#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/48/2014818.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_2014818
loop_
_publ_author_name
'M. Enriqueta Díaz de Vivar'
'Miguel Angel Harvey'
'María Teresa Garland'
'Sergio Baggio'
'Ricardo Baggio'
_publ_section_title
;
 Two Cd and Hg peroxodisulfate complexes with aromatic amines
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m240
_journal_page_last               m244
_journal_paper_doi               10.1107/S0108270105009273
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Hg (C10 H8 N2)2 (O8 S2)] , 0.4H2 O'
_chemical_formula_moiety         'C20 H16 Hg N4 O8 S2 , 0.4H2 O'
_chemical_formula_sum            'C20 H16.8 Hg N4 O8.4 S2'
_chemical_formula_weight         712.28
_chemical_name_systematic
;
catena-poly[[[bis(2,2'-bipyridine-κ²N,N')mercury(II)]-μ-peroxodisulfato-
κ²O:O'] 0.4-hydrate]
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.689(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3340(11)
_cell_length_b                   30.125(6)
_cell_length_c                   10.4340(17)
_cell_measurement_reflns_used    2344
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      22.65
_cell_measurement_theta_min      3.12
_cell_volume                     2239.8(7)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL-PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13178
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.12
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.118
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.715
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4938
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.035P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                4000
_reflns_number_total             4938
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ga1102.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C20 H16.80 Hg N4 O8.40 S2'
_cod_database_code               2014818
_cod_database_fobs_code          2014818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Hg1 0.58598(2) 0.134014(4) 0.411176(15) 0.03693(6) Uani d . 1 . . Hg
S1 0.11191(13) 0.13232(3) 0.40925(9) 0.0345(2) Uani d . 1 . . S
S2 -0.15321(16) 0.10384(3) 0.06340(10) 0.0411(2) Uani d . 1 . . S
O1 0.2183(4) 0.15490(9) 0.3295(3) 0.0469(7) Uani d . 1 . . O
O2 0.2204(4) 0.10251(9) 0.5050(3) 0.0495(7) Uani d . 1 . . O
O3 -0.0162(4) 0.16044(8) 0.4552(3) 0.0466(7) Uani d . 1 . . O
O4 -0.0180(4) 0.09509(7) 0.3123(2) 0.0384(6) Uani d . 1 . . O
O5 -0.1627(4) 0.11929(9) 0.2149(3) 0.0435(7) Uani d . 1 . . O
O6 0.0108(5) 0.12427(11) 0.0378(3) 0.0677(10) Uani d . 1 . . O
O7 -0.1519(5) 0.05695(9) 0.0632(3) 0.0673(9) Uani d . 1 . . O
O8 -0.3275(5) 0.12412(11) -0.0029(3) 0.0717(10) Uani d . 1 . . O
N1A 0.5151(4) 0.06822(9) 0.3137(3) 0.0349(7) Uani d . 1 . . N
N2A 0.7551(4) 0.08067(9) 0.5529(3) 0.0377(7) Uani d . 1 . . N
C1A 0.3953(6) 0.06403(14) 0.1958(4) 0.0440(10) Uani d . 1 . . C
H1AA 0.3278 0.0887 0.1576 0.053 Uiso calc R 1 . . H
C2A 0.3692(6) 0.02447(14) 0.1300(4) 0.0514(11) Uani d . 1 . . C
H2AA 0.2845 0.0223 0.0483 0.062 Uiso calc R 1 . . H
C3A 0.4693(6) -0.01192(13) 0.1856(5) 0.0492(11) Uani d . 1 . . C
H3AA 0.4566 -0.0389 0.1410 0.059 Uiso calc R 1 . . H
C4A 0.5899(6) -0.00806(12) 0.3095(4) 0.0426(10) Uani d . 1 . . C
H4AA 0.6555 -0.0327 0.3498 0.051 Uiso calc R 1 . . H
C5A 0.6120(5) 0.03268(11) 0.3727(4) 0.0331(8) Uani d . 1 . . C
C6A 0.7366(5) 0.03912(11) 0.5057(4) 0.0322(8) Uani d . 1 . . C
C7A 0.8301(6) 0.00434(12) 0.5800(4) 0.0394(9) Uani d . 1 . . C
H7AA 0.8168 -0.0244 0.5466 0.047 Uiso calc R 1 . . H
C8A 0.9421(6) 0.01231(13) 0.7029(4) 0.0468(10) Uani d . 1 . . C
H8AA 1.0046 -0.0109 0.7539 0.056 Uiso calc R 1 . . H
C9A 0.9608(6) 0.05524(13) 0.7497(4) 0.0475(10) Uani d . 1 . . C
H9AA 1.0372 0.0616 0.8323 0.057 Uiso calc R 1 . . H
C10A 0.8647(6) 0.08822(13) 0.6725(4) 0.0486(11) Uani d . 1 . . C
H10A 0.8762 0.1172 0.7045 0.058 Uiso calc R 1 . . H
N1B 0.5838(4) 0.20230(9) 0.3285(3) 0.0339(7) Uani d . 1 . . N
N2B 0.5553(4) 0.18388(9) 0.5769(3) 0.0364(7) Uani d . 1 . . N
C1B 0.5835(6) 0.20982(13) 0.2020(4) 0.0457(10) Uani d . 1 . . C
H1BA 0.5916 0.1857 0.1479 0.055 Uiso calc R 1 . . H
C2B 0.5717(7) 0.25141(14) 0.1495(4) 0.0553(12) Uani d . 1 . . C
H2BA 0.5697 0.2556 0.0609 0.066 Uiso calc R 1 . . H
C3B 0.5629(7) 0.28699(13) 0.2299(5) 0.0561(12) Uani d . 1 . . C
H3BA 0.5573 0.3157 0.1968 0.067 Uiso calc R 1 . . H
C4B 0.5625(6) 0.27972(12) 0.3599(4) 0.0432(10) Uani d . 1 . . C
H4BA 0.5560 0.3036 0.4152 0.052 Uiso calc R 1 . . H
C5B 0.5717(5) 0.23702(12) 0.4077(4) 0.0336(8) Uani d . 1 . . C
C6B 0.5667(5) 0.22705(11) 0.5458(4) 0.0340(8) Uani d . 1 . . C
C7B 0.5678(6) 0.25949(12) 0.6389(4) 0.0466(10) Uani d . 1 . . C
H7BA 0.5737 0.2893 0.6166 0.056 Uiso calc R 1 . . H
C8B 0.5601(7) 0.24782(13) 0.7644(4) 0.0574(12) Uani d . 1 . . C
H8BA 0.5622 0.2696 0.8280 0.069 Uiso calc R 1 . . H
C9B 0.5493(7) 0.20356(13) 0.7958(4) 0.0554(12) Uani d . 1 . . C
H9BA 0.5438 0.1949 0.8804 0.066 Uiso calc R 1 . . H
C10B 0.5468(6) 0.17285(13) 0.6996(4) 0.0466(10) Uani d . 1 . . C
H10B 0.5389 0.1430 0.7201 0.056 Uiso calc R 1 . . H
O1W 0.2977(19) 0.1213(5) -0.1050(15) 0.128(4) Uani d PD 0.3994(10) . . O
H1WA 0.27(2) 0.139(6) -0.054(17) 0.154 Uiso d PD 0.3994(10) . . H
H1WB 0.412(5) 0.118(6) -0.089(19) 0.154 Uiso d PD 0.3994(10) . . H
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'
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
_geom_angle_publ_flag
N1B Hg1 N1A 131.56(12) ?
N1B Hg1 N2A 146.65(11) ?
N1A Hg1 N2A 73.05(11) ?
N1B Hg1 N2B 72.59(10) ?
N1A Hg1 N2B 148.59(11) ?
N2A Hg1 N2B 95.93(11) ?
N1B Hg1 O1 75.40(9) ?
N1A Hg1 O1 87.47(10) ?
N2A Hg1 O1 134.53(9) ?
N2B Hg1 O1 79.65(10) ?
O3 S1 O2 115.92(18) y
O3 S1 O1 113.78(17) y
O2 S1 O1 114.27(17) y
O3 S1 O4 106.13(15) y
O2 S1 O4 98.38(15) y
O1 S1 O4 106.24(15) y
O7 S2 O6 115.1(2) y
O7 S2 O8 115.4(2) y
O6 S2 O8 114.7(2) y
O7 S2 O5 106.41(17) y
O6 S2 O5 106.43(17) y
O8 S2 O5 96.09(17) y
S1 O1 Hg1 110.17(15) ?
O5 O4 S1 107.62(17) ?
O4 O5 S2 109.31(18) ?
C1A N1A C5A 120.3(3) ?
C1A N1A Hg1 122.3(3) ?
C5A N1A Hg1 117.1(2) ?
C10A N2A C6A 119.3(3) ?
C10A N2A Hg1 126.0(3) ?
C6A N2A Hg1 114.7(3) ?
N1A C1A C2A 121.9(4) ?
N1A C1A H1AA 119.1 ?
C2A C1A H1AA 119.1 ?
C1A C2A C3A 119.2(4) ?
C1A C2A H2AA 120.4 ?
C3A C2A H2AA 120.4 ?
C2A C3A C4A 119.2(4) ?
C2A C3A H3AA 120.4 ?
C4A C3A H3AA 120.4 ?
C5A C4A C3A 119.7(4) ?
C5A C4A H4AA 120.1 ?
C3A C4A H4AA 120.1 ?
N1A C5A C4A 119.7(4) ?
N1A C5A C6A 117.7(3) ?
C4A C5A C6A 122.6(3) ?
N2A C6A C7A 120.5(4) ?
N2A C6A C5A 116.9(3) ?
C7A C6A C5A 122.6(3) ?
C8A C7A C6A 119.9(4) ?
C8A C7A H7AA 120.0 ?
C6A C7A H7AA 120.0 ?
C7A C8A C9A 118.9(4) ?
C7A C8A H8AA 120.6 ?
C9A C8A H8AA 120.6 ?
C10A C9A C8A 118.7(4) ?
C10A C9A H9AA 120.7 ?
C8A C9A H9AA 120.7 ?
N2A C10A C9A 122.7(4) ?
N2A C10A H10A 118.6 ?
C9A C10A H10A 118.6 ?
C1B N1B C5B 119.2(3) ?
C1B N1B Hg1 122.4(2) ?
C5B N1B Hg1 118.3(2) ?
C10B N2B C6B 119.3(3) ?
C10B N2B Hg1 125.6(2) ?
C6B N2B Hg1 114.8(2) ?
N1B C1B C2B 122.5(4) ?
N1B C1B H1BA 118.7 ?
C2B C1B H1BA 118.7 ?
C1B C2B C3B 118.7(4) ?
C1B C2B H2BA 120.7 ?
C3B C2B H2BA 120.7 ?
C2B C3B C4B 119.4(4) ?
C2B C3B H3BA 120.3 ?
C4B C3B H3BA 120.3 ?
C3B C4B C5B 119.7(4) ?
C3B C4B H4BA 120.2 ?
C5B C4B H4BA 120.2 ?
N1B C5B C4B 120.5(3) ?
N1B C5B C6B 117.4(3) ?
C4B C5B C6B 122.1(3) ?
N2B C6B C7B 120.4(3) ?
N2B C6B C5B 116.5(3) ?
C7B C6B C5B 123.0(3) ?
C8B C7B C6B 119.8(4) ?
C8B C7B H7BA 120.1 ?
C6B C7B H7BA 120.1 ?
C7B C8B C9B 119.5(4) ?
C7B C8B H8BA 120.3 ?
C9B C8B H8BA 120.3 ?
C10B C9B C8B 118.3(4) ?
C10B C9B H9BA 120.9 ?
C8B C9B H9BA 120.9 ?
N2B C10B C9B 122.7(4) ?
N2B C10B H10B 118.6 ?
C9B C10B H10B 118.6 ?
H1WA O1W H1WB 110(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
Hg1 N1B . 2.229(3) y
Hg1 N1A . 2.232(3) y
Hg1 N2A . 2.332(3) y
Hg1 N2B . 2.341(3) y
Hg1 O1 . 2.703(3) y
Hg1 O3 1_655 2.953(3) y
S1 O3 . 1.430(3) y
S1 O2 . 1.436(3) y
S1 O1 . 1.439(3) y
S1 O4 . 1.653(3) y
S2 O7 . 1.413(3) y
S2 O6 . 1.431(3) y
S2 O8 . 1.438(3) y
S2 O5 . 1.665(3) y
O4 O5 . 1.477(3) y
N1A C1A . 1.338(5) ?
N1A C5A . 1.350(4) ?
N2A C10A . 1.334(5) ?
N2A C6A . 1.340(4) ?
C1A C2A . 1.366(5) ?
C1A H1AA . 0.9300 ?
C2A C3A . 1.370(6) ?
C2A H2AA . 0.9300 ?
C3A C4A . 1.387(6) ?
C3A H3AA . 0.9300 ?
C4A C5A . 1.385(5) ?
C4A H4AA . 0.9300 ?
C5A C6A . 1.482(5) ?
C6A C7A . 1.385(5) ?
C7A C8A . 1.371(6) ?
C7A H7AA . 0.9300 ?
C8A C9A . 1.378(5) ?
C8A H8AA . 0.9300 ?
C9A C10A . 1.366(5) ?
C9A H9AA . 0.9300 ?
C10A H10A . 0.9300 ?
N1B C1B . 1.338(5) ?
N1B C5B . 1.349(4) ?
N2B C10B . 1.339(5) ?
N2B C6B . 1.348(4) ?
C1B C2B . 1.362(5) ?
C1B H1BA . 0.9300 ?
C2B C3B . 1.372(6) ?
C2B H2BA . 0.9300 ?
C3B C4B . 1.374(6) ?
C3B H3BA . 0.9300 ?
C4B C5B . 1.376(5) ?
C4B H4BA . 0.9300 ?
C5B C6B . 1.481(5) ?
C6B C7B . 1.376(5) ?
C7B C8B . 1.370(5) ?
C7B H7BA . 0.9300 ?
C8B C9B . 1.380(5) ?
C8B H8BA . 0.9300 ?
C9B C10B . 1.362(5) ?
C9B H9BA . 0.9300 ?
C10B H10B . 0.9300 ?
O1W H1WA . 0.82(2) ?
O1W H1WB . 0.82(2) ?
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
O1W H1WB O8 1_655 0.82(2) 1.92(7) 2.703(13) 160(16)
C7A H7AA O2 3_656 0.93 2.41 3.336(5) 170.8
C8A H8AA O7 3_656 0.93 2.40 3.301(5) 163.1
C1A H1AA O6 . 0.93 2.60 3.430(5) 149.5
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
_geom_torsion_publ_flag
S1 O4 O5 S2 125.56(17) y
O1 S1 O4 O5 -69.8(2) y
O2 S1 O4 O5 171.8(2) y
O3 S1 O4 O5 51.6(2) y
O6 S2 O4 O5 112.3(3) y
O7 S2 O5 O4 49.3(3) y
O8 S2 O5 O4 168.1(2) y
