#------------------------------------------------------------------------------
#$Date: 2022-04-20 02:10:13 +0300 (Wed, 20 Apr 2022) $
#$Revision: 274588 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/00/7710058.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_7710058
loop_
_publ_author_name
'Viau, Lydie'
'Knorr, Michael'
'Knauer, Lena'
'Brieger, Lukas'
'Strohman, Carsten'
_publ_section_title
;
 2,2’-Ethylenebis(1,3-dithiane) as polydentate m2-, m4- and
 m5-assembling ligand for the construction of sulphur-rich Cu(I), Hg(II)
 and heterometallic Cu(I)/Hg(II) coordination polymers featuring uncommon
 network architectures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00800A
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H20 Br2 Hg S4'
_chemical_formula_sum            'C10 H20 Br2 Hg S4'
_chemical_formula_weight         628.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2203(3)
_cell_length_b                   22.7657(9)
_cell_length_c                   4.4494(2)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.63
_cell_volume                     832.66(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker, 2021)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CPAD PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            18946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.981
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.521
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.3910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0857 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.6928.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0192
_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)+(0.0058P)²+0.9928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0326
_refine_ls_wR_factor_ref         0.0334
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1923
_reflns_number_total             2004
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00800a2.cif
_cod_data_source_block           b2065
_cod_database_code               7710058
_shelx_shelxl_version_number     2018/3
_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. Twinned data refinement
 Scales: 0.502(8)
 0.498(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Hg1A(0.4875) Hg1B(0.0125)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_file
;
TITL b2065_b.res in P2(1)2(1)2
    b2065.res
    created by SHELXL-2018/3 at 09:51:57 on 30-Mar-2022
REM Old TITL B2065 in P21212 #18
REM SHELXT solution in P2(1)2(1)2
REM R1 0.039, Rweak 0.020, Alpha 0.007, Orientation as input
REM Flack x = 0.499 ( 0.004 ) from Parsons' quotients
REM Formula found by SHELXT: C10 Br2 Hg S4
CELL 0.71073 8.2203 22.7657 4.4494 90 90 90
ZERR 2 0.0003 0.0009 0.0002 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br Hg S
UNIT 20 40 4 2 8

L.S. 10
PLAN  5
TEMP -173.15
CONF
BOND $H
LIST 6
MORE -1
fmap 2
ACTA
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT -3 56
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\B2065.hkl">
REM </olex2.extras>

WGHT    0.005800    0.992800
BASF   0.49783
FVAR       0.46243
PART 1
HG1A  4    0.500000    0.500000    0.434054    10.48750    0.01212    0.01375 =
         0.01822    0.00000    0.00000    0.00011
PART 2
HG1B  4    0.500000    0.500000    0.044927    10.01250    0.04150    0.03555 =
         0.05101    0.00000    0.00000    0.02192
PART 0
BR1   3    0.736147    0.545200    0.743124    11.00000    0.01561    0.01688 =
         0.01757   -0.00093   -0.00124   -0.00250
S1    5    0.646939    0.416338    0.135191    11.00000    0.01234    0.01430 =
         0.01679    0.00055   -0.00046   -0.00036
S2    5    0.717638    0.288288    0.172826    11.00000    0.01588    0.01490 =
         0.02510   -0.00283   -0.00087    0.00178
C1    1    0.588747    0.346852    0.310537    11.00000    0.01733    0.01132 =
         0.01643    0.00166    0.00316    0.00065
AFIX  13
H1    2    0.600958    0.350145    0.533515    11.00000   -1.20000
AFIX   0
C2    1    0.852077    0.423041    0.282177    11.00000    0.01366    0.01460 =
         0.02038   -0.00325   -0.00514   -0.00160
AFIX  23
H2A   2    0.899347    0.460611    0.211967    11.00000   -1.20000
H2B   2    0.847038    0.424410    0.504374    11.00000   -1.20000
AFIX   0
C3    1    0.963983    0.372838    0.187795    11.00000    0.01357    0.02076 =
         0.02175   -0.00032    0.00005    0.00287
AFIX  23
H3A   2    0.966878    0.370994   -0.034443    11.00000   -1.20000
H3B   2    1.075612    0.381568    0.258353    11.00000   -1.20000
AFIX   0
C4    1    0.913553    0.313231    0.308078    11.00000    0.01670    0.02052 =
         0.02709   -0.00052   -0.00252    0.00611
AFIX  23
H4A   2    0.910328    0.315090    0.530297    11.00000   -1.20000
H4B   2    0.997176    0.283987    0.251073    11.00000   -1.20000
AFIX   0
C5    1    0.413243    0.332640    0.234652    11.00000    0.01631    0.01614 =
         0.02594    0.00006    0.00005   -0.00134
AFIX 137
H5A   2    0.342358    0.363811    0.311628    11.00000   -1.50000
H5B   2    0.383034    0.295134    0.327231    11.00000   -1.50000
H5C   2    0.400927    0.329792    0.016061    11.00000   -1.50000
AFIX   0
HKLF 4




REM  b2065_b.res in P2(1)2(1)2
REM wR2 = 0.033356, GooF = S = 1.13864, Restrained GooF = 1.13864 for all data
REM R1 = 0.019182 for 1923 Fo > 4sig(Fo) and 0.021330 for all 2004 data
REM 85 parameters refined using 0 restraints

END

WGHT      0.0058      0.9928

REM Highest difference peak  0.763,  deepest hole -0.923,  1-sigma level  0.126
Q1    1   0.5000  0.5000  0.3140  10.50000  0.05    0.76
Q2    1   0.5000  0.5000  0.7089  10.50000  0.05    0.75
Q3    1   0.5655  0.5410  0.6194  11.00000  0.05    0.71
Q4    1   0.4363  0.5378  0.6305  11.00000  0.05    0.67
Q5    1   0.7475  0.4523  0.1177  11.00000  0.05    0.51
;
_shelx_res_checksum              1291
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1A Hg 0.500000 0.500000 0.43405(6) 0.01470(7) Uani 0.975 2 d S T P A 1
Hg1B Hg 0.500000 0.500000 0.045(3) 0.043(3) Uani 0.025 2 d S T P A 2
Br1 Br 0.73615(6) 0.54520(2) 0.74312(12) 0.01669(11) Uani 1 1 d . . . . .
S1 S 0.64694(16) 0.41634(6) 0.1352(3) 0.0145(3) Uani 1 1 d . . . . .
S2 S 0.71764(17) 0.28829(6) 0.1728(3) 0.0186(3) Uani 1 1 d . . . . .
C1 C 0.5887(7) 0.3469(2) 0.3105(14) 0.0150(13) Uani 1 1 d . . . . .
H1 H 0.600958 0.350145 0.533515 0.018 Uiso 1 1 calc R U . . .
C2 C 0.8521(6) 0.4230(2) 0.2822(13) 0.0162(11) Uani 1 1 d . . . . .
H2A H 0.899347 0.460611 0.211967 0.019 Uiso 1 1 calc R U . . .
H2B H 0.847038 0.424410 0.504374 0.019 Uiso 1 1 calc R U . . .
C3 C 0.9640(6) 0.3728(2) 0.1878(12) 0.0187(12) Uani 1 1 d . . . . .
H3A H 0.966878 0.370994 -0.034443 0.022 Uiso 1 1 calc R U . . .
H3B H 1.075612 0.381568 0.258353 0.022 Uiso 1 1 calc R U . . .
C4 C 0.9136(6) 0.3132(2) 0.3081(14) 0.0214(13) Uani 1 1 d . . . . .
H4A H 0.910328 0.315090 0.530297 0.026 Uiso 1 1 calc R U . . .
H4B H 0.997176 0.283987 0.251073 0.026 Uiso 1 1 calc R U . . .
C5 C 0.4132(7) 0.3326(2) 0.2347(16) 0.0195(13) Uani 1 1 d . . . . .
H5A H 0.342358 0.363811 0.311628 0.029 Uiso 1 1 calc R U . . .
H5B H 0.383034 0.295134 0.327231 0.029 Uiso 1 1 calc R U . . .
H5C H 0.400927 0.329792 0.016061 0.029 Uiso 1 1 calc R U . . .
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
Hg1A 0.01212(12) 0.01375(12) 0.01822(12) 0.000 0.000 0.00011(19)
Hg1B 0.041(7) 0.036(7) 0.051(8) 0.000 0.000 0.022(11)
Br1 0.0156(3) 0.0169(2) 0.0176(2) -0.0009(2) -0.0012(2) -0.0025(2)
S1 0.0123(6) 0.0143(6) 0.0168(7) 0.0005(5) -0.0005(5) -0.0004(5)
S2 0.0159(7) 0.0149(6) 0.0251(7) -0.0028(5) -0.0009(6) 0.0018(5)
C1 0.017(3) 0.011(3) 0.016(3) 0.002(2) 0.003(2) 0.001(2)
C2 0.014(2) 0.015(2) 0.020(3) -0.003(2) -0.005(2) -0.002(2)
C3 0.014(3) 0.021(3) 0.022(3) 0.000(2) 0.000(2) 0.003(2)
C4 0.017(3) 0.021(3) 0.027(3) -0.001(2) -0.003(2) 0.006(2)
C5 0.016(3) 0.016(3) 0.026(3) 0.000(3) 0.000(3) -0.001(2)
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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 -1.00 0.1460
-1.00 0.00 0.00 0.1660
-1.00 -1.00 1.00 0.1460
0.00 1.00 -1.00 0.0190
0.00 -1.00 1.00 0.0160
-1.00 1.00 -1.00 0.1470
1.00 -1.00 1.00 0.0920
0.00 -1.00 -1.00 0.0220
0.00 1.00 1.00 0.0150
0.00 1.00 0.00 0.0180
0.00 -1.00 0.00 0.0170
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
_geom_angle_publ_flag
Br1 Hg1A Br1 115.91(3) 2_665 . ?
Br1 Hg1A S1 109.04(3) . 2_665 ?
Br1 Hg1A S1 109.04(3) 2_665 . ?
Br1 Hg1A S1 102.28(3) . . ?
Br1 Hg1A S1 102.28(3) 2_665 2_665 ?
S1 Hg1A S1 118.95(6) . 2_665 ?
Br1 Hg1B Br1 117.1(6) 2_664 1_554 ?
S1 Hg1B Br1 91.50(15) 2_665 2_664 ?
S1 Hg1B Br1 91.50(15) . 1_554 ?
S1 Hg1B Br1 99.02(16) 2_665 1_554 ?
S1 Hg1B Br1 99.02(16) . 2_664 ?
S1 Hg1B S1 159.8(8) . 2_665 ?
C1 S1 Hg1A 106.98(18) . . ?
C1 S1 Hg1B 131.0(2) . . ?
C2 S1 Hg1A 100.63(17) . . ?
C2 S1 Hg1B 118.9(2) . . ?
C2 S1 C1 99.3(3) . . ?
C1 S2 C4 100.2(3) . . ?
S1 C1 H1 109.4 . . ?
S2 C1 S1 109.9(3) . . ?
S2 C1 H1 109.4 . . ?
C5 C1 S1 109.8(4) . . ?
C5 C1 S2 108.9(4) . . ?
C5 C1 H1 109.4 . . ?
S1 C2 H2A 108.9 . . ?
S1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 S1 113.4(3) . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 C2 114.1(4) . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
S2 C4 H4A 108.8 . . ?
S2 C4 H4B 108.8 . . ?
C3 C4 S2 114.0(4) . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1A Br1 2.5919(5) 2_665 ?
Hg1A Br1 2.5920(5) . ?
Hg1A S1 2.6182(13) . ?
Hg1A S1 2.6182(13) 2_665 ?
Hg1B Br1 2.575(8) 1_554 ?
Hg1B Br1 2.575(8) 2_664 ?
Hg1B S1 2.291(3) . ?
Hg1B S1 2.291(3) 2_665 ?
S1 C1 1.828(6) . ?
S1 C2 1.815(5) . ?
S2 C1 1.810(5) . ?
S2 C4 1.811(6) . ?
C1 H1 1.0000 . ?
C1 C5 1.517(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.526(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hg1A S1 C1 S2 -167.7(2) . . . . ?
Hg1A S1 C1 C5 72.6(4) . . . . ?
Hg1A S1 C2 C3 170.5(4) . . . . ?
Hg1B S1 C1 S2 154.2(5) . . . . ?
Hg1B S1 C1 C5 34.4(7) . . . . ?
Hg1B S1 C2 C3 -150.6(5) . . . . ?
S1 C2 C3 C4 -64.2(6) . . . . ?
C1 S1 C2 C3 61.1(4) . . . . ?
C1 S2 C4 C3 -59.8(4) . . . . ?
C2 S1 C1 S2 -63.4(3) . . . . ?
C2 S1 C1 C5 176.8(4) . . . . ?
C2 C3 C4 S2 63.2(6) . . . . ?
C4 S2 C1 S1 62.8(3) . . . . ?
C4 S2 C1 C5 -176.9(5) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.502(8)
2 0.498(8)
