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_4324293
_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_absolute_configuration ad
_chemical_formula_moiety         '(Re 7+)2, (O 2-)5, (SO4 2-)2'
_chemical_formula_sum            'O13 Re2 S2'
_chemical_formula_weight         644.52
_chemical_name_common            Dirhenium(VII)-pentaoxide-bis(sulfate)
_space_group_IT_number           32
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      32
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6485(11)
_cell_length_b                   8.4260(8)
_cell_length_c                   5.9075(7)
_cell_measurement_reflns_used    164
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     480.27(9)
_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 0.850
_diffrn_measured_fraction_theta_max 0.850
_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  0.1762
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4142
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         4.22
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    25.688
_exptl_absorpt_correction_T_max  0.0747
_exptl_absorpt_correction_T_min  0.0601
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED 1.22 (Stoe, 2001)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    4.457
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.491
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.408
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.0020(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   0.882
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         855
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                764
_reflns_number_total             855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101455z_si_003.cif
_cod_data_source_block           Re2O5(SO4)2_I
_cod_database_code               4324293