Liquid silver tris(perfluoroethyl)trifluorophosphate salts as new media for propene/propane separation.
Pliquett, Daniel; Schulz, Peter S.; Heinemann, Frank W.; Bause, Angela; Wasserscheid, Peter; Physical chemistry chemical physics : PCCP 18 (2016) 28242–28253; doi:10.1039/c6cp05653a

data_7226665
_publ_section_title
;
 Liquid silver tris(perfluoroethyl)trifluorophosphate salts as new media
 for propene/propane separation.
;
_journal_issue                   40
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              28242
_journal_page_last               28253
_journal_paper_doi               10.1039/c6cp05653a
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C8 H12 Ag N4, C6 F18 P'
_chemical_formula_sum            'C14 H12 Ag F18 N4 P'
_chemical_formula_weight         717.12
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Light-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-08-08 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6078(6)
_cell_length_b                   15.0214(5)
_cell_length_c                   18.0740(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.53
_cell_volume                     4780.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Triumph curved graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72757
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.729
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0526 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.8943.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         6118
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0343P)^2^+6.1280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4548
_reflns_number_total             6118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cp05653a1.cif
_cod_data_source_block           crt1501
_cod_depositor_comments
'Adding full bibliography for 7226665--7226667.cif.'
_cod_database_code               7226665
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.721
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13A-C14A \\sim C13-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10 \\sim C10A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C10) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(F16A) \\sim Ueq, Uanis(F17A)
\\sim Ueq, Uanis(F18A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Sof(P1A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(F1A)=
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=
 Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=
 Sof(F17A)=Sof(F18A)=1-FVAR(1)
 Sof(P1)=Sof(C9)=Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(F1)=Sof(F2)=
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=
 Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              78927
_olex2_submission_special_instructions 'No special instructions were received'