2D and 3D Polymeric Wells-Dawson Polyoxometelates: Synthesis, Crystal Structures, and Cyclic Voltammetry of [(M(H2O)4)x][H6-2xP2W18-nMonO62] (M = CuII, CoII, NiII)
Robila Belghiche; Ouahiba Bechiri; Mostefa Abbessi; Stéphane Golhen; Yann Le Gal; Lahcène Ouahab; Inorganic Chemistry 48 (2009) 6026–6033; doi:10.1021/ic9003406

data_4302489
_publ_contact_author_address
;Organom\'etalliques et Mat\'eriaux Mol\'eculaires
UMR 6226 CNRS-Universit\'e de Rennes 1
Sciences Chimiques de Rennes
Avenue G\'en\'eral Leclerc
35042 Rennes Cedex
France
;
_publ_contact_author_email       lahcene.ouahab@univ-rennes1.fr
_publ_contact_author_fax         +33(0)223236840
_publ_contact_author_name        'Lahc\`ene Ouahab'
_publ_contact_author_phone       +33(0)223235659
_publ_section_title
;
2D and 3D Polymeric Wells-Dawson Polyoxometelates: Synthesis, Crystal
Structures, and Cyclic Voltammetry of [(M(H2O)4)x][H6-2xP2W18-nMonO62]
(M = CuII, CoII, NiII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6026
_journal_page_last               6033
_journal_paper_doi               10.1021/ic9003406
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[Cu(H2O)4]2.5[HP2W18O62],11.33H2O'
_chemical_formula_sum            'Cu2.5 H43.67 O83.33 P2 W18'
_chemical_formula_weight         4907.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   none
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.2890(9)
_cell_length_b                   15.2890(9)
_cell_length_c                   55.9800(10)
_cell_measurement_reflns_used    56784
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.910
_cell_volume                     11332.4(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            66668
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    28.130
_exptl_crystal_density_diffrn    4.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             12869
_refine_diff_density_max         3.262
_refine_diff_density_min         -4.210
_refine_diff_density_rms         0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+266.2549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                4307
_reflns_number_total             6056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003406_si_001_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'H43.67 Cu2.50 O83.33 P2 W18'
_cod_database_code               4302489