Studies of Dirhodium(II) Tetra(trifluoroacetate). 5. Remarkable Examples of the Ambidentate Character of Dimethyl Sulfoxide
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Salah-Eddine Stiriba; Inorganic Chemistry 39 (2000) 1748–1754; doi:10.1021/ic9913076

data_4320881
_publ_section_title
;
 Studies of Dirhodium(II) Tetra(trifluoroacetate). 5. Remarkable Examples
 of the Ambidentate Character of Dimethyl Sulfoxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1748
_journal_page_last               1754
_journal_paper_doi               10.1021/ic9913076
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 [Rh2 (O2 C C F3)4 (O S (C H3)2)]2 [Rh2 (O2 C C F3)4] 
;
_chemical_formula_structural
;
 [Rh2(O2CCF3)4(\m2-DMSO-O,S)]2[Rh2(O2CCF3)4]
;
_chemical_formula_sum            'C28 H12 F36 O26 Rh6 S2'
_chemical_formula_weight         2129.96
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Catena(bis(\m2-dimethylsulfoxide-O,S)-bis(\m3-trifluoroacetato)-
 -hexakis(\m2-trifluoroacetato)-tetra-rhodium(II)-tetrakis
 (\m2-trifluoroacetato)-di-rhodium(II))
;
_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
_cell_angle_alpha                101.91(2)
_cell_angle_beta                 97.144(8)
_cell_angle_gamma                100.206(9)
_cell_formula_units_Z            1
_cell_length_a                   8.876(2)
_cell_length_b                   9.017(2)
_cell_length_c                   19.841(3)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.00
_cell_volume                     1507.7(5)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6789
_diffrn_reflns_theta_max         22.65
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.148
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_obs          0.0532
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+21.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1416
_refine_ls_wR_factor_obs         0.1231
_reflns_number_observed          3185
_reflns_number_total             3624
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9913076_1.cif
_cod_data_source_block           '[Rh2(O2CCF3)4]3(DMSO)2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+21.8090P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+21.8090P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320881