Reactivity of tetrel functionalized heptapnictogen clusters towards heteroallenes.
Jobbins, William D.; van IJzendoorn, Bono; Vitorica-Yrezabal, Inigo J; Whitehead, George F. S.; Mehta, Meera; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2384–2391; doi:10.1039/d2dt04074c

data_7712254
_publ_section_title
;
 Reactivity of tetrel functionalized heptapnictogen clusters towards
 heteroallenes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2384
_journal_page_last               2391
_journal_paper_doi               10.1039/d2dt04074c
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C33 H48 As7 N3 O9 S3 Si3'
_chemical_formula_sum            'C33 H48 As7 N3 O9 S3 Si3'
_chemical_formula_weight         1335.63
_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             2021-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-01-19 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                94.859(2)
_cell_angle_beta                 93.493(2)
_cell_angle_gamma                91.697(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0823(3)
_cell_length_b                   13.5652(3)
_cell_length_c                   14.0438(3)
_cell_measurement_reflns_used    24418
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.5150
_cell_measurement_theta_min      3.1570
_cell_volume                     2477.18(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_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    -19.00   6.00   1.00    1.00    --    5.00 -34.00 167.00   25
  2  \w    -46.00  -5.00   1.00    1.00    --  -44.02  34.00 -34.00   41
  3  \w    -69.00 -38.00   1.00    1.00    --  -44.02 -34.00 167.00   31
  4  \w   -125.00 -95.00   1.00    1.00    --  -44.02 -34.00 167.00   30
  5  \w    -99.00 -44.00   1.00    1.00    -- -107.20  34.00 -34.00   55
  6  \w   -191.00-164.00   1.00    1.00    -- -107.20 -34.00 167.00   27
  7  \w   -105.00 -67.00   1.00    1.00    -- -107.20 -34.00 167.00   38
  8  \w   -143.00-110.00   1.00    1.00    -- -107.20 -34.00 167.00   33
  9  \w    -11.00  79.00   1.00    1.00    --    5.00  34.00 -34.00   90
 10  \w    -84.00  44.00   1.00    1.00    --  -44.02  37.00  90.00  128
 11  \w    -75.00  44.00   1.00    1.00    --  -44.02  57.00 -60.00  119
 12  \w    -87.00  43.00   1.00    1.00    --  -46.18  76.00 120.00  130
 13  \w    -95.00 -70.00   1.00    1.00    --  -46.18 -34.00 167.00   25
 14  \w    -47.00 -22.00   1.00    1.00    --  -46.18  34.00 -34.00   25
 15  \w   -141.00-109.00   1.00    1.00    -- -107.20  76.00  30.00   32
 16  \w   -148.00 -19.00   1.00    1.00    -- -107.20  76.00 -60.00  129
 17  \w   -197.00 -68.00   1.00    1.00    -- -107.20 -37.00 -60.00  129
 18  \w   -144.00 -18.00   1.00    1.00    -- -107.20  37.00 150.00  126
 19  \w   -110.00 -19.00   1.00    1.00    -- -107.20  76.00 120.00   91
 20  \w   -196.00 -71.00   1.00    1.00    -- -107.20 -37.00-150.00  125
 21  \w   -135.00 -28.00   1.00    1.00    -- -107.20  76.00   0.00  107
 22  \w   -126.00-100.00   1.00    1.00    -- -107.20  76.00-180.00   26
 23  \w   -130.00-103.00   1.00    1.00    -- -107.20  76.00 -90.00   27
 24  \w    -43.00 -18.00   1.00    1.00    -- -107.20  76.00 150.00   25
 25  \w   -186.00-161.00   1.00    1.00    -- -107.20   0.00-150.00   25
 26  \w   -116.00 -90.00   1.00    1.00    -- -107.20  76.00  60.00   26
 27  \w   -155.00-130.00   1.00    1.00    -- -107.20   0.00-150.00   25
 28  \w    -74.00 -37.00   1.00    1.00    -- -107.20   0.00-150.00   37
 29  \w   -126.00 -46.00   1.00    1.00    -- -107.20  76.00-150.00   80
 30  \w   -101.00 -59.00   1.00    1.00    -- -107.20  76.00-120.00   42
 31  \w    -91.00 -54.00   1.00    1.00    -- -107.20  76.00-180.00   37
 32  \w   -107.00 -20.00   1.00    1.00    -- -107.20  76.00  30.00   87
 33  \w   -133.00 -74.00   1.00    1.00    -- -107.20  76.00 150.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0746153000
_diffrn_orient_matrix_UB_12      -0.0905128000
_diffrn_orient_matrix_UB_13      -0.0189840000
_diffrn_orient_matrix_UB_21      -0.0813088000
_diffrn_orient_matrix_UB_22      0.0655566000
_diffrn_orient_matrix_UB_23      -0.0440099000
_diffrn_orient_matrix_UB_31      0.0419216000
_diffrn_orient_matrix_UB_32      -0.0227234000
_diffrn_orient_matrix_UB_33      -0.0993605000
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32941
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.832
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         9935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9436
_reflns_number_total             9935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04074c2.cif
_cod_data_source_block           s5984r
_cod_depositor_comments
'Adding full bibliography for 7712250--7712254.cif.'
_cod_original_cell_volume        2477.18(11)
_cod_database_code               7712254
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.539
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C6(H6), C20(H20), C17(H17), C28(H28), C10(H10), C32(H32), C31(H31),
 C18(H18), C29(H29), C9(H9), C7(H7)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C13(H13A,H13B,
 H13C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C), C15(H15A,
 H15B,H15C), C22(H22A,H22B,H22C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C3(H3A,H3B,
 H3C)
;
_shelx_res_checksum              45106
_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 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.755