Substituted aromatic pentaphosphole ligands ‒ a journey across the p-block
Riesinger, Christoph; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC04296C

data_1564644
_publ_section_title
;
 Substituted aromatic pentaphosphole ligands -- a journey across the
 p-block
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04296C
_journal_year                    2021
_chemical_formula_moiety         'C38 H58 B Br2 O4 P8 Ta2, Al C16 F36 O4'
_chemical_formula_sum            'C54 H58 Al B Br2 F36 O8 P8 Ta2'
_chemical_formula_weight         2326.27
_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             2021-07-21
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                73.344(2)
_cell_angle_beta                 86.2377(16)
_cell_angle_gamma                85.9405(15)
_cell_formula_units_Z            2
_cell_length_a                   10.70454(17)
_cell_length_b                   17.1553(4)
_cell_length_c                   22.3411(6)
_cell_measurement_reflns_used    38951
_cell_measurement_temperature    122.93(19)
_cell_measurement_theta_max      74.3670
_cell_measurement_theta_min      4.5130
_cell_volume                     3916.30(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.93(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -88.00  -9.00   0.50    4.00    --  -45.15 125.00 150.00  158
  2  \w     -4.00  30.00   0.50    4.00    --  -45.15  19.00 -60.00   68
  3  \w     -5.00  22.00   0.50    4.00    --  -45.15  19.00 150.00   54
  4  \w     -3.00  28.00   0.50    4.00    --  -45.15  19.00  90.00   62
  5  \w     -5.00  31.00   0.50    4.00    --  -45.15  19.00  60.00   72
  6  \w     21.00 115.00   0.50    4.00    --   45.15  57.00 -30.00  188
  7  \w     35.00  72.00   0.50    4.00    --   45.15-125.00  90.00   74
  8  \w     50.00  76.00   0.50   16.00    --  104.50-125.00-120.00   52
  9  \w     36.00 112.00   0.50   16.00    --  104.50-125.00-180.00  152
 10  \w     38.00  66.00   0.50   16.00    --  104.50 -45.00 -60.00   56
 11  \w     76.00 112.00   0.50   16.00    --  104.50-125.00  90.00   72
 12  \w    127.00 166.00   0.50   16.00    --  104.50  30.00  60.00   78
 13  \w     97.00 123.00   0.50   16.00    --  104.50 125.00 -60.00   52
 14  \w     78.00 112.00   0.50   16.00    --  104.50-125.00-120.00   68
 15  \w     33.00  60.00   0.50   16.00    --  104.50-125.00  90.00   54
 16  \w     90.00 116.00   0.50   16.00    --  104.50 -77.00 -90.00   52
 17  \w     36.00  70.00   0.50   16.00    --  104.50 -45.00  60.00   68
 18  \w     38.00  80.00   0.50   16.00    --  104.50 -77.00 -90.00   84
 19  \w     72.00 112.00   0.50   16.00    --  104.50-125.00  60.00   80
 20  \w    133.00 159.00   0.50   16.00    --  104.50  15.00 -90.00   52
 21  \w    106.00 161.00   0.50   16.00    --  104.50 125.00-120.00  110
 22  \w     33.00  58.00   0.50   16.00    --  104.50-125.00  30.00   50
 23  \w     76.00 112.00   0.50   16.00    --  104.50-125.00  30.00   72
 24  \w     85.00 111.00   0.50   16.00    --  104.50  30.00  60.00   52
 25  \w     99.00 132.00   0.50   16.00    --  104.50  30.00  90.00   66
 26  \w    131.00 165.00   0.50   16.00    --  104.50 125.00 -30.00   68
 27  \w    132.00 167.00   0.50   16.00    --  104.50  45.00 -60.00   70
 28  \w    135.00 165.00   0.50   16.00    --  104.50 125.00 -60.00   60
 29  \w     75.00 111.00   0.50   16.00    --  104.50-125.00 120.00   72
 30  \w     85.00 170.00   0.50   16.00    --  104.50  45.00 -90.00  170
 31  \w     74.00 110.00   0.50   16.00    --  104.50-125.00 150.00   72
 32  \w     34.00  83.00   0.50   16.00    --  104.50 -77.00   0.00   98
 33  \w     36.00  62.00   0.50   16.00    --  104.50-125.00 150.00   52
 34  \w     39.00  72.00   0.50   16.00    --  104.50 -45.00 -90.00   66
 35  \w     64.00  94.00   0.50   16.00    --  104.50 -94.00 -90.00   60
 36  \w    144.00 170.00   0.50   16.00    --  104.50 125.00 -90.00   52
 37  \w     76.00 112.00   0.50   16.00    --  104.50-125.00-150.00   72
 38  \w     39.00  67.00   0.50   16.00    --  104.50-125.00  60.00   56
 39  \w    100.00 134.00   0.50   16.00    --  104.50 125.00 -90.00   68
 40  \w     73.00 127.00   0.50   16.00    --  104.50  15.00 -90.00  108
 41  \w     31.00  58.00   0.50   16.00    --  104.50 -94.00 -90.00   54
 42  \w     88.00 168.00   0.50   16.00    --  104.50  45.00-180.00  160
 43  \w     38.00  63.00   0.50   16.00    --  104.50 -77.00  30.00   50
 44  \w     72.00  98.00   0.50   16.00    --  104.50 -77.00  30.00   52
 45  \w     40.00  73.00   0.50   16.00    --  104.50-125.00   0.00   66
 46  \w     85.00 112.00   0.50   16.00    --  104.50-125.00   0.00   54
 47  \w    103.00 129.00   0.50   16.00    --  104.50  30.00   0.00   52
 48  \w     29.00  56.00   0.50   16.00    --  104.50 -94.00-150.00   54
 49  \w     79.00 105.00   0.50   16.00    --  104.50 -94.00-150.00   52
 50  \w     34.00  72.00   0.50   16.00    --  104.50 -94.00-120.00   76
 51  \w     42.00  67.00   0.50   16.00    --  104.50 -61.00  30.00   50
 52  \w     46.00  89.00   0.50   16.00    --  104.50 -61.00 -90.00   86
 53  \w     35.00  61.00   0.50   16.00    --  104.50 -61.00  60.00   52
 54  \w     98.00 129.00   0.50   16.00    --  104.50  45.00 -60.00   62
 55  \w     74.00 108.00   0.50   16.00    --  104.50-105.00-104.65   68
 56  \w     43.00  69.00   0.50   16.00    --  104.50-105.00-104.65   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0829071000
_diffrn_orient_matrix_UB_12      0.0369426000
_diffrn_orient_matrix_UB_13      0.0450950000
_diffrn_orient_matrix_UB_21      0.0217316000
_diffrn_orient_matrix_UB_22      0.0862107000
_diffrn_orient_matrix_UB_23      -0.0431754000
_diffrn_orient_matrix_UB_31      -0.1162645000
_diffrn_orient_matrix_UB_32      -0.0038875000
_diffrn_orient_matrix_UB_33      -0.0359810000
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.898
_diffrn_reflns_theta_min         3.832
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.149
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.193
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       rods
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.067
_refine_diff_density_max         3.643
_refine_diff_density_min         -5.026
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         15822
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0942P)^2^+55.6010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14586
_reflns_number_total             15822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr386_cua_ap_abs_ana
_cod_original_cell_volume        3916.28(15)
_cod_database_code               1564644
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C54H58AlBBr2F36O8P8Ta2
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.130
_olex2_refinement_description
;
1. Restrained distances
 F13B-C45B = F15B-C45B = F14B-C45B
 1.35 with sigma of 0.02
 C45B-C43B = C46B-C43B = C44B-C43B
 1.55 with sigma of 0.02
 F13A-C45A = F14A-C45A = F15A-C45A
 1.35 with sigma of 0.02
 Br2A-B1A \\sim Br2B-B1B \\sim Br1B-B1B \\sim Br1A-B1A
 with sigma of 0.02
 P1-B1B \\sim P1-B1A \\sim P5-B1B \\sim P5-B1A
 with sigma of 0.02
 F3A-C40A \\sim F1A-C40A \\sim F2A-C40A
 with sigma of 0.02
 F3B-F1B \\sim F1B-F2B \\sim F2B-F3B
 with sigma of 0.02
 F4B-C41B \\sim F5B-C41B \\sim F6B-C41B
 with sigma of 0.02
 C40B-C39 \\sim C41B-C39 \\sim C42B-C39
 with sigma of 0.02
 Al1-O5A \\sim Al1-O5B
 with sigma of 0.02
 F6B-C41B \\sim F8A-C42A
 with sigma of 0.02
 F2B-C40B \\sim F3B-C40B \\sim F1B-C40B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O6B \\sim C43A \\sim C43B \\sim C46B \\sim C44B \\sim C45B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C21 \\sim O4: within 2.3A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2.3A
Br1B \\sim Br1A \\sim Br2A \\sim Br2B: within 2.2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2.2A
F15B \\sim C45B \\sim F13B \\sim F14B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
B1A \\sim B1B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F17B \\sim F18B \\sim C46B \\sim F16B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F11B \\sim C44B \\sim F12B \\sim F10B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C40B \\sim F2B \\sim F1B \\sim F3B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F1A \\sim F9B \\sim F7B \\sim C42B \\sim F8B: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
F4B \\sim F5B \\sim C41B \\sim F6B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C40B \\sim C39 \\sim C41A \\sim C41B \\sim C42A \\sim C42B \\sim C40A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O5B \\sim O5A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C40A \\sim F3A \\sim F1A \\sim F2A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
3. Others
 Fixed Sof: Br1A(0.94) Br2A(0.94) F8A(0.72) F14A(0.86) F1A(0.72) F16A(0.86)
 F9A(0.72) F15A(0.86) F17A(0.86) F18A(0.86) O5A(0.72) O6A(0.86) F11A(0.86)
 F5A(0.72) F10A(0.86) F12A(0.86) F13A(0.86) F2A(0.72) F6A(0.72) F7A(0.72)
 F3A(0.72) F4A(0.72) C43A(0.86) C46A(0.86) C45A(0.86) C42A(0.72) C44A(0.86)
 C40A(0.72) C41A(0.72) Br1B(0.06) Br2B(0.06) O5B(0.28) C40B(0.28) F3B(0.28)
 F1B(0.28) F2B(0.28) C42B(0.28) F8B(0.28) F9B(0.28) F7B(0.28) C41B(0.28)
 F6B(0.28) F4B(0.28) F5B(0.28) B1A(0.94) B1B(0.06) O6B(0.14) C43B(0.14)
 C44B(0.14) F12B(0.14) F10B(0.14) F11B(0.14) C46B(0.14) F17B(0.14) F18B(0.14)
 F16B(0.14) C45B(0.14) F13B(0.14) F14B(0.14) F15B(0.14)
4.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C5(H5), C7(H7), C26(H26)
4.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C34(H34A,H34B,
 H34C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C),
 C38(H38A,H38B,H38C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C15(H15A,H15B,H15C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              23511
_shelx_hkl_checksum              68311
_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 2.088
_oxdiff_exptl_absorpt_empirical_full_min 0.536