New Mercury Vanadium Phosphate Hydrate Hg4-xO1-y(VO)(PO4)2.H2O with Unprecedented Tetrahedral Oxo-Cluster [Hg~4O~5]
E. Le Fur; R. Gautier; E. Furet; J. Y. Pivan; Inorganic Chemistry 41 (2002) 4227–4231; doi:10.1021/ic020229a

data_4318323
_publ_contact_author
;
        Jean Yves Pivan
        Laboratoire de Physicochimie
        ecole Nationale Superieure de Chimie
        Campus de Beaulieu
        Avenue du General Leclerc
        35000 Rennes
        France
        Identification number       IC020229A
;
_publ_contact_author_email       jean-yves.pivan@ensc-rennes.fr
_publ_section_title
;
 New Mercury Vanadium Phosphate Hydrate Hg4-xO1-y(VO)(PO4)2.H2O with
 Unprecedented Tetrahedral Oxo-Cluster [Hg~4O~5]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4227
_journal_page_last               4231
_journal_paper_doi               10.1021/ic020229a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'H2 Hg3.87 O10.77 P2 V'
_chemical_formula_weight         1063.58
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   6.3632(2)
_cell_length_b                   12.4155(5)
_cell_length_c                   14.2292(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.04
_cell_measurement_theta_min      2.18
_cell_volume                     1124.14(7)
_computing_cell_refinement       'DENZO (Otwinowski, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski, 1997)'
_computing_molecular_graphics    'DIAMOND 2.0 (Brandenbourg, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare,1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'w-f 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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23705
_diffrn_reflns_theta_full        35.04
_diffrn_reflns_theta_max         35.04
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    53.803
_exptl_absorpt_correction_T_max  0.362
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   'SORTAV (Blessing 1995)'
_exptl_crystal_colour            greenish
_exptl_crystal_density_diffrn    6.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1803
_exptl_crystal_size_max          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.176
_refine_diff_density_min         -2.945
_refine_diff_density_rms         0.474
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(10)
_refine_ls_extinction_coef       0.00039(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   1.298
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.004
_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          0.0561
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                4014
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020229a.cif
_cod_data_source_block           hgvpo
_cod_database_code               4318323