#------------------------------------------------------------------------------
#$Date: 2018-01-17 08:25:23 +0200 (Wed, 17 Jan 2018) $
#$Revision: 205307 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/09/2020905.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_2020905
loop_
_publ_author_name
'Liu, Feng-Yi'
'Zhou, Dong-Mei'
'Zhao, Xiao-Lan'
'Kou, Jun-Feng'
_publ_section_title
;
 Complexes of nickel(II) and copper(II) with 1,2,4-triazole-3-carboxylic
 acid and of cobalt(III) with 3-amino-1,2,4-triazole-5-carboxylic acid
;
_journal_coeditor_code           FP3038
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1010
_journal_page_last               1016
_journal_paper_doi               10.1107/S2053229617012943
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ni2 (C3 H N3 O2)2 (N H3)6], 4H2 O'
_chemical_formula_moiety         'C6 H20 N12 Ni2 O4, 4(H2 O)'
_chemical_formula_sum            'C6 H28 N12 Ni2 O8'
_chemical_formula_weight         513.78
_chemical_name_systematic
;Bis(μ-1,2,4-triazol-4-ide-3-carboxylato)-κ³N²,O:N¹;κ³N¹:N²,O-bis[triamminenickel(II)]
tetrahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_cell_angle_alpha                103.16(3)
_cell_angle_beta                 107.48(3)
_cell_angle_gamma                106.69(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1226(14)
_cell_length_b                   9.0134(18)
_cell_length_c                   9.1203(18)
_cell_measurement_reflns_used    4751
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      3.226
_cell_volume                     502.4(3)
_computing_cell_refinement       CrystalStructure
_computing_data_collection
;
CrystalStructure (Rigaku/MSC, 2006)
;
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material  SHELXTL
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku MM007-HF CCD (Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3780
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.226
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1767
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0418P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                1641
_reflns_number_total             1767
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fp3038sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        502.4(2)
_cod_database_code               2020905
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.643
loop_
_space_group_symop_operation_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_occupancy
Ni Ni1 0.15773(4) 0.70968(3) 0.19786(3) 0.01892(12) Uani d 1
N N1 0.2355(3) 0.60104(19) 0.0094(2) 0.0205(4) Uani d 1
N N2 0.1393(3) 0.4702(2) -0.1341(2) 0.0215(4) Uani d 1
N N3 0.0181(3) 0.8213(2) 0.0404(2) 0.0273(4) Uani d 1
H H3A -0.038(4) 0.752(3) -0.054(2) 0.033 Uiso d 1
H H3B -0.085(3) 0.844(3) 0.049(3) 0.033 Uiso d 1
H H3C 0.111(3) 0.907(2) 0.057(3) 0.033 Uiso d 1
N N4 0.4447(3) 0.6379(2) -0.1301(2) 0.0303(4) Uani d 1
N N5 0.1380(3) 0.8683(2) 0.3970(2) 0.0313(4) Uani d 1
H H5A 0.069(4) 0.823(3) 0.454(3) 0.038 Uiso d 1
H H5B 0.069(4) 0.926(3) 0.368(3) 0.038 Uiso d 1
H H5C 0.260(3) 0.937(3) 0.471(3) 0.038 Uiso d 1
N N6 0.3062(3) 0.5928(2) 0.3453(3) 0.0322(4) Uani d 1
H H6A 0.219(4) 0.511(3) 0.356(3) 0.039 Uiso d 1
H H6B 0.377(4) 0.553(3) 0.299(3) 0.039 Uiso d 1
H H6C 0.397(4) 0.659(3) 0.442(2) 0.039 Uiso d 1
O O1 0.7153(3) 0.94905(19) 0.1455(2) 0.0432(5) Uani d 1
O O2 0.4696(2) 0.88761(18) 0.25157(18) 0.0277(4) Uani d 1
O O3W 0.9480(3) 0.7541(2) 0.6383(2) 0.0469(5) Uani d 1
H H3WA 1.070(3) 0.820(3) 0.694(4) 0.070 Uiso d 1
H H3WB 0.847(3) 0.775(4) 0.652(4) 0.070 Uiso d 1
O O4W 0.6083(3) 0.8219(2) 0.6953(2) 0.0375(4) Uani d 1
H H4WA 0.579(5) 0.769(3) 0.754(3) 0.056 Uiso d 1
H H4WB 0.571(5) 0.902(3) 0.700(4) 0.056 Uiso d 1
C C1 0.4131(3) 0.6969(2) 0.0054(2) 0.0222(4) Uani d 1
C C2 0.2697(4) 0.4977(3) -0.2127(3) 0.0294(5) Uani d 1
H H2 0.2422 0.4265 -0.3150 0.035 Uiso calc 1
C C3 0.5471(3) 0.8585(3) 0.1445(3) 0.0262(5) 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'
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
N2 Ni1 N1 2_565 . 99.08(7)
N2 Ni1 N3 2_565 . 90.35(8)
N1 Ni1 N3 . . 86.20(8)
N2 Ni1 N5 2_565 . 93.72(9)
N1 Ni1 N5 . . 166.82(7)
N3 Ni1 N5 . . 90.62(8)
N2 Ni1 N6 2_565 . 90.82(8)
N1 Ni1 N6 . . 90.24(8)
N3 Ni1 N6 . . 176.38(8)
N5 Ni1 N6 . . 92.72(9)
N2 Ni1 O2 2_565 . 176.40(6)
N1 Ni1 O2 . . 77.32(7)
N3 Ni1 O2 . . 89.58(8)
N5 Ni1 O2 . . 89.88(8)
N6 Ni1 O2 . . 89.05(8)
C1 N1 N2 . . 106.05(17)
C1 N1 Ni1 . . 114.02(13)
N2 N1 Ni1 . . 138.46(13)
C2 N2 N1 . . 104.97(16)
C2 N2 Ni1 . 2_565 133.02(14)
N1 N2 Ni1 . 2_565 121.86(14)
Ni1 N3 H3A . . 106.7(17)
Ni1 N3 H3B . . 118.6(19)
H3A N3 H3B . . 101(3)
Ni1 N3 H3C . . 106.5(19)
H3A N3 H3C . . 117(3)
H3B N3 H3C . . 107(3)
C1 N4 C2 . . 101.33(18)
Ni1 N5 H5A . . 118.3(16)
Ni1 N5 H5B . . 112.4(18)
H5A N5 H5B . . 101(2)
Ni1 N5 H5C . . 113.6(17)
H5A N5 H5C . . 104(2)
H5B N5 H5C . . 106(2)
Ni1 N6 H6A . . 114.2(19)
Ni1 N6 H6B . . 107.5(19)
H6A N6 H6B . . 106(2)
Ni1 N6 H6C . . 113.8(18)
H6A N6 H6C . . 108(3)
H6B N6 H6C . . 106(2)
C3 O2 Ni1 . . 115.74(12)
H3WA O3W H3WB . . 120(3)
H4WA O4W H4WB . . 116(3)
N1 C1 N4 . . 113.83(17)
N1 C1 C3 . . 118.14(18)
N4 C1 C3 . . 127.96(19)
N2 C2 N4 . . 113.81(18)
N2 C2 H2 . . 123.1
N4 C2 H2 . . 123.1
O1 C3 O2 . . 126.26(18)
O1 C3 C1 . . 119.6(2)
O2 C3 C1 . . 114.12(18)
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_565 2.0745(19) y
Ni1 N1 . 2.0825(18) y
Ni1 N3 . 2.106(2) y
Ni1 N5 . 2.110(2) y
Ni1 N6 . 2.114(2) y
Ni1 O2 . 2.1651(18) y
N1 C1 . 1.327(3) ?
N1 N2 . 1.367(2) ?
N2 C2 . 1.337(3) ?
N2 Ni1 2_565 2.0745(19) ?
N3 H3A . 0.831(16) ?
N3 H3B . 0.833(17) ?
N3 H3C . 0.805(16) ?
N4 C1 . 1.341(3) ?
N4 C2 . 1.348(3) ?
N5 H5A . 0.904(17) ?
N5 H5B . 0.848(17) ?
N5 H5C . 0.863(17) ?
N6 H6A . 0.861(17) ?
N6 H6B . 0.857(17) ?
N6 H6C . 0.864(17) ?
O1 C3 . 1.237(3) ?
O2 C3 . 1.272(3) ?
O3W H3WA . 0.814(17) ?
O3W H3WB . 0.835(17) ?
O4W H4WA . 0.827(17) ?
O4W H4WB . 0.833(17) ?
C1 C3 . 1.508(3) ?
C2 H2 . 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
N3 H3B O1 1_455 0.833(17) 2.204(18) 3.010(3) 163(2)
N3 H3C O4W 2_676 0.805(16) 2.65(2) 3.307(3) 139(2)
N5 H5A O3W 1_455 0.904(17) 2.232(18) 3.123(3) 168(2)
N5 H5C O2 2_676 0.863(17) 2.473(19) 3.286(3) 157(2)
N6 H6A O3W 2_666 0.861(17) 2.367(19) 3.193(3) 161(3)
N6 H6C O4W . 0.864(17) 2.205(17) 3.067(3) 175(3)
O3W H3WA O1 2_776 0.814(17) 2.07(2) 2.805(3) 151(3)
O3W H3WB O4W . 0.835(17) 1.987(18) 2.821(3) 177(4)
O4W H4WA N4 1_556 0.827(17) 1.988(19) 2.802(3) 168(3)
O4W H4WB O2 2_676 0.833(17) 1.973(18) 2.795(2) 169(3)

_cod_database_fobs_code 2020905
