Crystal structures of three novel dioxotetraperoxodi(molybdenum) heteropolyanions in [PPh4]2[R2SiO2{Mo2O2(mu-O2)2(O2)2}] (R2 = (CH3)2, (i-C4H9)2 or (CH3)(CH2Cl)) and characterization of their tungsten analogues
Salles, L; Piquemal, J Y; Mahha, Y; Gentil,M; Herson, P; Bregeault, M; Polyhedron 26 (2007) 4786–4792; doi:10.1016/j.poly.2007.06.007

data_1507783
_publ_section_title
;
 Crystal structures of three novel dioxotetraperoxodi(molybdenum)
 heteropolyanions in [PPh4]2[R2SiO2{Mo2O2(mu-O2)2(O2)2}] (R2 = (CH3)2,
 (i-C4H9)2 or (CH3)(CH2Cl)) and characterization of their tungsten
 analogues
;
_journal_issue                   17
_journal_name_full               Polyhedron
_journal_page_first              4786
_journal_page_last               4792
_journal_paper_doi               10.1016/j.poly.2007.06.007
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source
;
?
;
_chemical_formula_moiety         '(C2 H6 Mo2 O12  Si)2-, 2(C24 H20 P1)+'
_chemical_formula_sum            'C50 H46 Mo2 O12 P2 Si'
_chemical_formula_weight         1120.78
_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
_cell_angle_alpha                76.99(3)
_cell_angle_beta                 77.80(2)
_cell_angle_gamma                61.03(2)
_cell_formula_units_Z            2
_cell_length_a                   13.395(3)
_cell_length_b                   13.474(6)
_cell_length_c                   15.877(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      15
_cell_volume                     2425.0(14)
_computing_cell_refinement
; 
 USER DEFINED 6 
;
_computing_data_collection
; 
 DATA COLLECTION 
;
_computing_data_reduction
; 
 USER DEFINED 5 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 USER DEFINED STRUCTURE SOLUTION 
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
; 
Unknown 
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8900
_diffrn_reflns_theta_full        24.972
_diffrn_reflns_theta_max         24.972
_diffrn_reflns_theta_min         1.326
_diffrn_standards_decay_%        19.06
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             1140.000
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1236
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         5252
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.000279
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 4.56 -0.910 3.40 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0557
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0532
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5252
_reflns_number_total             8499
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            LS_1cif.cif
_cod_data_source_block           LS-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C50 H46 Mo2 O12 P2 Si '
_cod_database_code               1507783