Organo-Ru supported sandwich-type tungstoarsenates: synthesis, structure and catalytic properties
Meng, Rui-Qi; Suo, Lin; Hou, Guang-Feng; Liang, Jing; Bi, Li-Hua; Li, Hao-Long; Wu, Li-Xin; CrystEngComm 15 (2013) 5867–; doi:10.1039/c3ce00045a

data_7209848
_publ_section_title
;
 Organo-Ru supported sandwich-type tungstoarsenates: synthesis, structure
 and catalytic properties
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5867
_journal_paper_doi               10.1039/c3ce00045a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C18 H53 As2 Na6 Ni4 O83.5 Ru3 W17'
_chemical_formula_sum            'C18 H53 As2 Na6 Ni4 O83.5 Ru3 W17'
_chemical_formula_weight         5556.88 
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.222(3)
_cell_length_b                   21.526(4)
_cell_length_c                   26.316(9)
_cell_measurement_reflns_used    48665
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.01
_cell_volume                     9177(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 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      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1506
_diffrn_reflns_av_sigmaI/netI    0.1238
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67117
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.341
_exptl_absorpt_correction_T_max  0.1645
_exptl_absorpt_correction_T_min  0.1447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9852
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.892
_refine_diff_density_min         -2.672
_refine_diff_density_rms         0.462
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         15652
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0545P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                10199
_reflns_number_total             15652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce00045a.txt
_cod_data_source_block           1
_cod_depositor_comments
;

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H106 As4 Na12 Ni8 O167 Ru6 W34'
_cod_original_formula_weight         11113.77
_cod_original_formula_moiety         'C36 H106 As4 Na12 Ni8 O167 Ru6 W34'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7209848