#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/83/2228324.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_2228324
loop_
_publ_author_name
'Lv, Lei'
'Qiu, Xiumin'
'Yang, Jie'
'Liu, Shizheng'
'Li, Dacheng'
_publ_section_title
;
 Bis[2-(pyridin-2-yl)ethanol-κ²N,O]bis(thiocyanato-κN)nickel(II)
;
_journal_coeditor_code           GK2318
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1587
_journal_paper_doi               10.1107/S1600536810046647
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (N C S)2 (C7 H9 N O)2]'
_chemical_formula_moiety         'C16 H18 N4 Ni O2 S2'
_chemical_formula_sum            'C16 H18 N4 Ni O2 S2'
_chemical_formula_weight         421.17
_chemical_name_systematic
;
Bis[2-(pyridin-2-yl)ethanol-κ²N,O]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                 105.496(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7197(9)
_cell_length_b                   13.8634(15)
_cell_length_c                   7.8655(7)
_cell_measurement_reflns_used    2904
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.42
_cell_volume                     916.26(16)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'phi and omega 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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4493
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.6236
_exptl_absorpt_correction_T_min  0.6105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.552
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1616
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+0.5792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                1408
_reflns_number_total             1616
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2318.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228324
_cod_database_fobs_code          2228324
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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 1.0000 0.5000 0.0000 0.03039(15) Uani d SU 1 . .
S S1 1.22010(9) 0.69823(5) 0.50929(9) 0.0528(2) Uani d U 1 . .
N N1 0.7906(2) 0.54485(14) 0.0607(2) 0.0341(4) Uani d . 1 . .
N N2 1.1214(2) 0.57961(15) 0.2136(3) 0.0409(5) Uani d U 1 . .
O O1 0.9851(2) 0.62603(12) -0.1523(2) 0.0415(4) Uani d . 1 . .
H H1 1.0793 0.6489 -0.1717 0.050 Uiso calc R 1 . .
C C1 0.8438(3) 0.6798(2) -0.2289(4) 0.0498(7) Uani d . 1 . .
H H1A 0.8409 0.6968 -0.3493 0.060 Uiso calc R 1 . .
H H1B 0.8448 0.7391 -0.1630 0.060 Uiso calc R 1 . .
C C2 0.6971(3) 0.62185(19) -0.2278(3) 0.0452(6) Uani d . 1 . .
H H2A 0.6039 0.6570 -0.2936 0.054 Uiso calc R 1 . .
H H2B 0.7005 0.5613 -0.2886 0.054 Uiso calc R 1 . .
C C3 0.6788(3) 0.60033(17) -0.0472(3) 0.0373(5) Uani d . 1 . .
C C4 0.5510(3) 0.6363(2) 0.0063(4) 0.0484(6) Uani d . 1 . .
H H4 0.4762 0.6754 -0.0692 0.058 Uiso calc R 1 . .
C C5 0.5344(3) 0.6142(2) 0.1710(4) 0.0535(7) Uani d . 1 . .
H H5 0.4484 0.6374 0.2077 0.064 Uiso calc R 1 . .
C C6 0.6478(3) 0.5570(2) 0.2799(4) 0.0499(7) Uani d . 1 . .
H H6 0.6397 0.5409 0.3920 0.060 Uiso calc R 1 . .
C C7 0.7733(3) 0.52394(19) 0.2214(3) 0.0415(6) Uani d . 1 . .
H H7 0.8496 0.4854 0.2963 0.050 Uiso calc R 1 . .
C C8 1.1618(3) 0.62905(16) 0.3352(3) 0.0320(5) Uani d U 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'
O O 0.0106 0.0060 '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'
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
N2 Ni1 N2 3_765 . 180.00(9) ?
N2 Ni1 N1 3_765 3_765 86.82(8) ?
N2 Ni1 N1 . 3_765 93.18(8) ?
N2 Ni1 N1 3_765 . 93.18(8) ?
N2 Ni1 N1 . . 86.82(8) ?
N1 Ni1 N1 3_765 . 180.0 ?
N2 Ni1 O1 3_765 . 92.32(7) ?
N2 Ni1 O1 . . 87.68(7) ?
N1 Ni1 O1 3_765 . 92.38(7) ?
N1 Ni1 O1 . . 87.62(7) ?
N2 Ni1 O1 3_765 3_765 87.68(7) ?
N2 Ni1 O1 . 3_765 92.32(7) ?
N1 Ni1 O1 3_765 3_765 87.62(7) ?
N1 Ni1 O1 . 3_765 92.38(7) ?
O1 Ni1 O1 . 3_765 180.00(5) ?
C7 N1 C3 . . 118.1(2) ?
C7 N1 Ni1 . . 118.18(16) ?
C3 N1 Ni1 . . 123.47(16) ?
C8 N2 Ni1 . . 167.28(19) ?
C1 O1 Ni1 . . 126.06(15) ?
C1 O1 H1 . . 117.0 ?
Ni1 O1 H1 . . 117.0 ?
O1 C1 C2 . . 110.9(2) ?
O1 C1 H1A . . 109.5 ?
C2 C1 H1A . . 109.5 ?
O1 C1 H1B . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 108.1 ?
C3 C2 C1 . . 114.5(2) ?
C3 C2 H2A . . 108.6 ?
C1 C2 H2A . . 108.6 ?
C3 C2 H2B . . 108.6 ?
C1 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
N1 C3 C4 . . 121.2(2) ?
N1 C3 C2 . . 117.8(2) ?
C4 C3 C2 . . 120.9(2) ?
C5 C4 C3 . . 120.1(3) ?
C5 C4 H4 . . 119.9 ?
C3 C4 H4 . . 119.9 ?
C6 C5 C4 . . 118.5(3) ?
C6 C5 H5 . . 120.8 ?
C4 C5 H5 . . 120.8 ?
C5 C6 C7 . . 119.2(3) ?
C5 C6 H6 . . 120.4 ?
C7 C6 H6 . . 120.4 ?
N1 C7 C6 . . 122.8(3) ?
N1 C7 H7 . . 118.6 ?
C6 C7 H7 . . 118.6 ?
N2 C8 S1 . . 179.3(2) ?
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 N2 . 2.052(2) y
Ni1 N1 . 2.1011(19) y
Ni1 O1 . 2.1030(15) y
S1 C8 . 1.637(2) ?
N1 C7 . 1.344(3) ?
N1 C3 . 1.349(3) ?
N2 C8 . 1.153(3) ?
O1 C1 . 1.428(3) ?
O1 H1 . 0.9300 ?
C1 C2 . 1.513(4) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C3 . 1.501(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.386(4) ?
C4 C5 . 1.375(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.374(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.375(4) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
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
O1 H1 S1 4_575 0.93 2.66 3.2183(19) 119.0
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 Ni1 N1 C7 3_765 . . . 121.90(18) ?
N2 Ni1 N1 C7 . . . . -58.10(18) ?
O1 Ni1 N1 C7 . . . . -145.91(18) ?
O1 Ni1 N1 C7 3_765 . . . 34.09(18) ?
N2 Ni1 N1 C3 3_765 . . . -63.84(19) ?
N2 Ni1 N1 C3 . . . . 116.16(19) ?
O1 Ni1 N1 C3 . . . . 28.35(18) ?
O1 Ni1 N1 C3 3_765 . . . -151.65(18) ?
N1 Ni1 N2 C8 3_765 . . . 176.2(9) ?
N1 Ni1 N2 C8 . . . . -3.8(9) ?
O1 Ni1 N2 C8 . . . . 84.0(9) ?
O1 Ni1 N2 C8 3_765 . . . -96.0(9) ?
N2 Ni1 O1 C1 3_765 . . . 69.2(2) ?
N2 Ni1 O1 C1 . . . . -110.8(2) ?
N1 Ni1 O1 C1 3_765 . . . 156.1(2) ?
N1 Ni1 O1 C1 . . . . -23.9(2) ?
O1 C1 C2 C3 . . . . 65.5(3) ?
C7 N1 C3 C4 . . . . 1.0(3) ?
Ni1 N1 C3 C4 . . . . -173.23(18) ?
C7 N1 C3 C2 . . . . -178.9(2) ?
Ni1 N1 C3 C2 . . . . 6.9(3) ?
C1 C2 C3 N1 . . . . -63.6(3) ?
C1 C2 C3 C4 . . . . 116.5(3) ?
N1 C3 C4 C5 . . . . -1.2(4) ?
C2 C3 C4 C5 . . . . 178.7(2) ?
C3 C4 C5 C6 . . . . 0.7(4) ?
C4 C5 C6 C7 . . . . 0.0(4) ?
C3 N1 C7 C6 . . . . -0.4(4) ?
Ni1 N1 C7 C6 . . . . 174.2(2) ?
C5 C6 C7 N1 . . . . -0.1(4) ?
