#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:45:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179126 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/88/4308862.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_4308862
loop_
_publ_author_name
'Masahiro Kato'
'Kazunori Kojima'
'Taka-aki Okamura'
'Hitoshi Yamamoto'
'Takeshi Yamamura'
'Norikazu Ueyama'
_publ_section_title
;
Relation between Intramolecular NH...S Hydrogen Bonds and Coordination
Number in Mercury(II) Complexes with Carbamoylbenzenethiol Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4037
_journal_page_last               4044
_journal_paper_doi               10.1021/ic0481780
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C28 H24 Hg N2 O2 S2'
_chemical_formula_weight         685.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             'Tue Dec 21 23:22:12 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.389(13)
_cell_angle_beta                 100.939(18)
_cell_angle_gamma                92.295(17)
_cell_formula_units_Z            1
_cell_length_a                   4.6960(13)
_cell_length_b                   11.8346(18)
_cell_length_c                   12.327(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      13.4
_cell_measurement_theta_min      11.2
_cell_volume                     651.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4195
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    6.091
_exptl_absorpt_correction_T_max  0.544
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0211P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                2023
_reflns_number_total             3778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0481780si20041224_115539.cif
_cod_data_source_block           complex3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4308862
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 0.0000 0.0000 0.0000 0.06466(13) Uani 1 2 d S . .
S1 S 0.3996(3) 0.09991(11) 0.13704(10) 0.0669(4) Uani 1 1 d . . .
O1 O 0.6457(8) 0.2114(5) -0.0684(3) 0.1035(15) Uani 1 1 d . . .
N1 N 0.1655(8) 0.1889(4) -0.1405(3) 0.0551(10) Uani 1 1 d . . .
H1 H -0.0027 0.2062 -0.1271 0.066 Uiso 1 1 calc R . .
C11 C 0.3239(10) 0.2467(4) 0.1429(3) 0.0507(12) Uani 1 1 d . . .
C12 C 0.2636(13) 0.3134(5) 0.2420(4) 0.0728(16) Uani 1 1 d . . .
H12 H 0.2592 0.2799 0.3030 0.087 Uiso 1 1 calc R . .
C13 C 0.2100(15) 0.4283(5) 0.2525(5) 0.091(2) Uani 1 1 d . . .
H13 H 0.1704 0.4720 0.3201 0.109 Uiso 1 1 calc R . .
C14 C 0.2148(14) 0.4786(5) 0.1629(5) 0.0848(19) Uani 1 1 d . . .
H14 H 0.1795 0.5565 0.1698 0.102 Uiso 1 1 calc R . .
C15 C 0.2728(11) 0.4126(4) 0.0622(4) 0.0666(15) Uani 1 1 d . . .
H15 H 0.2723 0.4459 0.0008 0.080 Uiso 1 1 calc R . .
C16 C 0.3311(9) 0.2980(4) 0.0526(4) 0.0479(11) Uani 1 1 d . . .
C17 C 0.3953(11) 0.2289(4) -0.0577(4) 0.0544(12) Uani 1 1 d . . .
C18 C 0.1767(12) 0.1172(5) -0.2536(3) 0.0670(15) Uani 1 1 d . . .
H18A H 0.0570 0.0445 -0.2678 0.080 Uiso 1 1 calc R . .
H18B H 0.3754 0.0986 -0.2552 0.080 Uiso 1 1 calc R . .
C101 C 0.0712(11) 0.1784(4) -0.3469(3) 0.0523(12) Uani 1 1 d . . .
C102 C 0.1972(14) 0.2810(5) -0.3507(5) 0.0829(18) Uani 1 1 d . . .
H102 H 0.3511 0.3179 -0.2922 0.099 Uiso 1 1 calc R . .
C103 C 0.1049(16) 0.3336(6) -0.4394(6) 0.096(2) Uani 1 1 d . . .
H103 H 0.1975 0.4042 -0.4402 0.116 Uiso 1 1 calc R . .
C104 C -0.1181(17) 0.2822(7) -0.5238(5) 0.097(2) Uani 1 1 d . . .
H104 H -0.1807 0.3167 -0.5837 0.116 Uiso 1 1 calc R . .
C105 C -0.2524(17) 0.1793(8) -0.5214(5) 0.111(2) Uani 1 1 d . . .
H105 H -0.4102 0.1441 -0.5791 0.133 Uiso 1 1 calc R . .
C106 C -0.1557(14) 0.1262(6) -0.4336(5) 0.0886(19) Uani 1 1 d . . .
H106 H -0.2458 0.0547 -0.4337 0.106 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 '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'
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
S1 Hg1 S1 180.0 . 2 ?
C11 S1 Hg1 100.88(15) . . ?
C17 N1 C18 124.7(4) . . ?
C17 N1 H1 117.6 . . ?
C18 N1 H1 117.6 . . ?
C12 C11 C16 118.8(4) . . ?
C12 C11 S1 118.6(4) . . ?
C16 C11 S1 122.6(4) . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C14 C13 C12 120.0(5) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.6(5) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 120.3(5) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C11 120.1(4) . . ?
C15 C16 C17 119.0(4) . . ?
C11 C16 C17 120.8(4) . . ?
O1 C17 N1 123.0(5) . . ?
O1 C17 C16 121.4(5) . . ?
N1 C17 C16 115.5(4) . . ?
N1 C18 C101 112.0(4) . . ?
N1 C18 H18A 109.2 . . ?
C101 C18 H18A 109.2 . . ?
N1 C18 H18B 109.2 . . ?
C101 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C102 C101 C106 117.9(5) . . ?
C102 C101 C18 122.9(5) . . ?
C106 C101 C18 119.2(5) . . ?
C101 C102 C103 122.1(6) . . ?
C101 C102 H102 119.0 . . ?
C103 C102 H102 119.0 . . ?
C104 C103 C102 119.7(7) . . ?
C104 C103 H103 120.1 . . ?
C102 C103 H103 120.1 . . ?
C103 C104 C105 119.6(6) . . ?
C103 C104 H104 120.2 . . ?
C105 C104 H104 120.2 . . ?
C104 C105 C106 120.4(7) . . ?
C104 C105 H105 119.8 . . ?
C106 C105 H105 119.8 . . ?
C101 C106 C105 120.3(6) . . ?
C101 C106 H106 119.8 . . ?
C105 C106 H106 119.8 . . ?
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 S1 2.3384(15) . ?
Hg1 S1 2.3384(15) 2 ?
S1 C11 1.775(5) . ?
O1 C17 1.229(5) . ?
N1 C17 1.322(6) . ?
N1 C18 1.466(5) . ?
N1 H1 0.8600 . ?
C11 C12 1.378(6) . ?
C11 C16 1.391(6) . ?
C12 C13 1.374(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.386(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.505(6) . ?
C18 C101 1.513(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C101 C102 1.344(7) . ?
C101 C106 1.367(7) . ?
C102 C103 1.388(7) . ?
C102 H102 0.9300 . ?
C103 C104 1.338(9) . ?
C103 H103 0.9300 . ?
C104 C105 1.358(9) . ?
C104 H104 0.9300 . ?
C105 C106 1.388(8) . ?
C105 H105 0.9300 . ?
C106 H106 0.9300 . ?
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
Hg1 S1 C11 C12 114.3(4) . . . . ?
Hg1 S1 C11 C16 -67.6(4) . . . . ?
C16 C11 C12 C13 0.3(8) . . . . ?
S1 C11 C12 C13 178.5(5) . . . . ?
C11 C12 C13 C14 0.2(10) . . . . ?
C12 C13 C14 C15 0.3(10) . . . . ?
C13 C14 C15 C16 -1.3(9) . . . . ?
C14 C15 C16 C11 1.9(8) . . . . ?
C14 C15 C16 C17 -179.6(5) . . . . ?
C12 C11 C16 C15 -1.3(7) . . . . ?
S1 C11 C16 C15 -179.5(4) . . . . ?
C12 C11 C16 C17 -179.9(5) . . . . ?
S1 C11 C16 C17 2.0(6) . . . . ?
C18 N1 C17 O1 1.5(8) . . . . ?
C18 N1 C17 C16 -178.3(4) . . . . ?
C15 C16 C17 O1 101.1(6) . . . . ?
C11 C16 C17 O1 -80.4(7) . . . . ?
C15 C16 C17 N1 -79.1(6) . . . . ?
C11 C16 C17 N1 99.4(5) . . . . ?
C17 N1 C18 C101 -116.2(5) . . . . ?
N1 C18 C101 C102 59.6(7) . . . . ?
N1 C18 C101 C106 -122.7(5) . . . . ?
C106 C101 C102 C103 -0.4(9) . . . . ?
C18 C101 C102 C103 177.4(5) . . . . ?
C101 C102 C103 C104 0.6(10) . . . . ?
C102 C103 C104 C105 0.3(11) . . . . ?
C103 C104 C105 C106 -1.4(12) . . . . ?
C102 C101 C106 C105 -0.7(9) . . . . ?
C18 C101 C106 C105 -178.6(6) . . . . ?
C104 C105 C106 C101 1.7(11) . . . . ?
