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_7712253
_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 Ge3 N3 O9 P7 S3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C35 H53 Ge3 N3 O9.5 P7 S3'
_chemical_formula_weight         1198.54
_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             2021-10-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                73.987(2)
_cell_angle_beta                 87.041(2)
_cell_angle_gamma                89.564(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2603(3)
_cell_length_b                   13.7420(3)
_cell_length_c                   14.7414(3)
_cell_measurement_reflns_used    23456
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.8810
_cell_measurement_theta_min      3.0520
_cell_volume                     2578.49(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.943
_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     41.00 107.00   1.00    1.00    --   43.53  50.00 -30.00   66
  2  \w    -45.00   6.00   1.00    1.00    --   43.53  60.00-150.00   51
  3  \w     93.00 133.00   1.00    1.00    --   43.53  60.00-150.00   40
  4  \w    -44.00 133.00   1.00    1.00    --   43.53  60.00  90.00  177
  5  \w      9.00  51.00   1.00    1.00    --   46.07  60.00 -60.00   42
  6  \w    -43.00 135.00   1.00    1.00    --   46.07  60.00  30.00  178
  7  \w     96.00 134.00   1.00    1.00    --   46.07  60.00 -60.00   38
  8  \w    -42.00  -7.00   1.00    1.00    --   46.07  60.00 -60.00   35
  9  \w     19.00  92.00   1.00    1.00    --  108.20  50.00-150.00   73
 10  \w    120.00 198.00   1.00    1.00    --  108.20  50.00-120.00   78
 11  \w    148.00 197.00   1.00    1.00    --  108.20  50.00  90.00   49
 12  \w    120.00 198.00   1.00    1.00    --  108.20  50.00   0.00   78
 13  \w     44.00  87.00   1.00    1.00    --  108.20  50.00 -60.00   43
 14  \w    103.00 128.00   1.00    1.00    --  108.20  50.00 -60.00   25
 15  \w    106.00 132.00   1.00    1.00    --  108.20  50.00  90.00   26
 16  \w     53.00  91.00   1.00    1.00    --  108.20  50.00  90.00   38
 17  \w     70.00  96.00   1.00    1.00    --  108.20  50.00   0.00   26
 18  \w     20.00 187.00   1.00    1.00    --  108.20  50.00  60.00  167
 19  \w    136.00 197.00   1.00    1.00    --  108.20  50.00 -60.00   61
 20  \w     19.00 198.00   1.00    1.00    --  108.20  50.00 150.00  179
 21  \w     24.00 191.00   1.00    1.00    --  108.20  10.00 -30.00  167
 22  \w     83.00 113.00   1.00    1.00    --  108.20  50.00-120.00   30
 23  \w    103.00 197.00   1.00    1.00    --  108.20  50.00-150.00   94
 24  \w    140.00 167.00   1.00    1.00    --  108.20  50.00 120.00   27
 25  \w     22.00  47.00   1.00    1.00    --  108.20  50.00   0.00   25
 26  \w    126.00 169.00   1.00    1.00    --  108.20  50.00 -90.00   43
 27  \w    142.00 168.00   1.00    1.00    --  108.20  50.00 -30.00   26
 28  \w    145.00 170.00   1.00    1.00    --  108.20  50.00  30.00   25
 29  \w     31.00  57.00   1.00    1.00    --  108.20  50.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0207985000
_diffrn_orient_matrix_UB_12      0.1112925000
_diffrn_orient_matrix_UB_13      -0.0031149000
_diffrn_orient_matrix_UB_21      -0.0584793000
_diffrn_orient_matrix_UB_22      -0.0346776000
_diffrn_orient_matrix_UB_23      0.0965960000
_diffrn_orient_matrix_UB_31      0.0983958000
_diffrn_orient_matrix_UB_32      0.0038675000
_diffrn_orient_matrix_UB_33      0.0501190000
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32445
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.409
_diffrn_reflns_theta_min         3.123
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
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    1.544
_exptl_crystal_description       plank
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.131
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10226
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0300
_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/[\s^2^(Fo^2^)+(0.0355P)^2^+3.1773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9771
_reflns_number_total             10226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04074c2.cif
_cod_data_source_block           s5950l
_cod_depositor_comments
'Adding full bibliography for 7712250--7712254.cif.'
_cod_original_formula_sum        'C35 H53 Ge3 N3 O9.50 P7 S3'
_cod_database_code               7712253
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.320
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O14-C1B
 1.41 with sigma of 0.02
 C1C-C1D
 1.5 with sigma of 0.02
 O14-C1C
 1.42 with sigma of 0.02
 C1A-C1B
 1.48 with sigma of 0.02
 O14-C1A = O14-C1D
 2.37 with sigma of 0.04
 C17-C22 \\sim C17-C22A
 with sigma of 0.02
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20
 with sigma of 0.02
 C17-C21 \\sim C17-C21A
 with sigma of 0.04
 C20-C21 \\sim C20-C21A
 with sigma of 0.02
 C20-C22 \\sim C20-C22A
 with sigma of 0.04
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C22 \\sim C23 \\sim C21 \\sim C18A
\\sim C22A \\sim C21A \\sim C19A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
C19 \\sim C19A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Rigid body (RIGU) restrains
 C1B, O14, C1C, C1A, C1D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C18A)=Sof(H18A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=Sof(C19A)=
 Sof(H19A)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C22)=Sof(H22)=Sof(C21)=Sof(H21)=FVAR(1)
 Fixed Sof: O14(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB)
6.b Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C28(H28), C7(H7), C18(H18), C29(H29), C11(H11), C19(H19),
 C8(H8), C10(H10), C22(H22), C21(H21), C18A(H18A), C22A(H22A), C21A(H21A),
 C19A(H19A)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              27896
_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.732