##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Bis(3-acetylpyridine-κN)bis(methanol-
κO)bis(thiocyanato-κN)nickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C18 H22 N4 Ni O4 S2'
_chemical_formula_sum     'C18 H22 N4 Ni O4 S2'
_chemical_formula_iupac     '[Ni (N C S)2 (C7 H7 N O) (C H4 O)2]'
_chemical_formula_weight     481.23
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
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'
_cell_length_a     7.7088(7)
_cell_length_b     14.6893(9)
_cell_length_c     9.6887(8)
_cell_angle_alpha     90.00
_cell_angle_beta     96.782(10)
_cell_angle_gamma     90.00
_cell_volume     1089.44(15)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     9642
_cell_measurement_theta_min     2.53
_cell_measurement_theta_max     28.03
_cell_measurement_temperature     180(2)
_exptl_crystal_description     block
_exptl_crystal_colour     blue
_exptl_crystal_size_max     0.19
_exptl_crystal_size_mid     0.14
_exptl_crystal_size_min     0.11
_exptl_crystal_density_diffrn     1.467
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     500
_exptl_absorpt_coefficient_mu     1.113
_exptl_absorpt_correction_type     numerical
_exptl_absorpt_process_details     '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_absorpt_correction_T_min     0.826
_exptl_absorpt_correction_T_max     0.881
_exptl_special_details     ?
_diffrn_ambient_temperature     180(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Stoe IPDS-1'
_diffrn_measurement_method     'φ scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     9642
_diffrn_reflns_av_R_equivalents     0.0603
_diffrn_reflns_av_sigmaI/netI     0.0418
_diffrn_reflns_theta_min     2.53
_diffrn_reflns_theta_max     28.03
_diffrn_reflns_theta_full     28.03
_diffrn_measured_fraction_theta_max     0.968
_diffrn_measured_fraction_theta_full     0.968
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_h_max     10
_diffrn_reflns_limit_k_min     -19
_diffrn_reflns_limit_k_max     18
_diffrn_reflns_limit_l_min     -12
_diffrn_reflns_limit_l_max     12
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     2555
_reflns_number_gt     2041
_reflns_threshold_expression     I>2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0523
_refine_ls_R_factor_gt     0.0390
_refine_ls_wR_factor_gt     0.0947
_refine_ls_wR_factor_ref     0.1011
_refine_ls_goodness_of_fit_ref     0.989
_refine_ls_restrained_S_all     0.989
_refine_ls_number_reflns     2555
_refine_ls_number_parameters     134
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.411
_refine_diff_density_min     -0.655
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_extinction_coef     0.028(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
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'
    'Ni' 'Ni' 0.3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'X-AREA (Stoe & Cie, 2008)'
_computing_cell_refinement     'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction     'XRED32 (Stoe & Cie, 2008)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'publCIF (Westrip, 2010)'
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_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Ni Ni1 0.5000 0.5000 0.5000 0.01655(14) Uani d S 1 2 . .
    N N1 0.6742(2) 0.59365(12) 0.5873(2) 0.0254(4) Uani d . 1 1 . .
    C C1 0.7710(3) 0.62982(13) 0.6700(2) 0.0205(4) Uani d . 1 1 . .
    S S1 0.90677(8) 0.68081(4) 0.78668(7) 0.03342(18) Uani d . 1 1 . .
    N N11 0.6038(2) 0.51317(11) 0.30841(19) 0.0195(4) Uani d . 1 1 . .
    O O11 0.6251(2) 0.28548(11) 0.0710(2) 0.0333(4) Uani d . 1 1 . .
    C C11 0.6169(3) 0.43931(14) 0.2295(2) 0.0203(4) Uani d . 1 1 . .
    H H11 0.5778 0.3827 0.2619 0.024 Uiso calc R 1 1 . .
    C C12 0.6841(3) 0.44086(14) 0.1032(2) 0.0199(4) Uani d . 1 1 . .
    C C13 0.7383(3) 0.52410(16) 0.0541(2) 0.0248(5) Uani d . 1 1 . .
    H H13 0.7830 0.5280 -0.0330 0.030 Uiso calc R 1 1 . .
    C C14 0.7256(3) 0.60105(15) 0.1351(3) 0.0265(5) Uani d . 1 1 . .
    H H14 0.7621 0.6586 0.1044 0.032 Uiso calc R 1 1 . .
    C C15 0.6593(3) 0.59317(14) 0.2609(2) 0.0228(4) Uani d . 1 1 . .
    H H15 0.6525 0.6462 0.3162 0.027 Uiso calc R 1 1 . .
    C C16 0.6908(3) 0.35298(15) 0.0263(2) 0.0249(5) Uani d . 1 1 . .
    C C17 0.7795(4) 0.3502(2) -0.1025(3) 0.0365(6) Uani d . 1 1 . .
    H H17A 0.7727 0.2884 -0.1408 0.055 Uiso calc R 1 1 . .
    H H17B 0.9023 0.3677 -0.0800 0.055 Uiso calc R 1 1 . .
    H H17C 0.7217 0.3927 -0.1711 0.055 Uiso calc R 1 1 . .
    O O21 0.3202(2) 0.60443(10) 0.44475(18) 0.0242(3) Uani d . 1 1 . .
    H H1O 0.3466 0.6599 0.4452 0.036 Uiso d R 1 1 . .
    C C21 0.1344(3) 0.59987(17) 0.4463(3) 0.0311(5) Uani d . 1 1 . .
    H H21A 0.0818 0.6583 0.4156 0.047 Uiso calc R 1 1 . .
    H H21B 0.1085 0.5868 0.5409 0.047 Uiso calc R 1 1 . .
    H H21C 0.0862 0.5515 0.3835 0.047 Uiso calc R 1 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ni1 0.0195(2) 0.01456(19) 0.0153(2) -0.00132(13) 0.00091(13) -0.00197(13)
    N1 0.0268(9) 0.0240(9) 0.0251(11) -0.0070(7) 0.0017(8) -0.0042(7)
    C1 0.0229(10) 0.0166(9) 0.0223(11) -0.0008(7) 0.0047(8) 0.0015(7)
    S1 0.0345(3) 0.0316(3) 0.0306(3) -0.0083(2) -0.0113(2) -0.0015(2)
    N11 0.0215(9) 0.0202(8) 0.0167(9) 0.0005(6) 0.0018(7) 0.0007(6)
    O11 0.0400(10) 0.0245(8) 0.0364(10) 0.0004(7) 0.0085(8) -0.0078(7)
    C11 0.0229(10) 0.0192(9) 0.0183(11) 0.0000(7) 0.0004(8) -0.0006(8)
    C12 0.0190(9) 0.0224(10) 0.0176(10) 0.0017(7) -0.0003(7) -0.0003(8)
    C13 0.0238(11) 0.0308(11) 0.0202(11) -0.0013(8) 0.0040(8) 0.0046(9)
    C14 0.0285(11) 0.0226(10) 0.0285(12) -0.0024(8) 0.0035(9) 0.0050(9)
    C15 0.0239(10) 0.0192(10) 0.0249(12) -0.0024(8) 0.0010(8) -0.0003(8)
    C16 0.0244(10) 0.0274(11) 0.0218(11) 0.0039(8) -0.0013(8) -0.0046(8)
    C17 0.0398(13) 0.0476(15) 0.0224(13) 0.0060(11) 0.0044(10) -0.0088(11)
    O21 0.0221(7) 0.0184(7) 0.0318(9) 0.0034(5) 0.0019(6) 0.0038(6)
    C21 0.0231(11) 0.0335(12) 0.0368(14) 0.0041(9) 0.0046(9) 0.0042(10)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
    Ni1 N1 3_666 2.0357(18) y
    Ni1 N1 . 2.0357(18) y
    Ni1 O21 3_666 2.0943(14) y
    Ni1 O21 . 2.0943(14) y
    Ni1 N11 . 2.1154(19) y
    Ni1 N11 3_666 2.1154(19) y
    N1 C1 . 1.157(3) ?
    C1 S1 . 1.629(2) ?
    N11 C11 . 1.338(3) ?
    N11 C15 . 1.350(3) ?
    O11 C16 . 1.216(3) ?
    C11 C12 . 1.384(3) ?
    C11 H11 . 0.9500 ?
    C12 C13 . 1.394(3) ?
    C12 C16 . 1.494(3) ?
    C13 C14 . 1.386(3) ?
    C13 H13 . 0.9500 ?
    C14 C15 . 1.380(3) ?
    C14 H14 . 0.9500 ?
    C15 H15 . 0.9500 ?
    C16 C17 . 1.493(4) ?
    C17 H17A . 0.9800 ?
    C17 H17B . 0.9800 ?
    C17 H17C . 0.9800 ?
    O21 C21 . 1.435(3) ?
    O21 H1O . 0.8399 ?
    C21 H21A . 0.9800 ?
    C21 H21B . 0.9800 ?
    C21 H21C . 0.9800 ?
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 Ni1 N1 3_666 . 180.00(13) y
    N1 Ni1 O21 3_666 3_666 89.75(7) y
    N1 Ni1 O21 . 3_666 90.25(7) y
    N1 Ni1 O21 3_666 . 90.25(7) y
    N1 Ni1 O21 . . 89.75(7) y
    O21 Ni1 O21 3_666 . 180.00(9) y
    N1 Ni1 N11 3_666 . 89.80(7) y
    N1 Ni1 N11 . . 90.20(7) y
    O21 Ni1 N11 3_666 . 89.06(7) y
    O21 Ni1 N11 . . 90.94(7) y
    N1 Ni1 N11 3_666 3_666 90.20(7) y
    N1 Ni1 N11 . 3_666 89.80(7) y
    O21 Ni1 N11 3_666 3_666 90.94(7) y
    O21 Ni1 N11 . 3_666 89.06(7) y
    N11 Ni1 N11 . 3_666 180.0 y
    C1 N1 Ni1 . . 159.66(19) ?
    N1 C1 S1 . . 179.8(2) ?
    C11 N11 C15 . . 117.6(2) ?
    C11 N11 Ni1 . . 119.28(14) ?
    C15 N11 Ni1 . . 123.16(15) ?
    N11 C11 C12 . . 123.58(19) ?
    N11 C11 H11 . . 118.2 ?
    C12 C11 H11 . . 118.2 ?
    C11 C12 C13 . . 118.3(2) ?
    C11 C12 C16 . . 117.70(19) ?
    C13 C12 C16 . . 124.0(2) ?
    C14 C13 C12 . . 118.6(2) ?
    C14 C13 H13 . . 120.7 ?
    C12 C13 H13 . . 120.7 ?
    C15 C14 C13 . . 119.3(2) ?
    C15 C14 H14 . . 120.3 ?
    C13 C14 H14 . . 120.3 ?
    N11 C15 C14 . . 122.6(2) ?
    N11 C15 H15 . . 118.7 ?
    C14 C15 H15 . . 118.7 ?
    O11 C16 C17 . . 121.8(2) ?
    O11 C16 C12 . . 119.1(2) ?
    C17 C16 C12 . . 119.1(2) ?
    C16 C17 H17A . . 109.5 ?
    C16 C17 H17B . . 109.5 ?
    H17A C17 H17B . . 109.5 ?
    C16 C17 H17C . . 109.5 ?
    H17A C17 H17C . . 109.5 ?
    H17B C17 H17C . . 109.5 ?
    C21 O21 Ni1 . . 126.46(13) ?
    C21 O21 H1O . . 106.7 ?
    Ni1 O21 H1O . . 123.8 ?
    O21 C21 H21A . . 109.5 ?
    O21 C21 H21B . . 109.5 ?
    H21A C21 H21B . . 109.5 ?
    O21 C21 H21C . . 109.5 ?
    H21A C21 H21C . . 109.5 ?
    H21B C21 H21C . . 109.5 ?
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
    O21 H1O O11 2_655 0.84 1.87 2.700(2) 171.6
data_global
_journal_date_recd_electronic     2012-02-13
_journal_date_accepted     2012-02-28
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2012
_journal_volume     68
_journal_issue      4
_journal_page_first     m441
_journal_page_last     m442
_journal_paper_category     QM
_journal_paper_doi     10.1107/S1600536812008860
_journal_coeditor_code     JJ2122
_publ_contact_author
;
      Julia Werner
      Institut für Anorganische Chemie
      Christian-Albrechts-Universität Kiel
      Max-Eyth Strasse 2
      D-24118 Kiel
      Germany
;
_publ_contact_author_email     jwerner@ac.uni-kiel.de
_publ_contact_author_fax     '(+)431-880-1520'
_publ_contact_author_phone     '(+)431-880-5546'
_publ_section_title
;\
Bis(3-acetylpyridine-κN)bis(methanol-κO)bis(thiocyanato-\
κN)nickel(II)
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Werner, Julia' .
;
Institut für Anorganische Chemie
Christian-Albrechts-Universität Kiel
Max-Eyth-Strasse 2
24118 Kiel
Germany
;
    'Boeckmann, Jan' .
;
Institut für Anorganische Chemie
Christian-Albrechts-Universität Kiel
Max-Eyth-Strasse 2
24118 Kiel
Germany
;
    'Jeß, Inke' .
;
Institut für Anorganische Chemie
Christian-Albrechts-Universität Kiel
Max-Eyth-Strasse 2
24118 Kiel
Germany
;
    'Näther, Christian' .
;
Institut für Anorganische Chemie
Christian-Albrechts-Universität Kiel
Max-Eyth-Strasse 2
24118 Kiel
Germany
;
_publ_section_synopsis     .
