#------------------------------------------------------------------------------
#$Date: 2020-01-17 07:16:26 +0200 (Fri, 17 Jan 2020) $
#$Revision: 246947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/19/2021955.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_2021955
loop_
_publ_author_name
'Cai, Hua'
'Li, Na'
'Zhang, Nan'
'Yang, Zhenyun'
'Cao, Jing'
'Lin, Yating'
'Min, Nan'
'Wang, Jia'
_publ_section_title
;
 Metal-directed supramolecular architectures based on the bifunctional
 ligand 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalic acid
;
_journal_coeditor_code           LF3111
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229620000248
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ni (C12 H6 N6 O4) (H2 O)2], 2H2 O'
_chemical_formula_sum            'C12 H14 N6 Ni O8'
_chemical_formula_weight         429.00
_chemical_name_systematic
'Poly[[diaqua[μ₄-2,5-bis(1H-1,2,4-triazol-1-yl)terephthalato]nickel(II)] dihydrate]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                65.416(2)
_cell_angle_beta                 88.890(2)
_cell_angle_gamma                69.788(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3533(11)
_cell_length_b                   7.9541(12)
_cell_length_c                   8.1396(12)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      2.78
_cell_volume                     401.92(10)
_computing_cell_refinement
;
SMART (Bruker, 2010)
;
_computing_data_collection
;
SMART (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2010)
;
_computing_publication_material
;
SHELXTL (Bruker, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2275
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_correction_T_min  0.7507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2010)
;
_exptl_crystal_colour            pale-blue
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.352
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0325
_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)+(0.0290P)²+0.3943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                1404
_reflns_number_total             1554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lf3111sup1.cif
_cod_data_source_block           160716b
_cod_database_code               2021955
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_symmetry_multiplicity
Ni Ni1 0.0000 0.0000 0.0000 0.01590(14) Uani d S 1 2
O O1 0.1783(3) 0.0696(3) 0.1277(2) 0.0238(4) Uani d . 1 1
O O2 -0.0129(3) 0.2317(3) 0.2726(3) 0.0421(6) Uani d . 1 1
O O3 -0.2351(3) 0.0953(3) 0.1293(2) 0.0275(4) Uani d . 1 1
H H3A -0.3420 0.1628 0.0559 0.041 Uiso d R 1 1
H H3B -0.1994 0.1532 0.1825 0.041 Uiso d R 1 1
O O4 0.6086(3) 0.6950(4) 0.0815(3) 0.0509(6) Uani d . 1 1
H H4A 0.6568 0.6149 0.1923 0.076 Uiso d R 1 1
H H4B 0.6589 0.7818 0.0281 0.076 Uiso d R 1 1
N N1 0.0940(3) 0.7165(3) 0.2172(3) 0.0201(5) Uani d . 1 1
N N2 0.2247(3) 0.4829(3) 0.5033(3) 0.0223(5) Uani d . 1 1
N N3 0.2541(3) 0.4001(3) 0.3823(3) 0.0187(4) Uani d . 1 1
C C1 0.1760(4) 0.5418(4) 0.2138(3) 0.0214(5) Uani d . 1 1
H H1 0.1789 0.5208 0.1094 0.026 Uiso calc R 1 1
C C2 0.1266(4) 0.6718(4) 0.3973(3) 0.0220(5) Uani d . 1 1
H H2 0.0829 0.7674 0.4414 0.026 Uiso calc R 1 1
C C3 0.3723(4) 0.1949(3) 0.4425(3) 0.0175(5) Uani d . 1 1
C C4 0.3308(4) 0.0778(4) 0.3714(3) 0.0187(5) Uani d . 1 1
C C5 0.4630(4) -0.1177(4) 0.4310(3) 0.0197(5) Uani d . 1 1
H H5 0.4397 -0.1983 0.3844 0.024 Uiso calc R 1 1
C C6 0.1472(4) 0.1363(4) 0.2464(3) 0.0203(5) Uani d . 1 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'
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
O1 Ni1 O1 . 2 180.0
O1 Ni1 N1 . 2_565 91.32(8)
O1 Ni1 N1 2 2_565 88.68(8)
O1 Ni1 N1 . 1_545 88.68(8)
O1 Ni1 N1 2 1_545 91.32(8)
N1 Ni1 N1 2_565 1_545 180.0
O1 Ni1 O3 . 2 87.59(7)
O1 Ni1 O3 2 2 92.41(7)
N1 Ni1 O3 2_565 2 89.88(8)
N1 Ni1 O3 1_545 2 90.12(8)
O1 Ni1 O3 . . 92.41(7)
O1 Ni1 O3 2 . 87.59(7)
N1 Ni1 O3 2_565 . 90.12(8)
N1 Ni1 O3 1_545 . 89.88(8)
O3 Ni1 O3 2 . 180.0
C6 O1 Ni1 . . 130.31(17)
Ni1 O3 H3A . . 111.9
Ni1 O3 H3B . . 105.5
H3A O3 H3B . . 116.5
H4A O4 H4B . . 116.3
C1 N1 C2 . . 103.4(2)
C1 N1 Ni1 . 1_565 128.76(17)
C2 N1 Ni1 . 1_565 126.28(16)
C2 N2 N3 . . 102.5(2)
C1 N3 N2 . . 109.73(19)
C1 N3 C3 . . 129.8(2)
N2 N3 C3 . . 120.12(19)
N1 C1 N3 . . 109.9(2)
N1 C1 H1 . . 125.0
N3 C1 H1 . . 125.0
N2 C2 N1 . . 114.5(2)
N2 C2 H2 . . 122.8
N1 C2 H2 . . 122.8
C5 C3 C4 2_656 . 120.8(2)
C5 C3 N3 2_656 . 117.1(2)
C4 C3 N3 . . 122.0(2)
C5 C4 C3 . . 117.4(2)
C5 C4 C6 . . 116.0(2)
C3 C4 C6 . . 126.4(2)
C3 C5 C4 2_656 . 121.8(2)
C3 C5 H5 2_656 . 119.1
C4 C5 H5 . . 119.1
O2 C6 O1 . . 126.8(2)
O2 C6 C4 . . 119.5(2)
O1 C6 C4 . . 113.6(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 O1 . 2.0347(16) y
Ni1 O1 2 2.0347(16) ?
Ni1 N1 2_565 2.084(2) y
Ni1 N1 1_545 2.084(2) ?
Ni1 O3 2 2.0878(18) ?
Ni1 O3 . 2.0879(18) y
O1 C6 . 1.265(3) ?
O2 C6 . 1.231(3) ?
O3 H3A . 0.8500 ?
O3 H3B . 0.8500 ?
O4 H4A . 0.8500 ?
O4 H4B . 0.8501 ?
N1 C1 . 1.322(3) ?
N1 C2 . 1.361(3) ?
N1 Ni1 1_565 2.084(2) ?
N2 C2 . 1.311(3) ?
N2 N3 . 1.372(3) ?
N3 C1 . 1.333(3) ?
N3 C3 . 1.425(3) ?
C1 H1 . 0.9300 ?
C2 H2 . 0.9300 ?
C3 C5 2_656 1.384(3) ?
C3 C4 . 1.395(3) ?
C4 C5 . 1.394(3) ?
C4 C6 . 1.517(3) ?
C5 C3 2_656 1.384(3) ?
C5 H5 . 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
_geom_hbond_publ_flag
O3 H3A O4 2_566 0.85 1.97 2.812(3) 171 yes
O3 H3B O2 . 0.85 1.95 2.749(3) 155 yes
O4 H4A N2 2_666 0.85 2.35 3.148(3) 157 yes
O4 H4B O1 2_665 0.85 2.03 2.852(3) 163 yes
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_4
_geom_torsion
O1 Ni1 O1 C6 2 . -5E1(10)
N1 Ni1 O1 C6 2_565 . 93.1(2)
N1 Ni1 O1 C6 1_545 . -86.9(2)
O3 Ni1 O1 C6 2 . -177.1(2)
O3 Ni1 O1 C6 . . 2.9(2)
C2 N2 N3 C1 . . 0.9(3)
C2 N2 N3 C3 . . 174.6(2)
C2 N1 C1 N3 . . -0.2(3)
Ni1 N1 C1 N3 1_565 . 166.03(16)
N2 N3 C1 N1 . . -0.5(3)
C3 N3 C1 N1 . . -173.3(2)
N3 N2 C2 N1 . . -1.1(3)
C1 N1 C2 N2 . . 0.8(3)
Ni1 N1 C2 N2 1_565 . -165.83(17)
C1 N3 C3 C5 . 2_656 134.2(3)
N2 N3 C3 C5 . 2_656 -38.0(3)
C1 N3 C3 C4 . . -42.7(4)
N2 N3 C3 C4 . . 145.1(2)
C5 C3 C4 C5 2_656 . -0.9(4)
N3 C3 C4 C5 . . 175.9(2)
C5 C3 C4 C6 2_656 . 173.8(2)
N3 C3 C4 C6 . . -9.4(4)
C3 C4 C5 C3 . 2_656 0.9(4)
C6 C4 C5 C3 . 2_656 -174.4(2)
Ni1 O1 C6 O2 . . -24.4(4)
Ni1 O1 C6 C4 . . 152.05(17)
C5 C4 C6 O2 . . 135.4(3)
C3 C4 C6 O2 . . -39.5(4)
C5 C4 C6 O1 . . -41.4(3)
C3 C4 C6 O1 . . 143.8(3)

_cod_database_fobs_code 2021955
