Crystal Structure and Replacement Reaction of Coordinated Water Molecules of the Heteropoly Compounds of Sandwich-Type Tungstoarsenates
Li-Hua Bi; En-Bo Wang; Jun Peng; Ru-Dan Huang; Lin Xu; Chang-Wen Hu; Inorganic Chemistry 39 (2000) 671–679; doi:10.1021/ic990596v

data_4300054
_publ_section_title
;
Crystal Structure and Replacement Reaction of Coordinated Water Molecules
of the Heteropoly Compounds of Sandwich-Type Tungstoarsenates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              671
_journal_page_last               679
_journal_paper_doi               10.1021/ic990596v
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'As4 Cu4 H98 Na16 O161 W30'
_chemical_formula_weight         9111.96
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                89.90(3)
_cell_angle_beta                 77.32(3)
_cell_angle_gamma                89.96(3)
_cell_formula_units_Z            2
_cell_length_a                   12.721(3)
_cell_length_b                   24.516(5)
_cell_length_c                   26.450(5)
_cell_measurement_temperature    293(2)
_cell_volume                     8048(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.1498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20958
_diffrn_reflns_theta_max         21.09
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    22.833
_exptl_crystal_density_diffrn    3.760
_exptl_crystal_F_000             8060
_refine_diff_density_max         4.144
_refine_diff_density_min         -3.498
_refine_diff_density_rms         0.628
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.889
_refine_ls_goodness_of_fit_obs   1.167
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         15816
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.1740
_refine_ls_R_factor_obs          0.0974
_refine_ls_shift/esd_max         12.530
_refine_ls_shift/esd_mean        0.477
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3109
_refine_ls_wR_factor_obs         0.2320
_reflns_number_observed          7882
_reflns_number_total             17317
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8047.7(28)
_cod_original_formula_sum        'H98 As4 Cu4 Na16 O161 W30'
_cod_database_code               4300054