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_7248508
_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         'Ag2 Br3, C8 H20 P'
_chemical_formula_sum            'C8 H20 Ag2 Br3 P'
_chemical_formula_weight         602.669
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_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            12
_cell_length_a                   21.3719(1)
_cell_length_b                   12.2556(1)
_cell_length_c                   17.2118(1)
_cell_measurement_reflns_used    43948
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.0790
_cell_measurement_theta_min      2.0540
_cell_volume                     4508.21(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      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2687
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9978
_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    -70.00  32.00   1.00    2.00    --  -41.26  57.00   0.00  102
  2  \w    -97.00 -12.00   1.00    2.00    --  -41.26 125.00 150.00   85
  3  \w   -117.00 -30.00   1.00    2.00    --  -41.26 -77.00-120.00   87
  4  \w   -117.00 -30.00   1.00    2.00    --  -41.26 -77.00 120.00   87
  5  \w     34.00  82.00   1.00    2.00    --   41.26 -99.00  30.00   48
  6  \w     78.00 158.00   1.00    8.00    --  109.50  30.00  30.00   80
  7  \w     43.00 108.00   1.00    8.00    --  109.50-111.00 150.00   65
  8  \w     37.00 137.00   1.00    8.00    --  109.50 -45.00  90.00  100
  9  \w     43.00 108.00   1.00    8.00    --  109.50-111.00  90.00   65
 10  \w     33.00 140.00   1.00    8.00    --  109.50 -30.00   0.00  107
 11  \w     79.00 158.00   1.00    8.00    --  109.50  61.00 -30.00   79
 12  \w     89.00 146.00   1.00    8.00    --  109.50 178.00 -30.00   57
 13  \w     29.00 106.00   1.00    8.00    --  109.50 -94.00 -60.00   77
 14  \w     28.00 158.00   1.00    8.00    --  109.50 -15.00-180.00  130
 15  \w     36.00 139.00   1.00    8.00    --  109.50 -61.00 -30.00  103
 16  \w    -33.00  67.00   1.00    2.00    --   41.26 -38.00-180.00  100
 17  \w    -33.00  67.00   1.00    2.00    --   41.26 -38.00  90.00  100
 18  \w      8.00  87.00   1.00    2.00    --   41.26  77.00 -30.00   79
 19  \w      8.00  87.00   1.00    2.00    --   41.26  77.00-150.00   79
 20  \w      8.00  87.00   1.00    2.00    --   41.26  77.00  60.00   79
 21  \w     82.00 158.00   1.00    8.00    --  109.50  45.00 -90.00   76
 22  \w     79.00 158.00   1.00    8.00    --  109.50  61.00 120.00   79
 23  \w     82.00 158.00   1.00    8.00    --  109.50  45.00-150.00   76
 24  \w     79.00 158.00   1.00    8.00    --  109.50  61.00 -60.00   79
 25  \w     82.00 158.00   1.00    8.00    --  109.50  45.00  60.00   76
 26  \w     79.00 158.00   1.00    8.00    --  109.50  61.00 150.00   79
 27  \w     82.00 158.00   1.00    8.00    --  109.50  45.00-120.00   76
 28  \w     79.00 158.00   1.00    8.00    --  109.50  61.00-180.00   79
 29  \w     43.00 108.00   1.00    8.00    --  109.50-111.00   0.00   65
 30  \w     79.00 158.00   1.00    8.00    --  109.50  61.00  90.00   79
 31  \w   -113.00 -12.00   1.00    2.00    --  -41.26 -57.00-120.00  101
 32  \w      8.00  87.00   1.00    2.00    --   41.26  77.00 150.00   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      0.0418854000
_diffrn_orient_matrix_UB_12      -0.0003728000
_diffrn_orient_matrix_UB_13      0.0728054000
_diffrn_orient_matrix_UB_21      0.0089336000
_diffrn_orient_matrix_UB_22      -0.1242151000
_diffrn_orient_matrix_UB_23      -0.0082446000
_diffrn_orient_matrix_UB_31      0.0579282000
_diffrn_orient_matrix_UB_32      0.0193909000
_diffrn_orient_matrix_UB_33      -0.0514782000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.9998
_diffrn_reflns_Laue_measured_fraction_max 0.9978
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69972
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.9978
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.33
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.990
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_correction_T_min  0.052
_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    2.664
_exptl_crystal_description       block
_exptl_crystal_F_000             3392.0
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.7741
_refine_diff_density_min         -2.3904
_refine_diff_density_rms         0.2060
_refine_ls_d_res_high            0.7969
_refine_ls_d_res_low             13.4051
_refine_ls_goodness_of_fit_ref   1.0433
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    63
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4892
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0432
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+24.2156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4807
_reflns_number_total             4892
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00210e2.cif
_cod_data_source_block           09
_cod_depositor_comments
'Adding full bibliography for 7248499--7248509.cif.'
_cod_database_code               7248508
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C8 H20 P Ag2 Br3'
_chemical_oxdiff_usercomment
'TJ421 (Et4P)2SO4 TEPS H-reactor site with AgBr'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 H00d, C00J, C00K, P00A
 with sigma of 0.2
3. Others
 Fixed Sof: H00a(0.5) H00b(0.5) H00p(0.5) H00q(0.5) H00c(0.5) H00d(0.5)
 H00e(0.5) H00z(0.5) H(0.5) H00c(0.5) H00d(0.5) H00e(0.5) H00f(0.5) H00g(0.5)
 H00j(0.5) H00k(0.5) H00l(0.5) H1(0.5) Ha(0.5) H00(0.5) Hc(0.5) Hd(0.5) H4(0.5)
 Hg(0.5) Hh(0.5) H5(0.5) Hi(0.5) Hj(0.5) H6(0.5) Hk(0.5) H00r(0.5) H00s(0.5)
 H00t(0.5) H00c(0.5) H00d(0.5) H00e(0.5) H00r(0.5) H00s(0.5) H00t(0.5)
 H00c(0.5) H00e(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C00D(H00a,H00b), C00E(H00p,H00q), C00G(H00u,H00v), C00I(H00z,H), C00K(H00f,
 H00g), C00L(H00h,H00i), C00N(H1,Ha), C00P(H2,Hb), C00U(H6,Hk)
4.b Idealised Me refined as rotating group:
 C00H(H00w,H00x,H00y), C00M(H00j,H00k,H00l), C00O(H00m,H00n,H00o), C00Q(H00,Hc,
 Hd), C00R(H3,He,Hf), C00S(H4,Hg,Hh), C00T(H5,Hi,Hj), C00F(H00r,H00s,H00t),
 C00J(H00c,H00d,H00e)
;
_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 1.808
_oxdiff_exptl_absorpt_empirical_full_min 0.727