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_7712250
_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         'C30 H75 As11 Ge5'
_chemical_formula_sum            'C30 H75 As11 Ge5'
_chemical_formula_weight         1622.97
_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             2022-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                85.802(3)
_cell_angle_beta                 84.724(3)
_cell_angle_gamma                82.011(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6695(3)
_cell_length_b                   14.0092(6)
_cell_length_c                   24.6674(7)
_cell_measurement_reflns_used    7278
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9940
_cell_measurement_theta_min      1.7920
_cell_volume                     2608.60(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_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      100.00(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 0.952
_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  45.00   1.00    3.00    --  -44.41  76.00 150.00   26
  2  \w    -73.00 -33.00   1.00    3.00    --  -44.41  76.00 150.00   40
  3  \w    -56.00  19.00   1.00    3.00    --  -44.41  57.00 -60.00   75
  4  \w    -78.00 -15.00   1.00    3.00    --  -46.39  57.00 120.00   63
  5  \w    -76.00  15.00   1.00    3.00    --  -46.39  76.00 -30.00   91
  6  \w   -131.00 -12.00   1.00    3.00    --  -46.39 -38.00 150.00  119
  7  \w    -56.00 -25.00   1.00   10.00    -- -107.20  76.00 -30.00   31
  8  \w   -195.00 -69.00   1.00   10.00    -- -107.20 -38.00   0.00  126
  9  \w   -145.00 -43.00   1.00   10.00    -- -107.20  76.00 -60.00  102
 10  \w   -192.00-114.00   1.00   10.00    -- -107.20 -38.00  30.00   78
 11  \w   -189.00 -72.00   1.00   10.00    -- -107.20 -38.00 -90.00  117
 12  \w   -123.00 -96.00   1.00   10.00    -- -107.20  76.00  60.00   27
 13  \w   -120.00 -62.00   1.00   10.00    -- -107.20  76.00 -30.00   58
 14  \w   -135.00 -85.00   1.00   10.00    -- -107.20  76.00 120.00   50
 15  \w   -122.00 -20.00   1.00   10.00    -- -107.20  76.00-120.00  102
 16  \w   -119.00 -85.00   1.00   10.00    -- -107.20  76.00-180.00   34
 17  \w   -116.00 -90.00   1.00   10.00    -- -107.20  57.00 150.00   26
 18  \w    -87.00 -18.00   1.00   10.00    -- -107.20  57.00 150.00   69
 19  \w   -131.00-102.00   1.00   10.00    -- -107.20  76.00 -90.00   29
 20  \w    -74.00 -47.00   1.00   10.00    -- -107.20  76.00 -90.00   27
 21  \w   -197.00-142.00   1.00   10.00    -- -107.20 -57.00  90.00   55
 22  \w   -105.00 -65.00   1.00   10.00    -- -107.20  76.00  30.00   40
 23  \w   -142.00 -26.00   1.00   10.00    -- -107.20  76.00  90.00  116
 24  \w   -188.00-104.00   1.00   10.00    -- -107.20 -38.00 -60.00   84
;
_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      -0.0700180000
_diffrn_orient_matrix_UB_12      0.0610634000
_diffrn_orient_matrix_UB_13      -0.0498615000
_diffrn_orient_matrix_UB_21      -0.0307975000
_diffrn_orient_matrix_UB_22      -0.0925952000
_diffrn_orient_matrix_UB_23      -0.0257043000
_diffrn_orient_matrix_UB_31      -0.1886219000
_diffrn_orient_matrix_UB_32      0.0084179000
_diffrn_orient_matrix_UB_33      0.0282994000
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.363
_diffrn_reflns_theta_min         1.802
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    11.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    2.066
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10433
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0853P)^2^+4.8257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7389
_reflns_number_total             10433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04074c2.cif
_cod_data_source_block           s6098r
_cod_depositor_comments
'Adding full bibliography for 7712250--7712254.cif.'
_cod_database_code               7712250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.347
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C33
 1.5 with sigma of 0.02
 C33-C15
 1.5 with sigma of 0.02
 Ge2-C8 \\sim Ge2-C8A
 with sigma of 0.02
 C8-C38 \\sim C8A-C38A
 with sigma of 0.02
 Ge2-C38 \\sim Ge2-C38A
 with sigma of 0.04
 Ge4-C35 \\sim Ge4-C35A
 with sigma of 0.02
 C35-C43 \\sim C35A-C43A
 with sigma of 0.02
 Ge5-C45 \\sim Ge5-C45A
 with sigma of 0.02
 Ge4-C43 \\sim Ge4-C43A
 with sigma of 0.04
 Ge1-C19 \\sim Ge1-C19A
 with sigma of 0.02
 C19-C42 \\sim C19A-C42A
 with sigma of 0.02
 C24-C45 \\sim C24A-C45A
 with sigma of 0.02
 Ge1-C42 \\sim Ge1-C42A
 with sigma of 0.04
 Ge5-C24 \\sim Ge5-C24A
 with sigma of 0.04
 Ge5-C15 \\sim Ge5-C15A
 with sigma of 0.02
 C15-C33 \\sim C15A-C33A
 with sigma of 0.02
 Ge5-C33 \\sim Ge5-C33A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C45A \\sim C45 \\sim C24 \\sim C24A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C15A \\sim C15 \\sim C33A \\sim C33: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C43 \\sim C35 \\sim C35A \\sim C43A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C19A \\sim C19 \\sim C42A \\sim C42: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C8A \\sim C8: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C8) = Uanis(C8A)
4. Rigid body (RIGU) restrains
 C19A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24A, C45A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15A, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(2)
 Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(3)
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(4)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(4)
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(5)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C45)=Sof(H45A)=Sof(H45B)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C13(H13A,H13B), C15(H15A,H15B),
 C18(H18A,H18B), C19(H19A,H19B), C35(H35A,H35B), C45(H45A,H45B), C8A(H8AA,H8AB),
  C35A(H35C,H35D), C19A(H19C,H19D), C15A(H15C,H15D), C45A(H45C,H45D)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C38A(H38D,H38E,H38F), C43A(H43D,H43E,H43F), C42A(H42D,H42E,H42F),
 C33A(H33D,H33E,H33F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              30507
_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 2.433
_oxdiff_exptl_absorpt_empirical_full_min 0.552