#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/97/2239792.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_2239792
loop_
_publ_author_name
'Weil, Matthias'
'Häusler, Thomas'
_publ_section_title
;
 Crystal structure of [NiHg(SCN)₄(CH₃OH)₂]ₙ
;
_journal_coeditor_code           HB0003
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              48
_journal_page_last               50
_journal_paper_doi               10.1107/S1600536814009532
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ni Hg (N C S)4 (C H4 O)2]'
_chemical_formula_moiety         'C6 H8 Hg N4 Ni O2 S4'
_chemical_formula_sum            'C6 H8 Hg N4 Ni O2 S4'
_chemical_formula_weight         555.70
_chemical_name_common
;
Nickel tetrathiocyanatomercurate(II) methanol disolvate
;
_chemical_name_systematic
catena-Poly[[bis(methanol-κO)nickel(II)]-di-μ-thiocyanato-κ⁴N:S-mercurate(II)-di-μ-thiocyanato-κ⁴N:S]
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1746(3)
_cell_length_b                   10.1746(3)
_cell_length_c                   29.5107(11)
_cell_measurement_reflns_used    9082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.947
_cell_measurement_theta_min      2.879
_cell_volume                     3055.02(17)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            17699
_diffrn_reflns_theta_full        39.99
_diffrn_reflns_theta_max         39.99
_diffrn_reflns_theta_min         2.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.814
_exptl_absorpt_correction_T_max  .7479
_exptl_absorpt_correction_T_min  .5665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       spherical
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.456
_refine_ls_abs_structure_details 'Flack (1983), 2098 Friedel pairs'
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0505
_reflns_number_gt                4214
_reflns_number_total             4684
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hb0003sup1.cf
_cod_data_source_block           I
_cod_database_code               2239792
_cod_database_fobs_code          2239792
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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 0.2500 0.529525(12) 0.8750 0.01652(3) Uani d S 1 2
Ni Ni1 0.0000 0.5000 1.050596(14) 0.01130(8) Uani d S 1 2
S S1 0.34284(7) 0.39974(6) 0.94163(2) 0.01777(12) Uani d . 1 1
S S2 0.07460(8) 0.66758(7) 0.91464(2) 0.02210(14) Uani d . 1 1
C C1 0.0628(3) 0.7838(2) 0.87530(12) 0.0204(4) Uani d . 1 1
C C2 0.2196(2) 0.4289(2) 0.97739(8) 0.0141(4) Uani d . 1 1
N N1 0.1356(2) 0.4484(2) 1.00263(8) 0.0177(4) Uani d . 1 1
N N2 0.0514(3) 0.8668(2) 0.84917(8) 0.0256(5) Uani d . 1 1
O O1 -0.0812(2) 0.3139(2) 1.05077(16) 0.0593(11) Uani d D 1 1
C C3 -0.0338(4) 0.1958(4) 1.0511(3) 0.075(2) Uani d . 1 1
H H2A -0.1061 0.1322 1.0511 0.112 Uiso calc PR 0.50 1
H H2B 0.0198 0.1834 1.0783 0.112 Uiso calc PR 0.50 1
H H2C 0.0207 0.1825 1.0241 0.112 Uiso calc PR 0.50 1
H H2D 0.0624 0.1999 1.0513 0.112 Uiso calc PR 0.50 1
H H2E -0.0635 0.1487 1.0240 0.112 Uiso calc PR 0.50 1
H H2F -0.0644 0.1495 1.0782 0.112 Uiso calc PR 0.50 1
H H1 -0.164(2) 0.331(5) 1.0596(16) 0.061(14) Uiso d D 1 1
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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
Ni Ni 0.3393 1.1124 '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
S1 Hg1 S1 5_556 . 117.62(3)
S1 Hg1 S2 5_556 . 112.27(2)
S1 Hg1 S2 . . 100.98(2)
S1 Hg1 S2 5_556 5_556 100.98(2)
S1 Hg1 S2 . 5_556 112.27(2)
S2 Hg1 S2 . 5_556 113.29(3)
N2 Ni1 N2 16_354 15_554 90.77(13)
N2 Ni1 N1 16_354 2_565 88.42(9)
N2 Ni1 N1 15_554 2_565 179.17(9)
N2 Ni1 N1 16_354 . 179.17(9)
N2 Ni1 N1 15_554 . 88.42(9)
N1 Ni1 N1 2_565 . 92.40(12)
N2 Ni1 O1 16_354 . 88.12(13)
N2 Ni1 O1 15_554 . 91.68(14)
N1 Ni1 O1 2_565 . 88.11(13)
N1 Ni1 O1 . . 92.08(13)
N2 Ni1 O1 16_354 2_565 91.68(14)
N2 Ni1 O1 15_554 2_565 88.12(13)
N1 Ni1 O1 2_565 2_565 92.08(13)
N1 Ni1 O1 . 2_565 88.11(13)
O1 Ni1 O1 . 2_565 179.7(3)
C2 S1 Hg1 . . 96.75(9)
C1 S2 Hg1 . . 97.01(10)
N2 C1 S2 . . 177.4(3)
N1 C2 S1 . . 179.0(2)
C2 N1 Ni1 . . 173.3(2)
C1 N2 Ni1 . 7_564 170.1(3)
C3 O1 Ni1 . . 134.5(2)
C3 O1 H1 . . 122(3)
Ni1 O1 H1 . . 101(3)
O1 C3 H2A . . 109.5
O1 C3 H2B . . 109.5
H2A C3 H2B . . 109.5
O1 C3 H2C . . 109.5
H2A C3 H2C . . 109.5
H2B C3 H2C . . 109.5
O1 C3 H2D . . 109.5
H2A C3 H2D . . 141.1
H2B C3 H2D . . 56.3
H2C C3 H2D . . 56.3
O1 C3 H2E . . 109.5
H2A C3 H2E . . 56.3
H2B C3 H2E . . 141.1
H2C C3 H2E . . 56.3
H2D C3 H2E . . 109.5
O1 C3 H2F . . 109.5
H2A C3 H2F . . 56.3
H2B C3 H2F . . 56.3
H2C C3 H2F . . 141.1
H2D C3 H2F . . 109.5
H2E C3 H2F . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 S1 5_556 2.5499(7) y
Hg1 S1 . 2.5499(7) y
Hg1 S2 . 2.5546(7) y
Hg1 S2 5_556 2.5546(7) y
Ni1 N2 16_354 2.041(2) y
Ni1 N2 15_554 2.041(2) y
Ni1 N1 2_565 2.045(2) y
Ni1 N1 . 2.045(2) y
Ni1 O1 . 2.066(2) y
Ni1 O1 2_565 2.066(2) y
S1 C2 . 1.666(2) ?
S2 C1 . 1.661(3) ?
C1 N2 . 1.149(4) ?
C2 N1 . 1.151(3) ?
N2 Ni1 7_564 2.041(2) ?
O1 C3 . 1.295(4) ?
O1 H1 . 0.897(10) ?
C3 H2A . 0.9800 ?
C3 H2B . 0.9800 ?
C3 H2C . 0.9800 ?
C3 H2D . 0.9800 ?
C3 H2E . 0.9800 ?
C3 H2F . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 S1 4_557 0.897(10) 2.40(2) 3.262(2) 160(4)
