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_4300778
_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
'(Cs+)3 (K+)3, C10 H16 O40 P1 Ru1 W11 6-,4(H20)'
_chemical_formula_sum            'C10 H24 Cs3 K3 O44 P Ru W11'
_chemical_formula_weight         3518.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-21-07
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 95.85(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.631(6)
_cell_length_b                   12.0258(17)
_cell_length_c                   21.892(4)
_cell_measurement_reflns_used    223
_cell_measurement_temperature    295
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      3.2
_cell_volume                     5665(2)
_computing_cell_refinement
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_computing_data_collection
; 

 COLLECT (Nonius BV, 1997) 

;
_computing_data_reduction
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_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 0.995
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type
; 

Nonius Kappa CCD 

;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32088
_diffrn_reflns_theta_full        22.803
_diffrn_reflns_theta_max         30.004
_diffrn_reflns_theta_min         2.024
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.734
_exptl_absorpt_correction_T_max  0.372
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 

 DIFABS (Walker & Stuart, 1983) 

;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    4.125
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             6028
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         16.63
_refine_diff_density_min         -5.84
_refine_ls_extinction_coef       30.165
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.002208
_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: 

 0.546 0.476 0.266 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1790
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0914
_reflns_limit_h_max              29
_reflns_limit_h_min              -29
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                6377
_reflns_number_total             15053
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic0482180si20041217_101512.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        'C10 H24 Cs3 K3 O44 P1 Ru1 W11'
_cod_database_code               4300778