Triniobium Polytungstophosphates. Syntheses, Structures, Clarification of Isomerism and Reactivity in the Presence of H2O2
Mason K. Harrup; Gyu-Shik Kim; Huadong Zeng; Rhoma P. Johnson; Don VanDerveer; Craig L. Hill; Inorganic Chemistry 37 (1998) 5550–5556; doi:10.1021/ic980467z

data_4323102
_publ_section_title
;
 Triniobium Polytungstophosphates. Syntheses, Structures, Clarification of
 Isomerism and Reactivity in the Presence of H2O2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5550
_journal_page_last               5556
_journal_paper_doi               10.1021/ic980467z
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'Cl Cs6 H14 Nb3 O49.5 P W9'
_chemical_formula_weight         3603.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.92360(10)
_cell_length_b                   13.5721(2)
_cell_length_c                   22.31890(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.2
_cell_volume                     5123.13(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0818
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31609
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    25.153
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.660
_exptl_crystal_description       'bar shape'
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.353
_refine_diff_density_min         -4.161
_refine_diff_density_rms         0.454
_refine_ls_extinction_coef       0.000025(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.981
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         11944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_restrained_S_obs      1.171
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_obs          0.0538
_refine_ls_shift/esd_max         0.024
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1474
_refine_ls_wR_factor_obs         0.1313
_reflns_number_observed          6892
_reflns_number_total             11944
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980467z.cif
_cod_data_source_block           Hill20(Cs1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0639P)^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^)+(0.0639P)^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_formula_sum        'H14 Cl Cs6 Nb3 O49.5 P W9'
_cod_database_code               4323102