#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208461.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_2208461
loop_
_publ_author_name
'Zhao, Qi-Hua'
'Mu, Xiu-Mei'
'Zhang, Mei-Su'
'Fang, Rui-Bing'
_publ_section_title
;Bis(thiocyanato-κN)bis(2,2'-thiodipyridine-κ²N,N')nickel(II)
 monohydrate
;
_journal_coeditor_code           XU6087
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m615
_journal_page_last               m616
_journal_paper_doi               10.1107/S1600536806006507
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (N C S)2 (C10 H8 N2 S)2] , H2 O'
_chemical_formula_moiety         'C22 H16 N6 Ni S4 , H2 O'
_chemical_formula_sum            'C22 H18 N6 Ni O S4'
_chemical_formula_weight         569.38
_chemical_name_systematic
;
Bis(thiocyanato-\kN)bis(2,2'-thiodipyridine-κ²N,N')nickel(II)
monohydrate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3379(5)
_cell_length_b                   29.3927(19)
_cell_length_c                   10.2119(7)
_cell_measurement_reflns_used    4506
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.4
_cell_volume                     2492.6(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      289(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16243
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5708
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0512P)²+1.153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.099
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                4345
_reflns_number_total             5708
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu6087.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208461
_cod_database_fobs_code          2208461
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
Ni Ni1 0.58750(4) 0.362796(10) 0.42512(3) 0.03727(10) Uani d . 1
S S1 0.45073(8) 0.40363(3) 0.71818(7) 0.05304(19) Uani d . 1
S S2 0.17063(7) 0.34870(2) 0.36259(7) 0.04650(17) Uani d . 1
S S3 0.92553(15) 0.45186(5) 0.16661(11) 0.1048(4) Uani d . 1
S S4 0.85797(10) 0.22061(3) 0.36455(11) 0.0775(3) Uani d . 1
O O1W 0.491(3) 0.4858(5) 0.0404(14) 0.221(7) Uani d PU 0.54(2)
O O1W' 0.331(4) 0.4744(5) 0.0091(15) 0.235(14) Uani d P 0.46(2)
N N1 0.7208(2) 0.38152(7) 0.6046(2) 0.0402(5) Uani d . 1
N N2 0.4444(2) 0.42109(7) 0.4568(2) 0.0436(5) Uani d . 1
N N3 0.4332(2) 0.31900(7) 0.51759(19) 0.0361(4) Uani d . 1
N N4 0.4506(2) 0.34625(7) 0.2458(2) 0.0402(5) Uani d . 1
N N5 0.7350(3) 0.40343(8) 0.3252(2) 0.0540(6) Uani d . 1
N N6 0.7323(2) 0.30683(8) 0.4031(2) 0.0477(5) Uani d . 1
C C1 0.7569(4) 0.40738(10) 0.8278(3) 0.0529(7) Uani d . 1
H H1 0.7112 0.4174 0.9025 0.063 Uiso calc R 1
C C2 0.9217(4) 0.40255(10) 0.8277(3) 0.0595(8) Uani d . 1
H H2 0.9890 0.4088 0.9031 0.071 Uiso calc R 1
C C3 0.9847(3) 0.38859(10) 0.7158(3) 0.0560(7) Uani d . 1
H H3 1.0955 0.3860 0.7130 0.067 Uiso calc R 1
C C4 0.8814(3) 0.37833(10) 0.6069(3) 0.0481(6) Uani d . 1
H H4 0.9253 0.3687 0.5310 0.058 Uiso calc R 1
C C5 0.6615(3) 0.39685(8) 0.7137(3) 0.0410(6) Uani d . 1
C C6 0.3929(3) 0.43393(9) 0.5717(3) 0.0456(6) Uani d . 1
C C7 0.3965(4) 0.44630(9) 0.3515(3) 0.0578(7) Uani d . 1
H H7 0.4365 0.4394 0.2716 0.069 Uiso calc R 1
C C8 0.2896(4) 0.48228(10) 0.3566(4) 0.0687(9) Uani d . 1
H H8 0.2557 0.4984 0.2808 0.082 Uiso calc R 1
C C9 0.2349(4) 0.49365(11) 0.4739(5) 0.0769(11) Uani d . 1
H H9 0.1624 0.5175 0.4788 0.092 Uiso calc R 1
C C10 0.2871(3) 0.46984(10) 0.5840(4) 0.0635(9) Uani d . 1
H H10 0.2528 0.4775 0.6654 0.076 Uiso calc R 1
C C11 0.1749(3) 0.29267(9) 0.5704(3) 0.0449(6) Uani d . 1
H H11 0.0641 0.2917 0.5496 0.054 Uiso calc R 1
C C12 0.2438(3) 0.27032(9) 0.6788(3) 0.0482(6) Uani d . 1
H H12 0.1800 0.2553 0.7352 0.058 Uiso calc R 1
C C13 0.4085(3) 0.27041(8) 0.7034(3) 0.0453(6) Uani d . 1
H H13 0.4582 0.2548 0.7750 0.054 Uiso calc R 1
C C14 0.4983(3) 0.29411(8) 0.6197(3) 0.0418(6) Uani d . 1
H H14 0.6099 0.2929 0.6345 0.050 Uiso calc R 1
C C15 0.2723(3) 0.31683(8) 0.4918(2) 0.0367(5) Uani d . 1
C C16 0.2894(3) 0.34376(8) 0.2288(3) 0.0413(6) Uani d . 1
C C17 0.5319(4) 0.33964(9) 0.1395(3) 0.0500(6) Uani d . 1
H H17 0.6438 0.3396 0.1506 0.060 Uiso calc R 1
C C18 0.4581(4) 0.33291(10) 0.0151(3) 0.0577(7) Uani d . 1
H H18 0.5187 0.3284 -0.0560 0.069 Uiso calc R 1
C C19 0.2922(4) 0.33303(11) -0.0018(3) 0.0631(8) Uani d . 1
H H19 0.2388 0.3298 -0.0852 0.076 Uiso calc R 1
C C20 0.2072(4) 0.33787(10) 0.1055(3) 0.0550(7) Uani d . 1
H H20 0.0952 0.3372 0.0962 0.066 Uiso calc R 1
C C21 0.8143(3) 0.42330(10) 0.2591(3) 0.0503(7) Uani d . 1
C C22 0.7849(3) 0.27134(10) 0.3869(3) 0.0451(6) 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'
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
_geom_angle_publ_flag
N5 Ni1 N6 . 91.57(10) y
N5 Ni1 N3 . 176.72(9) y
N6 Ni1 N3 . 87.04(8) y
N5 Ni1 N4 . 90.24(9) y
N6 Ni1 N4 . 89.89(8) y
N3 Ni1 N4 . 86.79(8) y
N5 Ni1 N1 . 89.29(9) y
N6 Ni1 N1 . 91.95(8) y
N3 Ni1 N1 . 93.73(8) y
N4 Ni1 N1 . 178.10(8) y
N5 Ni1 N2 . 88.62(9) y
N6 Ni1 N2 . 177.23(9) y
N3 Ni1 N2 . 92.91(8) y
N4 Ni1 N2 . 92.87(8) y
N1 Ni1 N2 . 85.29(8) y
C6 S1 C5 . 103.31(12) y
C16 S2 C15 . 105.62(11) y
O1W O1W O1W' 3_665 101(3) ?
C4 N1 C5 . 116.9(2) ?
C4 N1 Ni1 . 116.16(18) ?
C5 N1 Ni1 . 126.93(16) ?
C7 N2 C6 . 116.9(2) ?
C7 N2 Ni1 . 117.1(2) ?
C6 N2 Ni1 . 126.00(18) ?
C15 N3 C14 . 116.8(2) ?
C15 N3 Ni1 . 125.50(16) ?
C14 N3 Ni1 . 117.38(16) ?
C17 N4 C16 . 117.4(2) ?
C17 N4 Ni1 . 117.27(18) ?
C16 N4 Ni1 . 125.30(17) ?
C21 N5 Ni1 . 173.3(2) ?
C22 N6 Ni1 . 166.7(2) ?
C5 C1 C2 . 118.1(3) ?
C5 C1 H1 . 120.9 ?
C2 C1 H1 . 120.9 ?
C3 C2 C1 . 119.4(3) ?
C3 C2 H2 . 120.3 ?
C1 C2 H2 . 120.3 ?
C2 C3 C4 . 118.8(3) ?
C2 C3 H3 . 120.6 ?
C4 C3 H3 . 120.6 ?
N1 C4 C3 . 123.4(3) ?
N1 C4 H4 . 118.3 ?
C3 C4 H4 . 118.3 ?
N1 C5 C1 . 123.3(2) ?
N1 C5 S1 . 120.06(18) ?
C1 C5 S1 . 116.6(2) ?
N2 C6 C10 . 123.3(3) ?
N2 C6 S1 . 120.92(19) ?
C10 C6 S1 . 115.7(2) ?
N2 C7 C8 . 122.6(3) ?
N2 C7 H7 . 118.7 ?
C8 C7 H7 . 118.7 ?
C9 C8 C7 . 119.2(3) ?
C9 C8 H8 . 120.4 ?
C7 C8 H8 . 120.4 ?
C10 C9 C8 . 119.5(3) ?
C10 C9 H9 . 120.2 ?
C8 C9 H9 . 120.2 ?
C9 C10 C6 . 118.3(3) ?
C9 C10 H10 . 120.8 ?
C6 C10 H10 . 120.8 ?
C12 C11 C15 . 119.3(2) ?
C12 C11 H11 . 120.4 ?
C15 C11 H11 . 120.4 ?
C11 C12 C13 . 119.1(2) ?
C11 C12 H12 . 120.4 ?
C13 C12 H12 . 120.4 ?
C12 C13 C14 . 118.6(2) ?
C12 C13 H13 . 120.7 ?
C14 C13 H13 . 120.7 ?
N3 C14 C13 . 123.5(2) ?
N3 C14 H14 . 118.2 ?
C13 C14 H14 . 118.2 ?
N3 C15 C11 . 122.4(2) ?
N3 C15 S2 . 121.52(18) ?
C11 C15 S2 . 115.86(18) ?
N4 C16 C20 . 122.0(3) ?
N4 C16 S2 . 121.41(19) ?
C20 C16 S2 . 116.5(2) ?
N4 C17 C18 . 123.4(3) ?
N4 C17 H17 . 118.3 ?
C18 C17 H17 . 118.3 ?
C17 C18 C19 . 118.4(3) ?
C17 C18 H18 . 120.8 ?
C19 C18 H18 . 120.8 ?
C20 C19 C18 . 119.2(3) ?
C20 C19 H19 . 120.4 ?
C18 C19 H19 . 120.4 ?
C19 C20 C16 . 119.4(3) ?
C19 C20 H20 . 120.3 ?
C16 C20 H20 . 120.3 ?
N5 C21 S3 . 179.3(3) ?
N6 C22 S4 . 179.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 2.129(2) y
Ni1 N2 2.129(2) y
Ni1 N3 2.103(2) y
Ni1 N4 2.126(2) y
Ni1 N5 2.050(2) y
Ni1 N6 2.065(2) y
S1 C6 1.770(3) ?
S1 C5 1.774(3) ?
S2 C16 1.763(3) ?
S2 C15 1.771(2) ?
S3 C21 1.617(3) ?
S4 C22 1.634(3) ?
N1 C4 1.340(3) ?
N1 C5 1.337(3) ?
N2 C7 1.337(4) ?
N2 C6 1.340(3) ?
N3 C15 1.346(3) ?
N3 C14 1.348(3) ?
N4 C17 1.345(3) ?
N4 C16 1.342(3) ?
N5 C21 1.147(4) ?
N6 C22 1.149(3) ?
C1 C5 1.386(4) ?
C1 C2 1.382(4) ?
C1 H1 0.9300 ?
C2 C3 1.363(4) ?
C2 H2 0.9300 ?
C3 C4 1.378(4) ?
C3 H3 0.9300 ?
C4 H4 0.9300 ?
C6 C10 1.388(4) ?
C7 C8 1.387(4) ?
C7 H7 0.9300 ?
C8 C9 1.361(5) ?
C8 H8 0.9300 ?
C9 C10 1.363(5) ?
C9 H9 0.9300 ?
C10 H10 0.9300 ?
C11 C12 1.369(4) ?
C11 C15 1.387(4) ?
C11 H11 0.9300 ?
C12 C13 1.373(4) ?
C12 H12 0.9300 ?
C13 C14 1.375(4) ?
C13 H13 0.9300 ?
C14 H14 0.9300 ?
C16 C20 1.390(4) ?
C17 C18 1.375(4) ?
C17 H17 0.9300 ?
C18 C19 1.379(4) ?
C18 H18 0.9300 ?
C19 C20 1.364(4) ?
C19 H19 0.9300 ?
C20 H20 0.9300 ?
