#------------------------------------------------------------------------------
#$Date: 2017-04-05 11:35:42 +0200 (Wed 05 de Apr de 2017) $
#$Revision: 195034 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/77/7227751.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_7227751
loop_
_publ_author_name
'Azhdari Tehrani, Alireza'
'Ghasempour, Hosein'
'Morsali, Ali'
'Bauzá, Antonio'
'Frontera, Antonio'
'Retailleau, Pascal'
_publ_section_title
;
 Unraveling the dual character of sulfur atoms in a series of Hg(ii)
 coordination polymers containing bis(4-pyridyl)disulfide
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              1974
_journal_paper_doi               10.1039/C7CE00033B
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C10 H8 Hg I2 N2 S2'
_chemical_formula_sum            'C10 H8 Hg I2 N2 S2'
_chemical_formula_weight         674.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-02-15 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.445(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9527(11)
_cell_length_b                   10.2881(8)
_cell_length_c                   10.9667(9)
_cell_measurement_reflns_used    337
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.6
_cell_volume                     1569.5(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'HPAD Dectris Pilatus 200K'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 322
               Slice: -95.0000 - 66.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -24.0000
                 Phi: 108.0000
                 XTD: 35.0000
              2theta: -5.0000
scan:
    Number of images: 251
               Slice: -95.0000 - 30.5000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 108.0000
                 XTD: 35.0000
              2theta: -5.0000
scan:
    Number of images: 149
               Slice: -43.0000 - 31.5000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 56.0000
                 Phi: -36.0000
                 XTD: 35.0000
              2theta: -5.0000
scan:
    Number of images: 124
               Slice: -95.0000 - -33.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -24.0000
                 Phi: 72.0000
                 XTD: 35.0000
              2theta: -5.0000
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku XtalabPro mm003
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.003791
_diffrn_orient_matrix_UB_12      0.067740
_diffrn_orient_matrix_UB_13      -0.023310
_diffrn_orient_matrix_UB_21      -0.025113
_diffrn_orient_matrix_UB_22      0.029232
_diffrn_orient_matrix_UB_23      0.089033
_diffrn_orient_matrix_UB_31      0.087423
_diffrn_orient_matrix_UB_32      0.018690
_diffrn_orient_matrix_UB_33      0.018523
_diffrn_radiation_monochromator  'Confocal mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10991
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         3.961
_diffrn_source                   'Rigaku microsource mm003'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    13.987
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, Higashi 1998'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.855
_exptl_crystal_description       needle
_exptl_crystal_F_000             1200
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0213P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1688
_reflns_number_total             1810
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    hgi2.res created by SHELXL-2014/7

TITL shelx_a.res in C2/c
REM Old TITL shelx in C2/c #15
REM SHELXT solution in C2/c
REM R1 0.078, Rweak 0.005, Alpha 0.042, Orientation as input
REM Formula found by SHELXT: C12 Hg I2 S2
CELL 0.71075 13.9527 10.2881 10.9667 90 94.445 90
ZERR 4 0.0011 0.0008 0.0009 0 0.009 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Hg I N S
UNIT 40 32 4 8 8 8
 
L.S. 4
PLAN  20
  -100
BOND $H
LIST 4
MORE -1
CONF
fmap 2 53
acta
OMIT 3 1 10
OMIT -2 4 5
OMIT 4 10 7
OMIT -3 1 1
OMIT 0 2 1
OMIT 1 3 4
OMIT -1 1 2
OMIT 0 0 2
REM <olex2.extras>
REM <HklSrc "%./hgi2.hkl">
REM </olex2.extras>
 
WGHT    0.021300
FVAR       0.14249
HG1   3    0.500000    0.524744    0.250000    10.50000    0.01977    0.02576 =
         0.02545    0.00000    0.00472    0.00000
I1    4    0.319142    0.452400    0.268663    11.00000    0.02009    0.03563 =
         0.04038    0.00452    0.00630   -0.00258
S1    6    0.561017    0.998073    0.705322    11.00000    0.02194    0.02500 =
         0.01995   -0.00077    0.00285   -0.00334
N1    5    0.522506    0.686366    0.410158    11.00000    0.02824    0.02350 =
         0.02216   -0.00113    0.00497   -0.00140
C2    1    0.453079    0.707846    0.485233    11.00000    0.02701    0.02840 =
         0.02644   -0.00100    0.00817   -0.00603
AFIX  43
H2    2    0.396255    0.656901    0.474672    11.00000   -1.20000
AFIX   0
C3    1    0.459243    0.799832    0.577230    11.00000    0.02720    0.02752 =
         0.02390    0.00075    0.00793   -0.00403
AFIX  43
H3    2    0.408163    0.811260    0.628683    11.00000   -1.20000
AFIX   0
C4    1    0.541971    0.875351    0.592802    11.00000    0.02356    0.02176 =
         0.01838    0.00351    0.00251    0.00165
C5    1    0.602861    0.758709    0.427194    11.00000    0.02199    0.02923 =
         0.02335    0.00269    0.00733    0.00412
AFIX  43
H5    2    0.653480    0.743546    0.375802    11.00000   -1.20000
AFIX   0
C6    1    0.615205    0.854020    0.515937    11.00000    0.02177    0.02530 =
         0.02088    0.00400    0.00289   -0.00193
AFIX  43
H6    2    0.672596    0.903989    0.524266    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  shelx_a.res in C2/c
REM R1 =  0.0177 for    1688 Fo > 4sig(Fo)  and  0.0197 for all    1802 data
REM     78 parameters refined using      0 restraints
 
END  
     
WGHT      0.0213      0.0000 

REM Highest difference peak  1.184,  deepest hole -0.780,  1-sigma level  0.131
Q1    1   0.5032  0.5191  0.1632  11.00000  0.05    1.18
Q2    1   0.5026  0.5091  0.4498  11.00000  0.05    0.86
Q3    1   0.3213  0.4427  0.1921  11.00000  0.05    0.75
Q4    1   0.3172  0.4627  0.1005  11.00000  0.05    0.60
Q5    1   0.3171  0.5202  0.5037  11.00000  0.05    0.48
Q6    1   0.3019  0.5346  0.3921  11.00000  0.05    0.46
Q7    1   0.5415  0.5763  0.2519  11.00000  0.05    0.46
Q8    1   0.3151  0.4466  0.3723  11.00000  0.05    0.44
Q9    1   0.4316  0.4631  0.2977  11.00000  0.05    0.42
Q10   1   0.4170  0.5276  0.3926  11.00000  0.05    0.40
Q11   1   0.5697  0.9851  0.4021  11.00000  0.05    0.40
Q12   1   0.4399  0.5239  0.3646  11.00000  0.05    0.37
Q13   1   0.3765  0.5977  0.6163  11.00000  0.05    0.37
Q14   1   0.2558  0.5259  0.3336  11.00000  0.05    0.35
Q15   1   0.3941  0.4040  0.2139  11.00000  0.05    0.35
Q16   1   0.2814  0.3966  0.2556  11.00000  0.05    0.34
Q17   1   0.4834  0.4598  0.3814  11.00000  0.05    0.34
Q18   1   0.4197  0.7033  0.7372  11.00000  0.05    0.34
Q19   1   0.5401  0.4582  0.3800  11.00000  0.05    0.34
Q20   1   0.5973  0.7507  0.2356  11.00000  0.05    0.33

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0177 for 1688 Fo > 4sig(Fo) and 0.0197 for all 11411 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.18, deepest hole -0.78
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0197
  REM R1_gt = 0.0177
  REM wR_ref = 0.0414
  REM GOOF = 1.035
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 11411
  REM Reflections_gt = 1688
  REM Parameters = n/a
  REM Hole = -0.78
  REM Peak = 1.18
  REM Flack = n/a
  
  
;
_cod_data_source_file            c7ce00033b2.cif
_cod_data_source_block           HgI2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7227749--7227751.cif.
;
_cod_database_code               7227751
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Hg1 Hg 0.5000 0.52474(2) 0.2500 0.02351(6) Uani 1 2 d S T P
I1 I 0.31914(2) 0.45240(2) 0.26866(2) 0.03183(8) Uani 1 1 d . . .
S1 S 0.56102(5) 0.99807(8) 0.70532(7) 0.02223(15) Uani 1 1 d . . .
N1 N 0.52251(19) 0.6864(3) 0.4102(2) 0.0245(5) Uani 1 1 d . . .
C2 C 0.4531(2) 0.7078(3) 0.4852(3) 0.0270(7) Uani 1 1 d . . .
H2 H 0.3963 0.6569 0.4747 0.032 Uiso 1 1 calc R . .
C3 C 0.4592(2) 0.7998(3) 0.5772(3) 0.0259(6) Uani 1 1 d . . .
H3 H 0.4082 0.8113 0.6287 0.031 Uiso 1 1 calc R . .
C4 C 0.5420(2) 0.8754(3) 0.5928(3) 0.0212(6) Uani 1 1 d . . .
C5 C 0.6029(2) 0.7587(3) 0.4272(3) 0.0246(6) Uani 1 1 d . . .
H5 H 0.6535 0.7435 0.3758 0.029 Uiso 1 1 calc R . .
C6 C 0.6152(2) 0.8540(3) 0.5159(3) 0.0226(6) Uani 1 1 d . . .
H6 H 0.6726 0.9040 0.5243 0.027 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hg1 0.01977(9) 0.02576(10) 0.02545(10) 0.000 0.00472(6) 0.000
I1 0.02009(12) 0.03563(12) 0.04038(15) 0.00452(9) 0.00630(9) -0.00258(8)
S1 0.0219(4) 0.0250(3) 0.0200(3) -0.0008(3) 0.0029(3) -0.0033(3)
N1 0.0282(14) 0.0235(13) 0.0222(12) -0.0011(10) 0.0050(10) -0.0014(10)
C2 0.0270(17) 0.0284(16) 0.0264(16) -0.0010(13) 0.0082(13) -0.0060(13)
C3 0.0272(16) 0.0275(15) 0.0239(15) 0.0007(13) 0.0079(12) -0.0040(12)
C4 0.0236(14) 0.0218(14) 0.0184(13) 0.0035(11) 0.0025(11) 0.0017(11)
C5 0.0220(15) 0.0292(16) 0.0233(15) 0.0027(13) 0.0073(12) 0.0041(12)
C6 0.0218(14) 0.0253(14) 0.0209(14) 0.0040(12) 0.0029(11) -0.0019(12)
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'
Hg Hg -2.3894 9.2266 '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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I1 Hg1 I1 147.427(12) . 2_655
N1 Hg1 I1 100.25(6) 2_655 .
N1 Hg1 I1 100.25(6) . 2_655
N1 Hg1 I1 101.96(6) . .
N1 Hg1 I1 101.96(6) 2_655 2_655
N1 Hg1 N1 93.26(12) 2_655 .
C4 S1 S1 104.49(11) . 2_656
C2 N1 Hg1 120.0(2) . .
C2 N1 C5 117.3(3) . .
C5 N1 Hg1 122.7(2) . .
N1 C2 H2 118.1 . .
N1 C2 C3 123.8(3) . .
C3 C2 H2 118.1 . .
C2 C3 H3 120.8 . .
C2 C3 C4 118.5(3) . .
C4 C3 H3 120.8 . .
C3 C4 S1 124.2(2) . .
C3 C4 C6 118.6(3) . .
C6 C4 S1 117.2(2) . .
N1 C5 H5 118.4 . .
N1 C5 C6 123.1(3) . .
C6 C5 H5 118.4 . .
C4 C6 H6 120.6 . .
C5 C6 C4 118.7(3) . .
C5 C6 H6 120.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 I1 2.6540(3) .
Hg1 I1 2.6540(3) 2_655
Hg1 N1 2.421(3) 2_655
Hg1 N1 2.421(3) .
S1 S1 2.0293(15) 2_656
S1 C4 1.771(3) .
N1 C2 1.337(4) .
N1 C5 1.347(4) .
C2 H2 0.9500 .
C2 C3 1.381(5) .
C3 H3 0.9500 .
C3 C4 1.391(4) .
C4 C6 1.392(4) .
C5 H5 0.9500 .
C5 C6 1.383(5) .
C6 H6 0.9500 .
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_site_symmetry_1
Hg1 N1 C2 C3 -178.7(2) .
Hg1 N1 C5 C6 177.9(2) .
S1 S1 C4 C3 -0.6(3) 2_656
S1 S1 C4 C6 179.6(2) 2_656
S1 C4 C6 C5 179.8(2) .
N1 C2 C3 C4 0.4(5) .
N1 C5 C6 C4 1.0(5) .
C2 N1 C5 C6 -1.3(4) .
C2 C3 C4 S1 179.5(2) .
C2 C3 C4 C6 -0.7(4) .
C3 C4 C6 C5 0.0(4) .
C5 N1 C2 C3 0.6(5) .
