#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:17:17 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180006 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/00/7030088.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_7030088
loop_
_publ_author_name
'Onwudiwe, Damian C.'
'Strydom, Christien A.'
'Oluwafemi, Oluwatobi S.'
'Hosten, Eric'
'Jordaan, Anine'
_publ_section_title
;
 Synthesis, spectral and thermal studies of pyridyl adducts of Zn(ii) and
 Cd(ii) dithiocarbamates, and their use as single source precursors for
 ZnS and CdS nanoparticles.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8703
_journal_page_last               8712
_journal_paper_doi               10.1039/c4dt00610k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C23 H25 N3 S4 Zn'
_chemical_formula_sum            'C23 H25 N3 S4 Zn'
_chemical_formula_weight         537.07
_chemical_melting_point          463
_chemical_name_common            'Damian (5) Znmepyd (2nd try)'
_chemical_name_systematic
'bis(N-ethyl-N-phenyldithiocarbamato-k²S,S')(pyridine)zinc (II)'
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.608(5)
_cell_length_b                   8.608(5)
_cell_length_c                   29.162(5)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.4919
_cell_measurement_theta_min      3.4500
_cell_volume                     1871.3(16)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11163
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.095
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.016(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0230
_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)+(0.0271P)²+0.0624P]
where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                2910
_reflns_number_total             3082
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt00610k1.cif
_cod_data_source_block           ca160
_cod_depositor_comments          'Adding full bibliography for 7030088.cif.'
_cod_original_cell_volume        1871(2)
_cod_database_code               7030088
#BEGIN Tags that were not found in dictionaries:
_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   0.653
_shelx_estimated_absorpt_t_max   0.854
_shelxl_version_number           2012-9
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.68355(3) 0.68355(3) 0.0000 0.03427(10) Uani 1 2 d S T P . .
S1 S 0.59064(7) 0.60694(8) 0.07679(2) 0.03919(14) Uani 1 1 d . . . . .
S2 S 0.43078(8) 0.75966(8) 0.01515(2) 0.04081(14) Uani 1 1 d . . . . .
N1 N 0.3064(3) 0.6319(4) 0.09897(7) 0.0610(7) Uani 1 1 d . . . . .
N2 N 0.9230(3) 0.9230(3) 0.0000 0.0304(5) Uani 1 2 d S T P . .
C1 C 0.4300(3) 0.6647(3) 0.06694(7) 0.0366(5) Uani 1 1 d . . . . .
C11 C 0.3052(4) 0.5464(4) 0.14164(7) 0.0496(7) Uani 1 1 d . . . . .
C12 C 0.3705(4) 0.6498(5) 0.18097(9) 0.0584(7) Uani 1 1 d . . . . .
H12 H 0.4197 0.7762 0.1801 0.070 Uiso 1 1 calc R U . . .
C13 C 0.3613(5) 0.5618(6) 0.22176(9) 0.0746(11) Uani 1 1 d . . . . .
H13 H 0.4039 0.6291 0.2493 0.090 Uiso 1 1 calc R U . . .
C14 C 0.2921(5) 0.3805(6) 0.22288(10) 0.0769(11) Uani 1 1 d . . . . .
H14 H 0.2882 0.3234 0.2511 0.092 Uiso 1 1 calc R U . . .
C15 C 0.2282(5) 0.2800(5) 0.18365(11) 0.0770(10) Uani 1 1 d . . . . .
H15 H 0.1810 0.1539 0.1845 0.092 Uiso 1 1 calc R U . . .
C16 C 0.2332(4) 0.3650(5) 0.14267(10) 0.0642(8) Uani 1 1 d . . . . .
H16 H 0.1864 0.2967 0.1154 0.077 Uiso 1 1 calc R U . . .
C21 C 1.0796(3) 0.9250(3) -0.00060(7) 0.0368(5) Uani 1 1 d . . . . .
H21 H 1.0786 0.8142 -0.0011 0.044 Uiso 1 1 calc R U . . .
C22 C 1.2424(3) 1.0827(3) -0.00053(8) 0.0477(6) Uani 1 1 d . . . . .
H22 H 1.3518 1.0808 -0.0008 0.057 Uiso 1 1 calc R U . . .
C23 C 1.2427(4) 1.2427(4) 0.0000 0.0518(9) Uani 1 2 d S T P . .
H23 H 1.3531 1.3531 0.0000 0.062 Uiso 1 2 calc R U P . .
C2 C 0.1291(8) 0.6327(7) 0.08873(13) 0.0481(12) Uani 0.668(9) 1 d . . P A 1
H2A H 0.1105 0.6322 0.0552 0.058 Uiso 0.668(9) 1 calc R U P A 1
H2B H 0.0255 0.5250 0.1021 0.058 Uiso 0.668(9) 1 calc R U P A 1
C3 C 0.1459(8) 0.7973(8) 0.10947(15) 0.0702(17) Uani 0.668(9) 1 d . . P A 1
H3A H 0.2521 0.9025 0.0970 0.105 Uiso 0.668(9) 1 calc R U P A 1
H3B H 0.1580 0.7933 0.1428 0.105 Uiso 0.668(9) 1 calc R U P A 1
H3C H 0.0387 0.8050 0.1023 0.105 Uiso 0.668(9) 1 calc R U P A 1
C4 C 0.2283(10) 0.7517(10) 0.1013(2) 0.033(2) Uani 0.332(9) 1 d . . P A 2
H4A H 0.2742 0.8424 0.0765 0.040 Uiso 0.332(9) 1 calc R U P A 2
H4B H 0.2502 0.8123 0.1314 0.040 Uiso 0.332(9) 1 calc R U P A 2
C5 C 0.0319(14) 0.6132(13) 0.0945(3) 0.052(3) Uani 0.332(9) 1 d . . P A 2
H5A H 0.0163 0.5534 0.0649 0.078 Uiso 0.332(9) 1 calc R U P A 2
H5B H -0.0399 0.6727 0.0951 0.078 Uiso 0.332(9) 1 calc R U P A 2
H5C H -0.0075 0.5241 0.1192 0.078 Uiso 0.332(9) 1 calc R U P A 2
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Zn1 S1 108.022(19) . 4
N2 Zn1 S1 108.022(19) . .
S1 Zn1 S1 143.96(4) 4 .
N2 Zn1 S2 106.97(8) . 4
S1 Zn1 S2 72.555(17) 4 4
S1 Zn1 S2 96.84(2) . 4
N2 Zn1 S2 106.97(8) . .
S1 Zn1 S2 96.84(2) 4 .
S1 Zn1 S2 72.555(17) . .
S2 Zn1 S2 146.05(3) 4 .
C1 S1 Zn1 88.26(7) . .
C1 S2 Zn1 80.45(8) . .
C1 N1 C11 120.8(2) . .
C1 N1 C4 118.3(3) . .
C11 N1 C4 115.1(3) . .
C1 N1 C2 122.9(2) . .
C11 N1 C2 114.2(2) . .
C21 N2 C21 118.7(3) . 4
C21 N2 Zn1 120.65(13) . .
C21 N2 Zn1 120.65(13) 4 .
N1 C1 S1 119.68(17) . .
N1 C1 S2 121.94(18) . .
S1 C1 S2 118.36(12) . .
C16 C11 C12 121.6(2) . .
C16 C11 N1 119.1(3) . .
C12 C11 N1 119.2(3) . .
C11 C12 C13 117.6(3) . .
C11 C12 H12 121.2 . .
C13 C12 H12 121.2 . .
C14 C13 C12 121.1(3) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
C13 C14 C15 120.6(3) . .
C13 C14 H14 119.7 . .
C15 C14 H14 119.7 . .
C14 C15 C16 119.2(4) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
C11 C16 C15 119.9(3) . .
C11 C16 H16 120.0 . .
C15 C16 H16 120.0 . .
N2 C21 C22 122.2(2) . .
N2 C21 H21 118.9 . .
C22 C21 H21 118.9 . .
C23 C22 C21 118.5(3) . .
C23 C22 H22 120.7 . .
C21 C22 H22 120.7 . .
C22 C23 C22 119.8(3) . 4
C22 C23 H23 120.1 . .
C22 C23 H23 120.1 4 .
C3 C2 N1 107.4(4) . .
C3 C2 H2A 110.2 . .
N1 C2 H2A 110.2 . .
C3 C2 H2B 110.2 . .
N1 C2 H2B 110.2 . .
H2A C2 H2B 108.5 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 C5 99.3(6) . .
N1 C4 H4A 111.9 . .
C5 C4 H4A 111.9 . .
N1 C4 H4B 111.9 . .
C5 C4 H4B 111.9 . .
H4A C4 H4B 109.6 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.061(3) .
Zn1 S1 2.3583(15) 4
Zn1 S1 2.3583(15) .
Zn1 S2 2.6046(16) 4
Zn1 S2 2.6047(16) .
S1 C1 1.711(3) .
S2 C1 1.716(2) .
N1 C1 1.336(3) .
N1 C11 1.443(3) .
N1 C4 1.488(8) .
N1 C2 1.559(6) .
N2 C21 1.340(3) .
N2 C21 1.340(3) 4
C11 C16 1.362(5) .
C11 C12 1.387(4) .
C12 C13 1.391(4) .
C12 H12 0.9500 .
C13 C14 1.364(6) .
C13 H13 0.9500 .
C14 C15 1.373(5) .
C14 H14 0.9500 .
C15 C16 1.391(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.380(3) .
C21 H21 0.9500 .
C22 C23 1.376(3) .
C22 H22 0.9500 .
C23 C22 1.376(3) 4
C23 H23 0.9500 .
C2 C3 1.480(7) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.517(12) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
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
C2 H2A S2 0.99 2.67 3.115(5) 107.4
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_4
C11 N1 C1 S1 -0.7(4) . .
C4 N1 C1 S1 151.1(4) . .
C2 N1 C1 S1 -163.6(3) . .
C11 N1 C1 S2 177.9(2) . .
C4 N1 C1 S2 -30.3(5) . .
C2 N1 C1 S2 15.0(4) . .
Zn1 S1 C1 N1 172.6(2) . .
Zn1 S1 C1 S2 -6.10(13) . .
Zn1 S2 C1 N1 -173.0(2) . .
Zn1 S2 C1 S1 5.60(12) . .
C1 N1 C11 C16 -79.7(4) . .
C4 N1 C11 C16 127.6(4) . .
C2 N1 C11 C16 84.5(3) . .
C1 N1 C11 C12 103.0(3) . .
C4 N1 C11 C12 -49.7(5) . .
C2 N1 C11 C12 -92.8(4) . .
C16 C11 C12 C13 0.5(4) . .
N1 C11 C12 C13 177.8(2) . .
C11 C12 C13 C14 0.6(4) . .
C12 C13 C14 C15 -0.6(4) . .
C13 C14 C15 C16 -0.6(5) . .
C12 C11 C16 C15 -1.7(4) . .
N1 C11 C16 C15 -178.9(3) . .
C14 C15 C16 C11 1.7(4) . .
C21 N2 C21 C22 0.12(16) 4 .
Zn1 N2 C21 C22 -179.88(16) . .
N2 C21 C22 C23 -0.2(3) . .
C21 C22 C23 C22 0.12(15) . 4
C1 N1 C2 C3 -107.1(4) . .
C11 N1 C2 C3 89.1(4) . .
C4 N1 C2 C3 -11.5(4) . .
C1 N1 C4 C5 121.6(5) . .
C11 N1 C4 C5 -85.0(5) . .
C2 N1 C4 C5 13.2(4) . .
