A polychloride-enabled synthesis of [NEt<sub>3</sub>Me][PCl<sub>6</sub>] serving as a potential PCl<sub>3</sub>-storage and PCl<sub>5</sub>-reagent.
Ernst, Moritz J.; Kleoff, Merlin; Voßnacker, Patrick; Thiele, Günther; Müller, Christian; Riedel, Sebastian; Chemical communications (Cambridge, England) 60 (2024) 13372–13375; doi:10.1039/d4cc04319g

data_7133878
_publ_section_title
;
 A polychloride-enabled synthesis of [NEt<sub>3</sub>Me][PCl<sub>6</sub>]
 serving as a potential PCl<sub>3</sub>-storage and
 PCl<sub>5</sub>-reagent.
;
_journal_issue                   91
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13372
_journal_page_last               13375
_journal_paper_doi               10.1039/d4cc04319g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '4(Cl1.5 P0.25), 4(C1.75 N0.25)'
_chemical_formula_sum            'C7 Cl6 N P'
_chemical_formula_weight         341.75
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_audit_creation_date             2024-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.2009(9)
_cell_length_b                   7.2009(9)
_cell_length_c                   7.2009(9)
_cell_measurement_reflns_used    1133
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.83
_cell_measurement_theta_min      2.83
_cell_volume                     373.39(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.939
_diffrn_reflns_theta_max         24.939
_diffrn_reflns_theta_min         2.829
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0841 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.7339.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             166
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         95
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+0.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                77
_reflns_number_total             95
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04319g2.cif
_cod_data_source_block           mo_mje204_dcm_0m
_cod_depositor_comments          'Adding full bibliography for 7133878.cif.'
_cod_original_cell_volume        373.39(14)
_cod_database_code               7133878
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl1(0.03125) Cl2(0.09375) C2(0.083325) C1(0.0625)
;
_olex2_submission_special_instructions 'No special instructions were received'