Ring Expansion vs. Addition – Reactivity of a cyclo-P4 Complex Towards Pnictogenium Cations
Riesinger, Christoph; Erhard, Alexander; Scheer, Manfred; Chemical Communications  (2023) –; doi:10.1039/D3CC03369D

data_7131938
_publ_section_title
;
 Ring Expansion vs. Addition -- Reactivity of a cyclo-P4 Complex Towards
 Pnictogenium Cations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03369D
_journal_year                    2023
_chemical_formula_moiety         'C42 H52 O4 P8 Sb Ta2, Al C16 F36 O4'
_chemical_formula_sum            'C58 H52 Al F36 O8 P8 Sb Ta2'
_chemical_formula_weight         2319.38
_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
_audit_creation_date             2023-03-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-10 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                111.931(2)
_cell_angle_beta                 96.332(2)
_cell_angle_gamma                90.449(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8387(3)
_cell_length_b                   17.1357(3)
_cell_length_c                   20.9703(5)
_cell_measurement_reflns_used    22606
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.5730
_cell_measurement_theta_min      3.7470
_cell_volume                     3916.65(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_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    -99.00 -22.00   1.00    5.00    --  -40.72 125.00-120.00   77
  2  \w    -99.00 -22.00   1.00    5.00    --  -40.72 125.00  60.00   77
  3  \w    -37.00  43.00   1.00    5.00    --   40.72 -38.00-180.00   80
  4  \w    -37.00  43.00   1.00    5.00    --   40.72 -38.00   0.00   80
  5  \w    -50.00 131.00   1.00    5.00    --   40.72   0.00  60.00  181
  6  \w     76.00 178.00   1.00   20.00    --  104.78  45.00  90.00  102
  7  \w     71.00 178.00   1.00   20.00    --  104.78  71.00 123.30  107
  8  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00-116.44  126
  9  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00 -87.21  126
 10  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00 104.94  126
 11  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00  -9.61  126
 12  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00-161.59  126
 13  \w     29.00  71.00   1.00   20.00    --  104.78 -61.00 -90.00   42
 14  \w     76.00 178.00   1.00   20.00    --  104.78  45.00-180.00  102
 15  \w     20.00  80.00   1.00   20.00    --  104.78 -95.00  30.00   60
 16  \w     71.00 178.00   1.00   20.00    --  104.78  30.00-120.00  107
 17  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00  60.75  126
 18  \w     25.00  84.00   1.00   20.00    --  104.78-111.00 -60.00   59
 19  \w      7.00 111.00   1.00    5.00    --   40.72  73.00 134.25  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43183
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.960
_diffrn_reflns_theta_min         3.762
_exptl_absorpt_coefficient_mu    10.640
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.27a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       plate
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1233
_refine_ls_number_reflns         15015
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13175
_reflns_number_total             15015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03369d2.cif
_cod_data_source_block           cr574_cua
_cod_database_code               7131938
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 F4-C57 = F15-C57 = F36-C57
 1.33 with sigma of 0.02
 F4-F15
 2.2 with sigma of 0.04
 F15-F36
 2.2 with sigma of 0.04
 F4-F36
 2.2 with sigma of 0.04
 F46-F35 \\sim F5-F11
 with sigma of 0.04
 F4-C57 \\sim F9-C15
 with sigma of 0.02
 F30-C55 \\sim F37-C29
 with sigma of 0.02
 F44-C55 \\sim F39-C29
 with sigma of 0.02
 F36-F15 \\sim F19-F21
 with sigma of 0.04
 F36-C57 \\sim F19-C15
 with sigma of 0.02
 F44-F29 \\sim F39-F41
 with sigma of 0.04
 F46-F17 \\sim F5-F43
 with sigma of 0.04
 F29-C55 \\sim F41-C29
 with sigma of 0.02
 F15-C48 \\sim F21-C48
 with sigma of 0.04
 F15-C57 \\sim F21-C15
 with sigma of 0.02
 F17-F35 \\sim F43-F11
 with sigma of 0.04
 F17-C7 \\sim F43-C59
 with sigma of 0.02
 C48-C55 \\sim C48-C29
 with sigma of 0.02
 F46-C7 \\sim F5-C59
 with sigma of 0.02
 F36-C48 \\sim F19-C48
 with sigma of 0.04
 C48-C57 \\sim C48-C15
 with sigma of 0.02
 F35-C7 \\sim F11-C59
 with sigma of 0.02
 F44-C48 \\sim F39-C48
 with sigma of 0.04
 F46-C48 \\sim F5-C48
 with sigma of 0.04
 F29-C48 \\sim F41-C48
 with sigma of 0.04
 F17-C48 \\sim F43-C48
 with sigma of 0.04
 F4-F36 \\sim F9-F19
 with sigma of 0.04
 F4-F15 \\sim F9-F21
 with sigma of 0.04
 C48-F35 \\sim C48-F11
 with sigma of 0.04
 F4-C48 \\sim F9-C48
 with sigma of 0.04
 F30-F44 \\sim F37-F39
 with sigma of 0.04
 F30-F29 \\sim F37-F41
 with sigma of 0.04
 C48-C7 \\sim C48-C59
 with sigma of 0.02
 F30-C48 \\sim F37-C48
 with sigma of 0.04
 F18-C27 \\sim F47-C63
 with sigma of 0.02
 F10-C25 \\sim F23-C61
 with sigma of 0.02
 F34-C53 \\sim F3-C31
 with sigma of 0.02
 F50-C27 \\sim F49-C63
 with sigma of 0.02
 F54-C46 \\sim F51-C46
 with sigma of 0.04
 F52-C27 \\sim F25-C63
 with sigma of 0.02
 F54-C53 \\sim F51-C31
 with sigma of 0.02
 F34-F33 \\sim F3-F53
 with sigma of 0.04
 F31-C25 \\sim F13-C61
 with sigma of 0.02
 F50-F52 \\sim F49-F25
 with sigma of 0.04
 F33-C53 \\sim F53-C31
 with sigma of 0.02
 C46-C25 \\sim C46-C61
 with sigma of 0.02
 C46-C53 \\sim C46-C31
 with sigma of 0.02
 C46-C27 \\sim C46-C63
 with sigma of 0.02
 F18-C46 \\sim F47-C46
 with sigma of 0.04
 F34-F54 \\sim F3-F51
 with sigma of 0.04
 F34-C46 \\sim F3-C46
 with sigma of 0.04
 F1-C25 \\sim F45-C61
 with sigma of 0.02
 F50-C46 \\sim F49-C46
 with sigma of 0.04
 F52-C46 \\sim F25-C46
 with sigma of 0.04
 F1-F10 \\sim F45-F23
 with sigma of 0.04
 F54-F33 \\sim F51-F53
 with sigma of 0.04
 F1-F31 \\sim F45-F13
 with sigma of 0.04
 F1-C46 \\sim F45-C46
 with sigma of 0.04
 F31-C46 \\sim F13-C46
 with sigma of 0.04
 F33-C46 \\sim F53-C46
 with sigma of 0.04
 F10-F31 \\sim F23-F13
 with sigma of 0.04
 F10-C46 \\sim F23-C46
 with sigma of 0.04
 F18-F50 \\sim F47-F49
 with sigma of 0.04
 F18-F52 \\sim F47-F25
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
F51 \\sim F54: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C31 \\sim C46: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(F44) = Uanis(F37)
Uanis(F23) = Uanis(F1)
Uanis(F34) = Uanis(F53)
Uanis(F25) = Uanis(F18)
3. Others
 Sof(F9)=Sof(F37)=Sof(F19)=Sof(F39)=Sof(F5)=Sof(F41)=Sof(F21)=Sof(F43)=
 Sof(F11)=Sof(C29)=Sof(C59)=Sof(C15)=1-FVAR(1)
 Sof(F4)=Sof(F30)=Sof(F36)=Sof(F44)=Sof(F46)=Sof(F29)=Sof(F15)=Sof(F17)=
 Sof(F35)=Sof(C55)=Sof(C7)=Sof(C57)=FVAR(1)
 Sof(F45)=Sof(F23)=Sof(F47)=Sof(F3)=Sof(F49)=Sof(F25)=Sof(F51)=Sof(F13)=
 Sof(F53)=Sof(C61)=Sof(C31)=Sof(C63)=1-FVAR(2)
 Sof(F1)=Sof(F10)=Sof(F18)=Sof(F34)=Sof(F50)=Sof(F52)=Sof(F54)=Sof(F31)=
 Sof(F33)=Sof(C25)=Sof(C53)=Sof(C27)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C14(H14), C20(H20), C26(H26), C30(H30), C34(H34),
 C38(H38), C42(H42), C58(H58), C62(H62), C64(H64), C2(H2), C17(H17), C11(H11)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C50(H50A,H50B,H50C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C23(H23A,
 H23B,H23C), C47(H47A,H47B,H47C), C3(H3A,H3B,H3C), C49(H49A,H49B,H49C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              83378
_shelx_hkl_checksum              85235
_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
;