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_7712252
_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         'C39 H60 Ge3 N3 O3 P7'
_chemical_formula_sum            'C39 H60 Ge3 N3 O3 P7'
_chemical_formula_weight         1053.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 94.2470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6729(2)
_cell_length_b                   20.5725(3)
_cell_length_c                   15.8849(2)
_cell_measurement_reflns_used    19305
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.7200
_cell_measurement_theta_min      2.0720
_cell_volume                     4781.82(11)
_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    'SHELXS  (Sheldrick, 2008)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.961
_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    -45.00 133.00   1.00    1.00    --   43.34  20.00-120.00  178
  2  \w     24.00 104.00   1.00    1.00    --   45.86  40.00-180.00   80
  3  \w     67.00 134.00   1.00    1.00    --   45.86  50.00-150.00   67
  4  \w    -23.00   3.00   1.00    1.00    --   45.86  40.00-180.00   26
  5  \w     33.00  60.00   1.00    1.00    --  108.20  50.00 120.00   27
  6  \w     21.00  46.00   1.00    1.00    --  108.20  30.00 150.00   25
  7  \w     20.00 142.00   1.00    1.00    --  108.20  50.00 150.00  122
  8  \w     89.00 137.00   1.00    1.00    --  108.20  50.00-180.00   48
  9  \w     94.00 196.00   1.00    1.00    --  108.20  30.00 150.00  102
 10  \w    152.00 195.00   1.00    1.00    --  108.20  50.00-180.00   43
 11  \w    150.00 198.00   1.00    1.00    --  108.20  50.00 150.00   48
 12  \w    135.00 191.00   1.00    1.00    --  108.20  50.00 120.00   56
 13  \w     84.00 198.00   1.00    1.00    --  108.20  20.00 -30.00  114
 14  \w    154.00 179.00   1.00    1.00    --  108.20  30.00-150.00   25
 15  \w     19.00  74.00   1.00    1.00    --  108.20  20.00 -30.00   55
;
_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      0.0930511000
_diffrn_orient_matrix_UB_12      -0.0345560000
_diffrn_orient_matrix_UB_13      0.0133234000
_diffrn_orient_matrix_UB_21      -0.0444917000
_diffrn_orient_matrix_UB_22      -0.0639337000
_diffrn_orient_matrix_UB_23      -0.0326634000
_diffrn_orient_matrix_UB_31      0.0213436000
_diffrn_orient_matrix_UB_32      0.0179474000
_diffrn_orient_matrix_UB_33      -0.0906233000
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29680
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.240
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46343
_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    1.463
_exptl_crystal_description       plank
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9613
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0274P)^2^+12.5994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9318
_reflns_number_total             9613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04074c2.cif
_cod_data_source_block           s5953l
_cod_depositor_comments
'Adding full bibliography for 7712250--7712254.cif.'
_cod_database_code               7712252
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.482
_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
 Ge3-N6 \\sim Ge3A-N6
 with sigma of 0.02
 C38A-C2 \\sim C38-C2A
 with sigma of 0.002
 C1-C2 \\sim C1A-C2A
 with sigma of 0.04
 Ge3-C2 \\sim Ge3A-C2A
 with sigma of 0.04
 Ge3-C1 \\sim Ge3A-C1A
 with sigma of 0.02
 N6-C2 \\sim N6-C2A
 with sigma of 0.04
 C1-C37 \\sim C1A-C37A
 with sigma of 0.02
 Ge3-C37 \\sim Ge3A-C37A
 with sigma of 0.04
 N6-C1 \\sim N6-C1A
 with sigma of 0.04
 C36-C3 \\sim C3A-C36A
 with sigma of 0.002
 Ge3-C3 \\sim Ge3A-C3A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C38A \\sim C2A \\sim C2 \\sim C38: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C4A \\sim C39A \\sim C39: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C4A \\sim C39 \\sim C39A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C39 \\sim C39A \\sim C4A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C3 \\sim C36 \\sim C3A \\sim C36A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Ge3A \\sim Ge3: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Rigid body (RIGU) restrains
 Ge3, C1, C2, C36, C37, C38, Ge3A, C38A, C2A, C1A, C37A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C36A, C3, C36, C3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(Ge3A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
 Sof(Ge3)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=FVAR(2)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B), C9(H9A,H9B), C4(H4A,
 H4B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C4A(H4AA,H4AB), C2A(H2AA,H2AB),
 C1A(H1AA,H1AB), C3A(H3AA,H3AB)
6.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C29(H29A,H29B,
 H29C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F),
 C37A(H37D,H37E,H37F), C36A(H36D,H36E,H36F)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23),
 C27(H27), C28(H28), C30(H30), C32(H32), C33(H33), C21(H21), C22(H22), C24(H24)
;
_shelx_res_checksum              13881
_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 2.410
_oxdiff_exptl_absorpt_empirical_full_min 0.661