Further Evidence for the Tetraoxoiodate(V) Anion, IO43-: Hydrothermal Syntheses and Structures of Ba[(MoO2)6(IO4)2O4].H2O and Ba3[(MoO2)2(IO6)2].2H2O
Richard E. Sykora; Daniel M. Wells; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 41 (2002) 2697–2703; doi:10.1021/ic0112746

data_4317984
_publ_contact_author
;
Prof. Thomas E. Albrecht-Schmitt
179 Chemistry Building
Department of Chemistry
Auburn University, AL
36849
;
_publ_contact_author_email       ' albreth@auburn.edu '
_publ_contact_author_fax         ' 334 844 6959 '
_publ_contact_author_phone       ' 334 844 6948 '
_publ_section_title
;
 Further Evidence for the Tetraoxoiodate(V) Anion, IO43-: Hydrothermal
 Syntheses and Structures of Ba[(MoO2)6(IO4)2O4].H2O and
 Ba3[(MoO2)2(IO6)2].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2697
_journal_page_last               2703
_journal_paper_doi               10.1021/ic0112746
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'original synthesis'
_chemical_formula_structural     'Ba3(MoO2)2(IO6)2 2H2O'
_chemical_formula_sum            'Ba3 H4 I2 Mo2 O18'
_chemical_formula_weight         1149.73
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.356(7)
_cell_length_b                   45.544(24)
_cell_length_c                   4.867(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.79
_cell_volume                     2961(3)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7240
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    13.779
_exptl_absorpt_correction_T_max  '0.605663 ratio of min/max'
_exptl_absorpt_correction_T_min  '0.605663 ratio of min/max'
_exptl_absorpt_correction_type   'multiscan (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.141
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    calcd
_exptl_crystal_description       prism
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.759
_refine_diff_density_rms         0.329
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.00000(2)
_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   0.987
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'not located'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_obs          0.0367
_refine_ls_shift/esd_max         -1.396
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0758
_refine_ls_wR_factor_obs         0.0747
_reflns_number_observed          1651
_reflns_number_total             1849
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0112746_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nm' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0316P)^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^)+(0.0316P)^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        2960.6(27)
_cod_original_formula_sum        'Ba3 I2 Mo2 O18 H4'
_cod_database_code               4317984