#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/90/2219083.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_2219083
loop_
_publ_author_name
'Kalaiselvi, D.'
'Kumar, R. Mohan'
'Jayavel, R.'
_publ_section_title
;Redetermination of
 poly[μ-chlorido-heptachlorido-μ₃-<small>L</small>-proline-μ₂-<small>L</small>-proline-tetramercury(II)]
;
_journal_coeditor_code           LH2640
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1048
_journal_page_last               m1049
_journal_paper_doi               10.1107/S160053680802196X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Hg4 Cl8 (C5 H9 N O2)2]'
_chemical_formula_moiety         'C10 H18 Cl8 Hg4 N2 O4'
_chemical_formula_sum            'C10 H18 Cl8 Hg4 N2 O4'
_chemical_formula_weight         1316.23
_chemical_name_systematic
poly[μ-chlorido-heptachlorido-μ₃-L-proline-μ₂-L-proline-tetramercury(II)]
_space_group_IT_number           1
_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-97
_cell_angle_alpha                108.621(3)
_cell_angle_beta                 107.260(2)
_cell_angle_gamma                97.353(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2742(4)
_cell_length_b                   9.4472(5)
_cell_length_c                   10.4767(6)
_cell_measurement_reflns_used    5619
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.5
_cell_measurement_theta_min      2.35
_cell_volume                     631.51(6)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII area-detector'
_diffrn_measurement_method       'ω and φ'
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10896
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.102
_exptl_absorpt_correction_T_max  0.1880
_exptl_absorpt_correction_T_min  0.0817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    3.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.750
_refine_diff_density_min         -2.507
_refine_ls_abs_structure_details 'Flack (1983), 1736 Friedel pairs'
_refine_ls_abs_structure_Flack   0.057(16)
_refine_ls_extinction_coef       0.0066(5)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0367
_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)+(0.0781P)²+1.0577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                3773
_reflns_number_total             3956
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2640.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2219083
_cod_database_fobs_code          2219083
loop_
_symmetry_equiv_pos_as_xyz
'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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.899(3) 0.4306(18) 0.7785(18) 0.028(4) Uani d . 1
C C2 0.969(2) 0.3323(15) 0.6707(14) 0.029(3) Uani d . 1
H H2 1.1092 0.3762 0.6931 0.034 Uiso calc R 1
C C3 0.849(3) 0.307(2) 0.515(2) 0.061(5) Uani d U 1
H H3A 0.7262 0.3395 0.5091 0.073 Uiso calc R 1
H H3B 0.9246 0.3647 0.4779 0.073 Uiso calc R 1
C C4 0.805(3) 0.135(2) 0.4312(19) 0.053(5) Uani d . 1
H H4A 0.6851 0.1011 0.3467 0.063 Uiso calc R 1
H H4B 0.9145 0.1099 0.4004 0.063 Uiso calc R 1
C C5 0.782(3) 0.063(2) 0.529(2) 0.054(5) Uani d . 1
H H5A 0.8072 -0.0391 0.5014 0.065 Uiso calc R 1
H H5B 0.6496 0.0542 0.5329 0.065 Uiso calc R 1
C C6 0.330(2) 0.4234(17) 1.0096(17) 0.029(4) Uani d . 1
C C7 0.286(2) 0.5707(15) 1.1024(14) 0.031(3) Uani d . 1
H H7 0.2394 0.6301 1.0431 0.037 Uiso calc R 1
C C8 0.224(3) 0.559(3) 1.308(2) 0.066(5) Uani d U 1
H H8A 0.2775 0.4742 1.3230 0.079 Uiso calc R 1
H H8B 0.1311 0.5775 1.3584 0.079 Uiso calc R 1
C C9 0.385(4) 0.700(3) 1.359(3) 0.074(7) Uani d U 1
H H9A 0.4888 0.7116 1.4480 0.089 Uiso calc R 1
H H9B 0.3341 0.7919 1.3756 0.089 Uiso calc R 1
C C10 0.463(3) 0.673(2) 1.237(2) 0.059(5) Uani d . 1
H H10A 0.5709 0.6227 1.2514 0.070 Uiso calc R 1
H H10B 0.5103 0.7701 1.2293 0.070 Uiso calc R 1
N N1 0.942(2) 0.1748(13) 0.6775(12) 0.040(3) Uani d . 1
H H1A 0.9010 0.1744 0.7504 0.048 Uiso calc R 1
H H1B 1.0575 0.1460 0.6915 0.048 Uiso calc R 1
N N2 0.1290(17) 0.5265(14) 1.1579(15) 0.042(3) Uani d . 1
H H2A 0.0369 0.5809 1.1448 0.050 Uiso calc R 1
H H2B 0.0685 0.4256 1.1103 0.050 Uiso calc R 1
O O1 0.9293(18) 0.5718(13) 0.7961(14) 0.044(3) Uani d . 1
O O2 0.8094(19) 0.3750(13) 0.8405(12) 0.050(3) Uani d . 1
O O3 0.457(2) 0.4477(15) 0.9648(17) 0.055(4) Uani d . 1
O O4 0.2390(17) 0.2970(11) 0.9976(12) 0.039(3) Uani d . 1
Cl Cl1 1.3639(8) 0.8860(6) 0.9691(6) 0.0403(14) Uani d . 1
Cl Cl2 0.9186(9) 0.6904(7) 0.5046(7) 0.0569(15) Uani d . 1
Cl Cl3 0.4113(9) 0.5596(8) 0.6683(7) 0.0463(14) Uani d . 1
Cl Cl4 0.8766(8) 0.7849(6) 1.1323(6) 0.0388(11) Uani d . 1
Cl Cl5 0.7759(8) 0.2678(7) 1.1413(6) 0.0430(13) Uani d . 1
Cl Cl6 0.3481(8) 0.0587(7) 0.6721(6) 0.0504(14) Uani d . 1
Cl Cl7 -0.1508(9) -0.0454(6) 0.8492(6) 0.0408(14) Uani d . 1
Cl Cl8 0.2824(12) 0.1691(10) 1.3145(8) 0.076(2) Uani d . 1
Hg Hg1 1.13721(7) 0.76197(5) 0.73403(5) 0.0368(2) Uani d . 1
Hg Hg2 0.65755(7) 0.64526(5) 0.89544(5) 0.0337(2) Uani d . 1
Hg Hg3 0.54733(7) 0.19563(5) 0.91009(5) 0.0357(2) Uani d . 1
Hg Hg4 0.07001(8) 0.06525(6) 1.08346(6) 0.0426(2) Uani 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_3
_geom_angle
O2 C1 O1 . 123.4(15)
O2 C1 C2 . 120.9(14)
O1 C1 C2 . 115.6(13)
C1 C2 N1 . 108.0(11)
C1 C2 C3 . 113.8(14)
N1 C2 C3 . 105.4(12)
C1 C2 H2 . 109.8
N1 C2 H2 . 109.8
C3 C2 H2 . 109.8
C4 C3 C2 . 105.3(13)
C4 C3 H3A . 110.7
C2 C3 H3A . 110.7
C4 C3 H3B . 110.7
C2 C3 H3B . 110.7
H3A C3 H3B . 108.8
C5 C4 C3 . 105.7(15)
C5 C4 H4A . 110.6
C3 C4 H4A . 110.6
C5 C4 H4B . 110.6
C3 C4 H4B . 110.6
H4A C4 H4B . 108.7
C4 C5 N1 . 103.2(14)
C4 C5 H5A . 111.1
N1 C5 H5A . 111.1
C4 C5 H5B . 111.1
N1 C5 H5B . 111.1
H5A C5 H5B . 109.1
O3 C6 O4 . 127.5(16)
O3 C6 C7 . 114.5(14)
O4 C6 C7 . 117.8(14)
N2 C7 C10 . 104.9(12)
N2 C7 C6 . 109.9(11)
C10 C7 C6 . 113.7(14)
N2 C7 H7 . 109.4
C10 C7 H7 . 109.4
C6 C7 H7 . 109.4
N2 C8 C9 . 103.9(17)
N2 C8 H8A . 111.0
C9 C8 H8A . 111.0
N2 C8 H8B . 111.0
C9 C8 H8B . 111.0
H8A C8 H8B . 109.0
C8 C9 C10 . 103.5(19)
C8 C9 H9A . 111.1
C10 C9 H9A . 111.1
C8 C9 H9B . 111.1
C10 C9 H9B . 111.1
H9A C9 H9B . 109.0
C9 C10 C7 . 104.8(16)
C9 C10 H10A . 110.8
C7 C10 H10A . 110.8
C9 C10 H10B . 110.8
C7 C10 H10B . 110.8
H10A C10 H10B . 108.9
C2 N1 C5 . 106.4(11)
C2 N1 H1A . 110.5
C5 N1 H1A . 110.5
C2 N1 H1B . 110.5
C5 N1 H1B . 110.5
H1A N1 H1B . 108.6
C8 N2 C7 . 107.8(12)
C8 N2 H2A . 110.2
C7 N2 H2A . 110.2
C8 N2 H2B . 110.2
C7 N2 H2B . 110.2
H2A N2 H2B . 108.5
C1 O1 Hg1 . 138.6(10)
C1 O1 Hg2 . 99.7(10)
Hg1 O1 Hg2 . 121.1(4)
C6 O3 Hg3 . 100.3(10)
C6 O3 Hg2 . 146.2(12)
Hg3 O3 Hg2 . 113.5(5)
Cl2 Hg1 Cl1 . 168.25(18)
Cl2 Hg1 O1 . 94.4(3)
Cl1 Hg1 O1 . 94.2(3)
Cl3 Hg2 Cl4 . 166.19(18)
Cl3 Hg2 O1 . 93.9(3)
Cl4 Hg2 O1 . 94.9(3)
Cl3 Hg2 O3 . 90.6(4)
Cl4 Hg2 O3 . 94.2(4)
O1 Hg2 O3 . 119.6(4)
Cl6 Hg3 Cl5 . 163.51(18)
Cl6 Hg3 O3 . 103.4(4)
Cl5 Hg3 O3 . 93.0(4)
Cl8 Hg4 Cl7 . 178.5(3)
Cl3 Hg2 O2 . 95.4(3)
Cl4 Hg2 O2 . 98.4(3)
O1 Hg2 O2 . 47.2(3)
O3 Hg2 O2 . 72.4(3)
C1 O2 Hg2 . 86.4(10)
C6 O4 Hg3 . 82.7(10)
C6 O4 Hg4 . 158.6(11)
Hg3 O4 Hg4 . 106.4(3)
Cl6 Hg3 O4 . 95.2(3)
Cl5 Hg3 O4 . 95.6(3)
O3 Hg3 O4 . 47.7(3)
Cl8 Hg4 O4 . 95.3(3)
Cl7 Hg4 O4 . 86.2(3)
Cl2 Hg1 Cl3 1_655 98.1(2)
Cl1 Hg1 Cl3 1_655 89.20(19)
O1 Hg1 Cl3 1_655 94.7(3)
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
C1 O2 . 1.224(19) ?
C1 O1 . 1.267(19) ?
C1 C2 . 1.480(19) ?
C2 N1 . 1.502(16) ?
C2 C3 . 1.53(2) ?
C2 H2 . 0.98 ?
C3 C4 . 1.52(2) ?
C3 H3A . 0.97 ?
C3 H3B . 0.97 ?
C4 C5 . 1.44(2) ?
C4 H4A . 0.97 ?
C4 H4B . 0.97 ?
C5 N1 . 1.57(2) ?
C5 H5A . 0.97 ?
C5 H5B . 0.97 ?
C6 O3 . 1.18(2) ?
C6 O4 . 1.236(17) ?
C6 C7 . 1.56(2) ?
C7 N2 . 1.495(18) ?
C7 C10 . 1.52(2) ?
C7 H7 . 0.98 ?
C8 N2 . 1.43(2) ?
C8 C9 . 1.49(3) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
C9 C10 . 1.51(3) ?
C9 H9A . 0.97 ?
C9 H9B . 0.97 ?
C10 H10A . 0.97 ?
C10 H10B . 0.97 ?
N1 H1A . 0.90 ?
N1 H1B . 0.90 ?
N2 H2A . 0.90 ?
N2 H2B . 0.90 ?
O4 Hg4 . 2.888(10) y
O4 Hg3 . 2.828(11) y
O2 Hg2 . 2.869(13) y
O1 Hg1 . 2.564(11) y
O1 Hg2 . 2.566(12) y
O3 Hg3 . 2.486(13) y
O3 Hg2 . 2.634(12) y
Cl1 Hg1 . 2.326(6) y
Cl2 Hg1 . 2.276(6) y
Cl3 Hg2 . 2.323(6) y
Cl4 Hg2 . 2.337(6) y
Cl5 Hg3 . 2.316(6) y
Cl6 Hg3 . 2.304(6) y
Cl7 Hg4 . 2.300(6) y
Cl8 Hg4 . 2.255(7) y
Hg1 Cl3 1_655 3.009(6) y
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
N1 H1A Cl7 1_655 0.90 2.63 3.282(14) 130
N1 H1B Cl6 1_655 0.90 2.40 3.290(16) 167
N2 H2A Cl4 1_455 0.90 2.40 3.267(15) 163
N2 H2B Cl5 1_455 0.90 2.60 3.234(15) 128
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_4
_geom_torsion
O2 C1 C2 N1 . -10(2)
O1 C1 C2 N1 . 173.3(15)
O2 C1 C2 C3 . 107.0(18)
O1 C1 C2 C3 . -70(2)
C1 C2 C3 C4 . -133.0(16)
N1 C2 C3 C4 . -14.8(19)
C2 C3 C4 C5 . 34(2)
C3 C4 C5 N1 . -38(2)
O3 C6 C7 N2 . -177.7(15)
O4 C6 C7 N2 . -1.7(19)
O3 C6 C7 C10 . -61(2)
O4 C6 C7 C10 . 115.4(17)
N2 C8 C9 C10 . -39(2)
C8 C9 C10 C7 . 29(2)
N2 C7 C10 C9 . -8(2)
C6 C7 C10 C9 . -128.2(17)
C1 C2 N1 C5 . 114.4(14)
C3 C2 N1 C5 . -7.6(16)
C4 C5 N1 C2 . 28.4(18)
C9 C8 N2 C7 . 35(2)
C10 C7 N2 C8 . -16.4(17)
C6 C7 N2 C8 . 106.1(15)
O2 C1 O1 Hg1 . 168.6(12)
C2 C1 O1 Hg1 . -15(3)
O2 C1 O1 Hg2 . -21(2)
C2 C1 O1 Hg2 . 156.4(12)
O4 C6 O3 Hg3 . -15(2)
C7 C6 O3 Hg3 . 160.2(10)
O4 C6 O3 Hg2 . 161.1(15)
C7 C6 O3 Hg2 . -23(3)
C1 O1 Hg1 Cl2 . 81.9(18)
Hg2 O1 Hg1 Cl2 . -87.5(6)
C1 O1 Hg1 Cl1 . -106.1(18)
Hg2 O1 Hg1 Cl1 . 84.4(6)
C1 O1 Hg2 Cl3 . -83.9(11)
Hg1 O1 Hg2 Cl3 . 89.1(6)
C1 O1 Hg2 Cl4 . 106.7(11)
Hg1 O1 Hg2 Cl4 . -80.4(5)
C1 O1 Hg2 O3 . 9.0(14)
Hg1 O1 Hg2 O3 . -178.1(4)
C6 O3 Hg2 Cl3 . -85(3)
Hg3 O3 Hg2 Cl3 . 91.5(6)
C6 O3 Hg2 Cl4 . 82(3)
Hg3 O3 Hg2 Cl4 . -101.5(6)
C6 O3 Hg2 O1 . -179(2)
Hg3 O3 Hg2 O1 . -3.4(10)
C6 O3 Hg3 Cl6 . 91.9(12)
Hg2 O3 Hg3 Cl6 . -85.9(6)
C6 O3 Hg3 Cl5 . -87.8(13)
Hg2 O3 Hg3 Cl5 . 94.5(6)
O1 C1 O2 Hg2 . 18.1(18)
C2 C1 O2 Hg2 . -158.7(15)
O3 C6 O4 Hg3 . 13.3(19)
C7 C6 O4 Hg3 . -162.1(13)
O3 C6 O4 Hg4 . 130(3)
C7 C6 O4 Hg4 . -45(4)
C1 O1 Hg2 O2 . 9.8(10)
Hg1 O1 Hg2 O2 . -177.2(8)
C6 O3 Hg2 O2 . 180(3)
Hg3 O3 Hg2 O2 . -4.0(6)
C1 O2 Hg2 Cl3 . 80.4(10)
C1 O2 Hg2 Cl4 . -99.0(10)
C1 O2 Hg2 O1 . -10.0(10)
C1 O2 Hg2 O3 . 169.2(11)
C6 O3 Hg3 O4 . 7.1(11)
Hg2 O3 Hg3 O4 . -170.7(9)
C6 O4 Hg3 Cl6 . -110.2(9)
Hg4 O4 Hg3 Cl6 . 89.7(4)
C6 O4 Hg3 Cl5 . 82.2(9)
Hg4 O4 Hg3 Cl5 . -77.9(3)
C6 O4 Hg3 O3 . -6.7(10)
Hg4 O4 Hg3 O3 . -166.9(7)
C6 O4 Hg4 Cl8 . -25(3)
Hg3 O4 Hg4 Cl8 . 87.9(4)
C6 O4 Hg4 Cl7 . 155(3)
Hg3 O4 Hg4 Cl7 . -92.1(3)
C1 O1 Hg1 Cl3 1_655 -16.5(18)
Hg2 O1 Hg1 Cl3 1_655 174.0(5)
