 1 d . . . . .
Si2 Si 0.2079(5) 0.8175(9) -0.2997(4) 0.030(3) Uani 1 1 d . . . . .
Si3 Si 0.3206(5) 0.7878(9) 0.1017(5) 0.017(4) Uani 1 1 d . . . . .
O1 O -0.0014(13) 0.871(3) -0.3702(13) 0.0135(8) Uiso 1 1 d . . . . .
O2 O 0.1834(13) 0.704(2) -0.1492(12) 0.0115(8) Uiso 1 1 d . . . . .
O3 O 0.4190(12) 1.074(2) -0.1618(12) 0.0108(8) Uiso 1 1 d . . . . .
O4 O 0.2731(11) 0.536(2) 0.0859(11) 0.0094(7) Uiso 1 1 d . . . . .
O5 O 0.2691(13) 0.233(2) 0.2063(12) 0.0123(8) Uiso 1 1 d . . . . .
O6 O 0.2348(16) 0.630(3) 0.4734(15) 0.0208(11) Uiso 1 1 d . . . . .
O7 O 0.2327(19) 0.933(3) 0.2919(18) 0.0237(13) Uiso 1 1 d . . . . .
O8 O 0.6170(12) 0.658(2) 0.4088(12) 0.0112(8) Uiso 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
Na1 O4 2.141(9) 2_665 ?
Na1 O1 2.219(6) 1_656 ?
Na1 O8 2.230(9) . ?
Na1 O7 2.257(9) 1_655 ?
Na1 O1 2.272(16) 2_675 ?
Na1 O2 2.599(18) 2_665 ?
Na1 B1 2.707(15) 2_666 ?
Na1 O3 2.831(18) 2_675 ?
Na1 B1 2.833(10) 1_665 ?
Na1 O6 2.987(19) 1_655 ?
Na1 Si3 2.989(9) 2_665 ?
Na1 Si2 3.176(6) 1_656 ?
B1 O7 1.42(4) 1_545 ?
B1 O5 1.437(7) . ?
B1 O1 1.44(2) 2_565 ?
B1 O8 1.476(11) 2_666 ?
Si1 O6 1.574(18) . ?
Si1 O8 1.588(6) . ?
Si1 O5 1.596(14) . ?
Si1 O4 1.627(6) . ?
Si2 O1 1.584(17) . ?
Si2 O3 1.600(7) . ?
Si2 O2 1.606(7) . ?
Si2 O6 1.611(18) 1_554 ?
Si3 O3 1.579(6) 2_675 ?
Si3 O7 1.58(2) . ?
Si3 O2 1.608(5) . ?
Si3 O4 1.612(13) . ?

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
O4 Na1 O1 155.0(6) 2_665 1_656 ?
O4 Na1 O8 104.1(3) 2_665 . ?
O1 Na1 O8 63.2(3) 1_656 . ?
O4 Na1 O7 101.8(5) 2_665 1_655 ?
O1 Na1 O7 91.6(3) 1_656 1_655 ?
O8 Na1 O7 153.9(4) . 1_655 ?
O4 Na1 O1 117.3(4) 2_665 2_675 ?
O1 Na1 O1 87.6(4) 1_656 2_675 ?
O8 Na1 O1 109.2(7) . 2_675 ?
O7 Na1 O1 60.2(8) 1_655 2_675 ?
O4 Na1 O2 63.5(4) 2_665 2_665 ?
O1 Na1 O2 92.2(5) 1_656 2_665 ?
O8 Na1 O2 79.5(5) . 2_665 ?
O7 Na1 O2 109.9(8) 1_655 2_665 ?
O1 Na1 O2 170.0(5) 2_675 2_665 ?
O4 Na1 B1 136.7(2) 2_665 2_666 ?
O1 Na1 B1 32.1(4) 1_656 2_666 ?
O8 Na1 B1 33.0(2) . 2_666 ?
O7 Na1 B1 120.9(4) 1_655 2_666 ?
O1 Na1 B1 91.7(6) 2_675 2_666 ?
O2 Na1 B1 93.4(5) 2_665 2_666 ?
O4 Na1 O3 82.7(5) 2_665 2_675 ?
O1 Na1 O3 112.0(7) 1_656 2_675 ?
O8 Na1 O3 75.0(5) . 2_675 ?
O7 Na1 O3 111.5(6) 1_655 2_675 ?
O1 Na1 O3 58.1(4) 2_675 2_675 ?
O2 Na1 O3 130.7(3) 2_665 2_675 ?
B1 Na1 O3 87.5(6) 2_666 2_675 ?
O4 Na1 B1 112.5(3) 2_665 1_665 ?
O1 Na1 B1 89.6(3) 1_656 1_665 ?
O8 Na1 B1 135.3(7) . 1_665 ?
O7 Na1 B1 29.8(9) 1_655 1_665 ?
O1 Na1 B1 30.3(6) 2_675 1_665 ?
O2 Na1 B1 139.7(7) 2_665 1_665 ?
B1 Na1 B1 108.4(3) 2_666 1_665 ?
O3 Na1 B1 84.8(5) 2_675 1_665 ?
O4 Na1 O6 109.3(7) 2_665 1_655 ?
O1 Na1 O6 57.2(6) 1_656 1_655 ?
O8 Na1 O6 102.1(4) . 1_655 ?
O7 Na1 O6 66.0(5) 1_655 1_655 ?
O1 Na1 O6 113.4(3) 2_675 1_655 ?
O2 Na1 O6 58.7(4) 2_665 1_655 ?
B1 Na1 O6 84.2(5) 2_666 1_655 ?
O3 Na1 O6 168.0(5) 2_675 1_655 ?
B1 Na1 O6 89.5(5) 1_665 1_655 ?
O4 Na1 Si3 31.4(3) 2_665 2_665 ?
O1 Na1 Si3 123.7(5) 1_656 2_665 ?
O8 Na1 Si3 88.8(4) . 2_665 ?
O7 Na1 Si3 112.4(7) 1_655 2_665 ?
O1 Na1 Si3 148.65(19) 2_675 2_665 ?
O2 Na1 Si3 32.51(16) 2_665 2_665 ?
B1 Na1 Si3 115.3(4) 2_666 2_665 ?
O3 Na1 Si3 105.2(2) 2_675 2_665 ?
B1 Na1 Si3 135.3(5) 1_665 2_665 ?
O6 Na1 Si3 86.3(4) 1_655 2_665 ?
O4 Na1 Si2 137.7(7) 2_665 1_656 ?
O1 Na1 Si2 27.5(5) 1_656 1_656 ?
O8 Na1 Si2 83.6(2) . 1_656 ?
O7 Na1 Si2 75.1(3) 1_655 1_656 ?
O1 Na1 Si2 98.0(2) 2_675 1_656 ?
O2 Na1 Si2 77.6(3) 2_665 1_656 ?
B1 Na1 Si2 57.5(4) 2_666 1_656 ?
O3 Na1 Si2 138.5(4) 2_675 1_656 ?
B1 Na1 Si2 86.1(2) 1_665 1_656 ?
O6 Na1 Si2 30.1(3) 1_655 1_656 ?
Si3 Na1 Si2 109.6(3) 2_665 1_656 ?
O7 B1 O5 111.6(17) 1_545 . ?
O7 B1 O1 104.8(9) 1_545 2_565 ?
O5 B1 O1 113.3(13) . 2_565 ?
O7 B1 O8 109.0(13) 1_545 2_666 ?
O5 B1 O8 111.6(7) . 2_666 ?
O1 B1 O8 106.1(14) 2_565 2_666 ?
O7 B1 Na1 100.6(5) 1_545 2_666 ?
O5 B1 Na1 147.7(17) . 2_666 ?
O1 B1 Na1 54.9(5) 2_565 2_666 ?
O8 B1 Na1 55.4(5) 2_666 2_666 ?
O7 B1 Na1 52.1(5) 1_545 1_445 ?
O5 B1 Na1 128.7(6) . 1_445 ?
O1 B1 Na1 52.8(7) 2_565 1_445 ?
O8 B1 Na1 119.6(4) 2_666 1_445 ?
Na1 B1 Na1 71.6(3) 2_666 1_445 ?
O6 Si1 O8 111.1(5) . . ?
O6 Si1 O5 109.8(6) . . ?
O8 Si1 O5 113.2(8) . . ?
O6 Si1 O4 109.8(8) . . ?
O8 Si1 O4 105.9(3) . . ?
O5 Si1 O4 106.9(5) . . ?
O6 Si1 Na1 123.2(4) . 2_665 ?
O8 Si1 Na1 116.0(3) . 2_665 ?
O5 Si1 Na1 78.9(2) . 2_665 ?
O4 Si1 Na1 28.1(5) . 2_665 ?
O6 Si1 Na1 133.0(3) . . ?
O8 Si1 Na1 27.8(2) . . ?
O5 Si1 Na1 110.0(5) . . ?
O4 Si1 Na1 81.1(3) . . ?
Na1 Si1 Na1 88.29(12) 2_665 . ?
O1 Si2 O3 104.9(8) . . ?
O1 Si2 O2 113.7(5) . . ?
O3 Si2 O2 110.5(3) . . ?
O1 Si2 O6 107.9(7) . 1_554 ?
O3 Si2 O6 111.1(5) . 1_554 ?
O2 Si2 O6 108.7(9) . 1_554 ?
O1 Si2 Na1 40.3(4) . 1_454 ?
O3 Si2 Na1 111.8(4) . 1_454 ?
O2 Si2 Na1 135.24(19) . 1_454 ?
O6 Si2 Na1 68.4(6) 1_554 1_454 ?
O1 Si2 Na1 42.3(4) . 2_675 ?
O3 Si2 Na1 62.8(6) . 2_675 ?
O2 Si2 Na1 131.2(7) . 2_675 ?
O6 Si2 Na1 118.8(6) 1_554 2_675 ?
Na1 Si2 Na1 61.3(2) 1_454 2_675 ?
O3 Si3 O7 112.1(6) 2_675 . ?
O3 Si3 O2 109.9(3) 2_675 . ?
O7 Si3 O2 116.0(9) . . ?
O3 Si3 O4 109.8(7) 2_675 . ?
O7 Si3 O4 105.1(6) . . ?
O2 Si3 O4 103.3(6) . . ?
O3 Si3 Na1 115.3(6) 2_675 2_665 ?
O7 Si3 Na1 130.0(3) . 2_665 ?
O2 Si3 Na1 60.3(6) . 2_665 ?
O4 Si3 Na1 43.8(2) . 2_665 ?
O3 Si3 Na1 148.6(5) 2_675 1_455 ?
O7 Si3 Na1 37.6(3) . 1_455 ?
O2 Si3 Na1 95.8(4) . 1_455 ?
O4 Si3 Na1 80.1(4) . 1_455 ?
Na1 Si3 Na1 92.7(3) 2_665 1_455 ?
B1 O1 Si2 141.7(8) 2_565 . ?
B1 O1 Na1 93.0(5) 2_565 1_454 ?
Si2 O1 Na1 112.2(9) . 1_454 ?
B1 O1 Na1 96.9(13) 2_565 2_675 ?
Si2 O1 Na1 109.8(3) . 2_675 ?
Na1 O1 Na1 92.4(4) 1_454 2_675 ?
Si2 O2 Si3 134.9(5) . . ?
Si2 O2 Na1 127.7(7) . 2_665 ?
Si3 O2 Na1 87.2(6) . 2_665 ?
Si3 O3 Si2 146.1(12) 2_675 . ?
Si3 O3 Na1 119.0(6) 2_675 2_675 ?
Si2 O3 Na1 87.0(5) . 2_675 ?
Si3 O4 Si1 124.3(6) . . ?
Si3 O4 Na1 104.7(4) . 2_665 ?
Si1 O4 Na1 130.9(8) . 2_665 ?
B1 O5 Si1 116.7(12) . . ?
Si1 O6 Si2 159.6(4) . 1_556 ?
Si1 O6 Na1 109.8(4) . 1_455 ?
Si2 O6 Na1 81.4(8) 1_556 1_455 ?
B1 O7 Si3 126.8(6) 1_565 . ?
B1 O7 Na1 98.1(13) 1_565 1_455 ?
Si3 O7 Na1 117.1(8) . 1_455 ?
B1 O8 Si1 133.9(10) 2_666 . ?
B1 O8 Na1 91.5(5) 2_666 . ?
Si1 O8 Na1 132.9(3) . . ?

_refine_diff_density_max         1.176
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.148


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.252 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.99 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT213_shelx               
;
PROBLEM: Atom Si2             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        691 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC8
_audit_block_doi                 10.5517/ccdc.csd.cc2b5z9t
_database_code_depnum_ccdc_archive 'CCDC 2150696'
loop_
_audit_author_name
_audit_author_address
'Liudmila Gorelova'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2022-02-08 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Na O8 Si3'
_chemical_formula_weight         246.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0016 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0081 0.0107 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.7686(19)
_cell_length_b                   7.1398(19)
_cell_length_c                   7.3847(8)
_cell_angle_alpha                115.761(17)
_cell_angle_beta                 100.558(15)
_cell_angle_gamma                106.86(2)
_cell_volume                     287.09(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    731
_cell_measurement_theta_min      2.008
_cell_measurement_theta_max      17.339

_exptl_crystal_description       isosymmetric
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.847
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.107
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.2896
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  
'esperanto-CrysAlsiPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1117
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.008
_diffrn_reflns_theta_max         17.339
_diffrn_reflns_theta_full        10.007
_diffrn_measured_fraction_theta_max 0.140
_diffrn_measured_fraction_theta_full 0.255
_diffrn_reflns_Laue_measured_fraction_max 0.140
_diffrn_reflns_Laue_measured_fraction_full 0.255
_diffrn_reflns_point_group_measured_fraction_max 0.140
_diffrn_reflns_point_group_measured_fraction_full 0.255
_reflns_number_total             731
_reflns_number_gt                681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0473P)²] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.35(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         731
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_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
Na1 Na 0.8678(3) 0.7345(4) 0.2516(2) 0.013(2) Uani 1 1 d . . . . .
B1 B 0.2211(7) 0.1700(9) 0.3511(5) 0.007(4) Uani 1 1 d . . . . .
Si1 Si 0.35321(16) 0.5425(2) 0.31593(12) 0.0062(11) Uani 1 1 d . . . . .
Si2 Si 0.20918(15) 0.8152(2) -0.30456(11) 0.0051(10) Uani 1 1 d . . . . .
Si3 Si 0.31979(16) 0.8010(2) 0.10058(12) 0.0068(11) Uani 1 1 d . . . . .
O1 O -0.0031(4) 0.8576(7) -0.3721(4) 0.015(4) Uani 1 1 d . . . . .
O2 O 0.2037(4) 0.7059(6) -0.1524(3) 0.011(3) Uani 1 1 d . . . . .
O3 O 0.4170(4) 1.0637(6) -0.1739(3) 0.012(3) Uani 1 1 d . . . . .
O4 O 0.2758(4) 0.5659(6) 0.1057(3) 0.010(3) Uani 1 1 d . . . . .
O5 O 0.2702(4) 0.2738(6) 0.2246(3) 0.012(3) Uani 1 1 d . . . . .
O6 O 0.2324(5) 0.6473(7) 0.4787(3) 0.011(3) Uani 1 1 d . . . . .
O7 O 0.2126(5) 0.9407(8) 0.2533(4) 0.020(4) Uani 1 1 d . . . . .
O8 O 0.6173(4) 0.6844(6) 0.4250(3) 0.019(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
Na1 O4 2.332(4) 2_665 ?
Na1 O8 2.342(4) . ?
Na1 O7 2.365(3) 1_655 ?
Na1 O1 2.4085(17) 1_656 ?
Na1 O1 2.452(5) 2_675 ?
Na1 O2 2.764(5) 2_665 ?
Na1 O3 2.837(6) 2_675 ?
Na1 B1 2.930(4) 2_666 ?
Na1 B1 2.997(3) 1_665 ?
Na1 Si3 3.213(3) 2_665 ?
Na1 Si2 3.274(4) 2_675 ?
Na1 Si2 3.3502(18) 1_656 ?
B1 O5 1.451(2) . ?
B1 O7 1.451(10) 1_545 ?
B1 O1 1.477(7) 2_565 ?
B1 O8 1.481(2) 2_666 ?
Si1 O5 1.600(4) . ?
Si1 O8 1.607(2) . ?
Si1 O6 1.614(5) . ?
Si1 O4 1.6405(18) . ?
Si2 O1 1.589(5) . ?
Si2 O6 1.600(5) 1_554 ?
Si2 O3 1.6197(19) . ?
Si2 O2 1.623(2) . ?
Si3 O7 1.592(6) . ?
Si3 O3 1.610(2) 2_675 ?
Si3 O2 1.6181(14) . ?
Si3 O4 1.636(4) . ?

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
O4 Na1 O8 110.67(9) 2_665 . ?
O4 Na1 O7 97.95(14) 2_665 1_655 ?
O8 Na1 O7 151.37(13) . 1_655 ?
O4 Na1 O1 147.95(19) 2_665 1_656 ?
O8 Na1 O1 59.20(10) . 1_656 ?
O7 Na1 O1 95.78(7) 1_655 1_656 ?
O4 Na1 O1 125.52(9) 2_665 2_675 ?
O8 Na1 O1 103.56(19) . 2_675 ?
O7 Na1 O1 57.6(2) 1_655 2_675 ?
O1 Na1 O1 86.16(12) 1_656 2_675 ?
O4 Na1 O2 59.15(11) 2_665 2_665 ?
O8 Na1 O2 81.72(15) . 2_665 ?
O7 Na1 O2 113.8(2) 1_655 2_665 ?
O1 Na1 O2 88.80(14) 1_656 2_665 ?
O1 Na1 O2 169.39(15) 2_675 2_665 ?
O4 Na1 O3 93.58(14) 2_665 2_675 ?
O8 Na1 O3 73.28(15) . 2_675 ?
O7 Na1 O3 106.69(16) 1_655 2_675 ?
O1 Na1 O3 110.0(2) 1_656 2_675 ?
O1 Na1 O3 57.41(12) 2_675 2_675 ?
O2 Na1 O3 133.20(8) 2_665 2_675 ?
O4 Na1 B1 137.70(7) 2_665 2_666 ?
O8 Na1 B1 30.08(7) . 2_666 ?
O7 Na1 B1 122.30(9) 1_655 2_666 ?
O1 Na1 B1 30.16(14) 1_656 2_666 ?
O1 Na1 B1 89.98(15) 2_675 2_666 ?
O2 Na1 B1 90.35(14) 2_665 2_666 ?
O3 Na1 B1 87.24(18) 2_675 2_666 ?
O4 Na1 B1 115.70(10) 2_665 1_665 ?
O8 Na1 B1 128.8(2) . 1_665 ?
O7 Na1 B1 28.4(2) 1_655 1_665 ?
O1 Na1 B1 89.24(7) 1_656 1_665 ?
O1 Na1 B1 29.34(19) 2_675 1_665 ?
O2 Na1 B1 141.4(2) 2_665 1_665 ?
O3 Na1 B1 83.14(16) 2_675 1_665 ?
B1 Na1 B1 106.40(8) 2_666 1_665 ?
O4 Na1 Si3 29.18(8) 2_665 2_665 ?
O8 Na1 Si3 94.65(10) . 2_665 ?
O7 Na1 Si3 110.78(18) 1_655 2_665 ?
O1 Na1 Si3 118.82(14) 1_656 2_665 ?
O1 Na1 Si3 154.47(6) 2_675 2_665 ?
O2 Na1 Si3 30.24(4) 2_665 2_665 ?
O3 Na1 Si3 112.95(7) 2_675 2_665 ?
B1 Na1 Si3 114.13(10) 2_666 2_665 ?
B1 Na1 Si3 136.57(16) 1_665 2_665 ?
O4 Na1 Si2 112.89(12) 2_665 2_675 ?
O8 Na1 Si2 87.91(16) . 2_675 ?
O7 Na1 Si2 81.57(17) 1_655 2_675 ?
O1 Na1 Si2 97.67(17) 1_656 2_675 ?
O1 Na1 Si2 27.79(10) 2_675 2_675 ?
O2 Na1 Si2 162.79(9) 2_665 2_675 ?
O3 Na1 Si2 29.65(5) 2_675 2_675 ?
B1 Na1 Si2 87.44(16) 2_666 2_675 ?
B1 Na1 Si2 55.04(16) 1_665 2_675 ?
Si3 Na1 Si2 138.81(6) 2_665 2_675 ?
O4 Na1 Si2 130.89(18) 2_665 1_656 ?
O8 Na1 Si2 80.74(7) . 1_656 ?
O7 Na1 Si2 79.85(8) 1_655 1_656 ?
O1 Na1 Si2 26.05(14) 1_656 1_656 ?
O1 Na1 Si2 94.84(7) 2_675 1_656 ?
O2 Na1 Si2 76.77(8) 2_665 1_656 ?
O3 Na1 Si2 134.45(12) 2_675 1_656 ?
B1 Na1 Si2 54.67(12) 2_666 1_656 ?
B1 Na1 Si2 84.96(8) 1_665 1_656 ?
Si3 Na1 Si2 105.77(10) 2_665 1_656 ?
Si2 Na1 Si2 115.19(7) 2_675 1_656 ?
O5 B1 O7 111.9(4) . 1_545 ?
O5 B1 O1 113.0(5) . 2_565 ?
O7 B1 O1 105.0(3) 1_545 2_565 ?
O5 B1 O8 111.00(17) . 2_666 ?
O7 B1 O8 110.6(4) 1_545 2_666 ?
O1 B1 O8 105.0(4) 2_565 2_666 ?
O5 B1 Na1 141.4(5) . 2_666 ?
O7 B1 Na1 106.73(14) 1_545 2_666 ?
O1 B1 Na1 55.01(13) 2_565 2_666 ?
O8 B1 Na1 52.44(17) 2_666 2_666 ?
O5 B1 Na1 133.42(13) . 1_445 ?
O7 B1 Na1 50.83(15) 1_545 1_445 ?
O1 B1 Na1 54.4(2) 2_565 1_445 ?
O8 B1 Na1 115.59(13) 2_666 1_445 ?
Na1 B1 Na1 73.60(8) 2_666 1_445 ?
O5 Si1 O8 114.3(3) . . ?
O5 Si1 O6 109.82(17) . . ?
O8 Si1 O6 111.40(17) . . ?
O5 Si1 O4 105.78(14) . . ?
O8 Si1 O4 106.28(9) . . ?
O6 Si1 O4 108.9(3) . . ?
O1 Si2 O6 107.4(2) . 1_554 ?
O1 Si2 O3 106.0(2) . . ?
O6 Si2 O3 110.80(17) 1_554 . ?
O1 Si2 O2 115.00(17) . . ?
O6 Si2 O2 109.0(3) 1_554 . ?
O3 Si2 O2 108.56(9) . . ?
O1 Si2 Na1 46.00(12) . 2_675 ?
O6 Si2 Na1 119.96(15) 1_554 2_675 ?
O3 Si2 Na1 60.07(19) . 2_675 ?
O2 Si2 Na1 130.7(2) . 2_675 ?
O1 Si2 Na1 41.72(12) . 1_454 ?
O6 Si2 Na1 66.87(17) 1_554 1_454 ?
O3 Si2 Na1 111.50(11) . 1_454 ?
O2 Si2 Na1 138.22(6) . 1_454 ?
Na1 Si2 Na1 64.81(7) 2_675 1_454 ?
O7 Si3 O3 113.80(18) . 2_675 ?
O7 Si3 O2 114.6(2) . . ?
O3 Si3 O2 109.36(11) 2_675 . ?
O7 Si3 O4 108.11(19) . . ?
O3 Si3 O4 107.3(2) 2_675 . ?
O2 Si3 O4 102.80(15) . . ?
O7 Si3 Na1 130.82(8) . 2_665 ?
O3 Si3 Na1 113.5(2) 2_675 2_665 ?
O2 Si3 Na1 59.36(15) . 2_665 ?
O4 Si3 Na1 44.01(8) . 2_665 ?
O7 Si3 Na1 37.53(8) . 1_455 ?
O3 Si3 Na1 147.01(13) 2_675 1_455 ?
O2 Si3 Na1 100.53(13) . 1_455 ?
O4 Si3 Na1 78.41(16) . 1_455 ?
Na1 Si3 Na1 93.38(8) 2_665 1_455 ?
B1 O1 Si2 143.0(2) 2_565 . ?
B1 O1 Na1 94.83(15) 2_565 1_454 ?
Si2 O1 Na1 112.2(3) . 1_454 ?
B1 O1 Na1 96.2(4) 2_565 2_675 ?
Si2 O1 Na1 106.22(10) . 2_675 ?
Na1 O1 Na1 93.84(12) 1_454 2_675 ?
Si3 O2 Si2 135.67(18) . . ?
Si3 O2 Na1 90.40(15) . 2_665 ?
Si2 O2 Na1 130.06(19) . 2_665 ?
Si3 O3 Si2 145.7(4) 2_675 . ?
Si3 O3 Na1 119.89(18) 2_675 2_675 ?
Si2 O3 Na1 90.27(17) . 2_675 ?
Si3 O4 Si1 127.69(17) . . ?
Si3 O4 Na1 106.82(8) . 2_665 ?
Si1 O4 Na1 124.8(2) . 2_665 ?
B1 O5 Si1 123.7(3) . . ?
Si2 O6 Si1 158.11(13) 1_556 . ?
B1 O7 Si3 137.45(16) 1_565 . ?
B1 O7 Na1 100.8(3) 1_565 1_455 ?
Si3 O7 Na1 118.3(2) . 1_455 ?
B1 O8 Si1 135.0(3) 2_666 . ?
B1 O8 Na1 97.5(2) 2_666 . ?
Si1 O8 Na1 127.39(10) . . ?

_refine_diff_density_max         0.222
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.057


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.255 Why?  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.14 Note  
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        763 Report
RESPONSE: Incomplete scans, based on small opening of the daimond anvil cell
;
# end Validation Reply Form
