Carbon Dioxide as a Solubility "Switch" for the Reversible Dissolution of Highly Fluorinated Complexes and Reagents in Organic Solvents: Application to Crystallization
Philip G. Jessop; Marilyn M. Olmstead; Christopher D. Ablan; Megan Grabenauer; Daniel Sheppard; Charles A. Eckert; Charles L. Liotta; Inorganic Chemistry 41 (2002) 3463–3468; doi:10.1021/ic020057h

data_4318158
_publ_section_title
;
 Carbon Dioxide as a Solubility "Switch" for the Reversible Dissolution of
 Highly Fluorinated Complexes and Reagents in Organic Solvents:
 Application to Crystallization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3463
_journal_page_last               3468
_journal_paper_doi               10.1021/ic020057h
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H9 F18 P'
_chemical_formula_weight         670.28
_chemical_name_common            P[3,5-(CF3)2C6H3]3
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.539(7)
_cell_angle_beta                 80.590(4)
_cell_angle_gamma                85.248(5)
_cell_formula_units_Z            8
_cell_length_a                   12.3803(15)
_cell_length_b                   12.9054(17)
_cell_length_c                   32.807(4)
_cell_measurement_reflns_used    809
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     5092.3(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            67417
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1581
_refine_ls_number_reflns         23017
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          1.237
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+13.0873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                17854
_reflns_number_total             23017
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic020057h_4.cif
_cod_data_source_block           mn1279
_cod_original_cell_volume        5092.4(11)
_cod_database_code               4318158