Cobalt, Manganese, Nickel, and Vanadium Derivatives of the Cyclic 48-Tungsto-8-Phosphate [H7P8W48O184]33-
Bassem S. Bassil; Masooma Ibrahim; Sib Sankar Mal; Andreas Suchopar; Rosa Ngo Biboum; Bineta Keita; Louis Nadjo; Saritha Nellutla; Johan van Tol; Naresh S. Dalal; Ulrich Kortz; Inorganic Chemistry 49 (2010) 4949–4959; doi:10.1021/ic100050r

data_4315583
_publ_contact_author_address
;
Jacobs University, School of Engineering and Science, P.O. Box 750 561, 
28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_fax         '+49-421-200 3229'
_publ_contact_author_name        'Ulrich Kortz'
_publ_section_title
;
 Cobalt, Manganese, Nickel, and Vanadium Derivatives of the Cyclic
 48-Tungsto-8-Phosphate [H7P8W48O184]33-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4949
_journal_page_last               4959
_journal_paper_doi               10.1021/ic100050r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'H96 K20 Li16 O240 P8 V4 W48'
_chemical_formula_weight         14106.0
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           83
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4'
_symmetry_space_group_name_H-M   'P 4/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.0881(3)
_cell_length_b                   24.0881(3)
_cell_length_c                   21.7879(7)
_cell_measurement_reflns_used    8058
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.67
_cell_volume                     12642.1(5)
_computing_cell_refinement       'Bruker SMART'
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1239
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            297704
_diffrn_reflns_theta_full        29.46
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    22.395
_exptl_absorpt_correction_T_max  0.4132
_exptl_absorpt_correction_T_min  0.1034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.689
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12352
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.224
_refine_diff_density_min         -2.719
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         17957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                13772
_reflns_number_total             17957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100050r_si_002_4.cif
_cod_data_source_block           p4m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_database_code               4315583