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_7131937
_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         'C36 H56 I O2 P4 Sb Ta, Al C16 F36 O4'
_chemical_formula_sum            'C52 H58 Al F36 I O6 P4 Sb Ta'
_chemical_formula_weight         2043.44
_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                109.867(3)
_cell_angle_beta                 91.228(3)
_cell_angle_gamma                98.222(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6596(4)
_cell_length_b                   16.9425(5)
_cell_length_c                   21.4058(7)
_cell_measurement_reflns_used    13446
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.8120
_cell_measurement_theta_min      4.1020
_cell_volume                     3588.2(2)
_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      123.00(10)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     19.00 114.00   1.00    7.50    --   44.62  57.00-150.00   95
  2  \w    -25.00  70.00   1.00    7.50    --   44.62 -57.00  60.00   95
  3  \w    -21.00  76.00   1.00    7.50    --   44.62 -77.00 -60.00   97
  4  \w     34.00  72.00   1.00   30.00    --  104.50 -45.00-150.00   38
  5  \w     31.00 112.00   1.00   30.00    --  104.50-125.00-180.00   81
  6  \w     21.00 107.00   1.00   30.00    --  104.50 -94.00   0.00   86
  7  \w     31.00  57.00   1.00   30.00    --  104.50 -30.00-180.00   26
  8  \w    103.00 178.00   1.00   30.00    --  104.50  77.00-180.00   75
  9  \w     21.00 107.00   1.00   30.00    --  104.50 -94.00-150.00   86
 10  \w     31.00 112.00   1.00   30.00    --  104.50-125.00 120.00   81
 11  \w     25.00 178.00   1.00   30.00    --  104.50   0.00   0.00  153
 12  \w     24.00 107.00   1.00   30.00    --  104.50-101.00 -45.17   83
 13  \w   -114.00 -19.00   1.00    7.50    --  -44.62 -57.00  60.00   95
 14  \w     12.00  42.00   1.00    7.50    --   44.62  80.00  10.96   30
 15  \w     13.00  42.00   1.00    7.50    --   44.62  77.00 -36.70   29
 16  \w     80.00 175.00   1.00   30.00    --  104.50  45.00 170.64   95
 17  \w     78.00 174.00   1.00   30.00    --  104.50  61.00  30.00   96
 18  \w     76.00 175.00   1.00   30.00    --  104.50  67.00-135.46   99
 19  \w     75.00 170.00   1.00   30.00    --  104.50  70.00 -32.37   95
 20  \w     78.00 178.00   1.00   30.00    --  104.50  30.00 120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38301
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         4.128
_exptl_absorpt_coefficient_mu    11.365
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.510
_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 intense yellow'
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.183
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0651P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9897
_reflns_number_total             12796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03369d2.cif
_cod_data_source_block           cr426_cua_abs
_cod_database_code               7131937
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 F41-C49
 1.33 with sigma of 0.02
 F43-C49
 1.33 with sigma of 0.02
 F9-C49
 1.33 with sigma of 0.02
 F17-C49
 1.33 with sigma of 0.02
 F9-F43
 2.2 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C51 \\sim C53: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C25 \\sim C13: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F21 \\sim F33: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F17 \\sim F43: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F29 \\sim F19: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F35 \\sim F11: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F37 \\sim F7: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F9 \\sim F27: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F15 \\sim F39: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F31 \\sim F5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
3. Rigid body (RIGU) restrains
 C13, F39, F11, F5
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C54, C49, F41, F2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 F17, F43, C49, C54, F41, F2, F9, F27
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 F21, F33, C51, C53
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(F9)=Sof(F37)=Sof(F19)=Sof(F39)=Sof(F5)=Sof(F41)=Sof(F21)=Sof(F43)=
 Sof(F11)=Sof(C13)=Sof(C53)=1-FVAR(1)
 Sof(F27)=Sof(F7)=Sof(F29)=Sof(F15)=Sof(F31)=Sof(F2)=Sof(F33)=Sof(F17)=
 Sof(F35)=Sof(C25)=Sof(C51)=FVAR(1)
 Fixed U11: F34(0.022339) O5(0.015738) C5(0.037049)
 Fixed U12: F34(-0.006957) O5(0.00108) C5(-0.007001)
 Fixed U13: F34(-0.012271) O5(0.008079) C5(-0.003712)
 Fixed U22: F34(0.071316) O5(0.136251) C5(0.048607)
 Fixed U23: F34(0.040541) O5(0.008718) C5(0.008961)
 Fixed U33: F34(0.124) O5(0.037) C5(0.045)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C52(H52A,H52B,
 H52C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C2(H2A,
 H2B,H2C), C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C),
 C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C23(H23A,H23B,H23C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              9614
_shelx_hkl_checksum              13360
_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
;