2CH3CN@(n-Bu4N)2[{Ir(1,5-COD)}6W4O16].2CH3CN: A Hybrid Inorganic-Organometallic, Flexible Cavity Host, Acetonitrile-Guest Complex Composed of a [W4O4]n+ Tetratungstate Cube and Six Polyoxoanion-Supported (1,5-COD)Ir+ Organometallic Groups
Yoshihito Hayashi; Frank Müller; Yin Lin; Susie M. Miller; Oren P. Anderson; Richard G. Finke; Journal of the American Chemical Society 119 (1997) 11401–11407; doi:10.1021/ja970336h

data_4117064
_publ_contact_author
;
Dr Richard G. Finke
Department of Chemistry
Colorado State University
Fort Collins, CO 80523
U. S. A.
;
_publ_contact_author_email       rfinke@lamar.colostate.edu
_publ_contact_author_fax         907(491)1801
_publ_contact_author_phone       907(491)2475
_publ_section_title
;
 2CH3CN@(n-Bu4N)2[{Ir(1,5-COD)}6W4O16].2CH3CN: A Hybrid
 Inorganic-Organometallic, Flexible Cavity Host, Acetonitrile-Guest
 Complex Composed of a [W4O4]n+ Tetratungstate Cube and Six
 Polyoxoanion-Supported (1,5-COD)Ir+ Organometallic Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11401
_journal_page_last               11407
_journal_paper_doi               10.1021/ja970336h
_journal_volume                  119
_journal_year                    1997
_chemical_compound_source        synthetic
_chemical_formula_analytical     '[(n-Bu4N)2[{Ir(1,5-COD)}6W4O16] 4CH3CN]'
_chemical_formula_moiety         'C80 H144 Ir6 N2 O16 W4,4(C2 H3 N)'
_chemical_formula_structural
;
[2CH3CN<(n-Bu4N)2[{Ir(1,5-COD)}6W4O16] 2CH3CN]
;
_chemical_formula_sum            'C88 H156 Ir6 N6 O16 W4'
_chemical_formula_weight         3442.79
_chemical_name_common
;
[(Bis-(tetrra-n-butylammonium))-hexa((\h4-1,5-cyclooctadienyl)iridium)-
tetratungstate 4-acetonitrile solvate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL, V. 5.0.3.'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.5450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.8856(6)
_cell_length_b                   18.6662(5)
_cell_length_c                   45.7427(12)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      1.36
_cell_volume                     21207.7(9)
_computing_cell_refinement       'SIEMENS SAINT'
_computing_data_collection       'SIEMENT SMART'
_computing_data_reduction        'SIEMENS SHELXTL'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SIEMENS SHELXTL'
_computing_structure_solution    'SIEMENS SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       SMART
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            42659
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    11.873
_exptl_absorpt_correction_T_max  0.089
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_description       pallarel-piped
_exptl_crystal_F_000             12896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.831
_refine_diff_density_min         -2.484
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         27435
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.170
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_obs          0.0655
_refine_ls_shift/esd_max         0.147
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+484.3376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1811
_refine_ls_wR_factor_obs         0.1340
_reflns_number_observed          17436
_reflns_number_total             27451
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970336h.cif
_cod_data_source_block           2CH3CN<(Ir(COD))6W4O16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+484.3376P] 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^)+(0.0474P)^2^+484.3376P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117064