#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:45 +0100 (mar 22 de mar de 2016) $
#$Revision: 179136 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/98/4309856.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_4309856
loop_
_publ_author_name
'Holger Fleischer'
'Yvonne Dienes'
'Bernd Mathiasch'
'Volker Schmitt'
'Dieter Schollmeyer'
_publ_section_title
;
Cysteamine and Its Homoleptic Complexes with Group 12 Metal Ions.
Differences in the Coordination Chemistry of ZnII, CdII, and HgII with a
Small N,S-Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8087
_journal_page_last               8096
_journal_paper_doi               10.1021/ic050814m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C4 H12 N2 S2 Zn'
_chemical_formula_weight         217.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.647(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2166(15)
_cell_length_b                   4.9242(3)
_cell_length_c                   10.0513(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      73
_cell_measurement_theta_min      65
_cell_volume                     868.21(11)
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_collection       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dräger, 1971)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       θ/2ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            910
_diffrn_reflns_theta_full        73.85
_diffrn_reflns_theta_max         73.85
_diffrn_reflns_theta_min         5.04
_diffrn_source                   'rotating anode'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.806
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_process_details   'Tompa (Spek, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0328
_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)+(0.0544P)²+0.9846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0949
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                854
_reflns_number_total             882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050814msi20050520_041633.cif
_cod_data_source_block           hfr526
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4309856
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.71766(10) 0.2500 0.0429(3) Uani 1 2 d S . .
S2 S 0.41010(4) 0.92493(15) 0.33607(8) 0.0548(3) Uani 1 1 d . . .
C3 C 0.3333(2) 0.7072(10) 0.2384(5) 0.0775(11) Uani 1 1 d . . .
H3A H 0.2844 0.8049 0.2235 0.135(16) Uiso 1 1 d R . .
H3B H 0.3300 0.5047 0.3025 0.135(16) Uiso 1 1 d R . .
C4 C 0.34393(17) 0.5991(9) 0.1068(4) 0.0657(9) Uani 1 1 d . . .
H4A H 0.3045 0.4664 0.0691 0.119(14) Uiso 1 1 calc R . .
H4B H 0.3385 0.7463 0.0407 0.119(14) Uiso 1 1 calc R . .
N5 N 0.41876(14) 0.4720(6) 0.1257(3) 0.0588(7) Uani 1 1 d . . .
H5A H 0.4232 0.4247 0.0452 0.121(14) Uiso 1 1 d R . .
H5B H 0.4118 0.2943 0.1856 0.121(14) Uiso 1 1 d 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
Zn1 0.0382(3) 0.0391(4) 0.0528(4) 0.000 0.0145(2) 0.000
S2 0.0612(5) 0.0455(4) 0.0650(5) 0.0008(3) 0.0297(4) 0.0096(3)
C3 0.0408(16) 0.108(3) 0.086(3) -0.003(2) 0.0210(16) 0.0061(17)
C4 0.0434(15) 0.082(2) 0.0644(18) -0.0007(17) 0.0023(13) -0.0018(16)
N5 0.0500(13) 0.0655(16) 0.0610(15) -0.0149(12) 0.0153(11) -0.0087(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
N5 Zn1 N5 107.81(18) 2_655 . ?
N5 Zn1 S2 120.30(8) 2_655 . ?
N5 Zn1 S2 91.20(8) . . ?
N5 Zn1 S2 91.20(8) 2_655 2_655 ?
N5 Zn1 S2 120.30(8) . 2_655 ?
S2 Zn1 S2 127.02(5) . 2_655 ?
C3 S2 Zn1 93.32(13) . . ?
C4 C3 S2 115.1(3) . . ?
C4 C3 H3A 111.6 . . ?
S2 C3 H3A 109.0 . . ?
C4 C3 H3B 102.6 . . ?
S2 C3 H3B 110.0 . . ?
H3A C3 H3B 108.3 . . ?
N5 C4 C3 112.2(3) . . ?
N5 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N5 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 N5 Zn1 108.6(2) . . ?
C4 N5 H5A 108.2 . . ?
Zn1 N5 H5A 119.5 . . ?
C4 N5 H5B 99.9 . . ?
Zn1 N5 H5B 108.0 . . ?
H5A N5 H5B 110.8 . . ?
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
Zn1 N5 2.054(3) 2_655 ?
Zn1 N5 2.054(3) . ?
Zn1 S2 2.2883(7) . ?
Zn1 S2 2.2884(7) 2_655 ?
S2 C3 1.825(4) . ?
C3 C4 1.486(6) . ?
C3 H3A 0.9873 . ?
C3 H3B 1.1974 . ?
C4 N5 1.465(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N5 H5A 0.8667 . ?
N5 H5B 1.0885 . ?
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
N5 H5A S2 0.87 2.68 3.474(3) 153.5 6_565
N5 H5B S2 1.09 2.37 3.454(3) 173.1 1_545
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
N5 Zn1 S2 C3 -108.6(2) 2_655 . . . ?
N5 Zn1 S2 C3 2.95(16) . . . . ?
S2 Zn1 S2 C3 133.34(16) 2_655 . . . ?
Zn1 S2 C3 C4 -27.9(3) . . . . ?
S2 C3 C4 N5 50.8(5) . . . . ?
C3 C4 N5 Zn1 -44.3(4) . . . . ?
N5 Zn1 N5 C4 143.5(2) 2_655 . . . ?
S2 Zn1 N5 C4 21.1(2) . . . . ?
S2 Zn1 N5 C4 -114.1(2) 2_655 . . . ?
