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#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308988.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308988
loop_
_publ_author_name
'Péter Nagy'
'Andreas Fischer'
'Julius Glaser'
'Andrey Ilyukhin'
'Mikhail Maliarik'
'Imre Tóth'
_publ_contact_author_address
;
IFM-Department of Chemistry
Linköping University
581 83 Linköping
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_sum            'C4 K N4 Tl'
_chemical_formula_weight         347.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_primary     direct
_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                   7.5470(9)
_cell_length_b                   7.5470(9)
_cell_length_c                   14.987(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      12
_cell_volume                     853.62(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.721
_diffrn_measured_fraction_theta_max 0.721
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1491
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1121
_diffrn_reflns_theta_full        42.58
_diffrn_reflns_theta_max         42.58
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    19.341
_exptl_absorpt_correction_T_max  0.3068
_exptl_absorpt_correction_T_min  0.2049
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.621
_refine_diff_density_min         -4.497
_refine_diff_density_rms         0.324
_refine_ls_extinction_coef       0.0012(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         1121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0583
_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/[σ²(Fo²)+(0.0360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                567
_reflns_number_total             1121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0485918si20041008_073324_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4308988
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.0000 0.2500 0.1250 0.0338(2) Uani 1 4 d S . .
K1 K 0.5000 0.2500 -0.1250 0.0579(9) Uani 1 4 d S . .
N1 N 0.2817(14) 0.4710(15) -0.0046(10) 0.060(2) Uani 1 1 d . . .
C1 C 0.1838(13) 0.3947(14) 0.0403(6) 0.0454(19) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tl1 0.0383(3) 0.0383(3) 0.0249(2) 0.000 0.000 0.000
K1 0.0562(13) 0.0562(13) 0.061(2) 0.000 0.000 0.000
N1 0.053(5) 0.069(6) 0.059(5) 0.018(6) 0.024(5) -0.015(4)
C1 0.045(4) 0.053(5) 0.038(4) 0.010(4) 0.000(4) 0.011(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Tl1 C1 109.9(3) 6_454 15 ?
C1 Tl1 C1 109.9(3) 6_454 12_666 ?
C1 Tl1 C1 108.5(5) 15 12_666 ?
C1 Tl1 C1 108.5(5) 6_454 . ?
C1 Tl1 C1 109.9(3) 15 . ?
C1 Tl1 C1 109.9(3) 12_666 . ?
N1 K1 N1 111.8(3) 16_655 . ?
N1 K1 N1 104.8(6) 16_655 11_665 ?
N1 K1 N1 111.8(3) . 11_665 ?
N1 K1 N1 111.8(3) 16_655 6_554 ?
N1 K1 N1 104.8(6) . 6_554 ?
N1 K1 N1 111.8(3) 11_665 6_554 ?
N1 K1 N1 173.9(3) 16_655 9_665 ?
N1 K1 N1 63.9(3) . 9_665 ?
N1 K1 N1 73.90(19) 11_665 9_665 ?
N1 K1 N1 73.93(15) 6_554 9_665 ?
N1 K1 N1 63.9(3) 16_655 4_454 ?
N1 K1 N1 73.90(19) . 4_454 ?
N1 K1 N1 73.93(15) 11_665 4_454 ?
N1 K1 N1 173.9(3) 6_554 4_454 ?
N1 K1 N1 110.2(2) 9_665 4_454 ?
N1 K1 N1 73.90(19) 16_655 14_545 ?
N1 K1 N1 73.93(15) . 14_545 ?
N1 K1 N1 173.9(3) 11_665 14_545 ?
N1 K1 N1 63.9(3) 6_554 14_545 ?
N1 K1 N1 108.0(4) 9_665 14_545 ?
N1 K1 N1 110.2(2) 4_454 14_545 ?
N1 K1 N1 73.93(15) 16_655 7_544 ?
N1 K1 N1 173.9(3) . 7_544 ?
N1 K1 N1 63.9(3) 11_665 7_544 ?
N1 K1 N1 73.90(19) 6_554 7_544 ?
N1 K1 N1 110.2(2) 9_665 7_544 ?
N1 K1 N1 108.0(4) 4_454 7_544 ?
N1 K1 N1 110.2(2) 14_545 7_544 ?
C1 N1 K1 115.6(8) . . ?
C1 N1 K1 107.1(10) . 9_665 ?
K1 N1 K1 116.1(3) . 9_665 ?
N1 C1 Tl1 179.8(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 C1 2.175(10) 6_454 ?
Tl1 C1 2.175(10) 15 ?
Tl1 C1 2.175(10) 12_666 ?
Tl1 C1 2.175(10) . ?
K1 N1 2.958(12) 16_655 ?
K1 N1 2.958(12) . ?
K1 N1 2.958(12) 11_665 ?
K1 N1 2.958(12) 6_554 ?
K1 N1 3.305(14) 9_665 ?
K1 N1 3.305(14) 4_454 ?
K1 N1 3.305(14) 14_545 ?
K1 N1 3.305(14) 7_544 ?
N1 C1 1.153(14) . ?
N1 K1 3.305(14) 9_665 ?
