Solubility, Complex Formation, and Redox Reactions in the Tl2O3-HCN/CN‒H2O System. Crystal Structures of the Cyano Compounds Tl(CN)3.H2O, Na[Tl(CN)4].3H2O, K[Tl(CN)4], and TlI[TlIII(CN)4] and of TlI2C2O4
Péter Nagy; Andreas Fischer; Julius Glaser; Andrey Ilyukhin; Mikhail Maliarik; Imre Tóth; Inorganic Chemistry 44 (2005) 2347–2357; doi:10.1021/ic0485918

data_4308989
_publ_contact_author_address
;
IFM-Department of Chemistry
Link\"oping University
581 83 Link\"oping
Sweden
;
_publ_contact_author_email       ' misha@ifm.liu.se'
_publ_contact_author_name        'Mikhail Maliarik'
_publ_section_title
;
Solubility, Complex Formation, and Redox Reactions in the
Tl2O3-HCN/CN--H2O System. Crystal Structures of the Cyano Compounds
Tl(CN)3.H2O, Na[Tl(CN)4].3H2O, K[Tl(CN)4], and TlI[TlIII(CN)4] and of
TlI2C2O4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2347
_journal_page_last               2357
_journal_paper_doi               10.1021/ic0485918
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C4 H6 N4 Na1 O3 Tl1'
_chemical_formula_sum            'C4 H6 N4 Na O3 Tl'
_chemical_formula_weight         385.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 96.96(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6136(11)
_cell_length_b                   10.7203(14)
_cell_length_c                   19.161(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      13.1
_cell_measurement_wavelength     0.71073
_cell_volume                     2164.1(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.005997
_diffrn_orient_matrix_UB_12      0.093088
_diffrn_orient_matrix_UB_13      -0.001057
_diffrn_orient_matrix_UB_21      -0.024319
_diffrn_orient_matrix_UB_22      -0.000328
_diffrn_orient_matrix_UB_23      0.048814
_diffrn_orient_matrix_UB_31      0.091554
_diffrn_orient_matrix_UB_32      0.005983
_diffrn_orient_matrix_UB_33      0.019502
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3232
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    14.95
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.537
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.28
_refine_ls_extinction_coef       0.0036(2)
_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   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                1679
_reflns_number_total             2258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485918si20041008_073324_4.cif
_cod_data_source_block           3
_cod_database_code               4308989
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1