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_7712251
_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 H42 Ge3 N3 O3 P7, C2.5 H2.5 N0.5'
_chemical_formula_sum            'C32.5 H44.5 Ge3 N3.5 O3 P7'
_chemical_formula_weight         966.77
_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
_audit_creation_date             2021-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.9510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.93920(10)
_cell_length_b                   20.9710(2)
_cell_length_c                   18.2317(2)
_cell_measurement_reflns_used    13788
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4370
_cell_measurement_theta_min      3.1720
_cell_volume                     4182.46(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.938
_diffrn_measured_fraction_theta_max 0.891
_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      2.00  44.00   1.00    1.00    --  -43.99  34.00  89.00   42
  2  \w    -92.00 -67.00   1.00    1.00    --  -43.99 -34.00 -68.00   25
  3  \w    -60.00  -4.00   1.00    1.00    --  -43.99  34.00  89.00   56
  4  \w   -115.00 -70.00   1.00    1.00    --  -46.21 -34.00 -68.00   45
  5  \w    -89.00 -62.00   1.00    1.00    -- -107.20  34.00  89.00   27
  6  \w   -168.00 -70.00   1.00    1.00    -- -107.20 -34.00 -68.00   98
  7  \w      5.00  30.00   1.00    1.00    --    5.00  34.00  89.00   25
  8  \w   -132.00 -12.00   1.00    1.00    --  -43.99 -57.00-150.00  120
  9  \w   -148.00 -23.00   1.00    1.00    -- -107.20  37.00 -60.00  125
 10  \w   -103.00 -22.00   1.00    1.00    -- -107.20  57.00  30.00   81
 11  \w   -108.00 -79.00   1.00    1.00    -- -107.20  57.00-120.00   29
 12  \w   -129.00 -30.00   1.00    1.00    -- -107.20  57.00 -60.00   99
;
_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      0.1260860000
_diffrn_orient_matrix_UB_12      0.0061916000
_diffrn_orient_matrix_UB_13      -0.0367102000
_diffrn_orient_matrix_UB_21      -0.0184034000
_diffrn_orient_matrix_UB_22      0.0726141000
_diffrn_orient_matrix_UB_23      -0.0065331000
_diffrn_orient_matrix_UB_31      0.0596904000
_diffrn_orient_matrix_UB_32      0.0093437000
_diffrn_orient_matrix_UB_33      0.0758919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19585
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.884
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0430P)^2^+5.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7327
_reflns_number_total             7766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04074c2.cif
_cod_data_source_block           s5961r
_cod_depositor_comments
'Adding full bibliography for 7712250--7712254.cif.'
_cod_original_formula_sum        'C32.50 H44.50 Ge3 N3.50 O3 P7'
_cod_database_code               7712251
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P N O'
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.435
_diffrn_oxdiff_digest_frames
;
01852a298a5c9f582c02d593b74a51bfb700772ff84
;
_diffrn_oxdiff_digest_hkl
;
010413becc803543a55eb050db4a97f940b589
;
_reflns_odcompleteness_completeness 93.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Shared sites
{N4, C32}
3. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(C32)
4. Others
 Fixed Sof: C32(0.5) H32(0.5) H31(0.5) H31A(0.5) H33(0.5) H33A(0.5) N4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C16(H16), C28(H28), C10(H10), C17(H17), C9(H9), C26(H26),
 C20(H20), C7(H7), C19(H19), C8(H8), C6(H6), C18(H18), C27(H27), C32(H32),
 C31(H31), C31(H31A), C33(H33), C33(H33A)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C),
  C12(H12A,H12B,H12C)
;
_shelx_res_checksum              63314
_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 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.779