Hydrothermal Syntheses: A Route to the Stepwise Condensation of Reduced Keggin Polyanions. From Reduced β-[HmSiMo12O40]n- Monomers to Bicapped Dimerized [Si2Mo28O84(H2O)2]6- Anions
Anne Dolbecq; Emmanuel Cadot; Dirk Eisner; Francis Sécheresse; Inorganic Chemistry 38 (1999) 4217–4223; doi:10.1021/ic990420t

data_4322479
_publ_contact_author
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      Prof. F. S\'echeresse
      Institut Lavoisier, IREM, UMR C 0173
      Universit\'e de Versailles Saint Quentin
      45 Avenue des Etats Unis
      78035 Versailles cedex
      France
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_publ_contact_author_email       secheres@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 89'
_publ_section_title
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 Hydrothermal Syntheses: A Route to the Stepwise Condensation of Reduced
 Keggin Polyanions. From Reduced \b-[HmSiMo12O40]n- Monomers to Bicapped
 Dimerized [Si2Mo28O84(H2O)2]6- Anions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4217
_journal_page_last               4223
_journal_paper_doi               10.1021/ic990420t
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H48 Mo12 N3 O43.5 Si'
_chemical_formula_weight         2109.90
_chemical_name_systematic
; 
 ? 
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_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.037(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7763(5)
_cell_length_b                   20.2277(8)
_cell_length_c                   20.9784(9)
_cell_measurement_reflns_used    16173
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      1.4
_cell_volume                     5368.3(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24317
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4028
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.00015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         -0.354
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+89.6954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1364
_refine_ls_wR_factor_obs         0.1243
_reflns_number_observed          6070
_reflns_number_total             7733
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990420t_3.cif
_cod_data_source_block           de33
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+89.6954P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+89.6954P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_formula_sum        'C12 H48 Mo12 N3 O43.50 Si'
_cod_database_code               4322479