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_4318042
_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_formula_moiety
;
  {[Rh2 (O2 C C F3)4]3, [(O H) C (N C5 H4)3], (C6 H6)}, (C6 H6)0.5
;
_chemical_formula_structural
;
  {[Rh2(O2CCF3)4]3((OH)C(C5H4N)3)(\h1-C6H6)},0.5(C6H6)
;
_chemical_formula_sum            'C49 H22 F36 N3 O25 Rh6'
_chemical_formula_weight         2354.16
_chemical_melting_point          ?
_chemical_name_systematic
;
  Catena-{tris[tetrakis(trifluoroacetato)dirhodium(II,II)]-tris
  (4'-pyridyl)methanol-(\h1-benzene)}, benzene solvate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.101(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.175(2)
_cell_length_b                   16.1746(7)
_cell_length_c                   23.782(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     8901.5(17)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  '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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46593
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4524
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         15590
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+156.4058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2309
_reflns_number_gt                12839
_reflns_number_total             15590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020051s_1.cif
_cod_data_source_block
{[Rh2(O2CCF3)4]3,(OH)C(NC5H4)3,C6H6},0.5C6H6_(4,0.5C6H6)
_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:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        8902(2)
_cod_database_code               4318042