Supramolecular Assemblies of Dimetal Complexes with Polydentate N-Donor Ligands: From a Discrete Pyramid to a 3D Channel Network
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Marion Schmitz; Peter J. Stang; Inorganic Chemistry 41 (2002) 2903–2908; doi:10.1021/ic020051s

data_4318044
_publ_section_title
;
 Supramolecular Assemblies of Dimetal Complexes with Polydentate N-Donor
 Ligands: From a Discrete Pyramid to a 3D Channel Network
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2903
_journal_page_last               2908
_journal_paper_doi               10.1021/ic020051s
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
  [Rh2 (O2 C2 F3)4]2, [(C6 H5)2 Si (C5 H4 N)2]
;
_chemical_formula_structural
;
  {[Rh2(O2CCF3)4]2(Ph2Si(C5H4N)2)}
;
_chemical_formula_sum            'C38 H18 F24 N2 O16 Rh4 Si'
_chemical_formula_weight         1654.27
_chemical_melting_point          ?
_chemical_name_systematic
;
  Catena-{bis[tetrakis(trifluoroacetato)dirhodium(II,II)]-
  -bis(4'-pyridyl)diphenylsilane}
;
_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                 90.14(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.726(6)
_cell_length_b                   16.795(1)
_cell_length_c                   17.798(3)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     6494(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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21531
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0677
_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^)+(0.1050P)^2^+85.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2047
_refine_ls_wR_factor_obs         0.1854
_reflns_number_observed          4948
_reflns_number_total             5749
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020051s_3.cif
_cod_data_source_block           {[Rh2(O2CCF3)4]2,(C6H5)2Si(C5H4N)2}_(3)
_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 1569 2011-02-09 13:29:24Z 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^)+(0.1050P)^2^+85.7000P] 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^)+(0.1050P)^2^+85.7000P] 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               4318044