Synthesis, Characterization, and Photochemical Behavior of {Ru(arene)}2+Derivatives of α-[PW11O39]7-: An Organometallic Way to Ruthenium-Substituted Heteropolytungstates
Artero, V.; Laurencin, D.; Villanneau, R.; Thouvenot, R.; Herson, P.; Gouzerh, P.; Proust, A.; Inorganic Chemistry 44 (2005) 2826–2835; doi:10.1021/ic0482180

data_4300777
_publ_section_title
;
 Synthesis, Characterization, and Photochemical Behavior of
 {Ru(arene)}2+Derivatives of \a-[PW11O39]7-: An Organometallic
 Way to Ruthenium-Substituted Heteropolytungstates
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2826
_journal_page_last               2835
_journal_paper_doi               10.1021/ic0482180
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
' 4(K+) 3(Na+),(C12 H12 O80 Ru2 W23) 7-, 6(H20) '
_chemical_formula_sum            'C12 H24 K4 Na3 O86 P2 Ru2 W23'
_chemical_formula_weight         6262.27
_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
_audit_creation_date             04-29-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                95.20(1)
_cell_angle_beta                 97.82(4)
_cell_angle_gamma                97.33(3)
_cell_formula_units_Z            2
_cell_length_a                   13.387(13)
_cell_length_b                   19.829(3)
_cell_length_c                   20.249(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      11.30
_cell_measurement_theta_min      11.00
_cell_volume                     5250(5)
_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 2003) 

;
_computing_structure_refinement
; 

 CRYSTALS (Watkin et al 2003) 

;
_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
; 

 Nonius CAD4 

;
_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  0.076
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19290
_diffrn_reflns_theta_full        24.973
_diffrn_reflns_theta_max         24.973
_diffrn_reflns_theta_min         1.021
_diffrn_standards_decay_%        8.07
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    25.657
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 

 Azimutal absorption correction (North et al, 1968) 

;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    3.96
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.06
_refine_diff_density_min         -3.70
_refine_ls_extinction_coef       30.674
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8070
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.028156
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 

 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 

 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 

 Method = Robust Weighting (Prince, 1982) 

 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 

 A~i~ are: 

 7.11 -2.40 5.34 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0793
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0744
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8070
_reflns_number_total             18420
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic0482180si20041217_101446.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;

The following automatic conversions were performed:

_cell_measurement_temperature value 'ambient' changed to '295(2)' -

took room/ambient temperature average value [293;298] in Kelvins(K).

Automatic conversion script

Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5249(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C12 H24 K4 Na3 O86 P2 Ru2 W23 '
_cod_database_code               4300777