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_4320882
_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]7[(C H3)2 S O]8
;
_chemical_formula_structural
;
 Rh2(O2CCF3)4{[Rh2(O2CCF3)4]3(\m2-DMSO-O,S)3(DMSO-O)}2
;
_chemical_formula_sum            'C72 H48 F84 O64 Rh14 S8'
_chemical_formula_weight         5230.32
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Hexakis(\m2-dimethylsulfoxide,-O,S)-bis(dimethylsulfoxide-O)-
 -heptakis(tetrakis(\m2-trifluoroacetato)-di-rhodium(II))
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.40(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.261(2)
_cell_length_b                   16.059(4)
_cell_length_c                   17.636(2)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      5.0
_cell_volume                     7997(2)
_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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18994
_diffrn_reflns_theta_max         19.02
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             5012
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.135
_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_obs          0.0584
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0004P)^2^+264.5537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1437
_refine_ls_wR_factor_obs         0.1280
_reflns_number_observed          5244
_reflns_number_total             6191
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9913076_2.cif
_cod_data_source_block           '[Rh2(O2CCF3)4]7(DMSO)8'
_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^)+(0.0004P)^2^+264.5537P] 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^)+(0.0004P)^2^+264.5537P] 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               4320882