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_4318155
_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            'C29 H22 F28 N2 O10 Rh2'
_chemical_formula_weight         1296.31
_chemical_name_common            '[Rh2(F-O2But)8(DMF)2].toluene'
_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                82.103(8)
_cell_angle_beta                 82.239(7)
_cell_angle_gamma                63.296(8)
_cell_formula_units_Z            2
_cell_length_a                   10.559(2)
_cell_length_b                   10.578(2)
_cell_length_c                   22.015(4)
_cell_measurement_reflns_used    4602
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.2
_cell_volume                     2168.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.1, XP (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      92(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.055
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29485
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.7798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         13233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+10.8942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                9760
_reflns_number_total             13233
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic020057h_1.cif
_cod_data_source_block           mn1219
_cod_original_cell_volume        2168.5(10)
_cod_database_code               4318155