Studies of Dirhodium Tetra(trifluoroacetate). 3. Solid State Isomers of the Compound Rh2(O2CCF3)4(THF) Prepared by Sublimation
F. Albert Cotton; Evgeny V. Dikarev; Salah-Eddine Stiriba; Inorganic Chemistry 38 (1999) 4877–4881; doi:10.1021/ic990618d

data_4322333
_publ_section_title
;
 Studies of Dirhodium Tetra(trifluoroacetate). 3. Solid State Isomers of
 the Compound Rh2(O2CCF3)4(THF) Prepared by Sublimation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4877
_journal_page_last               4881
_journal_paper_doi               10.1021/ic990618d
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '[Rh2 (O2 C C F3)4 (O C4 H8)]2'
_chemical_formula_structural     '[Rh2(O2CCF3)4(THF)]2'
_chemical_formula_sum            'C12 H8 F12 O9 Rh2'
_chemical_formula_weight         730.00
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(tetrahydrofuran)-bis(\m3-trifluoroacetato)-hexakis
 (\m2-trifluoroacetato)-tetra-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                73.182(5)
_cell_angle_beta                 74.622(5)
_cell_angle_gamma                89.76(1)
_cell_formula_units_Z            2
_cell_length_a                   8.6347(3)
_cell_length_b                   9.678(1)
_cell_length_c                   13.773(4)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      6.85
_cell_volume                     1059.0(3)
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5688
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         2665
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_obs          0.0556
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+12.4337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1441
_refine_ls_wR_factor_obs         0.1283
_reflns_number_observed          2207
_reflns_number_total             2665
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990618d_1.cif
_cod_data_source_block           '[Rh2(O2CCF3)4(THF)]2(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 1673 2011-04-08 12:14:43Z 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^)+(0.0552P)^2^+12.4337P] 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^)+(0.0552P)^2^+12.4337P] 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               4322333