#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005484.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_7005484
loop_
_publ_author_name
'Seredyuk, Maksym'
'Haukka, Matti'
'Fritsky, Igor O.'
'Kozłowski, Henryk'
'Krämer, Roland'
'Pavlenko, Vadim A.'
'Gütlich, Philipp'
_publ_section_title
;
 Bis(3,5-dimethyl-1H-pyrazolyl)selenide--a new bidentate bent connector
 for preparation of 1D and 2D co-ordination polymers.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3183
_journal_page_last               3194
_journal_paper_doi               10.1039/b702574b
_journal_year                    2007
_chemical_formula_moiety         'C14 H14 Hg2 N8 S4 Se'
_chemical_formula_sum            'C14 H14 Hg2 N8 S4 Se'
_chemical_formula_weight         902.71
_chemical_name_common
;
catena-((mu-trans-bis(3,5-dimethyl-1H-pyrazolyl)selenide)bis
(thiocyanato)mercury(ii)) hexakix(bis)mercurate(ii)
;
_chemical_name_systematic
;
catena-{[mu-trans-bis(3,5-dimethyl-1H-pyrazolyl)selenide]bis
[thiocyanato]mercury(II)} hexakix(bis)mercurate(II)
;
_space_group_IT_number           2
_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                110.626(6)
_cell_angle_beta                 97.843(3)
_cell_angle_gamma                91.907(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3331(3)
_cell_length_b                   10.4321(8)
_cell_length_c                   12.8190(9)
_cell_measurement_reflns_used    5225
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1152.71(13)
_computing_cell_refinement       'EvalCCD (Duisenberg, 1998-2003)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998-2003)'
_computing_molecular_graphics    'Diamond v.3.1d (Crystal Impact GbR, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23114
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    15.262
_exptl_absorpt_correction_T_max  0.1861
_exptl_absorpt_correction_T_min  0.1160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.640
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0169P)²+0.3972P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0390
_reflns_number_gt                4479
_reflns_number_total             5289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702574b.txt
_cod_data_source_block           2
_cod_database_code               7005484
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.797505(14) 0.352615(14) 0.776516(11) 0.01672(4) Uani 1 1 d . . .
Hg2 Hg 0.329759(14) 0.178338(13) 0.923891(10) 0.01546(4) Uani 1 1 d . . .
Se1 Se 1.25401(4) 0.49093(4) 0.51248(3) 0.01646(8) Uani 1 1 d . . .
S1 S 0.77485(9) 0.50306(9) 0.97545(7) 0.01703(18) Uani 1 1 d . . .
S2 S 0.86648(11) 0.12570(9) 0.78003(8) 0.0255(2) Uani 1 1 d . . .
S3 S 0.25155(9) 0.10408(9) 1.06498(7) 0.01652(18) Uani 1 1 d . . .
S4 S 0.29534(11) 0.24648(9) 0.76346(8) 0.0239(2) Uani 1 1 d . . .
N1 N 0.9709(3) 0.4535(3) 0.7170(2) 0.0146(6) Uani 1 1 d . . .
N2 N 1.0259(3) 0.5866(3) 0.7697(2) 0.0172(6) Uani 1 1 d . . .
H2N H 1.002(5) 0.639(4) 0.840(4) 0.037(12) Uiso 1 1 d . . .
N3 N 1.6073(3) 0.3482(3) 0.6463(2) 0.0136(6) Uani 1 1 d . . .
N4 N 1.5523(3) 0.2364(3) 0.5532(2) 0.0150(6) Uani 1 1 d . . .
H4N H 1.597(5) 0.162(4) 0.530(3) 0.030(12) Uiso 1 1 d . . .
N5 N 0.5686(3) 0.3210(3) 1.0049(2) 0.0232(7) Uani 1 1 d . . .
N6 N 0.9980(3) 0.2396(3) 1.0072(3) 0.0221(7) Uani 1 1 d . . .
N7 N 0.5110(3) 0.0115(3) 1.1419(3) 0.0212(7) Uani 1 1 d . . .
N8 N 0.3104(4) -0.0033(3) 0.5844(3) 0.0272(8) Uani 1 1 d . . .
C1 C 1.0354(4) 0.4033(3) 0.6262(3) 0.0134(7) Uani 1 1 d . . .
C2 C 0.9988(4) 0.2591(4) 0.5449(3) 0.0202(8) Uani 1 1 d . . .
H2A H 1.0256 0.1950 0.5832 0.030 Uiso 1 1 calc R . .
H2B H 1.0525 0.2433 0.4816 0.030 Uiso 1 1 calc R . .
H2C H 0.8943 0.2443 0.5166 0.030 Uiso 1 1 calc R . .
C3 C 1.1349(4) 0.5048(4) 0.6237(3) 0.0147(7) Uani 1 1 d . . .
C4 C 1.1261(4) 0.6213(4) 0.7172(3) 0.0173(7) Uani 1 1 d . . .
C5 C 1.2007(4) 0.7615(4) 0.7597(3) 0.0273(9) Uani 1 1 d . . .
H5A H 1.1284 0.8292 0.7720 0.041 Uiso 1 1 calc R . .
H5B H 1.2586 0.7714 0.7043 0.041 Uiso 1 1 calc R . .
H5C H 1.2645 0.7770 0.8312 0.041 Uiso 1 1 calc R . .
C6 C 1.5175(4) 0.4455(3) 0.6489(3) 0.0143(7) Uani 1 1 d . . .
C7 C 1.5421(4) 0.5842(3) 0.7378(3) 0.0208(8) Uani 1 1 d . . .
H7A H 1.4854 0.5877 0.7976 0.031 Uiso 1 1 calc R . .
H7B H 1.5118 0.6528 0.7051 0.031 Uiso 1 1 calc R . .
H7C H 1.6456 0.6039 0.7697 0.031 Uiso 1 1 calc R . .
C8 C 1.4046(3) 0.3946(3) 0.5567(3) 0.0131(7) Uani 1 1 d . . .
C9 C 1.4318(4) 0.2612(3) 0.4977(3) 0.0140(7) Uani 1 1 d . . .
C10 C 1.3514(4) 0.1540(4) 0.3940(3) 0.0222(8) Uani 1 1 d . . .
H10A H 1.4206 0.0992 0.3498 0.033 Uiso 1 1 calc R . .
H10B H 1.2934 0.1981 0.3486 0.033 Uiso 1 1 calc R . .
H10C H 1.2871 0.0941 0.4149 0.033 Uiso 1 1 calc R . .
C11 C 0.6514(4) 0.3949(4) 0.9913(3) 0.0160(7) Uani 1 1 d . . .
C12 C 0.9436(4) 0.1926(3) 0.9145(3) 0.0160(7) Uani 1 1 d . . .
C13 C 0.4070(4) 0.0484(3) 1.1068(3) 0.0157(7) Uani 1 1 d . . .
C14 C 0.3055(4) 0.0951(4) 0.6600(3) 0.0190(8) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Hg1 N1 98.97(10) 1_455 . ?
N3 Hg1 S2 116.28(7) 1_455 . ?
N1 Hg1 S2 110.59(8) . . ?
N3 Hg1 S1 114.19(7) 1_455 . ?
N1 Hg1 S1 108.67(7) . . ?
S2 Hg1 S1 107.70(3) . . ?
S4 Hg2 S3 154.83(3) . . ?
S4 Hg2 N7 100.18(7) . 2_657 ?
S3 Hg2 N7 94.85(7) . 2_657 ?
S4 Hg2 N5 93.26(8) . . ?
S3 Hg2 N5 108.63(7) . . ?
N7 Hg2 N5 82.90(10) 2_657 . ?
C8 Se1 C3 100.52(14) . . ?
C11 S1 Hg1 94.79(12) . . ?
C12 S2 Hg1 92.80(12) . . ?
C13 S3 Hg2 98.58(12) . . ?
C14 S4 Hg2 100.22(13) . . ?
C1 N1 N2 106.2(3) . . ?
C1 N1 Hg1 129.9(2) . . ?
N2 N1 Hg1 123.9(2) . . ?
C4 N2 N1 112.1(3) . . ?
C4 N2 H2N 127(3) . . ?
N1 N2 H2N 121(3) . . ?
C6 N3 N4 106.0(3) . . ?
C6 N3 Hg1 128.3(2) . 1_655 ?
N4 N3 Hg1 125.4(2) . 1_655 ?
C9 N4 N3 111.7(3) . . ?
C9 N4 H4N 125(3) . . ?
N3 N4 H4N 123(3) . . ?
C11 N5 Hg2 144.5(3) . . ?
C13 N7 Hg2 138.0(3) . 2_657 ?
N1 C1 C3 109.3(3) . . ?
N1 C1 C2 121.6(3) . . ?
C3 C1 C2 129.1(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C1 106.5(3) . . ?
C4 C3 Se1 126.0(3) . . ?
C1 C3 Se1 127.4(3) . . ?
N2 C4 C3 105.9(3) . . ?
N2 C4 C5 121.5(3) . . ?
C3 C4 C5 132.7(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C8 109.5(3) . . ?
N3 C6 C7 122.2(3) . . ?
C8 C6 C7 128.3(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C6 106.0(3) . . ?
C9 C8 Se1 125.9(2) . . ?
C6 C8 Se1 127.9(3) . . ?
N4 C9 C8 106.8(3) . . ?
N4 C9 C10 121.5(3) . . ?
C8 C9 C10 131.7(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 S1 178.2(3) . . ?
N6 C12 S2 179.2(4) . . ?
N7 C13 S3 175.7(3) . . ?
N8 C14 S4 175.3(3) . . ?
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
Hg1 N3 2.251(3) 1_455 ?
Hg1 N1 2.259(3) . ?
Hg1 S2 2.4877(10) . ?
Hg1 S1 2.5220(9) . ?
Hg2 S4 2.3881(9) . ?
Hg2 S3 2.3904(9) . ?
Hg2 N7 2.490(3) 2_657 ?
Hg2 N5 2.514(3) . ?
Se1 C8 1.894(3) . ?
Se1 C3 1.894(3) . ?
S1 C11 1.667(4) . ?
S2 C12 1.660(4) . ?
S3 C13 1.671(4) . ?
S4 C14 1.682(4) . ?
N1 C1 1.331(4) . ?
N1 N2 1.358(4) . ?
N2 C4 1.334(4) . ?
N2 H2N 0.93(4) . ?
N3 C6 1.333(4) . ?
N3 N4 1.364(4) . ?
N3 Hg1 2.251(3) 1_655 ?
N4 C9 1.329(4) . ?
N4 H4N 0.87(4) . ?
N5 C11 1.147(4) . ?
N6 C12 1.149(4) . ?
N7 C13 1.149(5) . ?
N7 Hg2 2.490(3) 2_657 ?
N8 C14 1.144(5) . ?
C1 C3 1.397(5) . ?
C1 C2 1.493(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.389(5) . ?
C4 C5 1.479(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C8 1.403(5) . ?
C6 C7 1.480(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.381(5) . ?
C9 C10 1.485(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N N6 0.93(4) 1.92(4) 2.839(4) 167(4) 2_767
