Redox mediated dimerisation of a cyclo-As8 complex
Riesinger, Christoph; Scheer, Manfred; Chemical Science 16 (2025) 8807–8811; doi:10.1039/D5SC01685A

data_1574358
_publ_section_title
;
 Redox mediated dimerisation of a cyclo-As8 complex
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              8807
_journal_page_last               8811
_journal_paper_doi               10.1039/D5SC01685A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C26 H42 As8 Ta2, C18 H36 K N2 O6, C4 H8 O, 2[C4H8O]'
_chemical_formula_sum            'C56 H102 As8 K N2 O9 Ta2'
_chemical_formula_weight         1947.75
_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             2024-11-13
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.02 svn.r19aeb66f for OlexSys, GUI svn.r7078)
;
_audit_update_record
;
2025-02-06 deposited with the CCDC.	2025-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                109.325(2)
_cell_angle_beta                 108.365(2)
_cell_angle_gamma                101.9440(10)
_cell_formula_units_Z            2
_cell_length_a                   15.0711(3)
_cell_length_b                   15.7076(2)
_cell_length_c                   17.5064(4)
_cell_measurement_reflns_used    30895
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.7940
_cell_measurement_theta_min      2.8950
_cell_volume                     3480.31(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     24.00  70.00   0.50    0.10    --   62.65-114.00 154.00   92
  2  \w    -77.00 -29.00   0.50    0.10    --  -63.52 114.00-114.00   96
  3  \w    -93.00 -62.00   0.50    0.10    --  -72.72 114.00-114.00   62
  4  \w     44.00  71.00   0.50    0.10    --   75.31-114.00 154.00   54
  5  \w    -63.00 -37.00   0.50    0.10    --  -76.44 114.00-114.00   52
  6  \w    -97.00 -71.00   0.50    0.10    --  -76.44 114.00-114.00   52
  7  \w     26.00  71.00   0.50    0.10    --   62.65 -95.00   0.00   90
  8  \w     31.00  93.00   0.50    0.10    --   62.65  15.00-180.00  124
  9  \w     21.00  89.00   0.50    0.10    --   62.65-125.00-120.00  136
 10  \w     25.00  94.00   0.50    0.10    --   62.65   0.00 -30.00  138
 11  \w     47.00 107.00   0.50    0.10    --   62.65  15.00  30.00  120
 12  \w     25.00  70.00   0.50    0.10    --   62.65 -95.00  60.00   90
 13  \w    -67.00 -33.00   0.50    0.10    --  -63.52 -15.00-150.00   68
 14  \w    -94.00 -29.00   0.50    0.10    --  -63.52   0.00  90.00  130
 15  \w   -108.00 -76.00   0.50    0.10    --  -63.52 -15.00-150.00   64
 16  \w     41.00 118.00   0.50    0.10    --   72.32  15.00-120.00  154
 17  \w     32.00  90.00   0.50    0.10    --   72.32-114.00 154.00  116
 18  \w    -99.00 -37.00   0.50    0.10    --  -72.72 125.00   0.00  124
 19  \w    -99.00 -34.00   0.50    0.10    --  -72.72 125.00-150.00  130
 20  \w   -114.00 -80.00   0.50    0.10    --  -72.72 -15.00-180.00   68
 21  \w    -57.00 -32.00   0.50    0.10    --  -72.72 114.00-114.00   50
 22  \w    -78.00 -41.00   0.50    0.10    --  -72.72 -15.00-180.00   74
 23  \w     38.00  83.00   0.50    0.10    --   75.31 -95.00-150.00   90
 24  \w   -103.00 -37.00   0.50    0.10    --  -76.44 125.00 120.00  132
 25  \w   -103.00 -77.00   0.50    0.10    --  -76.44 125.00  90.00   52
 26  \w   -102.00 -36.00   0.50    0.10    --  -76.44 125.00-180.00  132
 27  \w   -119.00 -51.00   0.50    0.10    --  -76.44 -15.00 -30.00  136
 28  \w   -103.00 -39.00   0.50    0.10    --  -76.44 125.00 -30.00  128
 29  \w   -117.00 -75.00   0.50    0.10    --  -76.44-125.00 -60.00   84
 30  \w    -62.00 -35.00   0.50    0.10    --  -76.44 125.00  90.00   54
 31  \w   -103.00 -35.00   0.50    0.10    --  -76.44 125.00 -90.00  136
 32  \w    -74.00 -39.00   0.50    0.10    --  -76.44 125.00 -60.00   70
 33  \w   -103.00 -77.00   0.50    0.10    --  -76.44 125.00 -60.00   52
 34  \w   -103.00 -36.00   0.50    0.10    --  -76.44 125.00  30.00  134
 35  \w   -114.00 -40.00   0.50    0.10    --  -76.44   0.00-120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0759426000
_diffrn_orient_matrix_UB_12      -0.0671596000
_diffrn_orient_matrix_UB_13      -0.0963300000
_diffrn_orient_matrix_UB_21      0.0523173000
_diffrn_orient_matrix_UB_22      0.0650266000
_diffrn_orient_matrix_UB_23      -0.0337409000
_diffrn_orient_matrix_UB_31      0.0684776000
_diffrn_orient_matrix_UB_32      -0.0595552000
_diffrn_orient_matrix_UB_33      -0.0096112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44802
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.919
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.856
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.087
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       plate
_exptl_crystal_F_000             1906
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.949
_refine_diff_density_min         -2.665
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         13412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0517
_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/[\s^2^(Fo^2^)+(0.0997P)^2^+1.5567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11738
_reflns_number_total             13412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01685a2.cif
_cod_data_source_block           cr1399
_cod_depositor_comments
'Adding full bibliography for 1574358--1574360.cif.'
_cod_original_cell_volume        3480.30(13)
_cod_database_code               1574358
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C60H110N2O10KAs8Ta2
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.115
_diffrn_oxdiff_ac3_digest_hkl    415c68365a302e2787e5d1c9bca20f363bc828
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C34(H34A,H34B), C42(H42A,H42B), C13(H13A,H13B), C27(H27A,
 H27B), C15(H15A,H15B), C31(H31A,H31B), C2(H2A,H2B), C33(H33A,H33B), C17(H17A,
 H17B), C35(H35A,H35B), C9(H9A,H9B), C37(H37A,H37B), C19(H19A,H19B), C5(H5A,
 H5B), C41(H41A,H41B), C21(H21A,H21B), C43(H43A,H43B), C11(H11A,H11B), C45(H45A,
 H45B), C23(H23A,H23B), C47(H47A,H47B)
1.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C24(H24), C40(H40), C44(H44), C7(H7)
1.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C38(H38A,
 H38B,H38C), C46(H46A,H46B,H46C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C),
 C39(H39A,H39B,H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 160 electrons were 
found in a volume of 985\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O] per formula unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.4
_shelx_res_checksum              15231
_shelx_fab_checksum              3957
_platon_squeeze_void_probe_radius 1.20
_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 5.154
_oxdiff_exptl_absorpt_empirical_full_min 0.274