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#$Date: 2016-03-23 00:56:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179136 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/98/4309857.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_4309857
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 Cd N2 S2'
_chemical_formula_weight         264.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.141(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0834(12)
_cell_length_b                   11.9530(16)
_cell_length_c                   8.2840(11)
_cell_measurement_reflns_used    5380
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.4
_cell_volume                     827.06(19)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       'CCD Scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9455
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'sealed Tube'
_exptl_absorpt_coefficient_mu    3.065
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0386P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0676
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                1721
_reflns_number_total             2017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050814msi20050520_041655.cif
_cod_data_source_block           hfr700
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4309857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cd1 Cd 0.70116(2) 0.298787(17) 0.46450(3) 0.02020(9) Uani 1 1 d . . .
S1 S 0.42430(8) 0.37088(6) 0.27591(10) 0.02372(17) Uani 1 1 d . . .
C2 C 0.3165(4) 0.2413(3) 0.2653(5) 0.0299(7) Uani 1 1 d . . .
H2A H 0.2828 0.2395 0.3654 0.036 Uiso 1 1 calc R . .
H2B H 0.2182 0.2416 0.1562 0.036 Uiso 1 1 calc R . .
C3 C 0.4094(3) 0.1355(3) 0.2691(4) 0.0257(6) Uani 1 1 d . . .
H3A H 0.3414 0.0696 0.2629 0.031 Uiso 1 1 calc R . .
H3B H 0.4377 0.1338 0.1652 0.031 Uiso 1 1 calc R . .
N4 N 0.5561(3) 0.1292(2) 0.4294(3) 0.0235(5) Uani 1 1 d . . .
H4A H 0.5264(8) 0.1170(4) 0.520(3) 0.028 Uiso 1 1 d R . .
H4B H 0.6025(13) 0.0695(17) 0.4136(5) 0.028 Uiso 1 1 d R . .
S2 S 0.87469(8) 0.24177(6) 0.78958(9) 0.02071(16) Uani 1 1 d . . .
C5 C 0.9518(4) 0.3806(2) 0.8695(4) 0.0241(6) Uani 1 1 d . . .
H5A H 0.8757 0.4192 0.9095 0.029 Uiso 1 1 calc R . .
H5B H 1.0549 0.3730 0.9718 0.029 Uiso 1 1 calc R . .
C6 C 0.9767(3) 0.4512(2) 0.7303(4) 0.0244(6) Uani 1 1 d . . .
H6A H 1.0271 0.5232 0.7822 0.029 Uiso 1 1 calc R . .
H6B H 1.0497 0.4118 0.6866 0.029 Uiso 1 1 calc R . .
N7 N 0.8240(3) 0.4725(2) 0.5842(3) 0.0224(5) Uani 1 1 d . . .
H7A H 0.8442(7) 0.5130(13) 0.507(2) 0.027 Uiso 1 1 d R . .
H7B H 0.7666(17) 0.5142(13) 0.6145(9) 0.027 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
Cd1 0.01971(13) 0.01933(13) 0.01985(13) -0.00206(7) 0.00593(9) -0.00094(7)
S1 0.0217(3) 0.0199(4) 0.0290(4) 0.0019(3) 0.0094(3) 0.0022(3)
C2 0.0209(14) 0.0264(17) 0.0377(18) 0.0025(14) 0.0065(13) -0.0026(13)
C3 0.0256(14) 0.0232(15) 0.0229(14) -0.0030(12) 0.0038(12) -0.0049(12)
N4 0.0221(11) 0.0193(12) 0.0261(13) -0.0007(10) 0.0062(10) -0.0019(10)
S2 0.0248(3) 0.0174(3) 0.0200(3) 0.0006(3) 0.0088(3) -0.0014(3)
C5 0.0254(14) 0.0197(14) 0.0217(14) -0.0014(11) 0.0032(12) -0.0051(12)
C6 0.0218(14) 0.0197(14) 0.0287(15) 0.0017(12) 0.0067(12) -0.0035(11)
N7 0.0277(12) 0.0155(11) 0.0228(11) 0.0014(10) 0.0086(11) 0.0025(10)
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'
Cd Cd -0.8075 1.2024 '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
_geom_angle_publ_flag
N4 Cd1 N7 160.54(9) . . ?
N4 Cd1 S1 81.15(6) . . ?
N7 Cd1 S1 98.59(6) . . ?
N4 Cd1 S2 101.75(7) . 4_565 ?
N7 Cd1 S2 96.22(7) . 4_565 ?
S1 Cd1 S2 113.35(3) . 4_565 ?
N4 Cd1 S2 89.12(6) . . ?
N7 Cd1 S2 78.73(6) . . ?
S1 Cd1 S2 140.59(3) . . ?
S2 Cd1 S2 106.00(3) 4_565 . ?
C2 S1 Cd1 97.22(10) . . ?
C3 C2 S1 115.2(2) . . ?
N4 C3 C2 111.2(2) . . ?
C3 N4 Cd1 109.27(18) . . ?
C5 S2 Cd1 101.53(11) . 4_566 ?
C5 S2 Cd1 97.29(9) . . ?
Cd1 S2 Cd1 111.95(3) 4_566 . ?
C6 C5 S2 112.4(2) . . ?
N7 C6 C5 110.5(2) . . ?
C6 N7 Cd1 109.25(17) . . ?
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
Cd1 N4 2.373(2) . ?
Cd1 N7 2.382(2) . ?
Cd1 S1 2.5337(8) . ?
Cd1 S2 2.5719(8) 4_565 ?
Cd1 S2 2.6200(8) . ?
S1 C2 1.816(3) . ?
C2 C3 1.514(4) . ?
C3 N4 1.468(4) . ?
S2 C5 1.821(3) . ?
S2 Cd1 2.5719(8) 4_566 ?
C5 C6 1.517(4) . ?
C6 N7 1.461(4) . ?
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
N4 H4A S1 0.91 2.63 3.518(3) 167.2 4_566
N4 H4B S1 0.86 2.80 3.563(3) 147.5 2_645
N7 H7B S1 0.83 2.64 3.462(3) 174.3 3_666
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
N4 Cd1 S1 C2 3.68(14) . . . . ?
N7 Cd1 S1 C2 -156.64(14) . . . . ?
S2 Cd1 S1 C2 102.72(13) 4_565 . . . ?
S2 Cd1 S1 C2 -73.96(13) . . . . ?
Cd1 S1 C2 C3 -32.1(2) . . . . ?
S1 C2 C3 N4 59.0(3) . . . . ?
C2 C3 N4 Cd1 -51.1(3) . . . . ?
N7 Cd1 N4 C3 114.6(3) . . . . ?
S1 Cd1 N4 C3 23.89(19) . . . . ?
S2 Cd1 N4 C3 -88.28(19) 4_565 . . . ?
S2 Cd1 N4 C3 165.56(19) . . . . ?
N4 Cd1 S2 C5 -161.49(12) . . . . ?
N7 Cd1 S2 C5 3.23(12) . . . . ?
S1 Cd1 S2 C5 -86.62(11) . . . . ?
S2 Cd1 S2 C5 96.54(11) 4_565 . . . ?
N4 Cd1 S2 Cd1 -55.90(7) . . . 4_566 ?
N7 Cd1 S2 Cd1 108.82(7) . . . 4_566 ?
S1 Cd1 S2 Cd1 18.97(5) . . . 4_566 ?
S2 Cd1 S2 Cd1 -157.87(4) 4_565 . . 4_566 ?
Cd1 S2 C5 C6 -147.65(19) 4_566 . . . ?
Cd1 S2 C5 C6 -33.4(2) . . . . ?
S2 C5 C6 N7 64.0(3) . . . . ?
C5 C6 N7 Cd1 -57.9(3) . . . . ?
N4 Cd1 N7 C6 79.4(3) . . . . ?
S1 Cd1 N7 C6 167.17(17) . . . . ?
S2 Cd1 N7 C6 -78.02(18) 4_565 . . . ?
S2 Cd1 N7 C6 27.11(17) . . . . ?
