Studies of Dirhodium(II) Tetrakis(trifluoroacetate). 6. The First Structural Characterization of Axial Alkyne Complexes, Rh2(O2CCF3)4(Ph2C2)n(n= 1, 2): Diphenylacetylene as a Bifunctional Ligand
Cotton, F. Albert; Dikarev, Evgeny V.; Petrukhina, Marina A.; Stiriba, Salah-Eddine; Organometallics 19 (2000) 1402–; doi:10.1021/om9909800

data_4077718
_publ_section_title
;
 Studies of Dirhodium(II) Tetrakis(trifluoroacetate). 6. The First
 Structural Characterization of Axial Alkyne Complexes,
 Rh2(O2CCF3)4(Ph2C2)n(n= 1, 2):&#x00A0; Diphenylacetylene as a
 Bifunctional Ligand
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1402
_journal_paper_doi               10.1021/om9909800
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Rh2 (O2 C C F3)4 (C6 H5 C C C6 H5)2'
_chemical_formula_structural     Rh2(O2CCF3)4(PhCCPh)2
_chemical_formula_sum            'C36 H20 F12 O8 Rh2'
_chemical_formula_weight         1014.34
_chemical_melting_point          ?
_chemical_name_systematic
; 
 [tetrakis(\m-trifluoroacetato-\kO,\kO')dirhodium(II,II)]-bis-
 (\h2-diphenylacetylene)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 124.368(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.700(1)
_cell_length_b                   9.7055(5)
_cell_length_c                   18.5448(4)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     3669.6(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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9818
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_obs          0.0359
_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^)+(0.0346P)^2^+27.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0874
_refine_ls_wR_factor_obs         0.0850
_reflns_number_observed          2249
_reflns_number_total             2396
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om9909800.cif
_cod_data_source_block           Rh2(O2CCF3)4(Ph2C2)2_(1)
_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 1715 2011-07-08 13:25:40Z 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^)+(0.0346P)^2^+27.6066P] 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^)+(0.0346P)^2^+27.6066P] 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               4077718