Hydrothermal Single-Crystal Growth in the Systems Ag/Hg/X/O (X = VV, AsV): Crystal Structures of (Ag3Hg)VO4, (Ag2Hg2)3(VO4)4, and (Ag2Hg2)2(HgO2)(AsO4)2 with the Unusual Tetrahedral Cluster Cations (Ag3Hg)3+ and (Ag2Hg2)4+ and Crystal Structure of AgHgVO4
Matthias Weil; Ekkehart Tillmanns; Dmitry Yu. Pushcharovsky; Inorganic Chemistry 44 (2005) 1443–1451; doi:10.1021/ic0484912

data_4308658
_publ_contact_author_address
;  
Institute for Chemical Technologies and Analytics
Division of Structural Chemistry
Vienna University of Technology
Getreidemarkt 9/164-SC
A-1060 Vienna
Austria       
;
_publ_contact_author_email       mweil@mail.zserv.tuwien.ac.at
_publ_contact_author_fax         '+43 1 58801 17199'
_publ_contact_author_name
;       
Matthias Weil       
;
_publ_contact_author_phone       '+43 1 58801 17122'
_publ_section_title
;
Hydrothermal Single-Crystal Growth in the Systems Ag/Hg/X/O (X = VV,
AsV): Crystal Structures of (Ag3Hg)VO4, (Ag2Hg2)3(VO4)4, and
(Ag2Hg2)2(HgO2)(AsO4)2 with the Unusual Tetrahedral Cluster Cations
(Ag3Hg)3+ and (Ag2Hg2)4+ and Crystal Structure of AgHgVO4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1443
_journal_page_last               1451
_journal_paper_doi               10.1021/ic0484912
_journal_volume                  44
_journal_year                    2005
_chemical_formula_structural     '(Ag2 Hg2)3 (V O4)4'
_chemical_formula_sum            'Ag6 Hg6 O16 V4'
_chemical_formula_weight         2310.52
_chemical_name_common            'Silver mercury vanadate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   none
_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            4
_cell_length_a                   12.6295(13)
_cell_length_b                   12.6295(13)
_cell_length_c                   12.566(3)
_cell_measurement_reflns_used    3378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.421
_cell_measurement_theta_min      3.955
_cell_volume                     2004.3(6)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SMART (SIEMENS)'
_diffrn_measurement_method       \w
_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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14721
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    53.301
_exptl_absorpt_correction_T_max  0.1226
_exptl_absorpt_correction_T_min  0.0904
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Habitus (Herrendorf, 1993-1997)
;
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    7.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       spheroid
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.013
_refine_diff_density_min         -2.033
_refine_diff_density_rms         0.534
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_coef       0.00057(6)
_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   1.062
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+138.8349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                1199
_reflns_number_total             1524
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0484912si20041027_114324_3.cif
_cod_data_source_block           AgHgVO
_cod_original_cell_volume        2004.3(5)
_cod_database_code               4308658