Synthesis and crystal structure of pseudo-sandwich-type heteropolytungstates functionalized by organometallic ruthenium(ii)
Bi, Li-Hua; Hou, Guang-Feng; Li, Bao; Wu, Li-Xin; Kortz, Ulrich; Dalton Transactions  (2009) 6345–6353; doi:10.1039/b821750e

data_7001816
_publ_section_title
;
 Synthesis and crystal structure of pseudo-sandwich-type
 heteropolytungstates functionalized by organometallic ruthenium(ii)
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              6345
_journal_page_last               6353
_journal_paper_doi               10.1039/b821750e
_journal_year                    2009
_chemical_formula_moiety         'C6 H28 Na7 O45 P Ru W9, 3(H2 O)'
_chemical_formula_sum            'C6 H34 Na7 O48 P Ru W9'
_chemical_formula_weight         2821.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.927(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.199(3)
_cell_length_b                   16.958(3)
_cell_length_c                   19.932(3)
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.0164
_cell_measurement_theta_min      2.4020
_cell_volume                     5136.7(16)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25651
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.551
_exptl_absorpt_correction_T_max  0.1900
_exptl_absorpt_correction_T_min  0.1722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.781
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8881
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+2.7977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                7770
_reflns_number_total             8881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821750e.txt
_cod_data_source_block           PWRu
_cod_original_cell_volume        5136.6(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001816