#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:29:35 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298156 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573233.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_1573233
loop_
_publ_author_name
'Sumida, Akifumi'
'Saeki, Akinori'
'Matsuo, Kyohei'
'Naka, Kensuke'
'Imoto, Hiroaki'
_publ_section_title
;
 Dithienoarsinines: stable and planar π-extended arsabenzenes.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1126
_journal_page_last               1135
_journal_paper_doi               10.1039/d4sc06590e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C14 H5 As O5 S2 W'
_chemical_formula_sum            'C14 H5 As O5 S2 W'
_chemical_formula_weight         576.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-10
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.355(6)
_cell_angle_beta                 106.909(6)
_cell_angle_gamma                100.480(6)
_cell_formula_units_Z            2
_cell_length_a                   7.3120(5)
_cell_length_b                   10.1653(8)
_cell_length_c                   11.2954(8)
_cell_measurement_reflns_used    2534
_cell_measurement_temperature    256.00
_cell_measurement_theta_max      32.7370
_cell_measurement_theta_min      3.1370
_cell_volume                     785.92(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      256.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -48.00   0.10    0.50    --   30.00  54.00 -90.00  250
  2  ω      5.00  32.00   0.10    0.50    --   30.00  54.00 -90.00  270
  3  ω    -70.00  31.00   0.10    0.50    --   30.00  54.00 150.00 1010
  4  ω    -74.00 110.00   0.10    0.50    --   30.00  54.00  30.00 1840
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0455688000
_diffrn_orient_matrix_UB_12      0.0016118000
_diffrn_orient_matrix_UB_13      0.0648637000
_diffrn_orient_matrix_UB_21      0.0494456000
_diffrn_orient_matrix_UB_22      0.0671154000
_diffrn_orient_matrix_UB_23      0.0011660000
_diffrn_orient_matrix_UB_31      -0.0787330000
_diffrn_orient_matrix_UB_32      0.0240645000
_diffrn_orient_matrix_UB_33      0.0119345000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.724
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.15
_refine_diff_density_max         6.699
_refine_diff_density_min         -5.056
_refine_diff_density_rms         0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1871P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2385
_reflns_number_total             3210
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc06590e2.cif
_cod_data_source_block           3a-W(CO)5
_cod_depositor_comments
'Adding full bibliography for 1573224--1573235.cif.'
_cod_database_code               1573233
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H5O5AsS2W
_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   0.323
_shelx_estimated_absorpt_t_min   0.039
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C009 \\sim O007: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O008 \\sim C00B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C00D \\sim O006: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00N(H00N)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.306
_oxdiff_exptl_absorpt_empirical_full_min 0.343
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
W001 W 0.70010(10) 0.20133(7) 0.77907(7) 0.0308(4) Uani 1 1 d . . . . .
S003 S 0.5397(8) 0.2435(6) 0.3670(5) 0.0381(11) Uani 1 1 d . . . . .
S004 S 0.9273(7) 0.6440(6) 0.8256(5) 0.0412(12) Uani 1 1 d . . . . .
O005 O 0.237(2) 0.0962(15) 0.6901(16) 0.043(4) Uani 1 1 d . . . . .
O006 O 1.164(2) 0.2903(16) 0.8920(15) 0.042(3) Uani 1 1 d . U . . .
O007 O 0.756(2) 0.0227(14) 0.5593(14) 0.037(3) Uani 1 1 d . U . . .
O008 O 0.629(2) 0.4010(16) 0.9745(12) 0.039(3) Uani 1 1 d . U . . .
C009 C 0.727(3) 0.0832(18) 0.634(2) 0.034(3) Uani 1 1 d . U . . .
O00A O 0.723(3) -0.0298(17) 0.9505(18) 0.058(5) Uani 1 1 d . . . . .
C00B C 0.663(3) 0.330(2) 0.9156(19) 0.038(3) Uani 1 1 d . U . . .
C00C C 0.401(3) 0.1351(18) 0.719(2) 0.033(4) Uani 1 1 d . . . . .
C00D C 0.995(3) 0.263(2) 0.851(2) 0.041(3) Uani 1 1 d . U . . .
C00E C 0.662(3) 0.379(2) 0.467(2) 0.038(5) Uani 1 1 d . . . . .
C00F C 0.883(3) 0.657(2) 0.590(2) 0.045(5) Uani 1 1 d . . . . .
C00G C 0.827(3) 0.618(2) 0.464(2) 0.038(5) Uani 1 1 d . . . . .
H00G H 0.859687 0.682976 0.413428 0.045 Uiso 1 1 calc R U . . .
C00H C 0.991(3) 0.786(2) 0.655(2) 0.044(5) Uani 1 1 d . . . . .
H00H H 1.035758 0.857447 0.614664 0.053 Uiso 1 1 calc R U . . .
C00I C 0.710(3) 0.052(3) 0.888(2) 0.050(7) Uani 1 1 d . . . . .
C00J C 0.725(3) 0.492(2) 0.404(2) 0.040(5) Uani 1 1 d . . . . .
C00K C 0.568(3) 0.325(2) 0.241(2) 0.043(5) Uani 1 1 d . . . . .
H00K H 0.525033 0.283582 0.160334 0.052 Uiso 1 1 calc R U . . .
C00L C 0.655(3) 0.449(2) 0.270(2) 0.038(5) Uani 1 1 d . . . . .
H00L H 0.672906 0.507285 0.211044 0.046 Uiso 1 1 calc R U . . .
C00M C 0.842(3) 0.566(2) 0.677(2) 0.037(5) Uani 1 1 d . . . . .
C00N C 1.018(3) 0.793(2) 0.774(2) 0.039(5) Uani 1 1 d . . . . .
H00N H 1.081466 0.870831 0.826684 0.047 Uiso 1 1 calc R U . . .
As As 0.7062(3) 0.3928(2) 0.6380(2) 0.0357(6) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1794
0 0 -1 0.2688
0 1 0 0.0629
0 -1 0 0.0835
-1 1 0 0.2156
1 -1 0 0.4137
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
C009 W001 C00B 175.6(7) . . ?
C009 W001 As 85.8(5) . . ?
C00B W001 As 90.3(6) . . ?
C00C W001 C009 90.6(8) . . ?
C00C W001 C00B 87.8(8) . . ?
C00C W001 As 95.8(5) . . ?
C00D W001 C009 92.0(8) . . ?
C00D W001 C00B 89.8(9) . . ?
C00D W001 C00C 175.9(8) . . ?
C00D W001 As 87.6(7) . . ?
C00I W001 C009 92.6(8) . . ?
C00I W001 C00B 91.4(8) . . ?
C00I W001 C00C 87.0(9) . . ?
C00I W001 C00D 89.7(10) . . ?
C00I W001 As 176.7(6) . . ?
C00E S003 C00K 92.3(11) . . ?
C00M S004 C00N 91.1(11) . . ?
O007 C009 W001 174.9(19) . . ?
O008 C00B W001 171.5(18) . . ?
O005 C00C W001 177.1(19) . . ?
O006 C00D W001 175.9(19) . . ?
S003 C00E As 126.0(12) . . ?
C00J C00E S003 112.1(16) . . ?
C00J C00E As 121.9(17) . . ?
C00G C00F C00H 128(2) . . ?
C00G C00F C00M 122(2) . . ?
C00M C00F C00H 110(2) . . ?
C00F C00G C00J 126(2) . . ?
C00N C00H C00F 114(2) . . ?
O00A C00I W001 177(2) . . ?
C00E C00J C00L 108(2) . . ?
C00G C00J C00E 125(2) . . ?
C00G C00J C00L 127.6(18) . . ?
C00L C00K S003 113.3(18) . . ?
C00K C00L C00J 114.4(19) . . ?
S004 C00M As 123.1(12) . . ?
C00F C00M S004 111.1(17) . . ?
C00F C00M As 125.7(18) . . ?
C00H C00N S004 114.1(19) . . ?
C00E As W001 127.9(6) . . ?
C00M As W001 128.9(7) . . ?
C00M As C00E 99.3(10) . . ?
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
W001 C009 2.07(2) . ?
W001 C00B 2.09(2) . ?
W001 C00C 2.07(2) . ?
W001 C00D 2.04(2) . ?
W001 C00I 1.98(3) . ?
W001 As 2.568(2) . ?
S003 C00E 1.68(2) . ?
S003 C00K 1.72(2) . ?
S004 C00M 1.71(2) . ?
S004 C00N 1.74(2) . ?
O005 C00C 1.13(3) . ?
O006 C00D 1.16(3) . ?
O007 C009 1.11(2) . ?
O008 C00B 1.07(2) . ?
O00A C00I 1.12(3) . ?
C00E C00J 1.44(3) . ?
C00E As 1.86(2) . ?
C00F C00G 1.38(3) . ?
C00F C00H 1.44(3) . ?
C00F C00M 1.43(3) . ?
C00G C00J 1.40(3) . ?
C00H C00N 1.30(3) . ?
C00J C00L 1.47(3) . ?
C00K C00L 1.29(3) . ?
C00M As 1.83(2) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0006 0.0014 0.9983 0.0647 0.0012 0.0120
0.0006 -0.0014 -0.9983 -0.0647 -0.0012 -0.0120
0.0018 0.9958 -0.0001 0.0017 0.0669 0.0238
-0.0018 -0.9958 0.0001 -0.0017 -0.0669 -0.0238
-0.9951 0.9947 0.0014 -0.0436 0.0176 0.1023
0.9951 -0.9947 -0.0014 0.0436 -0.0176 -0.1023
