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_7248504
_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         'H O4 S, C4 H12 P'
_chemical_formula_sum            'C4 H13 O4 P S'
_chemical_formula_weight         188.185
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-12 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.924(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2417(2)
_cell_length_b                   7.2041(1)
_cell_length_c                   26.6728(5)
_cell_measurement_reflns_used    4976
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.0410
_cell_measurement_theta_min      5.2660
_cell_volume                     1762.87(6)
_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      100.01(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 0.9937
_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   -116.00 -15.00   1.00    2.50    --  -41.39 -38.00-150.00  101
  2  \w   -116.00 -15.00   1.00    2.50    --  -41.39 -38.00 -60.00  101
  3  \w     34.00  82.00   1.00    2.50    --   41.39 -99.00-180.00   48
  4  \w      8.00  87.00   1.00    2.50    --   41.39  77.00 -30.00   79
  5  \w     82.00 158.00   1.00    8.00    --  109.50  45.00  60.00   76
  6  \w     43.00 108.00   1.00    8.00    --  109.50-111.00-180.00   65
  7  \w     78.00 158.00   1.00    8.00    --  109.50  30.00   0.00   80
  8  \w     78.00 158.00   1.00    8.00    --  109.50  30.00 120.00   80
  9  \w     43.00 108.00   1.00    8.00    --  109.50-111.00  60.00   65
 10  \w     43.00 108.00   1.00    8.00    --  109.50-111.00 -60.00   65
 11  \w     81.00 158.00   1.00    8.00    --  109.50  54.00   1.57   77
 12  \w     89.00 146.00   1.00    8.00    --  109.50 178.00 -60.00   57
 13  \w     29.00 106.00   1.00    8.00    --  109.50 -94.00-150.00   77
 14  \w     28.00 158.00   1.00    8.00    --  109.50 -15.00 -90.00  130
 15  \w     43.00 108.00   1.00    8.00    --  109.50-111.00 -90.00   65
 16  \w     37.00 137.00   1.00    8.00    --  109.50 -45.00   0.00  100
 17  \w     89.00 146.00   1.00    8.00    --  109.50 178.00  90.00   57
 18  \w    -71.00  23.00   1.00    2.50    --  -41.39  57.00   0.00   94
 19  \w      8.00  87.00   1.00    2.50    --   41.39  77.00  90.00   79
;
_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      0.0964043000
_diffrn_orient_matrix_UB_12      0.0339936000
_diffrn_orient_matrix_UB_13      0.0504266000
_diffrn_orient_matrix_UB_21      -0.1374810000
_diffrn_orient_matrix_UB_22      0.0175627000
_diffrn_orient_matrix_UB_23      0.0270831000
_diffrn_orient_matrix_UB_31      0.0038736000
_diffrn_orient_matrix_UB_32      -0.2104191000
_diffrn_orient_matrix_UB_33      0.0103232000
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9937
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15143
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9937
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.26
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.270
_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    1.418
_exptl_crystal_description       needle
_exptl_crystal_F_000             807.528
_exptl_crystal_size_max          0.656
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.6149
_refine_diff_density_min         -0.4870
_refine_diff_density_rms         0.0832
_refine_ls_d_res_high            0.7971
_refine_ls_d_res_low             13.2391
_refine_ls_goodness_of_fit_ref   1.0326
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0326
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.0037
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -9
_reflns_number_gt                2844
_reflns_number_total             3618
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00210e2.cif
_cod_data_source_block           20230426_TJ427_02
_cod_depositor_comments
'Adding full bibliography for 7248499--7248509.cif.'
_cod_database_code               7248504
_chemical_oxdiff_formula         'C4 H13 P S O4'
_chemical_oxdiff_usercomment     '20230426_TJ427_01 TMPHS needle'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Idealised Me refined as rotating group:
 C00D(H00a,H00b,H00c), C00E(H00m,H00n,H00o), C00F(H00d,H00e,H00f), C00G(H00p,
 H00q,H00r), C00H(H00s,H00t,H00u), C00I(H00v,H00w,H00x), C00J(H00g,H00h,H00i),
 C00K(H00j,H00k,H00l)
;
_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 46.689
_oxdiff_exptl_absorpt_empirical_full_min 0.515