Selective conversion of {Mo132} Keplerate ion into 4-electron reduced crown-capped Keggin derivative [Te5Mo15O57]^8-^. A key intermediate to single phase M1 multielement MoVTeO light alkanes oxidation catalyst
Romain Canioni; Catherine Marchal-Roch; Nathalie Leclerc-Laronze; Mohamed Haouas; Francis Taulèlle; Jérôme Marrot; Sebastien Paul; Carole Lamonier; Jean-François Paul; Stéphane Loridant; Jean-Marc M. Millet; Emmanuel Cadot; Chem.Commun. 47 (2011) 6413–; doi:10.1039/c1cc11296a

data_7106468
_publ_section_title
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 Selective conversion of {Mo132} Keplerate ion into 4-electron reduced
 crown-capped Keggin derivative [Te5Mo15O57]^8-^. A key intermediate to
 single phase M1 multielement MoVTeO light alkanes oxidation catalyst
;
_journal_name_full               Chem.Commun.
_journal_page_first              6413
_journal_paper_doi               10.1039/c1cc11296a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'H124 Mo30 N11 Na5 O154 Te10'
_chemical_formula_weight         7012.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.251(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8349(18)
_cell_length_b                   25.5476(18)
_cell_length_c                   26.003(2)
_cell_measurement_temperature    293(2)
_cell_volume                     14855.1(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            56074
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    4.510
_exptl_absorpt_correction_T_max  0.6612
_exptl_absorpt_correction_T_min  0.2656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    3.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             13072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.296
_refine_diff_density_min         -4.790
_refine_diff_density_rms         0.627
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         21571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2568
_reflns_number_gt                12815
_reflns_number_total             21571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11296a.txt
_cod_data_source_block           te5mo15
_cod_depositor_comments
;

2024-04-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         3506.13
_cod_original_formula_units_Z            8
_cod_original_cell_volume        14855.3(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'H62 Mo15 N5.50 Na2.50 O77 Te5'
_cod_database_code               7106468