Polyoxometalates Paneling through {Mo~2~O~2~S~2~} Coordination: Cation-Directed Conformations and Chemistry of a Supramolecular Hexameric Scaffold
Jérôme Marrot; Marie Anne Pilette; Mohamed Haouas; Sébastien Floquet; Francis Taulelle; Xavier López; Josep M. Poblet; Emmanuel Cadot; Journal of the American Chemical Society 134 (2012) 1724–1737; doi:10.1021/ja2090383

data_4117332
_publ_contact_author
; 
      Pr E. Cadot
      Institut Lavoisier de Versailles, ILV, UMR CNRS 8180
      Universit\'e de Versailles Saint-Quentin-en-Yvelines
      45 Avenue des Etats Unis
      78035 Versailles Cedex
      France
;
_publ_contact_author_email       cadot@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 82'
_publ_section_title
;
 Polyoxometalates Paneling through {Mo~2~O~2~S~2~} Coordination:
 Cation-Directed Conformations and Chemistry of a Supramolecular Hexameric
 Scaffold
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1724
_journal_page_last               1737
_journal_paper_doi               10.1021/ja2090383
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'As6 H192 K34.5 Mo18 Na1.5 O312 S18 W54'
_chemical_formula_weight         19250.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.196(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.1120(9)
_cell_length_b                   44.9910(17)
_cell_length_c                   38.4158(13)
_cell_measurement_reflns_used    8945
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.47
_cell_measurement_theta_min      2.27
_cell_volume                     36276(2)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_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      296(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            412250
_diffrn_reflns_theta_full        22.68
_diffrn_reflns_theta_max         22.68
_diffrn_reflns_theta_min         0.70
_exptl_absorpt_coefficient_mu    18.789
_exptl_absorpt_correction_T_max  0.3148
_exptl_absorpt_correction_T_min  0.1330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.525
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             34392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.477
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4009
_refine_ls_number_reflns         48232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+244.6541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                34609
_reflns_number_total             48232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2090383_si_003.cif
_cod_data_source_block           KNa_1b
_cod_original_formula_sum        'H192 As6 K34.50 Mo18 Na1.50 O312 S18 W54'
_cod_database_code               4117332