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_4308656
_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)(Hg O2)(As O4)2'
_chemical_formula_sum            'Ag4 As2 Hg5 O10'
_chemical_formula_weight         1744.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   6.0261(9)
_cell_length_b                   6.0261(9)
_cell_length_c                   21.577(4)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.329
_cell_measurement_theta_min      3.778
_cell_volume                     678.57(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7466
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    66.849
_exptl_absorpt_correction_T_max  0.4526
_exptl_absorpt_correction_T_min  0.0272
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Habitus (Herrendorf, 1993-1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    8.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.015
_refine_diff_density_max         7.963
_refine_diff_density_min         -4.577
_refine_diff_density_rms         0.867
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(15)
_refine_ls_extinction_coef       0.00030(15)
_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   1.132
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1362
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0920P)^2^+16.8144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                1292
_reflns_number_total             1362
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0484912si20041027_114324_1.cif
_cod_data_source_block           AgHgAsO
_cod_original_cell_volume        678.56(19)
_cod_database_code               4308656