Phase behaviour and conductivity of supporting electrolytes in supercritical difluoromethane and 1,1-difluoroethane.
Han, Xue; Ke, Jie; Suleiman, Norhidayah; Levason, William; Pugh, David; Zhang, Wenjian; Reid, Gillian; Licence, Peter; George, Michael W.; Physical chemistry chemical physics : PCCP 18 (2016) 14359–14369; doi:10.1039/c6cp00466k

data_7225211
_publ_section_title
;
 Phase behaviour and conductivity of supporting electrolytes in
 supercritical difluoromethane and 1,1-difluoroethane.
;
_journal_issue                   21
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              14359
_journal_page_last               14369
_journal_paper_doi               10.1039/c6cp00466k
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C16 H36 N, C2 F6 N O4 S2'
_chemical_formula_sum            'C18 H36 F6 N2 O4 S2'
_chemical_formula_weight         522.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.059(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.312(6)
_cell_length_b                   28.997(13)
_cell_length_c                   13.523(6)
_cell_measurement_reflns_used    10858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.2
_cell_volume                     5207(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21991
_diffrn_reflns_point_group_measured_fraction_full 0.836
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 3195 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         17489
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0947
_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^)+(0.0587P)^2^+7.6416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.674
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                12466
_reflns_number_total             17489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cp00466k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7225209--7225211.cif.'
_cod_database_code               7225211
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2013-4
_shelx_res_checksum              24753