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_4318043
_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]3, [(C H3) Si (C5 H4 N)3], (C6 H6)3}, (C6 H6)
;
_chemical_formula_structural
;
  {[Rh2(O2CCF3)4]3(MeSi(C5H4N)3)(\h1-C6H6)3},C6H6
;
_chemical_formula_sum            'C64 H39 F36 N3 O24 Rh6 Si'
_chemical_formula_weight         2563.53
_chemical_melting_point          ?
_chemical_name_systematic
;
  {Tris[tetrakis(trifluoroacetato)dirhodium(II,II)]-tris(4'-pyridyl)
  methylsilane-tris(\h1-benzene)}, benzene solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   25.160(2)
_cell_length_b                   25.160(2)
_cell_length_c                   23.382(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      7.50
_cell_volume                     12818(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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17654
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.61
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_obs          0.0475
_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^)+(0.0512P)^2^+253.0030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_obs         0.1132
_reflns_number_observed          3286
_reflns_number_total             3700
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020051s_2.cif
_cod_data_source_block
{[Rh2(O2CCF3)4]3,(CH3)Si(C5H4N)3,3(C6H6)},C6H6_(2,C6H6)
_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^)+(0.0512P)^2^+253.0030P] 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^)+(0.0512P)^2^+253.0030P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        12819(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4318043