#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003136.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_2003136
_journal_name_full               'Acta Crystallographica, Section B'
_journal_volume                  55
_journal_year     1999
_journal_page_first     396
_journal_page_last     409
_publ_section_title
;
Polynuclear Chloromercurate(II) Systems in their Chloropyridinium Salts
;
loop_
    _publ_author_name
    'Linden, Anthony'
    'James, Bruce D.'
    'Liesegang, John'
    'Gonis, Nick'
_publ_section_synopsis
;
The chloromercurate(II) salts of monochloropyridines display a variety of
anion stoichiometries and structures.  The 2-chloropridinium salt has the
[HgCl~3~]^-^ stoichiometry, but the anions are infinite chains composed of
[HgCl~3~]^-^, HgCl~2~ and Cl^-^ moieties linked by longer Hg...Cl contacts.
Chains of interconnected [HgCl~4~]^2-^ and HgCl~2~ entities in the 3- and
4-chloropridinium salts yield the rare [Hg~3~Cl~10~]^4-^ stoichiometry.
Second forms of the 3- and 4-chloropridinium salts contain distorted
[Hg~2~Cl~6~]^2-^ moieties linked into chains and symmetrical discrete
[Hg~2~Cl~6~]^2-^ anions, respectively.
;
_chemical_name_systematic
;
3-chloropyridinium trichloromercurate(II)
;
_chemical_name_common
; ?
;
_chemical_formula_moiety     'C5 H5 Cl N 1+, Hg Cl3 1-'
_chemical_formula_sum     'C5 H5 Cl4 Hg N'
_chemical_formula_structural     '(C5 H5 Cl N 1+)2, (Hg2 Cl6 2-)'
_chemical_formula_analytical     ?
_chemical_formula_iupac     ?
_chemical_formula_weight     421.49
_chemical_melting_point     '367-370'
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 1 21/c 1'
_symmetry_space_group_name_Hall     '-P 2ybc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x,y,z'
    '-x,1/2+y,1/2-z'
    '-x,-y,-z'
    'x,1/2-y,1/2+z'
_cell_length_a     7.243(5)
_cell_length_b     22.145(8)
_cell_length_c     12.320(3)
_cell_angle_alpha     90
_cell_angle_beta     99.52(3)
_cell_angle_gamma     90
_cell_volume     1948.8(13)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     25
_cell_measurement_theta_min     19.0
_cell_measurement_theta_max     20.0
_cell_measurement_temperature     173.0(10)
_exptl_crystal_description     prism
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.38
_exptl_crystal_size_mid     0.30
_exptl_crystal_size_min     0.28
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     2.873
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1520
_exptl_absorpt_coefficient_mu     16.83
_exptl_absorpt_correction_type     'empirical via psi-scan'
_exptl_absorpt_process_details     '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min     0.004
_exptl_absorpt_correction_T_max     0.009
_diffrn_ambient_temperature     173.0(10)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_source     'Rigaku rotating anode generator'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku AFC-5R diffractometer'
_diffrn_measurement_method     '\w--2\q'
_diffrn_reflns_number     6239
_diffrn_reflns_av_R_equivalents     0.073
_diffrn_reflns_av_sigmaI/netI     ?
_diffrn_reflns_theta_min     2.5
_diffrn_reflns_theta_max     30
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     10
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     31
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_limit_l_max     17
_diffrn_reflns_reduction_process     ?
_diffrn_standards_number     3
_diffrn_standards_interval_count     150
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     'no decay'
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    1 -5 1
    1 -2 -3
    2 3 0
_reflns_number_total     5681
_reflns_number_gt     4100
_reflns_threshold_expression     'I > 2\s(I)'
_refine_ls_structure_factor_coef     F
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0879
_refine_ls_R_factor_gt     0.0486
_refine_ls_wR_factor_all     0.0513
_refine_ls_wR_factor_ref     0.0489
_refine_ls_goodness_of_fit_all     ?
_refine_ls_goodness_of_fit_ref     2.014
_refine_ls_restrained_S_all     ?
_refine_ls_number_reflns     4100
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_number_constraints     0
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     sigma
_refine_ls_weighting_details     'w=1/[\s^2^(F~o~)+(0.005F~o~)^2^]'
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     ?
_refine_diff_density_max     4.06
_refine_diff_density_min     -2.79
_refine_ls_extinction_method     'Zachariasen (1963)'
_refine_ls_extinction_coef     1.9E-7(1)
_refine_ls_abs_structure_details
; ?
;
_refine_ls_abs_structure_Flack     ?
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 for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
    H H 0.0000 0.0000
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
    Cl Cl 0.1484 0.1585
; 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 0.0061 0.0033
; International Tables for Crystallography (1992).
Vol.C, Tables 4.2.6.8 and 6.1.1.1
;
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
;
TEXSAN PROCESS (Molecular Structure Corporation, 1989)
;
;
TEXSAN LS (Molecular Structure Corporation, 1989)
;
;
TEXSAN FINISH (Molecular Structure Corporation, 1989)
and local programs
;
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_disorder_group
    _atom_site_type_symbol
    Hg1 -0.05411(7) 0.57150(3) 0.36436(4) 0.02636(17) Uani d ? . 1 . Hg
    Hg2 0.38188(7) 0.60230(2) 0.21518(3) 0.01930(14) Uani d ? . 1 . Hg
    Cl1 -0.1703(4) 0.51782(13) 0.2032(2) 0.0214(9) Uani d ? . 1 . Cl
    Cl2 -0.0229(5) 0.58621(14) 0.5531(2) 0.0247(10) Uani d ? . 1 . Cl
    Cl3 0.1175(4) 0.66586(12) 0.2803(2) 0.0180(8) Uani d ? . 1 . Cl
    Cl4 0.6411(4) 0.66852(13) 0.2927(2) 0.0178(8) Uani d ? . 1 . Cl
    Cl5 0.3091(5) 0.56245(14) 0.0324(2) 0.0268(10) Uani d ? . 1 . Cl
    Cl6 0.3566(4) 0.52641(13) 0.3688(2) 0.0207(9) Uani d ? . 1 . Cl
    Cl7 0.1227(5) 0.23839(14) -0.0429(3) 0.0291(10) Uani d ? . 1 . Cl
    N1 0.1987(14) 0.4106(5) 0.0256(8) 0.022(3) Uani d ? . 1 . N
    C2 0.1859(18) 0.3567(6) -0.0270(9) 0.022(4) Uani d ? . 1 . C
    C3 0.1413(15) 0.3066(5) 0.0255(8) 0.016(3) Uani d ? . 1 . C
    C4 0.1031(16) 0.3099(6) 0.1328(9) 0.021(4) Uani d ? . 1 . C
    C5 0.1121(19) 0.3651(7) 0.1814(10) 0.029(4) Uani d ? . 1 . C
    C6 0.1569(18) 0.4175(6) 0.1280(10) 0.026(4) Uani d ? . 1 . C
    Cl8 0.6317(5) 0.22561(14) 0.4759(3) 0.0258(10) Uani d ? . 1 . Cl
    N21 0.5419(15) 0.3964(4) 0.4002(8) 0.024(3) Uani d ? . 1 . N
    C22 0.5583(18) 0.3430(6) 0.4581(9) 0.022(4) Uani d ? . 1 . C
    C23 0.6106(15) 0.2930(5) 0.4051(9) 0.015(3) Uani d ? . 1 . C
    C24 0.6498(15) 0.2970(5) 0.3008(9) 0.017(4) Uani d ? . 1 . C
    C25 0.6319(18) 0.3536(6) 0.2450(10) 0.024(4) Uani d ? . 1 . C
    C26 0.5820(16) 0.4024(6) 0.2989(10) 0.022(4) Uani d ? . 1 . C
    H1 0.238 0.445 -0.011 0.027 Uiso calc N1 ? 1 . H
    H2 0.208 0.354 -0.101 0.026 Uiso calc C2 ? 1 . H
    H4 0.072 0.275 0.170 0.026 Uiso calc C4 ? 1 . H
    H5 0.087 0.368 0.254 0.035 Uiso calc C5 ? 1 . H
    H6 0.158 0.456 0.162 0.031 Uiso calc C6 ? 1 . H
    H21 0.499 0.431 0.434 0.028 Uiso calc N21 ? 1 . H
    H22 0.534 0.341 0.532 0.027 Uiso calc C22 ? 1 . H
    H24 0.689 0.262 0.265 0.021 Uiso calc C24 ? 1 . H
    H25 0.655 0.357 0.171 0.028 Uiso calc C25 ? 1 . H
    H26 0.575 0.441 0.265 0.027 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 0.0309(3) 0.0359(3) 0.0121(2) -0.0066(2) 0.00277(18) -0.00733(19) Hg
    Hg2 0.0236(3) 0.0194(2) 0.0139(2) -0.0034(2) 0.00022(17) -0.00361(18) Hg
    Cl1 0.0343(18) 0.0170(14) 0.0117(12) -0.0061(12) 0.0000(12) -0.0016(10) Cl
    Cl2 0.0387(19) 0.0254(17) 0.0106(12) -0.0016(14) 0.0060(12) -0.0024(11) Cl
    Cl3 0.0137(13) 0.0147(13) 0.0267(14) 0.0011(12) 0.0068(11) 0.0023(11) Cl
    Cl4 0.0097(13) 0.0204(14) 0.0230(14) -0.0017(11) 0.0022(11) -0.0037(11) Cl
    Cl5 0.0393(19) 0.0243(17) 0.0151(13) -0.0049(14) -0.0005(12) -0.0080(11) Cl
    Cl6 0.0311(17) 0.0142(14) 0.0171(13) 0.0065(12) 0.0045(12) 0.0028(10) Cl
    Cl7 0.0308(18) 0.0218(17) 0.0314(17) 0.0047(14) -0.0045(14) -0.0081(13) Cl
    N1 0.021(6) 0.022(6) 0.024(5) -0.001(5) 0.003(4) 0.004(4) N
    C2 0.033(7) 0.022(7) 0.010(5) 0.006(6) 0.004(5) 0.001(4) C
    C3 0.013(6) 0.018(6) 0.014(5) -0.005(5) -0.002(4) 0.001(4) C
    C4 0.018(6) 0.030(7) 0.017(6) 0.002(5) 0.003(5) 0.000(5) C
    C5 0.032(8) 0.043(9) 0.013(6) 0.007(7) 0.005(5) 0.000(5) C
    C6 0.024(7) 0.024(7) 0.028(7) 0.003(6) -0.004(5) -0.004(5) C
    Cl8 0.0290(17) 0.0191(15) 0.0275(15) 0.0006(13) -0.0006(13) 0.0075(12) Cl
    N21 0.038(7) 0.009(5) 0.024(5) 0.006(5) 0.007(5) -0.004(4) N
    C22 0.028(7) 0.022(7) 0.020(6) -0.004(6) 0.009(5) -0.006(5) C
    C23 0.008(5) 0.014(6) 0.022(6) -0.002(4) 0.002(4) -0.003(4) C
    C24 0.009(6) 0.014(6) 0.030(6) 0.002(5) 0.006(5) -0.003(5) C
    C25 0.026(7) 0.024(7) 0.021(6) -0.001(6) 0.005(5) 0.000(5) C
    C26 0.016(6) 0.018(6) 0.033(7) -0.003(5) 0.005(5) 0.000(5) C
_cod_database_code 2003136
