#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/41/2224111.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_2224111
loop_
_publ_author_name
'Zhang, Yun-Liang'
'Liu, Ti-Lou'
'Sun, Shuang-Jiao'
_publ_section_title
;
 Tetraaquabis[3-(3-pyridyl)-5-(4-pyridyl)-1,2,4-triazolido]nickel(II)
 dihydrate
;
_journal_coeditor_code           BG2306
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1590
_journal_paper_doi               10.1107/S1600536809047102
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C12 H8 N5)2 (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C24 H24 N10 Ni O4, 2(H2 O)'
_chemical_formula_sum            'C24 H28 N10 Ni O6'
_chemical_formula_weight         611.25
_chemical_name_systematic
;
Tetraaquabis[3-(3-pyridyl)-5-(4-pyridyl)-1,2,4-triazolido]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                90.70(3)
_cell_angle_beta                 104.96(3)
_cell_angle_gamma                96.47(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2240(16)
_cell_length_b                   9.1990(18)
_cell_length_c                   9.3850(19)
_cell_measurement_reflns_used    2567
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      1.5
_cell_volume                     680.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4042
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         3.10
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.9433
_exptl_absorpt_correction_T_min  0.8663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1998)'
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.847
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0523
_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)+(0.0912P)²+0.8P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                2258
_reflns_number_total             2437
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg2306.cif
_cod_data_source_block           I
_cod_original_cell_volume        680.9(2)
_cod_database_code               2224111
_cod_database_fobs_code          2224111
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.0000 0.5000 0.5000 0.0217(2) Uani d S 1 . .
C C1 0.2767(4) 0.3042(4) 0.6004(4) 0.0291(7) Uani d . 1 . .
H H1 0.3256 0.3814 0.6683 0.035 Uiso calc R 1 . .
C C2 0.3637(5) 0.1847(4) 0.5989(4) 0.0347(8) Uani d . 1 . .
H H2 0.4679 0.1806 0.6663 0.042 Uiso calc R 1 . .
C C3 0.2938(4) 0.0712(4) 0.4959(4) 0.0299(8) Uani d . 1 . .
H H3 0.3508 -0.0100 0.4928 0.036 Uiso calc R 1 . .
C C4 0.1385(4) 0.0799(3) 0.3976(3) 0.0211(6) Uani d . 1 . .
C C5 0.0578(4) 0.2022(3) 0.4086(3) 0.0235(7) Uani d . 1 . .
H H5A -0.0480 0.2078 0.3440 0.028 Uiso calc R 1 . .
C C6 0.0580(4) -0.0361(3) 0.2837(3) 0.0214(6) Uani d . 1 . .
C C7 -0.1047(4) -0.1550(3) 0.1011(3) 0.0231(7) Uani d . 1 . .
C C8 -0.2408(4) -0.2007(4) -0.0305(4) 0.0270(7) Uani d . 1 . .
C C9 -0.2480(5) -0.3324(4) -0.1091(4) 0.0382(9) Uani d . 1 . .
H H9A -0.1643 -0.3938 -0.0785 0.046 Uiso calc R 1 . .
C C10 -0.3798(6) -0.3703(5) -0.2319(5) 0.0480(11) Uani d . 1 . .
H H10A -0.3804 -0.4570 -0.2841 0.058 Uiso calc R 1 . .
C C11 -0.4989(5) -0.1649(5) -0.2061(4) 0.0428(10) Uani d . 1 . .
H H11A -0.5863 -0.1074 -0.2379 0.051 Uiso calc R 1 . .
C C12 -0.3699(5) -0.1149(4) -0.0848(4) 0.0363(8) Uani d . 1 . .
H H12A -0.3689 -0.0242 -0.0395 0.044 Uiso calc R 1 . .
N N1 0.1255(4) 0.3132(3) 0.5083(3) 0.0253(6) Uani d . 1 . .
N N2 -0.0797(3) -0.0233(3) 0.1726(3) 0.0243(6) Uani d . 1 . .
N N3 0.1159(4) -0.1651(3) 0.2840(3) 0.0263(6) Uani d . 1 . .
N N4 0.0088(4) -0.2439(3) 0.1640(3) 0.0276(6) Uani d . 1 . .
N N5 -0.5067(4) -0.2906(4) -0.2810(4) 0.0442(9) Uani d . 1 . .
O O1 0.2181(3) 0.6258(3) 0.4839(3) 0.0321(6) Uani d D 1 . .
O O2 0.0796(4) 0.5155(3) 0.7297(3) 0.0353(6) Uani d D 1 . .
O O3 0.8076(4) 0.2539(3) 0.0662(3) 0.0405(7) Uani d D 1 . .
H H1A 0.302(4) 0.650(5) 0.555(3) 0.059(15) Uiso d D 1 . .
H H2A 0.122(5) 0.580(3) 0.796(4) 0.043(12) Uiso d D 1 . .
H H3A 0.850(8) 0.182(5) 0.103(6) 0.12(3) Uiso d D 1 . .
H H1B 0.210(5) 0.695(3) 0.427(4) 0.043(12) Uiso d D 1 . .
H H2B 0.051(6) 0.440(3) 0.771(4) 0.049(13) Uiso d D 1 . .
H H3B 0.836(7) 0.274(5) -0.009(4) 0.069(17) Uiso d 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'
Ni Ni 0.3393 1.1124 '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'
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
O1 Ni1 O1 2_566 . 180.00(15) ?
O1 Ni1 O2 2_566 . 88.62(11) ?
O1 Ni1 O2 . . 91.38(11) ?
O1 Ni1 O2 2_566 2_566 91.38(11) ?
O1 Ni1 O2 . 2_566 88.62(11) ?
O2 Ni1 O2 . 2_566 180.0 ?
O1 Ni1 N1 2_566 . 90.86(11) ?
O1 Ni1 N1 . . 89.14(11) ?
O2 Ni1 N1 . . 87.82(11) ?
O2 Ni1 N1 2_566 . 92.18(11) ?
O1 Ni1 N1 2_566 2_566 89.14(11) ?
O1 Ni1 N1 . 2_566 90.86(11) ?
O2 Ni1 N1 . 2_566 92.18(11) ?
O2 Ni1 N1 2_566 2_566 87.82(11) ?
N1 Ni1 N1 . 2_566 180.0000(10) ?
N1 C1 C2 . . 122.5(3) ?
N1 C1 H1 . . 118.7 ?
C2 C1 H1 . . 118.7 ?
C1 C2 C3 . . 119.1(3) ?
C1 C2 H2 . . 120.5 ?
C3 C2 H2 . . 120.5 ?
C4 C3 C2 . . 119.2(3) ?
C4 C3 H3 . . 120.4 ?
C2 C3 H3 . . 120.4 ?
C3 C4 C5 . . 118.1(3) ?
C3 C4 C6 . . 122.0(3) ?
C5 C4 C6 . . 119.9(3) ?
N1 C5 C4 . . 122.9(3) ?
N1 C5 H5A . . 118.5 ?
C4 C5 H5A . . 118.5 ?
N3 C6 N2 . . 114.0(3) ?
N3 C6 C4 . . 121.9(3) ?
N2 C6 C4 . . 124.1(3) ?
N4 C7 N2 . . 113.1(3) ?
N4 C7 C8 . . 121.9(3) ?
N2 C7 C8 . . 125.0(3) ?
C12 C8 C9 . . 116.5(3) ?
C12 C8 C7 . . 121.6(3) ?
C9 C8 C7 . . 121.9(3) ?
C10 C9 C8 . . 119.4(4) ?
C10 C9 H9A . . 120.3 ?
C8 C9 H9A . . 120.3 ?
N5 C10 C9 . . 124.1(4) ?
N5 C10 H10A . . 118.0 ?
C9 C10 H10A . . 118.0 ?
N5 C11 C12 . . 124.1(4) ?
N5 C11 H11A . . 117.9 ?
C12 C11 H11A . . 117.9 ?
C11 C12 C8 . . 119.5(4) ?
C11 C12 H12A . . 120.2 ?
C8 C12 H12A . . 120.2 ?
C1 N1 C5 . . 118.1(3) ?
C1 N1 Ni1 . . 122.7(2) ?
C5 N1 Ni1 . . 118.9(2) ?
C6 N2 C7 . . 101.9(3) ?
C6 N3 N4 . . 105.3(3) ?
C7 N4 N3 . . 105.8(3) ?
C10 N5 C11 . . 116.3(3) ?
Ni1 O1 H1A . . 125(3) ?
Ni1 O1 H1B . . 119(3) ?
H1A O1 H1B . . 107(3) ?
Ni1 O2 H2A . . 138(3) ?
Ni1 O2 H2B . . 114(3) ?
H2A O2 H2B . . 107(3) ?
H3A O3 H3B . . 111(3) ?
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 O1 2_566 2.063(3) ?
Ni1 O1 . 2.063(3) ?
Ni1 O2 . 2.083(2) ?
Ni1 O2 2_566 2.083(2) ?
Ni1 N1 . 2.094(3) ?
Ni1 N1 2_566 2.094(3) ?
C1 N1 . 1.330(4) ?
C1 C2 . 1.379(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.381(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.380(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(4) ?
C4 C6 . 1.472(4) ?
C5 N1 . 1.345(4) ?
C5 H5A . 0.9300 ?
C6 N3 . 1.327(4) ?
C6 N2 . 1.344(4) ?
C7 N4 . 1.337(4) ?
C7 N2 . 1.347(4) ?
C7 C8 . 1.456(5) ?
C8 C12 . 1.389(5) ?
C8 C9 . 1.398(5) ?
C9 C10 . 1.373(6) ?
C9 H9A . 0.9300 ?
C10 N5 . 1.331(6) ?
C10 H10A . 0.9300 ?
C11 N5 . 1.333(5) ?
C11 C12 . 1.373(5) ?
C11 H11A . 0.9300 ?
C12 H12A . 0.9300 ?
N3 N4 . 1.376(4) ?
O1 H1A . 0.836(19) ?
O1 H1B . 0.830(18) ?
O2 H2A . 0.828(18) ?
O2 H2B . 0.836(19) ?
O3 H3A . 0.82(5) ?
O3 H3B . 0.81(4) ?
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 H1A N5 1_666 0.83(2) 1.92(3) 2.751(4) 179(3)
O1 H1B N3 1_565 0.83(3) 1.95(3) 2.750(4) 162(3)
O2 H2A O3 2_666 0.83(3) 1.93(3) 2.751(4) 171(3)
O2 H2B N4 2_556 0.84(3) 1.96(3) 2.791(4) 169(3)
O3 H3A N2 1_655 0.82(5) 2.10(5) 2.911(4) 170(3)
O3 H3B N4 2_655 0.82(4) 2.20(5) 2.944(4) 151(3)
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
N1 C1 C2 C3 . . . . 1.6(6) ?
C1 C2 C3 C4 . . . . -0.3(5) ?
C2 C3 C4 C5 . . . . -1.0(5) ?
C2 C3 C4 C6 . . . . 179.1(3) ?
C3 C4 C5 N1 . . . . 1.3(5) ?
C6 C4 C5 N1 . . . . -178.8(3) ?
C3 C4 C6 N3 . . . . 11.2(5) ?
C5 C4 C6 N3 . . . . -168.7(3) ?
C3 C4 C6 N2 . . . . -169.8(3) ?
C5 C4 C6 N2 . . . . 10.3(5) ?
N4 C7 C8 C12 . . . . 172.1(3) ?
N2 C7 C8 C12 . . . . -7.2(5) ?
N4 C7 C8 C9 . . . . -8.3(5) ?
N2 C7 C8 C9 . . . . 172.4(3) ?
C12 C8 C9 C10 . . . . -0.7(6) ?
C7 C8 C9 C10 . . . . 179.7(4) ?
C8 C9 C10 N5 . . . . -1.7(7) ?
N5 C11 C12 C8 . . . . -2.7(6) ?
C9 C8 C12 C11 . . . . 2.8(5) ?
C7 C8 C12 C11 . . . . -177.6(3) ?
C2 C1 N1 C5 . . . . -1.3(5) ?
C2 C1 N1 Ni1 . . . . -175.7(3) ?
C4 C5 N1 C1 . . . . -0.1(5) ?
C4 C5 N1 Ni1 . . . . 174.5(2) ?
O1 Ni1 N1 C1 2_566 . . . -129.6(3) ?
O1 Ni1 N1 C1 . . . . 50.4(3) ?
O2 Ni1 N1 C1 . . . . -41.0(3) ?
O2 Ni1 N1 C1 2_566 . . . 139.0(3) ?
O1 Ni1 N1 C5 2_566 . . . 56.0(2) ?
O1 Ni1 N1 C5 . . . . -124.0(2) ?
O2 Ni1 N1 C5 . . . . 144.6(2) ?
O2 Ni1 N1 C5 2_566 . . . -35.4(2) ?
N3 C6 N2 C7 . . . . -0.4(4) ?
C4 C6 N2 C7 . . . . -179.4(3) ?
N4 C7 N2 C6 . . . . 0.5(4) ?
C8 C7 N2 C6 . . . . 179.8(3) ?
N2 C6 N3 N4 . . . . 0.1(4) ?
C4 C6 N3 N4 . . . . 179.2(3) ?
N2 C7 N4 N3 . . . . -0.5(4) ?
C8 C7 N4 N3 . . . . -179.8(3) ?
C6 N3 N4 C7 . . . . 0.2(3) ?
C9 C10 N5 C11 . . . . 2.0(6) ?
C12 C11 N5 C10 . . . . 0.2(6) ?
