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#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/16/2221615.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_2221615
loop_
_publ_author_name
'Terao, Hiromitsu'
'Gesing, Thorsten M.'
'Ishihara, Hideta'
'Furukawa, Yoshihiro'
'Gowda, B. Thimme'
_publ_section_title
;
 Bis(guanidinium) tetraiodidomercurate(II)
;
_journal_coeditor_code           BX2201
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m503
_journal_paper_doi               10.1107/S160053680901280X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_analytical     '[C(NH2)3]2HgI4'
_chemical_formula_iupac          '(C1 H6 N3)2 '[Hg I4]''
_chemical_formula_moiety         '2(C H6 N3 +), Hg I4 2-'
_chemical_formula_structural     '[C(NH2)3]2HgI4'
_chemical_formula_sum            'C2 H12 Hg I4 N6'
_chemical_formula_weight         828.37
_chemical_name_common            'Guanidine mercury iodid'
_chemical_name_systematic
;
Bis(guanidinium) tetraiodidomercurate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.80(3)
_cell_angle_beta                 95.79(4)
_cell_angle_gamma                118.46(2)
_cell_formula_units_Z            2
_cell_length_a                   8.981(2)
_cell_length_b                   8.996(2)
_cell_length_c                   12.302(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.65
_cell_volume                     808.9(5)
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_data_reduction        'XPREP (Bruker, 2003)'
_computing_molecular_graphics
;
DIAMOND (Crystal Impact, 2008) and PLATON (Spek, 2009)
;
_computing_publication_material  'SHELXL93 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 28.05
_diffrn_measurement_device       'Stoe IPDS-I'
_diffrn_measurement_method       'imaging plate dynamic profile intergration'
_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  0.1177
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14500
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    17.126
_exptl_absorpt_correction_T_max  0.0568
_exptl_absorpt_correction_T_min  0.0166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(XSHAPE; Stoe & Cie, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.401
_exptl_crystal_density_method    none
_exptl_crystal_description       cylindric
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         3.075
_refine_diff_density_min         -2.708
_refine_ls_extinction_coef       0.00075(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_all   0.810
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0587
_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)+(0.0353P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0699
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                1846
_reflns_number_total             3613
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bx2201.cif
_cod_data_source_block           I
_cod_database_code               2221615
_cod_database_fobs_code          2221615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
Hg Hg1 0.34641(9) 0.61562(10) 0.73508(6) 0.0667(3) Uani d . 1 .
I I1 0.0809(2) 0.5696(2) 0.84518(10) 0.0650(3) Uani d . 1 .
I I2 0.53156(14) 0.4740(2) 0.82071(9) 0.0607(3) Uani d . 1 .
I I3 0.58185(14) 0.9944(2) 0.80058(10) 0.0627(3) Uani d . 1 .
I I4 0.22651(14) 0.4550(2) 0.49342(9) 0.0673(3) Uani d . 1 .
C C1 0.0864(17) 0.0540(15) 0.8824(8) 0.051(3) Uani d D 1 .
N N11 0.2387(17) 0.0661(18) 0.9149(13) 0.072(4) Uani d D 1 .
H H11A 0.246(12) -0.030(7) 0.902(4) 0.12(3) Uiso d D 1 .
H H11B 0.333(7) 0.174(5) 0.9499(19) 0.12(3) Uiso d D 1 .
N N12 0.0824(14) 0.2000(14) 0.9034(11) 0.066(4) Uani d D 1 .
H H12A 0.179(2) 0.3056(13) 0.9387(16) 0.12(3) Uiso d D 1 .
H H12B -0.0169(19) 0.193(2) 0.8825(17) 0.12(3) Uiso d D 1 .
N N13 -0.0542(16) -0.1065(19) 0.8300(14) 0.080(4) Uani d D 1 .
H H13A -0.152(4) -0.111(8) 0.810(3) 0.12(3) Uiso d D 1 .
H H13B -0.054(9) -0.207(5) 0.815(3) 0.12(3) Uiso d D 1 .
C C2 0.2590(18) -0.012(2) 0.5152(16) 0.067(4) Uani d D 1 .
N N21 0.4067(18) 0.136(2) 0.5198(14) 0.086(5) Uani d D 1 .
H H21A 0.453(8) 0.138(11) 0.461(4) 0.12(3) Uiso d D 1 .
H H21B 0.457(8) 0.232(6) 0.584(3) 0.12(3) Uiso d D 1 .
N N22 0.1800(17) -0.158(2) 0.4211(13) 0.092(5) Uani d D 1 .
H H22A 0.085(3) -0.246(11) 0.427(11) 0.12(3) Uiso d D 1 .
H H22B 0.212(14) -0.173(18) 0.357(5) 0.12(3) Uiso d D 1 .
N N23 0.193(2) -0.009(3) 0.6078(14) 0.110(7) Uani d D 1 .
H H23A 0.098(3) -0.100(11) 0.610(12) 0.12(3) Uiso d D 1 .
H H23B 0.252(13) 0.093(8) 0.668(7) 0.12(3) Uiso d D 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'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
I4 Hg1 I1 . . 113.75(5) ?
I4 Hg1 I2 . . 109.54(5) ?
I1 Hg1 I2 . . 108.81(4) ?
I4 Hg1 I3 . . 109.38(6) ?
I1 Hg1 I3 . . 107.26(5) ?
I2 Hg1 I3 . . 107.93(5) ?
N13 C1 N12 . . 121.1(14) ?
N13 C1 N11 . . 119.7(14) ?
N12 C1 N11 . . 119.2(14) ?
H11A N11 H11B . . 120(7) ?
H11A N11 C1 . . 120(11) ?
H11B N11 C1 . . 118.(6) ?
H12A N12 H12B . . 120(2) ?
H12A N12 C1 . . 119.9(19) ?
H12B N12 C1 . . 120.0(18) ?
H13A N13 H13B . . 120(6) ?
H13A N13 C1 . . 117.(4) ?
H13B N13 C1 . . 123.(4) ?
N22 C2 N21 . . 120.3(17) ?
N22 C2 N23 . . 119.8(15) ?
N21 C2 N23 . . 119.9(17) ?
H21B N21 H21A . . 120(7) ?
H21B N21 C2 . . 119.(6) ?
H21A N21 C2 . . 121.(6) ?
H22B N22 H22A . . 120(11) ?
H22B N22 C2 . . 127.(9) ?
H22A N22 C2 . . 114.(9) ?
H23A N23 H23B . . 120(11) ?
H23A N23 C2 . . 125.(10) ?
H23B N23 C2 . . 115.(10) ?
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 I4 . 2.760(2) ?
Hg1 I1 . 2.7762(15) ?
Hg1 I2 . 2.8098(14) ?
Hg1 I3 . 2.833(2) ?
I1 H13B 1_565 2.87(7) ?
I1 H11A 1_565 3.00(4) ?
I2 H21B . 2.91(3) ?
I2 H23B . 2.99(5) ?
I3 H13A 1_665 2.97(5) ?
I3 H22B 2_666 3.05(7) ?
I3 H21A 2_666 3.03(4) ?
I3 H12B 1_665 3.057(19) ?
C1 N13 . 1.29(2) ?
C1 N12 . 1.29(2) ?
C1 N11 . 1.32(2) ?
N11 H11A . 0.88(8) ?
N11 H11B . 0.87(5) ?
N12 H12A . 0.87(2) ?
N12 H12B . 0.87(2) ?
N13 H13A . 0.87(5) ?
N13 H13B . 0.88(6) ?
C2 N22 . 1.30(2) ?
C2 N21 . 1.34(2) ?
C2 N23 . 1.34(2) ?
N21 H21B . 0.87(4) ?
N21 H21A . 0.87(7) ?
N22 H22B . 0.87(9) ?
N22 H22A . 0.87(9) ?
N23 H23A . 0.87(9) ?
N23 H23B . 0.87(8) ?
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
N11 H11A I1 1_545 0.87(4) 3.00(4) 3.78(2) 151(2)
N12 H12A I2 . 0.87(4) 3.46(2) 3.83(2) 123(2)
N13 H13A I3 1_445 0.87(4) 2.96(4) 3.80(2) 161(2)
N13 H13B I1 1_545 0.87(4) 2.88(4) 3.69(2) 156(2)
N21 H21A I3 2_666 0.87(4) 3.03(4) 3.82(2) 151(2)
N21 H21B I2 . 0.87(4) 2.91(4) 3.74(2) 162(6)
N22 H22A I4 2_556 0.87(9) 2.98(4) 3.82(2) 162(2)
N22 H22B I3 2_666 0.87(10) 3.05(4) 3.81(2) 147(2)
N23 H23A I4 2_556 0.87(9) 2.91(4) 3.71(2) 153(2)
N23 H23B I2 . 0.87(4) 2.99(4) 3.82(2) 161(6)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N13 C1 N11 H11A . . . . 0.0(6) ?
N12 C1 N11 H11A . . . . -180.0(5) ?
N13 C1 N11 H11B . . . . 180.0(6) ?
N12 C1 N11 H11B . . . . 0.0(5) ?
N13 C1 N12 H12A . . . . -180.0(6) ?
N11 C1 N12 H12A . . . . 0.0(4) ?
N13 C1 N12 H12B . . . . 0.1(9) ?
N11 C1 N12 H12B . . . . -180.0(8) ?
N12 C1 N13 H13A . . . . -0.1(10) ?
N11 C1 N13 H13A . . . . 179.9(7) ?
N12 C1 N13 H13B . . . . -179.9(7) ?
N11 C1 N13 H13B . . . . 0.1(10) ?
N22 C2 N21 H21B . . . . 180.0(5) ?
N23 C2 N21 H21B . . . . -0.1(6) ?
N22 C2 N21 H21A . . . . 0.0(5) ?
N23 C2 N21 H21A . . . . 179.9(6) ?
N21 C2 N22 H22B . . . . 0.1(6) ?
N23 C2 N22 H22B . . . . -179.9(6) ?
N21 C2 N22 H22A . . . . 180.0(5) ?
N23 C2 N22 H22A . . . . 0.1(6) ?
N22 C2 N23 H23A . . . . -0.2(11) ?
N21 C2 N23 H23A . . . . 179.9(8) ?
N22 C2 N23 H23B . . . . -179.9(7) ?
N21 C2 N23 H23B . . . . 0.1(9) ?
