Route for the Elaboration of Functionalized Hybrid 3d-Substituted Trivacant Keggin Anions
Guillaume Rousseau; Olivier Oms; Anne Dolbecq; Jérôme Marrot; Pierre Mialane; Inorganic Chemistry 50 (2011) 7376–7378; doi:10.1021/ic2011088

data_4325957
_publ_contact_author
; 
      Pr P. Mialane
      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       mialane@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83 '
_publ_section_title
;
 Route for the Elaboration of Functionalized Hybrid 3d-Substituted
 Trivacant Keggin Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7376
_journal_page_last               7378
_journal_paper_doi               10.1021/ic2011088
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H36 K24.75 Na1.75 Ni17.5 O219 Si4 W36'
_chemical_formula_weight         12666.93
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.291(4)
_cell_angle_beta                 81.552(5)
_cell_angle_gamma                87.936(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5203(13)
_cell_length_b                   28.513(3)
_cell_length_c                   37.719(4)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.25
_cell_volume                     13270(2)
_computing_cell_refinement       'Bruker SAINT'
_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      200(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            422308
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         0.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.249
_exptl_absorpt_correction_T_max  0.5454
_exptl_absorpt_correction_T_min  0.1299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.170
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             11335
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.669
_refine_diff_density_min         -2.850
_refine_diff_density_rms         0.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3163
_refine_ls_number_reflns         77308
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0494P)^2^+836.6871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                61663
_reflns_number_total             77308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2011088_si_002_4.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C30 H36 K24.75 Na1.75 Ni17.50 O219 Si4 W36'
_cod_database_code               4325957