#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/42/2234295.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_2234295
loop_
_publ_author_name
'Werner, Julia'
'Boeckmann, Jan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Bis(3-acetylpyridine-κN)bis(methanol-κO)bis(thiocyanato-κN)nickel(II)
;
_journal_coeditor_code           JJ2122
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m441
_journal_page_last               m442
_journal_paper_doi               10.1107/S1600536812008860
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (N C S)2 (C7 H7 N O) (C H4 O)2]'
_chemical_formula_moiety         'C18 H22 N4 Ni O4 S2'
_chemical_formula_sum            'C18 H22 N4 Ni O4 S2'
_chemical_formula_weight         481.23
_chemical_name_systematic
;
Bis(3-acetylpyridine-κN)bis(methanol-
κO)bis(thiocyanato-κN)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.782(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7088(7)
_cell_length_b                   14.6893(9)
_cell_length_c                   9.6887(8)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.53
_cell_volume                     1089.44(15)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'XRED32 (Stoe & Cie, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'φ scans'
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9642
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.655
_refine_ls_extinction_coef       0.028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                2041
_reflns_number_total             2555
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2122.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234295
_cod_database_fobs_code          2234295
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'
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
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_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'
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_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_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
