Synthesis and structural trends in a series of simple tetraalkylphosphonium salts
Gawraczyński, Jakub; Leszczyński, Piotr J.; Cyrański, Michał K.; Dobrzycki, Łukasz; Koźmiński, Wiktor; Fijałkowski, Karol J.; Grochala, Wojciech; Jaroń, Tomasz; CrystEngComm 26 (2024) 2673–2682; doi:10.1039/D4CE00210E

data_7248506
_publ_section_title
;
 Synthesis and structural trends in a series of simple
 tetraalkylphosphonium salts
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              2673
_journal_page_last               2682
_journal_paper_doi               10.1039/D4CE00210E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C4 H12 P, Al C16 F36 O4'
_chemical_formula_sum            'C20 H12 Al F36 O4 P'
_chemical_formula_weight         1058.214
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_Int_Tables_number      82
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4285(2)
_cell_length_b                   13.4285(2)
_cell_length_c                   9.4154(2)
_cell_measurement_reflns_used    5940
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4690
_cell_measurement_theta_min      4.6210
_cell_volume                     1697.83(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2687
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9979
_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     34.00  81.00   1.00    2.00    --   41.56 -99.00 150.00   47
  2  \w     10.00  87.00   1.00    2.00    --   41.56  77.00  30.00   77
  3  \w     34.00  81.00   1.00    2.00    --   41.56 -99.00-150.00   47
  4  \w     10.00  87.00   1.00    2.00    --   41.56  77.00-120.00   77
  5  \w     34.00  81.00   1.00    2.00    --   41.56 -99.00 120.00   47
  6  \w     18.00 114.00   1.00    2.00    --   41.56  38.00 -30.00   96
  7  \w     89.00 146.00   1.00    7.80    --  109.50 178.00 -60.00   57
  8  \w     84.00 158.00   1.00    7.80    --  109.50  45.00  30.00   74
  9  \w     80.00 158.00   1.00    7.80    --  109.50  67.00  42.75   78
 10  \w     89.00 146.00   1.00    7.80    --  109.50 178.00-180.00   57
 11  \w     82.00 158.00   1.00    7.80    --  109.50  58.00 114.51   76
 12  \w     81.00 158.00   1.00    7.80    --  109.50  61.00  30.00   77
 13  \w     89.00 146.00   1.00    7.80    --  109.50 178.00  60.00   57
 14  \w     89.00 146.00   1.00    7.80    --  109.50 178.00   0.00   57
 15  \w     39.00 138.00   1.00    7.80    --  109.50 -61.00  90.00   99
 16  \w     89.00 146.00   1.00    7.80    --  109.50 178.00  90.00   57
 17  \w     82.00 114.00   1.00    7.80    --  109.50  61.00   0.00   32
 18  \w     86.00 148.00   1.00    7.80    --  109.50  45.00 -90.00   62
 19  \w    117.00 150.00   1.00    7.80    --  109.50  15.00  90.00   33
 20  \w    126.00 158.00   1.00    7.80    --  109.50  65.00 -15.97   32
 21  \w     80.00 114.00   1.00    7.80    --  109.50  65.00 -15.97   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0504034000
_diffrn_orient_matrix_UB_12      0.0940434000
_diffrn_orient_matrix_UB_13      0.0600398000
_diffrn_orient_matrix_UB_21      -0.0973865000
_diffrn_orient_matrix_UB_22      -0.0587812000
_diffrn_orient_matrix_UB_23      0.0208400000
_diffrn_orient_matrix_UB_31      0.0336126000
_diffrn_orient_matrix_UB_32      -0.0292106000
_diffrn_orient_matrix_UB_33      0.1508814000
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6778
_diffrn_reflns_point_group_measured_fraction_full 0.9935
_diffrn_reflns_point_group_measured_fraction_max 0.9737
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.83
_diffrn_reflns_theta_min         4.66
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.186
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_description       block
_exptl_crystal_F_000             1039.676
_exptl_crystal_recrystallization_method
'Crystallized from water and acetone mixture (0.85:0.15 by volume) via acetone evaporation.'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.5519
_refine_diff_density_min         -0.2888
_refine_diff_density_rms         0.0672
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_d_res_high            0.7951
_refine_ls_d_res_low             9.4954
_refine_ls_goodness_of_fit_ref   1.0428
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0428
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+2.4011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.946
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              11
_reflns_limit_l_min              -11
_reflns_number_gt                1717
_reflns_number_total             1737
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00210e2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7248499--7248509.cif.'
_cod_original_sg_symbol_Hall     ' I -4'
_cod_database_code               7248506
_chemical_oxdiff_formula         'C20 H12 F36 P O4 Al'
_chemical_oxdiff_usercomment     TJ405
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C00E(H00a,H00b,H00c)
;
_olex2_exptl_crystal_mounting_method loop
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.712