#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/98/2239821.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2239821
loop_
_publ_author_name
'Weil, Matthias'
'Häusler, Thomas'
_publ_section_title
;
 Crystal structure of K[Hg(SCN)₃] -- a redetermination
;
_journal_coeditor_code           HB0013
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i46
_journal_paper_doi               10.1107/S1600536814013403
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'K [Hg (N C S)3]'
_chemical_formula_structural     'K [Hg (S C N)3]'
_chemical_formula_sum            'C3 Hg K N3 S3'
_chemical_formula_weight         413.93
_chemical_name_common            'Potassium mercury tris-thiocyanate'
_chemical_name_systematic
;
Potassium [trithiocyanatomercurate(II)]
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     isomor
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.951(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2727(11)
_cell_length_b                   4.0775(4)
_cell_length_c                   10.9764(10)
_cell_measurement_reflns_used    4570
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.696
_cell_measurement_theta_min      3.407
_cell_volume                     457.44(8)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ATOMS for Windows (Dowty, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω and φ scans'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11940
_diffrn_reflns_theta_full        44.43
_diffrn_reflns_theta_max         44.43
_diffrn_reflns_theta_min         3.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.899
_exptl_absorpt_correction_T_max  .5042
_exptl_absorpt_correction_T_min  .2258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.334
_refine_ls_extinction_coef       0.0219(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+0.0583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                2358
_reflns_number_total             3765
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hb0013sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2239821
_cod_database_fobs_code          2239821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Hg Hg1 0.145383(12) 0.2500 0.725128(12) 0.03813(6) Uani d S 1 2
K K1 0.59433(8) 0.7500 0.71536(7) 0.03802(15) Uani d S 1 2
S S1 0.12455(7) 0.2500 0.49391(8) 0.03495(17) Uani d S 1 2
S S2 0.32808(7) 0.7500 0.80993(8) 0.03121(14) Uani d S 1 2
S S3 0.06157(10) 0.2500 0.89262(10) 0.0704(4) Uani d S 1 2
C C1 0.2848(3) 0.2500 0.5314(3) 0.0313(6) Uani d S 1 2
C C2 0.3579(3) 0.7500 0.9719(3) 0.0312(6) Uani d S 1 2
C C3 0.9019(4) 0.2500 0.7977(4) 0.0357(6) Uani d S 1 2
N N1 0.3940(3) 0.2500 0.5574(3) 0.0477(8) Uani d S 1 2
N N2 0.6210(4) 0.2500 0.9165(3) 0.0500(8) Uani d S 1 2
N N3 0.7909(4) 0.2500 0.7382(4) 0.0601(10) Uani d S 1 2
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'
S S 0.1246 0.1234 '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'
Hg Hg -2.3894 9.2266 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
S3 Hg1 S1 . . 154.06(3)
S3 Hg1 S2 . . 102.74(2)
S1 Hg1 S2 . . 94.65(2)
S3 Hg1 S2 . 1_545 102.74(2)
S1 Hg1 S2 . 1_545 94.65(2)
S2 Hg1 S2 . 1_545 95.00(2)
N2 K1 N2 1_565 . 88.34(9)
N2 K1 N3 1_565 1_565 67.60(10)
N2 K1 N3 . 1_565 125.76(10)
N2 K1 N3 1_565 . 125.76(10)
N2 K1 N3 . . 67.60(10)
N3 K1 N3 1_565 . 87.70(10)
N2 K1 N1 1_565 . 136.39(10)
N2 K1 N1 . . 76.98(8)
N3 K1 N1 1_565 . 151.42(11)
N3 K1 N1 . . 86.24(8)
N2 K1 N1 1_565 1_565 76.98(8)
N2 K1 N1 . 1_565 136.39(10)
N3 K1 N1 1_565 1_565 86.24(7)
N3 K1 N1 . 1_565 151.42(11)
N1 K1 N1 . 1_565 85.87(8)
N2 K1 N1 1_565 3_666 135.00(5)
N2 K1 N1 . 3_666 135.00(5)
N3 K1 N1 1_565 3_666 75.01(9)
N3 K1 N1 . 3_666 75.01(9)
N1 K1 N1 . 3_666 76.45(8)
N1 K1 N1 1_565 3_666 76.45(8)
N2 K1 C1 1_565 3_666 129.27(7)
N2 K1 C1 . 3_666 129.27(7)
N3 K1 C1 1_565 3_666 62.76(8)
N3 K1 C1 . 3_666 62.76(8)
N1 K1 C1 . 3_666 89.79(8)
N1 K1 C1 1_565 3_666 89.79(8)
N1 K1 C1 3_666 3_666 18.38(8)
N2 K1 S2 1_565 . 67.14(8)
N2 K1 S2 . . 67.14(8)
N3 K1 S2 1_565 . 132.15(6)
N3 K1 S2 . . 132.15(6)
N1 K1 S2 . . 69.32(6)
N1 K1 S2 1_565 . 69.32(6)
N1 K1 S2 3_666 . 132.49(6)
C1 K1 S2 3_666 . 150.86(6)
N2 K1 K1 1_565 1_545 134.17(5)
N2 K1 K1 . 1_545 45.83(5)
N3 K1 K1 1_565 1_545 133.85(5)
N3 K1 K1 . 1_545 46.15(5)
N1 K1 K1 . 1_545 47.06(4)
N1 K1 K1 1_565 1_545 132.94(4)
N1 K1 K1 3_666 1_545 90.0
C1 K1 K1 3_666 1_545 90.0
S2 K1 K1 . 1_545 90.0
N2 K1 K1 1_565 1_565 45.83(5)
N2 K1 K1 . 1_565 134.17(5)
N3 K1 K1 1_565 1_565 46.15(5)
N3 K1 K1 . 1_565 133.85(5)
N1 K1 K1 . 1_565 132.94(4)
N1 K1 K1 1_565 1_565 47.06(4)
N1 K1 K1 3_666 1_565 90.0
C1 K1 K1 3_666 1_565 90.0
S2 K1 K1 . 1_565 90.0
K1 K1 K1 1_545 1_565 180.00(5)
N2 K1 K1 1_565 3_666 155.60(6)
N2 K1 K1 . 3_666 108.20(5)
N3 K1 K1 1_565 3_666 112.78(8)
N3 K1 K1 . 3_666 78.02(8)
N1 K1 K1 . 3_666 38.66(6)
N1 K1 K1 1_565 3_666 78.70(6)
N1 K1 K1 3_666 3_666 37.79(4)
C1 K1 K1 3_666 3_666 52.26(4)
S2 K1 K1 . 3_666 102.20(3)
K1 K1 K1 1_545 3_666 64.574(8)
K1 K1 K1 1_565 3_666 115.426(8)
C1 S1 Hg1 . . 97.08(11)
C2 S2 Hg1 . . 98.38(7)
C2 S2 Hg1 . 1_565 98.38(7)
Hg1 S2 Hg1 . 1_565 95.00(2)
C2 S2 K1 . . 119.70(11)
Hg1 S2 K1 . . 120.06(2)
Hg1 S2 K1 1_565 . 120.06(2)
C3 S3 Hg1 1_455 . 101.12(13)
N1 C1 S1 . . 179.8(3)
N1 C1 K1 . 3_666 57.5(2)
S1 C1 K1 . 3_666 122.68(14)
N2 C2 S2 3_667 . 179.7(3)
N3 C3 S3 . 1_655 176.4(4)
C1 N1 K1 . . 128.00(14)
C1 N1 K1 . 1_545 128.00(14)
K1 N1 K1 . 1_545 85.87(8)
C1 N1 K1 . 3_666 104.1(2)
K1 N1 K1 . 3_666 103.55(8)
K1 N1 K1 1_545 3_666 103.55(8)
C2 N2 K1 3_667 1_545 135.73(5)
C2 N2 K1 3_667 . 135.73(5)
K1 N2 K1 1_545 . 88.34(9)
C3 N3 K1 . 1_545 130.79(15)
C3 N3 K1 . . 130.79(15)
K1 N3 K1 1_545 . 87.70(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Hg1 S3 . 2.3954(11)
Hg1 S1 . 2.4481(8)
Hg1 S2 . 2.7653(6)
Hg1 S2 1_545 2.7653(6)
K1 N2 1_565 2.926(2)
K1 N2 . 2.926(2)
K1 N3 1_565 2.943(3)
K1 N3 . 2.943(3)
K1 N1 . 2.993(2)
K1 N1 1_565 2.993(2)
K1 N1 3_666 3.051(3)
K1 C1 3_666 3.508(3)
K1 S2 . 3.5657(12)
K1 K1 1_545 4.0775(4)
K1 K1 1_565 4.0775(4)
K1 K1 3_666 4.7485(14)
S1 C1 . 1.675(3)
S2 C2 . 1.664(3)
S2 Hg1 1_565 2.7653(6)
S3 C3 1_455 1.657(4)
C1 N1 . 1.140(4)
C1 K1 3_666 3.508(3)
C2 N2 3_667 1.145(5)
C3 N3 . 1.141(6)
C3 S3 1_655 1.657(4)
N1 K1 1_545 2.993(2)
N1 K1 3_666 3.051(3)
N2 C2 3_667 1.145(5)
N2 K1 1_545 2.926(2)
N3 K1 1_545 2.943(3)
