Sulfates of the Refractory Metals: Crystal Structure and Thermal Behavior of Nb2O2(SO4)3, MoO2(SO4), WO(SO4)2, and Two Modifications of Re2O5(SO4)2
Ulf Betke; Mathias S. Wickleder; Inorganic Chemistry 50 (2011) 858–872; doi:10.1021/ic101455z

data_4324291
_publ_contact_author_address
;
  Institut f\"ur Reine und Angewandte Chemie,
  Fakult\"at f\"ur Mathematik und Naturwissenschaften
  der Carl von Ossietzky Universit\"at Oldenburg
  Postfach 2503
  D-26111 Oldenburg
  Germany
;
_publ_contact_author_email       'mathias.wickleder@uni-oldenburg.de '
_publ_contact_author_fax         '049 441 798-3352'
_publ_contact_author_name        'Prof. Dr. Mathias S. Wickleder'
_publ_contact_author_phone       '049 441 798-3660'
_publ_section_title
;
 Sulfates of the Refractory Metals: Crystal Structure and Thermal Behavior
 of Nb2O2(SO4)3, MoO2(SO4), WO(SO4)2, and Two Modifications of Re2O5(SO4)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              858
_journal_page_last               872
_journal_paper_doi               10.1021/ic101455z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '(Mo 6+), (O 2-)2, (SO4 2-)'
_chemical_formula_sum            'Mo O6 S'
_chemical_formula_weight         224.00
_chemical_name_common            Molybdenum(VI)-dioxide-sulfate
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.567(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   8.5922(6)
_cell_length_b                   12.2951(6)
_cell_length_c                   25.671(2)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     2703.3(3)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED 1.22 (Stoe, 2001)'
_computing_molecular_graphics    'Diamond 3.2 (Brandenburg, 2010)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Stoe IPDS I'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16473
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.309
_exptl_absorpt_correction_T_max  0.6730
_exptl_absorpt_correction_T_min  0.3905
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED 1.22 (Stoe, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.302
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00110(4)
_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_ref   0.973
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0166
_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^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0399
_refine_ls_wR_factor_ref         0.0409
_reflns_number_gt                2215
_reflns_number_total             2609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101455z_si_001.cif
_cod_data_source_block           MoO2(SO4)
_cod_original_cell_volume        2703.4(3)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4324291