Hybrid Polyoxometalates: Keggin and Dawson Silyl Derivatives as Versatile Platforms
B. Matt; S. Renaudineau; L.-M. Chamoreau; C. Afonso; G. Izzet; A. Proust; Journal of Organic Chemistry 76 (2011) 3107–3112; doi:10.1021/jo102546v

data_4026231
_publ_section_title
;
 Hybrid Polyoxometalates: Keggin and Dawson Silyl Derivatives as Versatile
 Platforms
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3107
_journal_page_last               3112
_journal_paper_doi               10.1021/jo102546v
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C48 H26 O62 P2 Si2 W17, 6(C16 H36 N)'
_chemical_formula_sum            'C144 H242 N6 O62 P2 Si2 W17'
_chemical_formula_weight         6293.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   notdet
_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            4
_cell_length_a                   18.6980(5)
_cell_length_b                   30.7933(7)
_cell_length_c                   31.3930(8)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      3.3
_cell_volume                     18075.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56301
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.879
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.313
_exptl_crystal_description       prism
_exptl_crystal_F_000             11840
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.127
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.378
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         26138
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1430.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                22073
_reflns_number_total             26138
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo102546v_si_002.cif
_cod_data_source_block           bm158b_0m
_cod_database_code               4026231