Tetra-cationic imidazoliumyl-substituted phosphorus-sulfur heterocycles from a cationic organophosphorus sulfide.
Henne, Florian D.; Watt, Fabian A.; Schwedtmann, Kai; Hennersdorf, Felix; Kokoschka, Malte; Weigand, Jan J.; Chemical communications (Cambridge, England) 52 (2016) 2023–2026; doi:10.1039/c5cc08182c

data_7118623
_publ_section_title
;
 Tetra-cationic imidazoliumyl-substituted phosphorus-sulfur heterocycles
 from a cationic organophosphorus sulfide.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2023
_journal_page_last               2026
_journal_paper_doi               10.1039/c5cc08182c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C44 H80 N8 P4 S4, 4(C F3 O3 S)'
_chemical_formula_sum            'C48 H80 F12 N8 O12 P4 S8'
_chemical_formula_weight         1569.56
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.5055(4)
_cell_length_b                   17.5055(4)
_cell_length_c                   13.3734(6)
_cell_measurement_temperature    100.0
_cell_volume                     4098.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.93618
_exptl_absorpt_correction_T_min  0.93618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.32(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1052P)^2^+3.3272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4006
_reflns_number_total             5071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08182c6.cif
_cod_data_source_block
;
;
_cod_original_cell_volume        4098.2(3)
_cod_database_code               7118623
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.68(18) 0.32(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C2A-C4A \\sim C4B-C2B \\sim C5B-C3B \\sim C5A-C3A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C12A \\sim S2 \\sim O2B \\sim O3A \\sim O1B \\sim O2A \\sim O1A \\sim O3B \\sim
C12B \\sim F2A \\sim F1A \\sim F3A \\sim F2B \\sim F3B \\sim F1B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
N1B \\sim C1B \\sim N2B \\sim C2B \\sim C6B \\sim C3B \\sim C9B \\sim C4B \\sim
C7 \\sim C8 \\sim C5B \\sim C11 \\sim C10 \\sim C6A \\sim C9A \\sim N1A \\sim
N2A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(P1B)=Sof(C3B)=Sof(N1B)=Sof(C2B)=Sof(N2B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(H7BD)=Sof(H7BE)=Sof(H7BF)=Sof(H8BD)=Sof(H8BE)=Sof(H8BF)=Sof(C5B)=Sof(H5BA)=
 Sof(H5BB)=Sof(H5BC)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C9B)=Sof(H9B)=Sof(C6B)=
 Sof(H6B)=Sof(S1B)=Sof(C1B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(1)
 Sof(P1A)=Sof(S1A)=Sof(C1A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(N2A)=Sof(N1A)=Sof(C3A)=Sof(C2A)=Sof(C9A)=
 Sof(H9A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=FVAR(1)
 Sof(O1B)=Sof(O3B)=Sof(F2B)=Sof(F3B)=Sof(F1B)=Sof(C12B)=Sof(O2B)=1-FVAR(2)
 Sof(O2A)=Sof(C12A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=Sof(O3A)=Sof(O1A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C9B(H9B), C6B(H6B), C9A(H9A), C6A(H6A)
6.b Me refined with riding coordinates:
 C10(H10D,H10E,H10F), C10(H10A,H10B,H10C), C7(H7BD,H7BE,H7BF), C7(H7AA,H7AB,
 H7AC), C8(H8BD,H8BE,H8BF), C8(H8AA,H8AB,H8AC)
6.c Idealised Me refined as rotating group:
 C5B(H5BA,H5BB,H5BC), C11(H11D,H11E,H11F), C11(H11A,H11B,H11C), C4A(H4AA,H4AB,
 H4AC), C5A(H5AA,H5AB,H5AC), C4B(H4BA,H4BB,H4BC)
;
_shelx_fab_checksum              92010
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'