#------------------------------------------------------------------------------
#$Date: 2019-12-27 22:21:20 +0200 (Fri, 27 Dec 2019) $
#$Revision: 246248 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/20/2312019.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312019
loop_
_publ_author_name
'Arman, Hadi D.'
'Poplaukhin, Pavel'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Crystal structures of
 {μ₂-N,N'-bis-[(pyridin-3-yl)meth-yl]ethanedi-amide}tetra-kis-(di-methyl-carbamodi-thio-ato)dizinc(II)
 di-methyl-formamide disolvate and
 {μ₂-N,N'-bis-[(pyridin-3-yl)meth-yl]ethanedi-amide}tetra-kis-(di-n-propyl-carbamodi-thio-ato)dizinc(II).
;
_journal_coeditor_code           HB7704
_journal_issue                   'Pt 10'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1501
_journal_page_last               1507
_journal_paper_doi               10.1107/S2056989017012956
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Zn2 (C7 H14 N S2)4 (C14 H14 N4 O2)]'
_chemical_formula_moiety         'C42 H70 N8 O2 S8 Zn2'
_chemical_formula_sum            'C42 H70 N8 O2 S8 Zn2'
_chemical_formula_weight         1106.28
_chemical_name_systematic
{μ₂-N,N'-Bis[(pyridin-3-yl)methyl]ethanediamide}tetrakis(di-n-propylcarbamodithioato)dizinc(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.361(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.048(4)
_cell_length_b                   16.923(2)
_cell_length_c                   10.3453(14)
_cell_measurement_reflns_used    12374
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.7969
_cell_measurement_theta_min      2.3278
_cell_volume                     5347.0(12)
_computing_cell_refinement
;
CrystalClear (Molecular Structure Corporation & Rigaku, 2005)
;
_computing_data_collection
;
CrystalClear (Molecular Structure Corporation & Rigaku, 2005)
;
_computing_data_reduction
;
CrystalClear (Molecular Structure Corporation & Rigaku, 2005)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and  DIAMOND (Brandenburg,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC12K/SATURN724'
_diffrn_measurement_method       ω
_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  0.0312
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17361
_diffrn_reflns_theta_full        27.499
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.328
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0308P)²+4.5145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                5700
_reflns_number_total             6129
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7704sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        5347.1(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2312019
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.669
_shelx_estimated_absorpt_t_max   0.797
loop_
_space_group_symop_operation_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_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_occupancy
Zn Zn 0.13541(2) 0.24490(2) 0.60218(2) 0.01873(7) Uani d 1
S S1 0.08181(2) 0.25161(3) 0.73301(4) 0.01949(10) Uani d 1
S S2 0.17501(2) 0.28982(3) 0.83257(4) 0.01932(10) Uani d 1
S S3 0.17753(2) 0.13268(2) 0.57617(4) 0.01802(10) Uani d 1
S S4 0.09814(2) 0.17783(3) 0.38786(4) 0.01878(10) Uani d 1
O O1 0.03808(5) 0.50349(8) 0.14247(13) 0.0254(3) Uani d 1
N N1 0.11727(5) 0.25613(8) 0.98790(15) 0.0180(3) Uani d 1
N N2 0.14225(5) 0.04388(9) 0.36979(14) 0.0178(3) Uani d 1
N N3 0.14982(5) 0.34572(9) 0.50690(14) 0.0181(3) Uani d 1
N N4 0.04959(5) 0.51477(9) 0.36629(15) 0.0196(3) Uani d 1
H H4N 0.0375(7) 0.5160(12) 0.4359(15) 0.024 Uiso d 1
C C1 0.12447(6) 0.26513(10) 0.86517(17) 0.0178(3) Uani d 1
C C2 0.15269(6) 0.26758(11) 1.10193(17) 0.0199(4) Uani d 1
H H2A 0.1397 0.2798 1.1804 0.024 Uiso calc 1
H H2B 0.1708 0.3133 1.0852 0.024 Uiso calc 1
C C3 0.18182(7) 0.19481(11) 1.12973(17) 0.0215(4) Uani d 1
H H3A 0.1636 0.1490 1.1458 0.026 Uiso calc 1
H H3B 0.1949 0.1828 1.0514 0.026 Uiso calc 1
C C4 0.21819(7) 0.20604(12) 1.24757(18) 0.0243(4) Uani d 1
H H4A 0.2338 0.2554 1.2378 0.036 Uiso calc 1
H H4B 0.2387 0.1616 1.2532 0.036 Uiso calc 1
H H4C 0.2056 0.2083 1.3278 0.036 Uiso calc 1
C C5 0.07487(6) 0.22987(11) 1.01677(18) 0.0211(4) Uani d 1
H H5A 0.0800 0.1975 1.0978 0.025 Uiso calc 1
H H5B 0.0603 0.1959 0.9440 0.025 Uiso calc 1
C C6 0.04457(7) 0.29765(13) 1.0347(2) 0.0285(4) Uani d 1
H H6A 0.0384 0.3295 0.9532 0.034 Uiso calc 1
H H6B 0.0589 0.3323 1.1068 0.034 Uiso calc 1
C C7 0.00182(8) 0.26606(17) 1.0668(2) 0.0407(6) Uani d 1
H H7A -0.0130 0.2338 0.9935 0.061 Uiso calc 1
H H7B -0.0171 0.3104 1.0813 0.061 Uiso calc 1
H H7C 0.0080 0.2336 1.1465 0.061 Uiso calc 1
C C8 0.13929(6) 0.11097(10) 0.43552(16) 0.0169(3) Uani d 1
C C9 0.17538(6) -0.01696(10) 0.41526(17) 0.0192(4) Uani d 1
H H9A 0.1633 -0.0694 0.3855 0.023 Uiso calc 1
H H9B 0.1816 -0.0172 0.5125 0.023 Uiso calc 1
C C10 0.21794(6) -0.00422(11) 0.36546(17) 0.0205(4) Uani d 1
H H10A 0.2313 0.0464 0.4000 0.025 Uiso calc 1
H H10B 0.2119 -0.0011 0.2683 0.025 Uiso calc 1
C C11 0.24983(7) -0.07212(12) 0.4094(2) 0.0274(4) Uani d 1
H H11A 0.2547 -0.0766 0.5053 0.041 Uiso calc 1
H H11B 0.2777 -0.0616 0.3809 0.041 Uiso calc 1
H H11C 0.2374 -0.1216 0.3699 0.041 Uiso calc 1
C C12 0.11177(6) 0.02471(10) 0.24797(17) 0.0193(4) Uani d 1
H H12A 0.1276 -0.0055 0.1893 0.023 Uiso calc 1
H H12B 0.1013 0.0745 0.2026 0.023 Uiso calc 1
C C13 0.07247(7) -0.02322(12) 0.27126(18) 0.0242(4) Uani d 1
H H13A 0.0561 0.0068 0.3289 0.029 Uiso calc 1
H H13B 0.0826 -0.0733 0.3160 0.029 Uiso calc 1
C C14 0.04240(7) -0.04110(13) 0.1408(2) 0.0309(5) Uani d 1
H H14A 0.0313 0.0085 0.0987 0.046 Uiso calc 1
H H14B 0.0178 -0.0736 0.1568 0.046 Uiso calc 1
H H14C 0.0588 -0.0697 0.0831 0.046 Uiso calc 1
C C15 0.12006(6) 0.40358(10) 0.47673(17) 0.0192(4) Uani d 1
H H15 0.0928 0.3991 0.5059 0.023 Uiso calc 1
C C16 0.12765(6) 0.46989(10) 0.40430(17) 0.0180(3) Uani d 1
C C17 0.16739(7) 0.47512(11) 0.36094(18) 0.0220(4) Uani d 1
H H17 0.1734 0.5191 0.3099 0.026 Uiso calc 1
C C18 0.19815(7) 0.41597(11) 0.39255(18) 0.0232(4) Uani d 1
H H18 0.2255 0.4188 0.3640 0.028 Uiso calc 1
C C19 0.18838(6) 0.35269(11) 0.46629(18) 0.0211(4) Uani d 1
H H19 0.2097 0.3125 0.4892 0.025 Uiso calc 1
C C20 0.09527(6) 0.53720(11) 0.38052(19) 0.0218(4) Uani d 1
H H20A 0.1021 0.5748 0.4546 0.026 Uiso calc 1
H H20B 0.0995 0.5654 0.2999 0.026 Uiso calc 1
C C21 0.02463(6) 0.50634(10) 0.24787(18) 0.0195(4) 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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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_3
_geom_angle
N3 Zn S1 . 118.51(4)
N3 Zn S3 . 116.21(5)
S1 Zn S3 . 125.225(18)
N3 Zn S4 . 93.20(4)
S1 Zn S4 . 105.351(19)
S3 Zn S4 . 73.615(17)
N3 Zn S2 . 95.11(4)
S1 Zn S2 . 73.841(18)
S3 Zn S2 . 99.247(17)
S4 Zn S2 . 170.877(16)
C1 S1 Zn . 86.60(6)
C1 S2 Zn . 79.03(6)
C8 S3 Zn . 87.51(6)
C8 S4 Zn . 81.18(6)
C1 N1 C5 . 122.43(16)
C1 N1 C2 . 121.12(16)
C5 N1 C2 . 116.34(14)
C8 N2 C12 . 122.13(15)
C8 N2 C9 . 122.71(15)
C12 N2 C9 . 115.15(14)
C19 N3 C15 . 118.52(16)
C19 N3 Zn . 120.34(12)
C15 N3 Zn . 121.01(12)
C21 N4 C20 . 121.14(16)
C21 N4 H4N . 119.8(16)
C20 N4 H4N . 118.0(15)
N1 C1 S2 . 121.99(15)
N1 C1 S1 . 119.86(15)
S2 C1 S1 . 118.16(10)
N1 C2 C3 . 112.14(14)
N1 C2 H2A . 109.2
C3 C2 H2A . 109.2
N1 C2 H2B . 109.2
C3 C2 H2B . 109.2
H2A C2 H2B . 107.9
C4 C3 C2 . 112.39(15)
C4 C3 H3A . 109.1
C2 C3 H3A . 109.1
C4 C3 H3B . 109.1
C2 C3 H3B . 109.1
H3A C3 H3B . 107.9
C3 C4 H4A . 109.5
C3 C4 H4B . 109.5
H4A C4 H4B . 109.5
C3 C4 H4C . 109.5
H4A C4 H4C . 109.5
H4B C4 H4C . 109.5
N1 C5 C6 . 113.23(16)
N1 C5 H5A . 108.9
C6 C5 H5A . 108.9
N1 C5 H5B . 108.9
C6 C5 H5B . 108.9
H5A C5 H5B . 107.7
C5 C6 C7 . 110.23(18)
C5 C6 H6A . 109.6
C7 C6 H6A . 109.6
C5 C6 H6B . 109.6
C7 C6 H6B . 109.6
H6A C6 H6B . 108.1
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
N2 C8 S4 . 122.11(14)
N2 C8 S3 . 120.36(14)
S4 C8 S3 . 117.52(10)
N2 C9 C10 . 113.16(14)
N2 C9 H9A . 108.9
C10 C9 H9A . 108.9
N2 C9 H9B . 108.9
C10 C9 H9B . 108.9
H9A C9 H9B . 107.8
C9 C10 C11 . 110.41(15)
C9 C10 H10A . 109.6
C11 C10 H10A . 109.6
C9 C10 H10B . 109.6
C11 C10 H10B . 109.6
H10A C10 H10B . 108.1
C10 C11 H11A . 109.5
C10 C11 H11B . 109.5
H11A C11 H11B . 109.5
C10 C11 H11C . 109.5
H11A C11 H11C . 109.5
H11B C11 H11C . 109.5
N2 C12 C13 . 113.16(14)
N2 C12 H12A . 108.9
C13 C12 H12A . 108.9
N2 C12 H12B . 108.9
C13 C12 H12B . 108.9
H12A C12 H12B . 107.8
C12 C13 C14 . 110.26(16)
C12 C13 H13A . 109.6
C14 C13 H13A . 109.6
C12 C13 H13B . 109.6
C14 C13 H13B . 109.6
H13A C13 H13B . 108.1
C13 C14 H14A . 109.5
C13 C14 H14B . 109.5
H14A C14 H14B . 109.5
C13 C14 H14C . 109.5
H14A C14 H14C . 109.5
H14B C14 H14C . 109.5
N3 C15 C16 . 122.43(17)
N3 C15 H15 . 118.8
C16 C15 H15 . 118.8
C17 C16 C15 . 118.11(17)
C17 C16 C20 . 120.22(16)
C15 C16 C20 . 121.55(17)
C18 C17 C16 . 119.57(17)
C18 C17 H17 . 120.2
C16 C17 H17 . 120.2
C19 C18 C17 . 118.81(18)
C19 C18 H18 . 120.6
C17 C18 H18 . 120.6
N3 C19 C18 . 122.55(17)
N3 C19 H19 . 118.7
C18 C19 H19 . 118.7
N4 C20 C16 . 115.44(15)
N4 C20 H20A . 108.4
C16 C20 H20A . 108.4
N4 C20 H20B . 108.4
C16 C20 H20B . 108.4
H20A C20 H20B . 107.5
O1 C21 N4 . 125.54(18)
O1 C21 C21 2 121.4(2)
N4 C21 C21 2 112.96(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn N3 . 2.0595(15)
Zn S1 . 2.3289(5)
Zn S3 . 2.3484(5)
Zn S4 . 2.5731(5)
Zn S2 . 2.5917(6)
S1 C1 . 1.7391(19)
S2 C1 . 1.715(2)
S3 C8 . 1.7435(19)
S4 C8 . 1.7114(19)
O1 C21 . 1.237(2)
N1 C1 . 1.337(2)
N1 C5 . 1.470(2)
N1 C2 . 1.474(2)
N2 C8 . 1.335(2)
N2 C12 . 1.470(2)
N2 C9 . 1.472(2)
N3 C19 . 1.343(2)
N3 C15 . 1.344(2)
N4 C21 . 1.334(2)
N4 C20 . 1.450(2)
N4 H4N . 0.870(9)
C2 C3 . 1.524(3)
C2 H2A . 0.9900
C2 H2B . 0.9900
C3 C4 . 1.517(3)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C5 C6 . 1.516(3)
C5 H5A . 0.9900
C5 H5B . 0.9900
C6 C7 . 1.522(3)
C6 H6A . 0.9900
C6 H6B . 0.9900
C7 H7A . 0.9800
C7 H7B . 0.9800
C7 H7C . 0.9800
C9 C10 . 1.518(3)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 C11 . 1.531(3)
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 H11A . 0.9800
C11 H11B . 0.9800
C11 H11C . 0.9800
C12 C13 . 1.520(3)
C12 H12A . 0.9900
C12 H12B . 0.9900
C13 C14 . 1.527(3)
C13 H13A . 0.9900
C13 H13B . 0.9900
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
C15 C16 . 1.393(2)
C15 H15 . 0.9500
C16 C17 . 1.389(3)
C16 C20 . 1.510(3)
C17 C18 . 1.382(3)
C17 H17 . 0.9500
C18 C19 . 1.380(3)
C18 H18 . 0.9500
C19 H19 . 0.9500
C20 H20A . 0.9900
C20 H20B . 0.9900
C21 C21 2 1.538(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
N4 H4N O1 4_565 0.870(18) 2.159(16) 2.959(2) 152.6(19)

_cod_database_fobs_code 2312019
