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_4318156
_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            'C44 H16 F76 O12 Rh2'
_chemical_formula_weight         2386.39
_chemical_name_common            {(MeOH)2Rh2(OAc(CF2)9F)4}.2MeOH
_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                90.917(4)
_cell_angle_beta                 95.208(4)
_cell_angle_gamma                107.581(4)
_cell_formula_units_Z            1
_cell_length_a                   9.665(3)
_cell_length_b                   13.903(4)
_cell_length_c                   14.195(4)
_cell_measurement_reflns_used    410
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.2
_cell_volume                     1808.9(9)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.095
_diffrn_reflns_av_sigmaI/netI    0.162
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13954
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.890
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       0.025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6585
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.2150
_refine_ls_R_factor_gt           0.1574
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1722P)^2^+105.3087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4379
_refine_ls_wR_factor_ref         0.4641
_reflns_number_gt                3769
_reflns_number_total             6585
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic020057h_2.cif
_cod_data_source_block           mn1192
_cod_original_cell_volume        1808.9(8)
_cod_database_code               4318156