Asymmetric Sandwich-Type Polyoxoanions. Synthesis, Characterization, and X-ray Crystal Structures of Diferric Complexes [TMIIFeIII2(P2W15O56)(P2TMII2W13O52)]16-, TM = Cu or Co
Travis M. Anderson; Kenneth I. Hardcastle; Nelya Okun; Craig L. Hill; Inorganic Chemistry 40 (2001) 6418–6425; doi:10.1021/ic0105314

data_4320642
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Laboratory
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Kenneth I. Hardcastle'
_publ_contact_author_phone       404-727-6140
_publ_section_title
;
 Asymmetric Sandwich-Type Polyoxoanions. Synthesis, Characterization, and
 X-ray Crystal Structures of Diferric Complexes
 [TMIIFeIII2(P2W15O56)(P2TMII2W13O52)]16-, TM = Cu or Co
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6418
_journal_page_last               6425
_journal_paper_doi               10.1021/ic0105314
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Cu3 Fe2 H0 Na16 O142.75 P4 W28'
_chemical_formula_weight         8225.84
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.475(2)
_cell_angle_beta                 85.555(2)
_cell_angle_gamma                89.563(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4413(9)
_cell_length_b                   21.2590(15)
_cell_length_c                   25.5207(18)
_cell_measurement_reflns_used    8587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.505
_cell_measurement_theta_min      2.467
_cell_volume                     7170.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            96539
_diffrn_reflns_theta_full        30.60
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    23.192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.432568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             7178
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.046
_refine_diff_density_min         -2.566
_refine_diff_density_rms         0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         43097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                30877
_reflns_number_total             43097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105314_1.cif
_cod_data_source_block           cu3fe2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'H0 Cu3 Fe2 Na16 O142.75 P4 W28'
_cod_database_code               4320642