#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/95/2219565.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_2219565
loop_
_publ_author_name
'Yang, Ming-Hua'
_publ_section_title
;Diaqua(2,5-di-4-pyridyl-1,3,4-thiadiazole-κN²)bis(thiocyanato-κN)nickel(II)
 dihydrate
;
_journal_coeditor_code           DN2378
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1331
_journal_paper_doi               10.1107/S1600536808030444
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (N C S)2 (C12 H8 N4 S)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C26 H20 N10 Ni O2 S4, 2(H2 O)'
_chemical_formula_sum            'C26 H24 N10 Ni O4 S4'
_chemical_formula_weight         727.50
_chemical_name_systematic
;Diaqua(2,5-di-4-pyridyl-1,3,4-thiadiazole-\kN²)bis(thiocyanato-\kN)nickel(II)
dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.629(2)
_cell_angle_beta                 93.067(2)
_cell_angle_gamma                112.228(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0555(11)
_cell_length_b                   8.3034(13)
_cell_length_c                   14.849(2)
_cell_measurement_reflns_used    2721
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      1.44
_cell_volume                     768.3(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
CAMERON (Pearce et al.,  2000)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3967
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.44
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.8545
_exptl_absorpt_correction_T_min  0.7893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0553
_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)+(0.0643P)²+0.1149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                1810
_reflns_number_total             2747
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2378.cif
_cod_data_source_block           I
_cod_database_code               2219565
_cod_database_fobs_code          2219565
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.5000 0.5000 0.0397(3) Uani d S 1
S S1 -0.0367(2) 0.2796(2) 0.90422(9) 0.0507(4) Uani d . 1
S S2 0.7893(2) 0.05582(18) 0.46356(10) 0.0499(4) Uani d . 1
N N1 0.4008(5) 0.4385(5) 0.6282(3) 0.0370(9) Uani d . 1
N N2 0.3264(6) 0.2926(6) 0.9413(3) 0.0507(11) Uani d . 1
N N3 0.2307(7) 0.2566(6) 1.0167(3) 0.0512(11) Uani d . 1
N N4 -0.3536(7) 0.1274(6) 1.2103(3) 0.0530(11) Uani d . 1
N N5 0.6832(6) 0.3540(6) 0.4939(3) 0.0439(10) Uani d . 1
O O1W 0.2492(4) 0.2685(4) 0.4104(2) 0.0456(8) Uani d . 1
H H1WA 0.1300 0.2324 0.4268 0.068 Uiso d R 1
H H1WB 0.2655 0.1751 0.3792 0.068 Uiso d R 1
C C1 0.2114(7) 0.4119(6) 0.6465(3) 0.0448(12) Uani d . 1
H H1 0.1217 0.4267 0.6042 0.054 Uiso calc R 1
C C2 0.1394(7) 0.3639(7) 0.7239(3) 0.0479(13) Uani d . 1
H H2 0.0026 0.3409 0.7317 0.058 Uiso calc R 1
C C3 0.2717(7) 0.3502(6) 0.7897(3) 0.0392(11) Uani d . 1
C C4 0.4712(8) 0.3790(7) 0.7725(3) 0.0490(13) Uani d . 1
H H4 0.5656 0.3697 0.8149 0.059 Uiso calc R 1
C C5 0.5267(7) 0.4217(7) 0.6915(3) 0.0454(12) Uani d . 1
H H5 0.6606 0.4399 0.6803 0.054 Uiso calc R 1
C C6 0.2059(7) 0.3069(6) 0.8769(3) 0.0408(12) Uani d . 1
C C7 0.0422(8) 0.2485(7) 1.0080(3) 0.0435(12) Uani d . 1
C C8 -0.0933(7) 0.2144(6) 1.0799(3) 0.0395(11) Uani d . 1
C C9 -0.0247(8) 0.1812(7) 1.1595(3) 0.0514(13) Uani d . 1
H H9 0.1090 0.1867 1.1704 0.062 Uiso calc R 1
C C10 -0.1584(8) 0.1398(8) 1.2222(4) 0.0573(15) Uani d . 1
H H10 -0.1108 0.1191 1.2760 0.069 Uiso calc R 1
C C11 -0.4142(8) 0.1632(7) 1.1355(4) 0.0516(13) Uani d . 1
H H11 -0.5477 0.1593 1.1273 0.062 Uiso calc R 1
C C12 -0.2923(7) 0.2065(7) 1.0682(3) 0.0459(12) Uani d . 1
H H12 -0.3433 0.2298 1.0160 0.055 Uiso calc R 1
C C13 0.7270(6) 0.2306(7) 0.4811(3) 0.0366(11) Uani d . 1
O O2W 0.3283(5) -0.0225(5) 0.3113(2) 0.0604(10) Uani d . 1
H H2WA 0.3641 -0.0509 0.3583 0.091 Uiso d R 1
H H2WB 0.4342 0.0242 0.2871 0.091 Uiso d R 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'
Ni Ni 0.3393 1.1124 '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'
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
N5 Ni1 N5 . 2_666 180.000(2)
N5 Ni1 O1W . 2_666 88.99(14)
N5 Ni1 O1W 2_666 2_666 91.01(14)
N5 Ni1 O1W . . 91.01(14)
N5 Ni1 O1W 2_666 . 88.99(14)
O1W Ni1 O1W 2_666 . 180.0
N5 Ni1 N1 . . 91.17(14)
N5 Ni1 N1 2_666 . 88.83(14)
O1W Ni1 N1 2_666 . 86.52(12)
O1W Ni1 N1 . . 93.48(13)
N5 Ni1 N1 . 2_666 88.83(14)
N5 Ni1 N1 2_666 2_666 91.17(14)
O1W Ni1 N1 2_666 2_666 93.48(13)
O1W Ni1 N1 . 2_666 86.52(12)
N1 Ni1 N1 . 2_666 180.0000(10)
C7 S1 C6 . . 87.2(2)
C1 N1 C5 . . 116.3(4)
C1 N1 Ni1 . . 122.2(3)
C5 N1 Ni1 . . 121.4(3)
C6 N2 N3 . . 112.5(4)
C7 N3 N2 . . 112.7(4)
C11 N4 C10 . . 116.8(4)
C13 N5 Ni1 . . 159.3(4)
Ni1 O1W H1WA . . 120.3
Ni1 O1W H1WB . . 121.7
H1WA O1W H1WB . . 107.7
N1 C1 C2 . . 124.1(4)
N1 C1 H1 . . 118.0
C2 C1 H1 . . 118.0
C1 C2 C3 . . 119.1(5)
C1 C2 H2 . . 120.5
C3 C2 H2 . . 120.5
C2 C3 C4 . . 117.8(4)
C2 C3 C6 . . 121.6(4)
C4 C3 C6 . . 120.5(4)
C5 C4 C3 . . 118.6(4)
C5 C4 H4 . . 120.7
C3 C4 H4 . . 120.7
N1 C5 C4 . . 124.0(4)
N1 C5 H5 . . 118.0
C4 C5 H5 . . 118.0
N2 C6 C3 . . 123.7(4)
N2 C6 S1 . . 113.8(3)
C3 C6 S1 . . 122.4(4)
N3 C7 C8 . . 123.5(4)
N3 C7 S1 . . 113.8(3)
C8 C7 S1 . . 122.7(4)
C12 C8 C9 . . 118.1(4)
C12 C8 C7 . . 121.8(4)
C9 C8 C7 . . 119.9(4)
C10 C9 C8 . . 118.5(5)
C10 C9 H9 . . 120.7
C8 C9 H9 . . 120.7
N4 C10 C9 . . 123.8(5)
N4 C10 H10 . . 118.1
C9 C10 H10 . . 118.1
N4 C11 C12 . . 124.1(5)
N4 C11 H11 . . 117.9
C12 C11 H11 . . 117.9
C8 C12 C11 . . 118.6(4)
C8 C12 H12 . . 120.7
C11 C12 H12 . . 120.7
N5 C13 S2 . . 179.7(4)
H2WA O2W H2WB . . 109.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 N5 . 2.072(4)
Ni1 N5 2_666 2.072(4)
Ni1 O1W 2_666 2.116(3)
Ni1 O1W . 2.116(3)
Ni1 N1 . 2.176(4)
Ni1 N1 2_666 2.176(4)
S1 C7 . 1.723(5)
S1 C6 . 1.724(5)
S2 C13 . 1.635(5)
N1 C1 . 1.325(6)
N1 C5 . 1.328(6)
N2 C6 . 1.304(6)
N2 N3 . 1.376(5)
N3 C7 . 1.303(6)
N4 C11 . 1.310(6)
N4 C10 . 1.340(6)
N5 C13 . 1.153(6)
O1W H1WA . 0.8510
O1W H1WB . 0.8497
C1 C2 . 1.371(6)
C1 H1 . 0.9300
C2 C3 . 1.371(6)
C2 H2 . 0.9300
C3 C4 . 1.385(6)
C3 C6 . 1.481(6)
C4 C5 . 1.374(6)
C4 H4 . 0.9300
C5 H5 . 0.9300
C7 C8 . 1.480(6)
C8 C12 . 1.380(6)
C8 C9 . 1.383(6)
C9 C10 . 1.373(7)
C9 H9 . 0.9300
C10 H10 . 0.9300
C11 C12 . 1.382(7)
C11 H11 . 0.9300
C12 H12 . 0.9300
O2W H2WA . 0.8456
O2W H2WB . 0.8472
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
O1W H1WB O2W . 0.85 1.91 2.762(5) 174.9
O2W H2WB N4 1_654 0.85 2.00 2.833(5) 169.5
O1W H1WA S2 1_455 0.85 2.47 3.303(3) 166.3
O2W H2WA S2 2_656 0.85 2.92 3.540(4) 132.2
