#------------------------------------------------------------------------------
#$Date: 2016-06-11 05:09:59 +0300 (Sat, 11 Jun 2016) $
#$Revision: 183352 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/17/2241715.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_2241715
loop_
_publ_author_name
'Neumann, Tristan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 bis(isonicotinamide-κN¹)bis(thiocyanato-κN)zinc
;
_journal_coeditor_code           WM5297
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              922
_journal_page_last               925
_journal_paper_doi               10.1107/S2056989016008963
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Zn (N C S)2 (C6 H6 N2 O)2]'
_chemical_formula_moiety         'C14 H12 N6 O2 S2 Zn'
_chemical_formula_sum            'C14 H12 N6 O2 S2 Zn'
_chemical_formula_weight         425.79
_chemical_name_systematic
;
Bis(isonicotinamide-κN¹)bis(thiocyanato-κN)zinc
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.1926(9)
_cell_length_b                   36.3044(12)
_cell_length_c                   5.2930(2)
_cell_measurement_reflns_used    15683
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      56.2
_cell_measurement_theta_min      4.2
_cell_volume                     3688.0(3)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            15338
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.077
_diffrn_reflns_theta_min         2.244
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.7416
_exptl_absorpt_correction_T_min  0.5947
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.266
_refine_ls_abs_structure_details
;
Flack x determined using 819 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al., 2013).
;
_refine_ls_abs_structure_Flack   -0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2132
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0282P)²+4.6943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                2012
_reflns_number_total             2132
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5297sup1.cif
_cod_data_source_block           I
_cod_database_code               2241715
_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.
;
_shelxl_version_number           2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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 Zn1 0.5000 0.5000 0.00134(10) 0.04197(15) Uani d 1
N N1 0.41911(18) 0.48143(9) -0.1702(7) 0.0562(8) Uani d 1
C C1 0.3688(2) 0.46990(10) -0.2648(9) 0.0514(9) Uani d 1
S S1 0.29987(6) 0.45456(4) -0.4003(3) 0.0802(4) Uani d 1
N N11 0.46205(13) 0.53943(7) 0.2367(6) 0.0399(6) Uani d 1
C C11 0.39419(17) 0.54254(10) 0.2958(8) 0.0465(9) Uani d 1
H H11 0.3616 0.5266 0.2164 0.056 Uiso calc 1
C C12 0.37026(17) 0.56804(10) 0.4673(8) 0.0466(8) Uani d 1
H H12 0.3219 0.5697 0.5036 0.056 Uiso calc 1
C C13 0.41714(16) 0.59132(9) 0.5870(7) 0.0373(7) Uani d 1
C C14 0.48690(15) 0.58811(9) 0.5240(9) 0.0438(8) Uani d 1
H H14 0.5205 0.6037 0.6011 0.053 Uiso calc 1
C C15 0.50720(17) 0.56217(10) 0.3489(7) 0.0428(8) Uani d 1
H H15 0.5552 0.5604 0.3063 0.051 Uiso calc 1
C C16 0.39066(16) 0.61924(9) 0.7711(8) 0.0429(7) Uani d 1
N N12 0.43541(15) 0.63295(9) 0.9372(6) 0.0486(8) Uani d 1
H H12A 0.4215 0.6495 1.0479 0.058 Uiso calc 1
H H12B 0.4791 0.6255 0.9367 0.058 Uiso calc 1
O O11 0.32905(12) 0.62889(8) 0.7653(7) 0.0590(8) 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_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Zn1 N1 2_665 . 123.6(2)
N1 Zn1 N11 2_665 . 109.39(13)
N1 Zn1 N11 . . 104.32(13)
N1 Zn1 N11 2_665 2_665 104.32(13)
N1 Zn1 N11 . 2_665 109.40(13)
N11 Zn1 N11 . 2_665 104.42(17)
C1 N1 Zn1 . . 177.2(4)
N1 C1 S1 . . 178.8(5)
C15 N11 C11 . . 118.2(3)
C15 N11 Zn1 . . 118.4(2)
C11 N11 Zn1 . . 123.3(2)
N11 C11 C12 . . 122.3(3)
N11 C11 H11 . . 118.9
C12 C11 H11 . . 118.9
C11 C12 C13 . . 119.7(3)
C11 C12 H12 . . 120.2
C13 C12 H12 . . 120.2
C14 C13 C12 . . 117.8(3)
C14 C13 C16 . . 122.9(3)
C12 C13 C16 . . 119.3(3)
C15 C14 C13 . . 119.5(3)
C15 C14 H14 . . 120.2
C13 C14 H14 . . 120.2
N11 C15 C14 . . 122.6(3)
N11 C15 H15 . . 118.7
C14 C15 H15 . . 118.7
O11 C16 N12 . . 122.1(4)
O11 C16 C13 . . 120.1(3)
N12 C16 C13 . . 117.8(3)
C16 N12 H12A . . 120.0
C16 N12 H12B . . 120.0
H12A N12 H12B . . 120.0
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_665 1.921(3) ?
Zn1 N1 . 1.921(3) y
Zn1 N11 . 2.033(3) y
Zn1 N11 2_665 2.033(3) ?
N1 C1 . 1.165(5) ?
C1 S1 . 1.605(4) ?
N11 C15 . 1.336(4) ?
N11 C11 . 1.344(4) ?
C11 C12 . 1.376(5) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.387(5) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.385(4) ?
C13 C16 . 1.495(5) ?
C14 C15 . 1.378(5) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 O11 . 1.233(4) ?
C16 N12 . 1.326(5) ?
N12 H12A . 0.8800 ?
N12 H12B . 0.8800 ?
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
C14 H14 O11 3_565 0.95 2.54 3.365(6) 144.9
N12 H12A S1 12_556 0.88 2.62 3.407(3) 149.6
N12 H12B O11 3_565 0.88 1.97 2.821(4) 162.1

_cod_database_fobs_code 2241715
