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_4308987
_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_compound_source        'Local laboratory'
_chemical_formula_moiety         'C3 N3 O Tl'
_chemical_formula_sum            'C3 N3 O Tl'
_chemical_formula_weight         298.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5729(7)
_cell_length_b                   8.0012(7)
_cell_length_c                   17.765(1)
_cell_measurement_reflns_used    1254
_cell_measurement_temperature    200
_cell_volume                     1502.85(19)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction
;
Denzo and Scalepak (Otwinowski & Minor, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.11441
_diffrn_orient_matrix_UB_12      -0.02790
_diffrn_orient_matrix_UB_13      0.04052
_diffrn_orient_matrix_UB_21      -0.02789
_diffrn_orient_matrix_UB_22      -0.01464
_diffrn_orient_matrix_UB_23      -0.08885
_diffrn_orient_matrix_UB_31      0.01468
_diffrn_orient_matrix_UB_32      -0.05397
_diffrn_orient_matrix_UB_33      0.00428
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5769
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.59
_exptl_absorpt_coefficient_mu    21.414
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.162
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Herrendorf, W. & B/"arnighausen, H.:
HABITUS, a program for numerical absorption
correction, University of Giessen, Germany, 1997.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.64
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.180
_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   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0073P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0343
_reflns_number_gt                744
_reflns_number_total             908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485918si20041008_073324_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1502.8(2)
_cod_database_code               4308987