Wheel-Shaped Cu20-Tungstophosphate [Cu20X(OH)24(H2O)12(P8W48O184)]25- Ion (X = Cl, Br, I) and the Role of the Halide Guest
Sib Sankar Mal; Bassem S. Bassil; Masooma Ibrahim; Saritha Nellutla; Johan van Tol; Naresh S. Dalal; Jorge A. Fernández; Xavier López; Josep M. Poblet; Rosa Ngo Biboum; Bineta Keita; Ulrich Kortz; Inorganic Chemistry 48 (2009) 11636–11645; doi:10.1021/ic901641f

data_4303850
_publ_contact_author_address
;
School of Engineering and Science, 
Jacobs University, P.O. Box 750 561, 
28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_name        'Ulrich Kortz'
_publ_section_title
;
Wheel-Shaped Cu20-Tungstophosphate [Cu20X(OH)24(H2O)12(P8W48O184)]25- Ion
(X = Cl, Br, I) and the Role of the Halide Guest
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11636
_journal_page_last               11645
_journal_paper_doi               10.1021/ic901641f
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Cu20 H148 I K12 Li13 O270 P8 W48'
_chemical_formula_weight         15498.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 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                   26.9335(3)
_cell_length_b                   26.9335(3)
_cell_length_c                   21.0993(7)
_cell_measurement_reflns_used    6921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.39
_cell_volume                     15305.7(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1378
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            170034
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    20.260
_exptl_absorpt_correction_T_max  0.3518
_exptl_absorpt_correction_T_min  0.1494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             13460
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         5.086
_refine_diff_density_min         -9.898
_refine_diff_density_rms         0.579
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         9467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1170P)^2^+1967.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                7293
_reflns_number_total             9467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901641f_si_001_2.cif
_cod_data_source_block           i4m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'H148 Cu20 I K12 Li13 O270 P8 W48'
_cod_database_code               4303850