#------------------------------------------------------------------------------
#$Date: 2016-02-04 03:14:23 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175649 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/48/4344814.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4344814
loop_
_publ_author_name
'Xu, Caixia'
'Zhang, Jianguo'
'Yin, Xin'
'Cheng, Zhenxuan'
_publ_section_title
;
 Structural Diversity and Properties of M(II) Coordination Compounds
 Constructed by 3-Hydrazino-4-amino-1,2,4-triazole Dihydrochloride as
 Starting Material.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              322
_journal_paper_doi               10.1021/acs.inorgchem.5b02434
_journal_volume                  55
_journal_year                    2015
_chemical_formula_sum            'C4 H30 Cl4 N12 Ni2 O16'
_chemical_formula_weight         761.62
_chemical_name_systematic
; 
 ? 
;
_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                71.1180(10)
_cell_angle_beta                 72.4340(10)
_cell_angle_gamma                86.012(2)
_cell_formula_units_Z            1
_cell_length_a                   7.6985(5)
_cell_length_b                   8.6832(6)
_cell_length_c                   10.9672(11)
_cell_measurement_reflns_used    1973
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4780
_cell_measurement_theta_min      3.4600
_cell_volume                     661.01(9)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4021
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.5790
_exptl_absorpt_correction_T_min  0.4792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0413
_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)+(0.0477P)²+0.3038P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                2088
_reflns_number_total             2327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02434_si_009.cif
_cod_data_source_block           141022k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4344814
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.39738(5) 0.28629(5) 0.49901(4) 0.01329(19) Uani 1 1 d .
Cl1 Cl 0.30503(12) 0.16237(10) 0.35304(9) 0.0195(2) Uani 1 1 d .
Cl2 Cl 0.12838(12) 0.69729(10) 0.00992(9) 0.0227(3) Uani 1 1 d .
N1 N 0.5110(4) 0.5039(3) 0.6589(3) 0.0155(6) Uani 1 1 d .
N2 N 0.4554(4) 0.3644(3) 0.6412(3) 0.0152(6) Uani 1 1 d .
N3 N 0.4342(4) 0.3129(3) 0.8538(3) 0.0152(6) Uani 1 1 d .
N4 N 0.3543(4) 0.1007(4) 0.7843(3) 0.0231(7) Uani 1 1 d .
H4A H 0.2540 0.0752 0.8562 0.028 Uiso 1 1 calc R
H4B H 0.4418 0.0324 0.8056 0.028 Uiso 1 1 calc R
N5 N 0.3138(4) 0.0755(3) 0.6733(3) 0.0179(7) Uani 1 1 d .
H5A H 0.1933 0.0561 0.6943 0.021 Uiso 1 1 calc R
H5B H 0.3725 -0.0118 0.6558 0.021 Uiso 1 1 calc R
N6 N 0.3796(4) 0.2234(4) 0.9930(3) 0.0210(7) Uani 1 1 d .
H6A H 0.2900 0.2743 1.0362 0.032 Uiso 1 1 d R
H6B H 0.4741 0.2165 1.0251 0.032 Uiso 1 1 d R
O1 O 0.2087(5) 0.8318(3) 0.0279(3) 0.0413(8) Uani 1 1 d .
O2 O 0.1176(5) 0.7424(4) -0.1245(3) 0.0489(9) Uani 1 1 d .
O3 O 0.2428(4) 0.5595(4) 0.0365(3) 0.0440(8) Uani 1 1 d .
O4 O -0.0471(4) 0.6559(4) 0.1047(3) 0.0464(9) Uani 1 1 d .
O5 O 0.1339(3) 0.3676(3) 0.5460(2) 0.0204(6) Uani 1 1 d .
H5E H 0.1096 0.4443 0.5803 0.025 Uiso 1 1 d R
H5F H 0.0639 0.2862 0.5981 0.025 Uiso 1 1 d R
O6 O 0.6505(3) 0.1836(3) 0.4524(2) 0.0180(5) Uani 1 1 d .
H6E H 0.7484 0.2415 0.4196 0.022 Uiso 1 1 d R
H6F H 0.6702 0.0917 0.5040 0.022 Uiso 1 1 d R
O7 O 0.0535(3) 0.6167(3) 0.6594(3) 0.0229(6) Uani 1 1 d .
H7C H 0.0533 0.5569 0.7380 0.027 Uiso 1 1 d R
H7D H -0.0454 0.6678 0.6643 0.027 Uiso 1 1 d R
O8 O 0.0962(4) 0.8981(3) 0.2818(3) 0.0352(7) Uani 1 1 d .
H8C H 0.1411 0.8883 0.2038 0.042 Uiso 1 1 d R
H8D H 0.1601 0.9686 0.2894 0.042 Uiso 1 1 d R
C1 C 0.4099(5) 0.2538(4) 0.7603(3) 0.0151(7) Uani 1 1 d .
C2 C 0.4950(5) 0.4690(4) 0.7863(3) 0.0171(8) Uani 1 1 d .
H2 H 0.5215 0.5411 0.8256 0.021 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ni1 N2 95.74(11) 2_666 .
N1 Ni1 O5 92.43(10) 2_666 .
N2 Ni1 O5 91.53(11) . .
N1 Ni1 O6 91.22(10) 2_666 .
N2 Ni1 O6 92.42(10) . .
O5 Ni1 O6 174.33(9) . .
N1 Ni1 N5 174.93(11) 2_666 .
N2 Ni1 N5 79.33(11) . .
O5 Ni1 N5 88.91(11) . .
O6 Ni1 N5 87.83(11) . .
N1 Ni1 Cl1 91.59(8) 2_666 .
N2 Ni1 Cl1 172.51(8) . .
O5 Ni1 Cl1 86.66(7) . .
O6 Ni1 Cl1 88.91(7) . .
N5 Ni1 Cl1 93.37(8) . .
O4 Cl2 O2 110.8(2) . .
O4 Cl2 O3 108.44(19) . .
O2 Cl2 O3 110.9(2) . .
O4 Cl2 O1 109.6(2) . .
O2 Cl2 O1 109.38(18) . .
O3 Cl2 O1 107.65(19) . .
C2 N1 N2 107.1(3) . .
C2 N1 Ni1 130.6(2) . 2_666
N2 N1 Ni1 122.3(2) . 2_666
C1 N2 N1 106.4(3) . .
C1 N2 Ni1 111.7(2) . .
N1 N2 Ni1 141.4(2) . .
C1 N3 C2 105.5(3) . .
C1 N3 N6 122.1(3) . .
C2 N3 N6 132.0(3) . .
C1 N4 N5 113.9(3) . .
C1 N4 H4A 108.8 . .
N5 N4 H4A 108.8 . .
C1 N4 H4B 108.8 . .
N5 N4 H4B 108.8 . .
H4A N4 H4B 107.7 . .
N4 N5 Ni1 109.80(19) . .
N4 N5 H5A 109.7 . .
Ni1 N5 H5A 109.7 . .
N4 N5 H5B 109.7 . .
Ni1 N5 H5B 109.7 . .
H5A N5 H5B 108.2 . .
N3 N6 H6A 109.3 . .
N3 N6 H6B 109.1 . .
H6A N6 H6B 109.5 . .
Ni1 O5 H5E 119.9 . .
Ni1 O5 H5F 107.9 . .
H5E O5 H5F 108.4 . .
Ni1 O6 H6E 121.4 . .
Ni1 O6 H6F 119.9 . .
H6E O6 H6F 108.5 . .
H7C O7 H7D 109.3 . .
H8C O8 H8D 108.7 . .
N2 C1 N4 124.4(3) . .
N2 C1 N3 110.5(3) . .
N4 C1 N3 125.0(3) . .
N1 C2 N3 110.5(3) . .
N1 C2 H2 124.8 . .
N3 C2 H2 124.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.053(3) 2_666
Ni1 N2 2.059(3) .
Ni1 O5 2.070(2) .
Ni1 O6 2.074(2) .
Ni1 N5 2.139(3) .
Ni1 Cl1 2.4768(9) .
Cl2 O4 1.419(3) .
Cl2 O2 1.425(3) .
Cl2 O3 1.440(3) .
Cl2 O1 1.452(3) .
N1 C2 1.298(4) .
N1 N2 1.401(4) .
N1 Ni1 2.053(3) 2_666
N2 C1 1.308(4) .
N3 C1 1.350(5) .
N3 C2 1.354(4) .
N3 N6 1.415(4) .
N4 C1 1.343(4) .
N4 N5 1.428(4) .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
N5 H5A 0.9000 .
N5 H5B 0.9000 .
N6 H6A 0.8900 .
N6 H6B 0.8900 .
O5 H5E 0.8500 .
O5 H5F 0.8501 .
O6 H6E 0.8499 .
O6 H6F 0.8500 .
O7 H7C 0.8499 .
O7 H7D 0.8500 .
O8 H8C 0.8500 .
O8 H8D 0.8501 .
C2 H2 0.9300 .
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
_geom_torsion_site_symmetry_1
C2 N1 N2 C1 -0.2(4) .
Ni1 N1 N2 C1 178.6(2) 2_666
C2 N1 N2 Ni1 170.9(3) .
Ni1 N1 N2 Ni1 -10.2(5) 2_666
N1 Ni1 N2 C1 179.5(2) 2_666
O5 Ni1 N2 C1 86.9(2) .
O6 Ni1 N2 C1 -89.0(2) .
N5 Ni1 N2 C1 -1.7(2) .
Cl1 Ni1 N2 C1 11.1(8) .
N1 Ni1 N2 N1 8.7(4) 2_666
O5 Ni1 N2 N1 -83.9(3) .
O6 Ni1 N2 N1 100.2(3) .
N5 Ni1 N2 N1 -172.5(4) .
Cl1 Ni1 N2 N1 -159.8(4) .
C1 N4 N5 Ni1 8.6(4) .
N1 Ni1 N5 N4 9.9(14) 2_666
N2 Ni1 N5 N4 -3.7(2) .
O5 Ni1 N5 N4 -95.5(2) .
O6 Ni1 N5 N4 89.1(2) .
Cl1 Ni1 N5 N4 177.9(2) .
N1 N2 C1 N4 -177.9(3) .
Ni1 N2 C1 N4 8.0(4) .
N1 N2 C1 N3 -0.5(4) .
Ni1 N2 C1 N3 -174.6(2) .
N5 N4 C1 N2 -11.7(5) .
N5 N4 C1 N3 171.3(3) .
C2 N3 C1 N2 1.0(4) .
N6 N3 C1 N2 174.1(3) .
C2 N3 C1 N4 178.4(3) .
N6 N3 C1 N4 -8.6(5) .
N2 N1 C2 N3 0.9(4) .
Ni1 N1 C2 N3 -177.8(2) 2_666
C1 N3 C2 N1 -1.2(4) .
N6 N3 C2 N1 -173.3(3) .
