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
Liu, Feng-Yi; Zhou, Dong-Mei; Zhao, Xiao-Lan; Kou, Jun-Feng; Acta Crystallographica Section C 73 (2017) 1010–1016; doi:10.1107/S2053229617012943

data_2020905
_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(\m-1,2,4-triazol-4-ide-3-carboxylato)-\k^3^<i>N</i>^2^,<i>O</i>:<i>N</i>^1^;\k^3^<i>N</i>^1^:<i>N</i>^2^,<i>O</i>-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       '\w scans at fixed \c = 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/[\s^2^(Fo^2^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            fp3038sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        502.4(2)
_cod_database_code               2020905
_cod_database_fobs_code          2020905
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.643
_shelx_hkl_checksum              47185
_shelx_res_checksum              97725