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_4337905
_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         'P2 O61 Ru W17, C2 H6 S O, K8, 16(H2 O)'
_chemical_formula_sum            'C2 H38 K8 O78 P2 Ru S W17'
_chemical_formula_weight         4943.4
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                97.9960(14)
_cell_angle_beta                 90.9513(15)
_cell_angle_gamma                112.9434(12)
_cell_formula_units_Z            2
_cell_length_a                   12.5844(5)
_cell_length_b                   15.1035(6)
_cell_length_c                   22.2140(9)
_cell_measurement_reflns_used    19905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.037
_cell_measurement_theta_min      2.103
_cell_volume                     3838.7(3)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.798
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_radiation_source         'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.83095
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.798
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19905
_diffrn_reflns_point_group_measured_fraction_full 0.798
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        29.905
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_min         2.103
_exptl_absorpt_coefficient_mu    38.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4158
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.001
_refine_diff_density_max         6.836
_refine_diff_density_min         -4.455
_refine_diff_density_rms         0.678
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11175
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1685P)^2^+256.4501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2547
_refine_ls_wR_factor_ref         0.2679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8715
_reflns_number_total             11175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic403041s_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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

 Adding full bibliography for 4337904--4337905.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C2 H38 K8 O78 P2 Ru S1 W17'
_cod_database_code               4337905
_shelx_estimated_absorpt_t_min   0.041
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-3
_shelx_res_checksum              46842
_shelx_hkl_checksum              2123