#------------------------------------------------------------------------------
#$Date: 2016-02-21 04:24:37 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176802 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/15/2241566.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_2241566
loop_
_publ_author_name
'Neumann, Tristan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 catena-poly[[[bis(pyridine-4-carbothioamide-κN¹)cadmium]-di-μ-thiocyanato-κ²N:S;κ²S:N]
 methanol disolvate]
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              370
_journal_page_last               373
_journal_paper_doi               10.1107/S2056989016002632
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cd (N C S)2 (C6 H6 N2 S)], 2C H4 O'
_chemical_formula_moiety         'C32 H40 Cd2 N12 O4 S8'
_chemical_formula_sum            'C32 H40 Cd2 N12 O4 S8'
_chemical_formula_weight         1138.04
_chemical_name_systematic
;catena-Poly[[[bis(pyridine-4-carbothioamide-κN¹)cadmium]-di-μ-thiocyanato-κ²N:S;κ²S:N] methanol
disolvate]
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.124(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.1891(10)
_cell_length_b                   5.8729(2)
_cell_length_c                   15.5080(6)
_cell_measurement_reflns_used    16834
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1.3
_cell_volume                     2294.14(15)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.617
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.8000
_exptl_absorpt_correction_T_min  0.6443
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.466
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0255
_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)+(0.0471P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                2208
_reflns_number_total             2515
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5271sup1.cif
_cod_data_source_block           I
_cod_database_code               2241566
_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+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd1 0.5000 0.5000 0.5000 0.02964(10) Uani d 1 . .
N N1 0.45141(7) 0.8201(3) 0.46141(12) 0.0363(4) Uani d 1 . .
C C1 0.44617(9) 1.0011(3) 0.43255(13) 0.0317(4) Uani d 1 . .
S S1 0.43930(2) 1.25424(10) 0.38878(4) 0.04069(15) Uani d 1 . .
N N11 0.43968(8) 0.4286(3) 0.61284(12) 0.0361(4) Uani d 1 . .
C C11 0.44093(9) 0.2407(4) 0.66130(15) 0.0426(5) Uani d 1 . .
H H11 0.4684 0.1332 0.6514 0.051 Uiso calc 1 . .
C C12 0.40419(9) 0.1946(4) 0.72524(14) 0.0405(5) Uani d 1 . .
H H12 0.4060 0.0563 0.7569 0.049 Uiso calc 1 . .
C C13 0.36515(9) 0.3512(4) 0.74238(13) 0.0353(5) Uani d 1 . .
C C14 0.36407(12) 0.5485(4) 0.6943(2) 0.0542(7) Uani d 1 . .
H H14 0.3381 0.6623 0.7050 0.065 Uiso calc 1 . .
C C15 0.40177(12) 0.5776(5) 0.62990(18) 0.0532(7) Uani d 1 . .
H H15 0.4002 0.7124 0.5962 0.064 Uiso calc 1 . .
C C16 0.32407(9) 0.3067(4) 0.81005(14) 0.0366(5) Uani d 1 . .
N N12 0.31373(11) 0.4768(4) 0.86169(16) 0.0540(6) Uani d 1 . .
H H12A 0.3305 0.6070 0.8554 0.065 Uiso calc 1 . .
H H12B 0.2900 0.4610 0.9028 0.065 Uiso calc 1 . .
S S11 0.29342(3) 0.05620(11) 0.81316(4) 0.04527(16) Uani d 1 . .
O O1 0.2777(4) 0.0596(16) 1.0276(8) 0.067(3) Uani d 0.5 A 1
H H1 0.2760 0.0718 0.9737 0.100 Uiso calc 0.5 A 1
C C17 0.3143(5) -0.101(3) 1.0489(13) 0.062(3) Uani d 0.5 A 1
H H17A 0.3476 -0.0703 1.0185 0.093 Uiso calc 0.5 A 1
H H17B 0.3010 -0.2520 1.0324 0.093 Uiso calc 0.5 A 1
H H17C 0.3206 -0.0978 1.1113 0.093 Uiso calc 0.5 A 1
O O1' 0.2639(4) -0.0102(19) 1.0155(8) 0.079(3) Uani d 0.5 B 2
H H1' 0.2637 0.0358 0.9642 0.118 Uiso calc 0.5 B 2
C C17' 0.3144(8) -0.019(4) 1.0447(17) 0.113(8) Uani d 0.5 B 2
H H17D 0.3348 0.1072 1.0201 0.169 Uiso calc 0.5 B 2
H H17E 0.3306 -0.1640 1.0274 0.169 Uiso calc 0.5 B 2
H H17F 0.3146 -0.0074 1.1077 0.169 Uiso calc 0.5 B 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'
Cd Cd -0.8075 1.2024 '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'
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 Cd1 N1 5_666 . 180.00(9)
N1 Cd1 N11 5_666 5_666 89.72(7)
N1 Cd1 N11 . 5_666 90.28(7)
N1 Cd1 N11 5_666 . 90.28(7)
N1 Cd1 N11 . . 89.72(7)
N11 Cd1 N11 5_666 . 180.0
N1 Cd1 S1 5_666 1_545 91.67(5)
N1 Cd1 S1 . 1_545 88.33(5)
N11 Cd1 S1 5_666 1_545 89.20(5)
N11 Cd1 S1 . 1_545 90.80(5)
N1 Cd1 S1 5_666 5_676 88.33(5)
N1 Cd1 S1 . 5_676 91.67(5)
N11 Cd1 S1 5_666 5_676 90.80(5)
N11 Cd1 S1 . 5_676 89.20(5)
S1 Cd1 S1 1_545 5_676 180.0
C1 N1 Cd1 . . 154.23(17)
N1 C1 S1 . . 178.2(2)
C1 S1 Cd1 . 1_565 99.19(7)
C15 N11 C11 . . 116.8(2)
C15 N11 Cd1 . . 119.86(16)
C11 N11 Cd1 . . 123.37(15)
N11 C11 C12 . . 123.3(2)
N11 C11 H11 . . 118.3
C12 C11 H11 . . 118.3
C13 C12 C11 . . 119.2(2)
C13 C12 H12 . . 120.4
C11 C12 H12 . . 120.4
C12 C13 C14 . . 118.2(2)
C12 C13 C16 . . 121.0(2)
C14 C13 C16 . . 120.8(2)
C13 C14 C15 . . 118.6(2)
C13 C14 H14 . . 120.7
C15 C14 H14 . . 120.7
N11 C15 C14 . . 123.9(2)
N11 C15 H15 . . 118.1
C14 C15 H15 . . 118.1
N12 C16 C13 . . 115.8(2)
N12 C16 S11 . . 124.43(17)
C13 C16 S11 . . 119.74(16)
C16 N12 H12A . . 120.0
C16 N12 H12B . . 120.0
H12A N12 H12B . . 120.0
C17 O1 H1 . . 109.5
O1 C17 H17A . . 109.5
O1 C17 H17B . . 109.5
H17A C17 H17B . . 109.5
O1 C17 H17C . . 109.5
H17A C17 H17C . . 109.5
H17B C17 H17C . . 109.5
C17' O1' H1' . . 109.5
O1' C17' H17D . . 109.5
O1' C17' H17E . . 109.5
H17D C17' H17E . . 109.5
O1' C17' H17F . . 109.5
H17D C17' H17F . . 109.5
H17E C17' H17F . . 109.5
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
Cd1 N1 5_666 2.3212(18) ?
Cd1 N1 . 2.3212(18) y
Cd1 N11 5_666 2.3575(18) ?
Cd1 N11 . 2.3576(18) y
Cd1 S1 1_545 2.7174(6) y
Cd1 S1 5_676 2.7174(6) ?
N1 C1 . 1.161(3) ?
C1 S1 . 1.643(2) ?
S1 Cd1 1_565 2.7174(6) ?
N11 C15 . 1.322(3) ?
N11 C11 . 1.335(3) ?
C11 C12 . 1.385(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.373(3) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.378(3) ?
C13 C16 . 1.498(3) ?
C14 C15 . 1.390(3) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 N12 . 1.307(3) ?
C16 S11 . 1.662(2) ?
N12 H12A . 0.8800 ?
N12 H12B . 0.8800 ?
O1 C17 . 1.361(13) ?
O1 H1 . 0.8400 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
O1' C17' . 1.351(15) ?
O1' H1' . 0.8400 ?
C17' H17D . 0.9800 ?
C17' H17E . 0.9800 ?
C17' H17F . 0.9800 ?
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
C11 H11 N1 5_666 0.95 2.69 3.335(3) 125.9
C12 H12 S1 6_566 0.95 2.86 3.762(2) 157.9
C15 H15 N1 . 0.95 2.54 3.230(3) 129.8
N12 H12B O1 7_557 0.88 2.02 2.883(10) 165.4
N12 H12B O1' 7_557 0.88 1.88 2.740(12) 164.7
N12 H12A S1 6_576 0.88 2.90 3.560(3) 132.7
N12 H12A S11 1_565 0.88 2.87 3.522(2) 131.8
O1 H1 S11 . 0.84 2.53 3.351(12) 165.4
O1' H1' S11 . 0.84 2.46 3.250(12) 156.2

_cod_database_fobs_code 2241566
