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_1507785
_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 H5 Cl1 Mo2 O12 Si)2-,2(C24 H20 P)+ '
_chemical_formula_sum            'C50 H45 Cl Mo2 O12 P2 Si'
_chemical_formula_weight         1155.22
_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                76.03(2)
_cell_angle_beta                 79.39(2)
_cell_angle_gamma                61.18(2)
_cell_formula_units_Z            2
_cell_length_a                   13.467(3)
_cell_length_b                   13.548(3)
_cell_length_c                   15.931(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      15
_cell_volume                     2463.4(10)
_computing_cell_refinement
; 
 Cad4 Express, (Enraf-Nonius, 1989) 
;
_computing_data_collection
; 
 Cad4 Express, (Enraf-Nonius, 1989) 
;
_computing_data_reduction
; 
 RC93 (Watkin, Prout & Lilley, 1994) 
;
_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
; 
 SHELXS 86 (Sheldrick, 1986) 
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
; 
Enraf-Nonius CAD4 
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10103
_diffrn_reflns_theta_full        25.976
_diffrn_reflns_theta_max         25.976
_diffrn_reflns_theta_min         1.321
_diffrn_standards_decay_%        7.79
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_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    1.557
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             1172.000
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.41
_refine_diff_density_min         -1.49
_refine_ls_extinction_coef       723.5
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0605
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7933
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001373
_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 
 
 8.83 0.697 7.24 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0589
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0583
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7931
_reflns_number_total             9666
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            LS_5cif.cif
_cod_data_source_block           LS-5
_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_formula_sum        ' C50 H45 Cl1 Mo2 O12 P2 Si '
_cod_database_code               1507785