Preparation and Redox Studies of α1- and α2-Isomers of Mono-Ru-Substituted Dawson-type Phosphotungstates with a DMSO Ligand: [α1/α2-P2W17O61Ru(II)(DMSO)](8-)
Ogo, Shuhei; Shimizu, Noriko; Nishiki, Kensuke; Yasuda, Nobuhiro; Mizuta, Tsutomu; Sano, Tsuneji; Sadakane, Masahiro; Inorganic chemistry 53 (2014) 3526–; doi:10.1021/ic403041s

data_4337904
_publ_section_title
;
 Preparation and Redox Studies of \a1- and \a2-Isomers of
 Mono-Ru-Substituted Dawson-type Phosphotungstates with a DMSO Ligand:
 [\a1/\a2-P2W17O61Ru(II)(DMSO)](8-)
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3526
_journal_paper_doi               10.1021/ic403041s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'(K +)8, (P2 W17 O61 Ru 8-), (C2 H6 O S), 16(H2 O)'
_chemical_formula_sum            'C2 H38 K8 O78 P2 Ru S W17'
_chemical_formula_weight         4943.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   no
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.395(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.173(2)
_cell_length_b                   20.597(4)
_cell_length_c                   14.857(3)
_cell_measurement_temperature    123
_cell_volume                     3641.6(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21081
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    27.580
_exptl_absorpt_correction_T_max  0.7700
_exptl_absorpt_correction_T_min  0.0959
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4348
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.638
_refine_diff_density_min         -3.003
_refine_diff_density_rms         0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8720
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+69.1709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                6086
_reflns_number_total             8720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403041s_si_003.cif
_cod_data_source_block           shimizu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337904--4337905.cif.
;
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               4337904