#------------------------------------------------------------------------------
#$Date: 2023-05-25 00:52:34 +0200 (Thu 25 de May de 2023) $
#$Revision: 283991 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/31/7713149.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7713149
loop_
_publ_author_name
'Huang, Yi'
'Chu, Dongdong'
'Yun, Yihan'
'Xie, Wenlong'
'Li, Guangmao'
'Zhang, Yong'
_publ_section_title
;
 From BPS4 to AB3P2S10 (A = Na, K): Cations Inducing Dimension Reduction
 and Bandgap Enlargement
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01337E
_journal_year                    2023
_chemical_formula_moiety         'B3 Na P2 S10'
_chemical_formula_sum            'B3 Na P2 S10'
_chemical_formula_weight         437.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-03-31 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.126(3)
_cell_length_b                   13.126(3)
_cell_length_c                   15.379(5)
_cell_measurement_reflns_used    3019
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      3.104
_cell_volume                     2649.7(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.040
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1680 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.7099.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0233P)²+6.3878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1170
_reflns_number_total             1517
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01337e2.cif
_cod_data_source_block           NaB3P2S10
_cod_original_cell_volume        2649.6(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7713149
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
;
_shelx_res_file
;
TITL shou2222_a.res in I4(1)/a
    shou2222.res
    created by SHELXL-2018/3 at 22:06:37 on 31-Mar-2023
REM Old TITL SHOU2222 in I4(1)/a
REM SHELXT solution in I4(1)/a: R1 0.119, Rweak 0.003, Alpha 0.020
REM <I/s> 0.225 for 57 systematic absences, Orientation as input
REM Formula found by SHELXT: B P S3
CELL 0.71073 13.1257 13.1257 15.3792 90 90 90
ZERR 8 0.0033 0.0033 0.0045 0 0 0
LATT 2
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.75-Y,0.25+X,0.25+Z
SYMM 0.75+Y,0.75-X,0.75+Z
SFAC B Na P S
UNIT 24 8 16 80

L.S. 40
PLAN  2
SIZE 0.13 0.14 0.12
TEMP 0
CONF
list 4
MORE -1
fmap 2 53
acta
OMIT 1 5 4
OMIT -3 5 6
REM <olex2.extras>
REM <HklSrc "%.\\shou2222.hkl">
REM </olex2.extras>

WGHT    0.023300    6.387800
FVAR       0.12713
S2    4    0.620304    0.218277    0.799464    11.00000    0.01299    0.01318 =
         0.01599   -0.00020    0.00033   -0.00035
S4    4    0.687051    0.448868    0.809865    11.00000    0.01506    0.01591 =
         0.02400    0.00434   -0.00087   -0.00283
P1    3    0.564282    0.482713    0.731956    11.00000    0.01599    0.01393 =
         0.01932    0.00399    0.00066   -0.00064
S3    4    0.764723    0.311833    0.942169    11.00000    0.01358    0.01761 =
         0.02472    0.00266   -0.00399   -0.00186
S1    4    0.468940    0.141922    0.653380    11.00000    0.02584    0.01752 =
         0.01533   -0.00259    0.00000   -0.00307
S5    4    0.596455    0.600089    0.658476    11.00000    0.02589    0.02012 =
         0.02709    0.01140    0.00089   -0.00280
NA1   2    0.500000    0.500000    0.500000    10.50000    0.17919    0.07773 =
         0.03432    0.00009   -0.02852    0.04832
B1    1    0.500000    0.250000    0.732688    10.50000    0.01566    0.01306 =
         0.01914    0.00000    0.00000    0.00040
B2    1    0.644227    0.333674    0.875860    11.00000    0.01329    0.01648 =
         0.01842    0.00105   -0.00019    0.00055
HKLF 4




REM  shou2222_a.res in I4(1)/a
REM wR2 = 0.0867, GooF = S = 1.071, Restrained GooF = 1.071 for all data
REM R1 = 0.0341 for 1170 Fo > 4sig(Fo) and 0.0499 for all 1517 data
REM 75 parameters refined using 0 restraints

END

WGHT      0.0233      6.3876

REM Highest difference peak  0.564,  deepest hole -0.409,  1-sigma level  0.114
Q1    1   0.4527  0.0838  0.6884  11.00000  0.05    0.56
Q2    1   0.6355  0.4608  0.7735  11.00000  0.05    0.50
;
_shelx_res_checksum              6736
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
S2 S 0.62030(5) 0.21828(5) 0.79946(4) 0.01405(17) Uani 1 1 d . . . . .
S4 S 0.68705(6) 0.44887(6) 0.80986(5) 0.01832(19) Uani 1 1 d . . . . .
P1 P 0.56428(6) 0.48271(6) 0.73196(5) 0.01641(19) Uani 1 1 d . . . . .
S3 S 0.76472(6) 0.31183(6) 0.94217(5) 0.01864(19) Uani 1 1 d . . . . .
S1 S 0.46894(6) 0.14192(6) 0.65338(5) 0.01956(19) Uani 1 1 d . . . . .
S5 S 0.59646(6) 0.60009(6) 0.65848(5) 0.0244(2) Uani 1 1 d . . . . .
Na1 Na 0.500000 0.500000 0.500000 0.0971(14) Uani 1 2 d S . P . .
B1 B 0.500000 0.250000 0.7327(3) 0.0160(9) Uani 1 2 d S T P . .
B2 B 0.6442(2) 0.3337(2) 0.8759(2) 0.0161(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S2 0.0130(3) 0.0132(3) 0.0160(3) -0.0002(3) 0.0003(3) -0.0003(3)
S4 0.0151(4) 0.0159(4) 0.0240(4) 0.0043(3) -0.0009(3) -0.0028(3)
P1 0.0160(4) 0.0139(4) 0.0193(4) 0.0040(3) 0.0007(3) -0.0006(3)
S3 0.0136(4) 0.0176(4) 0.0247(4) 0.0027(3) -0.0040(3) -0.0019(3)
S1 0.0258(4) 0.0175(4) 0.0153(4) -0.0026(3) 0.0000(3) -0.0031(3)
S5 0.0259(4) 0.0201(4) 0.0271(4) 0.0114(3) 0.0009(3) -0.0028(3)
Na1 0.179(4) 0.078(2) 0.0343(14) 0.0001(15) -0.029(2) 0.048(2)
B1 0.016(2) 0.013(2) 0.019(2) 0.000 0.000 0.0004(17)
B2 0.0133(15) 0.0165(16) 0.0184(16) 0.0011(13) -0.0002(12) 0.0006(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
B1 S2 B2 106.13(12) . 11_667 ?
B1 S2 B2 106.62(12) . . ?
B2 S2 B2 106.07(10) 11_667 . ?
B2 S4 P1 104.51(11) . . ?
S4 P1 S3 110.01(5) . 16_657 ?
S4 P1 S1 109.44(5) . 6_554 ?
S3 P1 S1 108.65(5) 16_657 6_554 ?
S5 P1 S4 109.72(5) . . ?
S5 P1 S3 109.79(5) . 16_657 ?
S5 P1 S1 109.21(5) . 6_554 ?
B2 S3 P1 104.71(11) . 11_667 ?
P1 S1 Na1 89.82(4) 6_554 6_554 ?
B1 S1 P1 104.91(12) . 6_554 ?
B1 S1 Na1 157.18(8) . 6_554 ?
P1 S5 Na1 91.88(4) . . ?
P1 S5 Na1 111.84(4) . 8_454 ?
Na1 S5 Na1 153.34(3) . 8_454 ?
S1 Na1 S1 180.0 14_556 6_554 ?
S1 Na1 S5 97.44(3) 6_554 15_566 ?
S1 Na1 S5 65.58(3) 6_554 . ?
S1 Na1 S5 82.56(3) 14_556 15_566 ?
S1 Na1 S5 65.58(3) 14_556 9_666 ?
S1 Na1 S5 97.44(3) 14_556 7_544 ?
S1 Na1 S5 82.56(3) 6_554 7_544 ?
S1 Na1 S5 114.42(3) 6_554 9_666 ?
S1 Na1 S5 114.42(3) 14_556 . ?
S5 Na1 S5 68.03(3) . 15_566 ?
S5 Na1 S5 68.03(3) 9_666 7_544 ?
S5 Na1 S5 111.97(3) 9_666 15_566 ?
S5 Na1 S5 180.0 15_566 7_544 ?
S5 Na1 S5 180.0 9_666 . ?
S5 Na1 S5 111.97(3) . 7_544 ?
S2 B1 S2 115.7(2) . 6_554 ?
S1 B1 S2 108.95(4) . 6_554 ?
S1 B1 S2 108.95(4) 6_554 . ?
S1 B1 S2 110.70(4) 6_554 6_554 ?
S1 B1 S2 110.70(4) . . ?
S1 B1 S1 100.9(2) 6_554 . ?
S2 B2 S2 115.48(17) 16_657 . ?
S4 B2 S2 110.13(16) . . ?
S4 B2 S2 110.16(16) . 16_657 ?
S3 B2 S2 109.93(16) . . ?
S3 B2 S2 110.74(16) . 16_657 ?
S3 B2 S4 99.19(15) . . ?
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
S2 B1 1.929(3) . ?
S2 B2 1.931(3) 11_667 ?
S2 B2 1.942(3) . ?
S4 P1 2.0566(11) . ?
S4 B2 1.906(3) . ?
P1 S3 2.0684(11) 16_657 ?
P1 S1 2.0801(11) 6_554 ?
P1 S5 1.9568(11) . ?
S3 B2 1.904(3) . ?
S1 Na1 3.0332(10) 6_554 ?
S1 B1 1.915(3) . ?
S5 Na1 3.0445(11) . ?
S5 Na1 3.1488(11) 8_454 ?
