Lamellar Structures in Fluorinated Phosphonium Ionic Liquids: the Roles of Fluorination and Chain Length
Zhang, Peng; Rauber, Daniel; Huch, Volker; Kraus, Tobias; Hempelmann, Rolf; Phys. Chem. Chem. Phys.  (2017) –; doi:10.1039/C7CP04814A

data_7229227
_publ_section_title
;
 Lamellar Structures in Fluorinated Phosphonium Ionic Liquids: the Roles
 of Fluorination and Chain Length
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP04814A
_journal_year                    2017
_chemical_formula_moiety         'C22 H31 F17 P, C2 N3'
_chemical_formula_sum            'C24 H31 F17 N3 P'
_chemical_formula_weight         715.49
_chemical_name_systematic
'tributyl(1H,1H,2H,2H-perfluorodecyl)phosphonium dicyanamide'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1mgjf1
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-09-09 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                102.184(4)
_cell_angle_beta                 97.398(4)
_cell_angle_gamma                94.832(5)
_cell_formula_units_Z            4
_cell_length_a                   10.1936(7)
_cell_length_b                   12.6081(10)
_cell_length_c                   25.0746(17)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.31
_cell_volume                     3103.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.949
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39865
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.722
_diffrn_reflns_theta_min         0.840
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichlormethane, heptane '
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         12493
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0738P)^2^+3.8539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8587
_reflns_number_total             12493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp04814a2.cif
_cod_data_source_block           sh3765a
_cod_database_code               7229227
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2014/6
_shelx_res_checksum              18020