Synthesis and Characterization of Copper-, Zinc-, Manganese-, and Cobalt-Substituted Dimeric Heteropolyanions, [(α-XW~9~O~33~)~2~M~3~(H~2~O)~3~]^n-^ (n = 12, X = As^III^, Sb^III^, M = Cu^2+^, Zn^2+^; n = 10, X = Se^IV^, Te^IV^, M = Cu^2+^) and [(α-AsW~9~O~33~)~2~WO(H~2~O)M~2~(H~2~O)~2~]^10-^ (M = Zn^2+^, Mn^2+^, Co^2+^)
Ulrich Kortz; Noha K. Al-Kassem; Masha G. Savelieff; Nisrine A. Al Kadi; Masahiro Sadakane; Inorganic Chemistry 40 (2001) 4742–4749; doi:10.1021/ic0101477

data_4320181
_publ_contact_author_address
;
Department of Chemistry
American University of Beirut
Bliss street, POB 11-0236
Beirut, LEBANON
;
_publ_contact_author_email
;
ulrich.kortz@aub.edu.lb
;
_publ_contact_author_fax
;
+961 1 744 461
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+961 3 776 439
;
_publ_section_title
;
 Synthesis and Characterization of Copper-, Zinc-, Manganese-, and
 Cobalt-Substituted Dimeric Heteropolyanions,
 [(\a-XW~9~O~33~)~2~M~3~(H~2~O)~3~]^n-^ (n = 12, X = As^III^, Sb^III^, M =
 Cu^2+^, Zn^2+^; n = 10, X = Se^IV^, Te^IV^, M = Cu^2+^) and
 [(\a-AsW~9~O~33~)~2~WO(H~2~O)M~2~(H~2~O)~2~]^10-^ (M = Zn^2+^, Mn^2+^,
 Co^2+^)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4742
_journal_page_last               4749
_journal_paper_doi               10.1021/ic0101477
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'As2 Cu3 Na12 O101 W18'
_chemical_formula_weight         5541.64
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.4050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4989(9)
_cell_length_b                   20.7463(14)
_cell_length_c                   16.7571(11)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.29
_cell_volume                     4426.3(5)
_computing_cell_refinement       'Bruker SMART (Siemens, 1995)'
_computing_data_collection       'Bruker SMART (Siemens, 1995)'
_computing_data_reduction        'Bruker SHELXTL (Sheldrick, 1993b)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 1993b)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 1993b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50077
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    24.917
_exptl_absorpt_correction_T_max  0.120
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4850
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.595
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.478
_refine_ls_extinction_coef       0.000604(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         11094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0408P)^2^+27.5188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                9914
_reflns_number_total             11094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic01014777_2.cif
_cod_data_source_block           na12cu3(asw9)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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               4320181