#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2003134.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_2003134
loop_
_publ_author_name
'Linden, Anthony'
'James, Bruce D.'
'Liesegang, John'
'Gonis, Nick'
_publ_section_title
;
 Polynuclear chloromercurate(II) systems in their chloropyridinium
 salts
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              396
_journal_page_last               409
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         '(C5 H5 Cl N 1+)4, Hg3 Cl10 4-'
_chemical_formula_structural     '(C5 H5 Cl N 1+)4, Hg Cl2, (Hg Cl4 2-)2'
_chemical_formula_sum            'C20 H20 Cl14 Hg3 N4'
_chemical_formula_weight         1414.52
_chemical_name_common            ' ?'
_chemical_name_systematic
;
tetrakis(3-chloropyridinium) decachlorotrimercurate(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.78(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.522(2)
_cell_length_b                   28.046(3)
_cell_length_c                   9.165(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.5
_cell_volume                     1860.6(7)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
_computing_data_reduction
;
TEXSAN PROCESS (Molecular Structure Corporation, 1989)
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
;
TEXSAN FINISH (Molecular Structure Corporation, 1989)
and local programs
;
_computing_structure_refinement
;
TEXSAN LS (Molecular Structure Corporation, 1989)
;
_computing_structure_solution    'DIRDIF92 Patterson (Beurskens et al., 1992)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measurement_device_type  'Rigaku AFC-5R diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .046
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5915
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.37
_exptl_absorpt_correction_T_max  .024
_exptl_absorpt_correction_T_min  .010
_exptl_absorpt_correction_type   'empirical via psi-scan'
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.524
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          .37
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .28
_refine_diff_density_max         2.15
_refine_diff_density_min         -2.32
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_coef       1.3E-7(2)
_refine_ls_extinction_method     'Zachariasen (1963)'
_refine_ls_goodness_of_fit_ref   1.950
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .0562
_refine_ls_R_factor_gt           .0357
_refine_ls_shift/su_max          .0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(F~o~)+(0.005F~o~)^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .0388
_refine_ls_wR_factor_ref         .0375
_reflns_number_gt                4337
_reflns_number_total             5426
_reflns_threshold_expression     'I > 2\s(I)'
_[local]_cod_data_source_file    sh0124.cif
_[local]_cod_data_source_block   II
_cod_original_cell_volume        1860.5(7)
_cod_database_code               2003134
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_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_calc_attached_atom
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Hg1 .0 .0 .0 .02077(13) Uani d ? S 1 Hg
Hg2 .44770(4) .126030(10) -.21367(3) .02059(9) Uani d ? . 1 Hg
Cl1 -.0673(3) -.04381(6) -.2260(2) .0243(6) Uani d ? . 1 Cl
Cl2 .2445(3) .06871(6) -.0959(2) .0238(6) Uani d ? . 1 Cl
Cl3 .3173(3) .12483(8) -.4810(2) .0368(7) Uani d ? . 1 Cl
Cl4 .4927(3) .18989(7) -.0298(2) .0326(7) Uani d ? . 1 Cl
Cl5 .7291(3) .07370(7) -.1353(3) .0315(7) Uani d ? . 1 Cl
Cl6 -.0203(3) .25279(8) -.2269(3) .0408(8) Uani d ? . 1 Cl
N1 .0286(10) .1501(2) .0704(8) .031(2) Uani d ? . 1 N
C2 .0188(11) .1736(3) -.0608(9) .026(3) Uani d ? . 1 C
C3 -.0109(10) .2217(3) -.0638(9) .023(2) Uani d ? . 1 C
C4 -.0348(12) .2441(3) .0637(11) .033(3) Uani d ? . 1 C
C5 -.0191(13) .2187(3) .1975(10) .036(3) Uani d ? . 1 C
C6 .0113(11) .1704(3) .1980(9) .028(3) Uani d ? . 1 C
Cl7 .8257(3) .15591(8) .5247(3) .0384(8) Uani d ? . 1 Cl
N21 .5482(9) .0657(3) .2230(7) .031(2) Uani d ? . 1 N
C22 .6193(12) .1067(3) .2914(9) .028(3) Uani d ? . 1 C
C23 .7391(11) .1037(3) .4323(9) .025(3) Uani d ? . 1 C
C24 .7860(12) .0592(3) .5012(10) .033(3) Uani d ? . 1 C
C25 .7089(12) .0196(3) .4243(10) .034(3) Uani d ? . 1 C
C26 .5876(12) .0236(3) .2864(10) .032(3) Uani d ? . 1 C
H1 .049 .117 .072 .037 Uiso calc N1 ? 1 H
H2 .032 .157 -.148 .031 Uiso calc C2 ? 1 H
H4 -.062 .277 .060 .040 Uiso calc C4 ? 1 H
H5 -.029 .234 .287 .043 Uiso calc C5 ? 1 H
H6 .020 .152 .287 .034 Uiso calc C6 ? 1 H
H21 .466 .067 .124 .037 Uiso calc N21 ? 1 H
H22 .587 .137 .243 .034 Uiso calc C22 ? 1 H
H24 .870 .057 .599 .039 Uiso calc C24 ? 1 H
H25 .741 -.011 .468 .040 Uiso calc C25 ? 1 H
H26 .530 -.004 .235 .039 Uiso calc C26 ? 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Hg1 .0241(2) .02007(19) .0191(2) -.00327(16) .00748(15) -.00288(16) Hg
Hg2 .02245(15) .02047(14) .01912(15) -.00038(12) .00612(11) .00143(11) Hg
Cl1 .0352(11) .0209(8) .0169(9) -.0024(8) .0073(8) -.0008(7) Cl
Cl2 .0244(9) .0218(9) .0289(10) -.0049(7) .0137(8) .0010(7) Cl
Cl3 .0376(12) .0498(13) .0191(10) -.0004(11) .0008(8) .0015(9) Cl
Cl4 .0497(13) .0231(9) .0255(10) -.0043(9) .0113(9) -.0053(8) Cl
Cl5 .0211(9) .0277(10) .0413(12) .0057(8) .0010(9) -.0011(9) Cl
Cl6 .0559(15) .0328(11) .0322(11) -.0076(11) .0096(10) .0087(10) Cl
N1 .039(4) .018(3) .038(4) .001(3) .013(3) .000(3) N
C2 .028(4) .022(4) .027(4) .003(3) .006(3) -.005(3) C
C3 .025(4) .021(4) .022(4) -.006(3) .005(3) .004(3) C
C4 .043(5) .019(4) .041(5) -.001(4) .017(4) -.003(4) C
C5 .047(6) .034(5) .029(5) -.001(4) .015(4) -.009(4) C
C6 .033(5) .028(4) .022(4) .000(3) .003(3) .003(3) C
Cl7 .0456(13) .0344(11) .0344(12) -.0078(10) .0093(10) -.0105(10) Cl
N21 .034(4) .035(4) .019(3) .002(3) -.001(3) -.002(3) N
C22 .036(5) .023(4) .023(4) .001(3) .005(4) .003(3) C
C23 .026(4) .030(4) .022(4) .000(3) .010(3) -.005(3) C
C24 .030(5) .038(5) .030(5) .005(4) .008(4) .004(4) C
C25 .046(5) .021(4) .037(5) .006(4) .017(4) .003(4) C
C26 .039(5) .025(4) .035(5) -.002(4) .015(4) -.003(4) C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
H H .0000 .0000
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
Cl Cl .1484 .1585
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
Hg Hg -2.3894 9.2266
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
N N .0061 .0033
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 5 -1
-1 1 -2
-1 -1 -2
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
Cl1 Hg1 Cl1 . 3 180.0 no
Cl1 Hg1 Cl2 . . 94.66(6) no
Cl1 Hg1 Cl2 . 3 85.34(6) no
Cl1 Hg1 Cl5 . 1_455 92.17(6) no
Cl1 Hg1 Cl5 . 3_655 87.83(6) no
Cl2 Hg1 Cl2 . 3 180.0 no
Cl2 Hg1 Cl5 . 1_455 80.31(6) no
Cl2 Hg1 Cl5 . 3_655 99.69(6) no
Cl5 Hg1 Cl5 1_455 3_655 180.0 no
Cl2 Hg2 Cl3 . . 106.84(7) no
Cl2 Hg2 Cl4 . . 98.77(7) no
Cl2 Hg2 Cl5 . . 93.66(7) no
Cl3 Hg2 Cl4 . . 131.94(8) no
Cl3 Hg2 Cl5 . . 111.43(8) no
Cl4 Hg2 Cl5 . . 106.60(7) no
Hg1 Cl2 Hg2 . . 173.34(8) no
Hg1 Cl5 Hg2 3_655 . 165.22(9) no
C2 N1 C6 . . 125.2(7) no
N1 C2 C3 . . 117.7(7) no
Cl6 C3 C2 . . 119.2(7) no
Cl6 C3 C4 . . 121.4(6) no
C2 C3 C4 . . 119.4(7) no
C3 C4 C5 . . 120.6(7) no
C4 C5 C6 . . 118.9(8) no
N1 C6 C5 . . 118.1(8) no
C22 N21 C26 . . 123.2(7) no
N21 C22 C23 . . 117.6(7) no
Cl7 C23 C22 . . 118.4(6) no
Cl7 C23 C24 . . 121.3(6) no
C22 C23 C24 . . 120.3(7) no
C23 C24 C25 . . 118.3(8) no
C24 C25 C26 . . 120.2(8) no
N21 C26 C25 . . 120.2(8) no
C2 N1 H1 . . 117.5 no
C6 N1 H1 . . 117.4 no
N1 C2 H2 . . 121.2 no
C3 C2 H2 . . 121.1 no
C3 C4 H4 . . 119.7 no
C5 C4 H4 . . 119.7 no
C4 C5 H5 . . 120.5 no
C6 C5 H5 . . 120.6 no
N1 C6 H6 . . 121.0 no
C5 C6 H6 . . 120.9 no
C22 N21 H21 . . 118.4 no
C26 N21 H21 . . 118.4 no
N21 C22 H22 . . 121.2 no
C23 C22 H22 . . 121.2 no
C23 C24 H24 . . 120.8 no
C25 C24 H24 . . 120.8 no
C24 C25 H25 . . 119.9 no
C26 C25 H25 . . 119.9 no
N21 C26 H26 . . 119.9 no
C25 C26 H26 . . 119.9 no
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 Cl1 . 2.3420(18) no
Hg1 Cl2 . 2.9575(18) no
Hg1 Cl5 1_455 2.9303(19) no
Hg2 Cl2 . 2.6427(18) no
Hg2 Cl3 . 2.379(2) no
Hg2 Cl4 . 2.4193(19) no
Hg2 Cl5 . 2.5148(19) no
Cl6 C3 . 1.716(8) no
N1 C2 . 1.354(10) no
N1 C6 . 1.338(10) no
C2 C3 . 1.367(10) no
C3 C4 . 1.382(11) no
C4 C5 . 1.396(12) no
C5 C6 . 1.373(11) no
Cl7 C23 . 1.729(8) no
N21 C22 . 1.349(10) no
N21 C26 . 1.313(10) no
C22 C23 . 1.362(10) no
C23 C24 . 1.398(11) no
C24 C25 . 1.359(11) no
C25 C26 . 1.347(12) no
N1 H1 . .95 no
C2 H2 . .95 no
C4 H4 . .95 no
C5 H5 . .95 no
C6 H6 . .95 no
N21 H21 . .95 no
C22 H22 . .95 no
C24 H24 . .95 no
C25 H25 . .95 no
C26 H26 . .95 no
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
_geom_hbond_publ_flag
N1 H1 Cl1 3_555 .95 2.47 3.284(7) 144 no
N1 H1 Cl2 . .95 2.75 3.395(7) 126 no
N21 H21 Cl2 . .95 2.24 3.184(7) 173 no