#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/46/2004695.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_2004695
loop_
_publ_author_name
'Sen, A. K.'
'Dubey, S. N.'
'Squattrito, P. J.'
_publ_section_title
;Diaquabis(4-amino-3-methyl-4,5-dihydro-1H-1,2,4-triazole-5-thione)nickel(II)
 Nitrate: a Sulfur--Nitrogen Chelate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              865
_journal_page_last               868
_journal_paper_doi               10.1107/S010827019501496X
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ni (C3 H6 N4 S)2 (H2 O)2] (N O3)2'
_chemical_formula_moiety         '[Ni (C3 H6 N4 S)2 (H2 O)2] (N O3)2'
_chemical_formula_structural     '[Ni (C3 H6 N4 S)2 (H2 O)2] (N O3)2'
_chemical_formula_sum            'C6 H16 N10 Ni O8 S2'
_chemical_formula_weight         479.07
_chemical_name_systematic
;
Diaquabis(1-H-3-methyl-4-amine-5-thione-1,2,4-triazole)nickel(II) nitrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.683(2)
_cell_length_b                   8.888(2)
_cell_length_c                   12.653(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    296
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      17.8
_cell_volume                     1763.7(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1991)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'MITHRIL (Gilmore, 1983)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC-6S'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_sigmaI/netI    0.074
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1796
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        -0.70
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'emerald green'
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.166
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1052
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_obs          0.035
_refine_ls_shift/esd_max         0.056
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fₒ²/σ²(Fₒ²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0355
_refine_ls_wR_factor_obs         0.033
_reflns_number_observed          1052
_reflns_number_total             1796
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            bk1184.cif
_cod_data_source_block           squattrito
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 4F~o~^2^/\s^2^(F~o~^2^)' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
4F~o~^2^/\s^2^(F~o~^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1763.8(9)
_cod_original_formula_sum        'C6 H16 N10 O8 Ni S2 '
_cod_database_code               2004695
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2-y,1/2+z
'1/2+x,1/2-y,   -z'
'   -x,   +y,1/2-z'
'   -x,   -y,   -z'
1/2+x,1/2+y,1/2-z
'1/2-x,1/2+y,   +z'
'   +x,   -y,1/2+z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni(1) 0.0204(4) 0.0273(4) 0.0388(4) 0.0000 -0.0023(4) 0.0000
S(1) 0.0278(6) 0.0376(7) 0.0425(7) 0.0014(6) -0.0067(5) -0.0060(6)
O(1) 0.027(2) 0.039(2) 0.061(2) -0.007(2) -0.004(2) 0.015(2)
O(2) 0.067(3) 0.063(3) 0.072(3) -0.010(2) 0.003(2) -0.032(2)
O(3) 0.060(2) 0.036(2) 0.078(3) 0.015(2) -0.016(2) -0.015(2)
O(4) 0.069(3) 0.112(3) 0.098(3) 0.043(3) -0.039(3) -0.025(3)
N(1) 0.021(2) 0.034(2) 0.043(2) 0.001(2) -0.005(2) -0.004(2)
N(2) 0.021(2) 0.029(2) 0.036(2) 0.001(2) -0.001(2) 0.004(2)
N(3) 0.026(2) 0.048(2) 0.049(3) 0.009(2) 0.000(2) -0.002(2)
N(4) 0.022(2) 0.052(2) 0.050(2) 0.006(2) -0.010(2) -0.008(2)
N(5) 0.044(2) 0.039(2) 0.039(2) 0.001(2) 0.001(2) 0.002(2)
C(1) 0.025(2) 0.028(2) 0.041(3) 0.002(2) 0.001(2) 0.007(2)
C(2) 0.035(2) 0.040(3) 0.053(3) 0.007(2) -0.003(2) -0.009(3)
C(3) 0.025(2) 0.027(2) 0.041(3) 0.000(2) -0.006(2) 0.008(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ni(1) 1 0.33325(8) 0.75 0.0289(2) Uij
S(1) 1.12925(7) 0.3282(1) 0.85303(9) 0.0360(3) Uij
O(1) 1.0469(2) 0.4935(3) 0.6441(2) 0.0424(9) Uij
O(2) 0.5907(2) 0.4160(4) 0.6894(3) 0.068(1) Uij
O(3) 0.5972(2) 0.2130(3) 0.5980(3) 0.058(1) Uij
O(4) 0.4891(3) 0.3549(5) 0.5870(3) 0.093(2) Uij
N(1) 1.0617(2) 0.1713(4) 0.6503(3) 0.0327(10) Uij
N(2) 1.1496(2) 0.1573(4) 0.6752(3) 0.0288(10) Uij
N(3) 1.2831(2) 0.0905(4) 0.6772(3) 0.041(1) Uij
N(4) 1.2636(2) 0.1815(4) 0.7628(3) 0.041(1) Uij
N(5) 0.5585(2) 0.3289(5) 0.6263(3) 0.041(1) Uij
C(1) 1.2125(3) 0.0747(4) 0.6258(3) 0.032(1) Uij
C(2) 1.2018(3) -0.0181(5) 0.5297(4) 0.043(1) Uij
C(3) 1.1825(2) 0.2231(4) 0.7638(3) 0.031(1) Uij
H(1) 1.1040 0.5389 0.6467 0.0517 Uij
H(2) 1.0009 0.5578 0.6006 0.0539 Uij
H(3) 1.3171 0.2023 0.8119 0.0477 Uij
H(4) 1.0398 0.0629 0.6491 0.0411 Uij
H(5) 1.0682 0.2230 0.5716 0.0403 Uij
H(6) 1.1511 -0.0680 0.5258 0.0495 Uij
H(7) 1.2547 -0.0853 0.5269 0.0495 Uij
H(8) 1.1888 0.0739 0.4687 0.0518 Uij
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni 0.285 1.113 'International Tables'
S 0.110 0.124 'International Tables'
O 0.008 0.006 'International Tables'
N 0.004 0.003 'International Tables'
C 0.002 0.002 'International Tables'
H 0.000 0.000 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 3 -1
1 2 -2
2 1 2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S(1) Ni(1) S(1) 4_756 177.86(7) yes
S(1) Ni(1) O(1) ? 93.62(8) yes
S(1) Ni(1) O(1) 4_756 87.84(8) yes
S(1) Ni(1) N(1) ? 85.76(9) yes
S(1) Ni(1) N(1) 4_756 92.80(9) yes
S(1) Ni(1) O(1) ? 87.84(8) no
S(1) Ni(1) O(1) ? 93.62(8) no
S(1) Ni(1) N(1) ? 92.80(9) no
O(1) Ni(1) O(1) 4_756 94.0(2) yes
O(1) Ni(1) N(1) ? 85.50(10) yes
O(1) Ni(1) N(1) 4_756 173.50(10) yes
O(1) Ni(1) N(1) ? 173.50(10) no
N(1) Ni(1) N(1) 4_756 95.7(2) yes
Ni(1) S(1) C(3) ? 93.70(10) yes
Ni(1) N(1) N(2) ? 111.5(2) yes
N(1) N(2) C(1) ? 129.8(4) yes
N(1) N(2) C(3) ? 120.8(3) yes
C(1) N(2) C(3) ? 109.2(3) yes
N(4) N(3) C(1) ? 105.5(3) yes
N(3) N(4) C(3) ? 112.4(3) yes
O(2) N(5) O(3) ? 120.6(4) yes
O(2) N(5) O(4) ? 121.1(5) yes
O(3) N(5) O(4) ? 118.3(4) yes
N(2) C(1) N(3) ? 109.1(4) yes
N(2) C(1) C(2) ? 126.0(4) yes
N(3) C(1) C(2) ? 124.9(4) yes
S(1) C(3) N(2) ? 126.8(3) yes
S(1) C(3) N(4) ? 129.5(4) yes
N(2) C(3) N(4) ? 103.7(4) yes
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
Ni(1) S(1) ? 2.4110(10) yes
Ni(1) S(1) 4_756 2.4110(10) no
Ni(1) O(1) ? 2.089(3) yes
Ni(1) O(1) 4_756 2.089(3) no
Ni(1) N(1) ? 2.144(3) yes
Ni(1) N(1) 4_756 2.144(3) no
S(1) C(3) ? 1.686(4) yes
O(2) N(5) ? 1.223(4) yes
O(3) N(5) ? 1.248(4) yes
O(4) N(5) ? 1.218(5) yes
N(1) N(2) ? 1.419(4) yes
N(2) C(1) ? 1.380(5) yes
N(2) C(3) ? 1.365(5) yes
N(3) N(4) ? 1.386(5) yes
N(3) C(1) ? 1.292(5) yes
N(4) C(3) ? 1.325(5) yes
C(1) C(2) ? 1.479(6) yes
