#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/81/2228129.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_2228129
loop_
_publ_author_name
'Zha, Mei-Qin'
'Li, Xing'
'Bing, Yue'
'Lu, Yue'
_publ_section_title
;
 (μ-4,4'-Bipyridine-κ²N:N')bis[bis(N,N-dimethyldithiocarbamato-κ²S,S')zinc(II)]
;
_journal_coeditor_code           XU5042
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1465
_journal_paper_doi               10.1107/S1600536810042650
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Zn2 (C3 H6 N S2)4 (C10 H8 N2)]'
_chemical_formula_moiety         'C22 H32 N6 S8 Zn2'
_chemical_formula_sum            'C22 H32 N6 S8 Zn2'
_chemical_formula_weight         767.76
_chemical_name_systematic
;
(μ-4,4'-Bipyridine-κ²N:N')bis[bis(N,N-
dimethyldithiocarbamato-κ²S,S')zinc(II)]
;
_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                 100.0700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0490(8)
_cell_length_b                   13.8770(14)
_cell_length_c                   14.8134(14)
_cell_measurement_reflns_used    14059
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.03
_cell_volume                     1629.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14059
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.947
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0401
_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)+(0.0365P)²+3.8184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                3205
_reflns_number_total             3754
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5042.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228129
_cod_database_fobs_code          2228129
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.13314(4) 0.27435(3) 0.24330(2) 0.02256(11) Uani d . 1 . .
S S1 0.08181(9) 0.16003(5) 0.10290(5) 0.02256(11) Uani d . 1 . .
S S2 -0.12799(10) 0.31820(6) 0.15575(6) 0.02636(18) Uani d . 1 . .
S S3 0.39861(9) 0.33093(6) 0.22187(5) 0.02260(17) Uani d . 1 . .
S S4 0.21808(10) 0.41611(6) 0.35942(6) 0.02694(18) Uani d . 1 . .
C C1 -0.0291(4) 0.1060(2) 0.3154(2) 0.0286(7) Uani d . 1 . .
H H1A -0.0887 0.1049 0.2541 0.034 Uiso calc R 1 . .
C C2 -0.0689(4) 0.0385(2) 0.3764(2) 0.0292(7) Uani d . 1 . .
H H2A -0.1562 -0.0069 0.3570 0.035 Uiso calc R 1 . .
C C3 0.0183(4) 0.0363(2) 0.46632(19) 0.0183(6) Uani d . 1 . .
C C4 0.1429(4) 0.1065(2) 0.4901(2) 0.0236(6) Uani d . 1 . .
H H4A 0.2065 0.1084 0.5504 0.028 Uiso calc R 1 . .
C C5 0.1731(4) 0.1731(2) 0.4255(2) 0.0235(6) Uani d . 1 . .
H H5A 0.2568 0.2209 0.4434 0.028 Uiso calc R 1 . .
C C6 -0.1905(5) 0.1389(3) -0.0636(3) 0.0444(10) Uani d . 1 . .
H H6A -0.0751 0.1136 -0.0503 0.067 Uiso calc R 1 . .
H H6B -0.2123 0.1658 -0.1257 0.067 Uiso calc R 1 . .
H H6C -0.2706 0.0867 -0.0591 0.067 Uiso calc R 1 . .
C C7 -0.3640(5) 0.2736(4) -0.0185(3) 0.0495(11) Uani d . 1 . .
H H7A -0.4042 0.2895 0.0385 0.074 Uiso calc R 1 . .
H H7B -0.4514 0.2375 -0.0591 0.074 Uiso calc R 1 . .
H H7C -0.3387 0.3332 -0.0489 0.074 Uiso calc R 1 . .
C C8 -0.0971(4) 0.2285(2) 0.0785(2) 0.0230(6) Uani d . 1 . .
C C9 0.6095(5) 0.5119(3) 0.2449(3) 0.0372(8) Uani d . 1 . .
H H9A 0.5971 0.4609 0.1985 0.056 Uiso calc R 1 . .
H H9B 0.7211 0.5072 0.2836 0.056 Uiso calc R 1 . .
H H9C 0.5976 0.5750 0.2147 0.056 Uiso calc R 1 . .
C C10 0.4667(5) 0.5812(3) 0.3652(3) 0.0362(8) Uani d . 1 . .
H H10A 0.3668 0.5723 0.3939 0.054 Uiso calc R 1 . .
H H10B 0.4570 0.6421 0.3312 0.054 Uiso calc R 1 . .
H H10C 0.5680 0.5825 0.4127 0.054 Uiso calc R 1 . .
C C11 0.3763(4) 0.4248(2) 0.2965(2) 0.0206(6) Uani d . 1 . .
N N1 0.0906(3) 0.17348(17) 0.33906(17) 0.0203(5) Uani d . 1 . .
N N2 -0.2105(3) 0.2147(2) 0.0027(2) 0.0331(7) Uani d . 1 . .
N N3 0.4789(3) 0.50091(19) 0.30182(18) 0.0255(6) Uani d . 1 . .
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'
Zn Zn 0.2839 1.4301 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Zn1 S2 . . 108.37(7) ?
N1 Zn1 S3 . . 125.72(7) ?
S2 Zn1 S3 . . 125.87(3) ?
N1 Zn1 S1 . . 96.55(7) ?
S2 Zn1 S1 . . 73.36(3) ?
S3 Zn1 S1 . . 96.74(3) ?
N1 Zn1 S4 . . 96.52(7) ?
S2 Zn1 S4 . . 105.85(3) ?
S3 Zn1 S4 . . 72.49(3) ?
S1 Zn1 S4 . . 166.41(3) ?
C8 S1 Zn1 . . 80.77(11) ?
C8 S2 Zn1 . . 87.75(11) ?
C11 S3 Zn1 . . 88.10(10) ?
C11 S4 Zn1 . . 80.15(10) ?
N1 C1 C2 . . 122.7(3) ?
N1 C1 H1A . . 118.6 ?
C2 C1 H1A . . 118.6 ?
C1 C2 C3 . . 120.4(3) ?
C1 C2 H2A . . 119.8 ?
C3 C2 H2A . . 119.8 ?
C2 C3 C4 . . 116.4(3) ?
C2 C3 C3 . 3_556 122.1(3) ?
C4 C3 C3 . 3_556 121.5(3) ?
C5 C4 C3 . . 119.8(3) ?
C5 C4 H4A . . 120.1 ?
C3 C4 H4A . . 120.1 ?
N1 C5 C4 . . 123.2(3) ?
N1 C5 H5A . . 118.4 ?
C4 C5 H5A . . 118.4 ?
N2 C6 H6A . . 109.5 ?
N2 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
N2 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N2 C7 H7A . . 109.5 ?
N2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
N2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
N2 C8 S1 . . 121.7(3) ?
N2 C8 S2 . . 120.2(3) ?
S1 C8 S2 . . 118.10(18) ?
N3 C9 H9A . . 109.5 ?
N3 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
N3 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
N3 C10 H10A . . 109.5 ?
N3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
N3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N3 C11 S4 . . 122.4(2) ?
N3 C11 S3 . . 119.9(2) ?
S4 C11 S3 . . 117.64(17) ?
C5 N1 C1 . . 117.4(3) ?
C5 N1 Zn1 . . 123.2(2) ?
C1 N1 Zn1 . . 119.4(2) ?
C8 N2 C6 . . 121.9(3) ?
C8 N2 C7 . . 121.8(3) ?
C6 N2 C7 . . 116.3(3) ?
C11 N3 C9 . . 123.2(3) ?
C11 N3 C10 . . 121.8(3) ?
C9 N3 C10 . . 115.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N1 . 2.064(2) y
Zn1 S1 . 2.5909(9) y
Zn1 S2 . 2.3488(9) y
Zn1 S3 . 2.3495(8) y
Zn1 S4 . 2.6239(9) y
S1 C8 . 1.710(3) ?
S2 C8 . 1.738(3) ?
S3 C11 . 1.738(3) ?
S4 C11 . 1.708(3) ?
C1 N1 . 1.345(4) ?
C1 C2 . 1.378(4) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.393(4) ?
C2 H2A . 0.9500 ?
C3 C4 . 1.398(4) ?
C3 C3 3_556 1.483(6) ?
C4 C5 . 1.383(4) ?
C4 H4A . 0.9500 ?
C5 N1 . 1.335(4) ?
C5 H5A . 0.9500 ?
C6 N2 . 1.467(5) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 N2 . 1.468(5) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 N2 . 1.331(4) ?
C9 N3 . 1.466(4) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 N3 . 1.471(4) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 N3 . 1.334(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C4 H4A S3 4_566 0.95 2.86 3.782(3) 164
