#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/92/1529226.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_1529226
loop_
_publ_author_name
'Golovnev, Nikolay'
'Molokeev, Maxim'
'Vereshchagin, Sergey'
'Atuchin, Victor'
'Sidorenko, Maxim'
'Dmitrushkov, Michael'
_publ_section_title
;
 Crystal structure and properties of the precursor [Ni(H2O)6](HTBA)2.2H2O
 and the complexes M(HTBA)2(H2O)2 (M=Ni, Co, Fe)
;
_journal_issue                   0
_journal_name_full               Polyhedron
_journal_page_first              71
_journal_paper_doi               10.1016/j.poly.2013.12.021
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety
;
2(C4 H3 N2 O2 S), H12 Ni O6, 4(H2 O)
;
_chemical_formula_sum            'C8 H26 N4 Ni O14 S2'
_chemical_formula_weight         525.16
_chemical_name_systematic
; 
Hexaaquanickel(II) bis(2-thiobarbiturate) dihydrate 
;
_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                101.278(8)
_cell_angle_beta                 96.786(8)
_cell_angle_gamma                108.066(8)
_cell_formula_units_Z            1
_cell_length_a                   7.389(6)
_cell_length_b                   7.631(6)
_cell_length_c                   10.082(8)
_cell_measurement_reflns_used    1833
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.90
_cell_volume                     520.2(7)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5052
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.81
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.39(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   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0467
_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)+(0.1083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                2188
_reflns_number_total             2698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NiHTBA2H2O10.cif
_cod_data_source_block           a
_cod_original_sg_symbol_Hall
;
-P 1
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1529226
_cod_database_fobs_code          1529226
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.0000 0.0233(2) Uani 1 2 d S . .
S S 0.00281(13) -0.00136(13) 0.27448(9) 0.0346(3) Uani 1 1 d . . .
O1 O 0.5811(4) 0.1966(3) 0.6358(3) 0.0346(6) Uani 1 1 d . . .
O2 O 0.1992(4) 0.5930(3) 0.6366(3) 0.0333(6) Uani 1 1 d . . .
N1 N 0.1282(4) 0.3171(4) 0.4754(3) 0.0270(6) Uani 1 1 d . . .
H1 H 0.0272 0.3380 0.4405 0.032 Uiso 1 1 calc R . .
N3 N 0.3150(4) 0.1284(4) 0.4729(3) 0.0270(6) Uani 1 1 d . . .
H3 H 0.3377 0.0280 0.4352 0.032 Uiso 1 1 calc R . .
C2 C 0.1565(5) 0.1566(4) 0.4135(3) 0.0255(6) Uani 1 1 d . . .
C4 C 0.4444(5) 0.2495(5) 0.5905(3) 0.0260(6) Uani 1 1 d . . .
C6 C 0.2494(5) 0.4510(4) 0.5911(3) 0.0264(6) Uani 1 1 d . . .
C5 C 0.4115(5) 0.4152(5) 0.6475(3) 0.0285(7) Uani 1 1 d . . .
H5 H 0.4982 0.5027 0.7238 0.034 Uiso 1 1 calc R . .
O3 O 0.4928(4) 0.2576(4) -0.0191(3) 0.0405(7) Uani 1 1 d D . .
H3A H 0.590(5) 0.367(5) 0.003(5) 0.049 Uiso 1 1 d D . .
H3B H 0.388(5) 0.284(7) -0.018(5) 0.049 Uiso 1 1 d D . .
O4 O 0.9166(4) 0.4614(4) 0.7954(3) 0.0439(7) Uani 1 1 d D . .
H4A H 0.820(5) 0.383(6) 0.733(4) 0.053 Uiso 1 1 d D . .
H4B H 0.995(6) 0.517(7) 0.748(5) 0.053 Uiso 1 1 d D . .
O5 O 0.5295(4) 0.0835(4) 0.2079(3) 0.0341(6) Uani 1 1 d D . .
H5A H 0.512(6) -0.004(5) 0.252(4) 0.041 Uiso 1 1 d D . .
H5B H 0.625(5) 0.181(5) 0.253(4) 0.041 Uiso 1 1 d D . .
O6 O 0.2059(4) -0.1061(4) -0.0096(3) 0.0364(6) Uani 1 1 d D . .
H6A H 0.139(6) -0.110(6) -0.086(3) 0.044 Uiso 1 1 d D . .
H6B H 0.168(6) -0.067(6) 0.064(3) 0.044 Uiso 1 1 d D . .
O7 O 0.7975(4) 0.5959(4) 0.0225(3) 0.0401(6) Uani 1 1 d D . .
H7A H 0.892(5) 0.622(7) 0.094(4) 0.048 Uiso 1 1 d D . .
H7B H 0.840(7) 0.570(7) -0.051(4) 0.048 Uiso 1 1 d D . .
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'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 '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'
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
O3 Ni1 O3 180.0 . 2_655
O3 Ni1 O5 90.69(12) . .
O3 Ni1 O5 89.31(12) 2_655 .
O3 Ni1 O5 89.31(12) . 2_655
O3 Ni1 O5 90.69(12) 2_655 2_655
O5 Ni1 O5 180.00(16) . 2_655
O3 Ni1 O6 87.41(11) . 2_655
O3 Ni1 O6 92.59(11) 2_655 2_655
O5 Ni1 O6 92.42(11) . 2_655
O5 Ni1 O6 87.58(11) 2_655 2_655
O3 Ni1 O6 92.59(11) . .
O3 Ni1 O6 87.41(11) 2_655 .
O5 Ni1 O6 87.59(11) . .
O5 Ni1 O6 92.41(11) 2_655 .
O6 Ni1 O6 180.0 2_655 .
C2 N1 C6 125.1(3) . .
C2 N1 H1 117.5 . .
C6 N1 H1 117.5 . .
C2 N3 C4 124.8(3) . .
C2 N3 H3 117.6 . .
C4 N3 H3 117.6 . .
N3 C2 N1 115.4(3) . .
N3 C2 S 121.8(2) . .
N1 C2 S 122.8(2) . .
O1 C4 C5 126.3(3) . .
O1 C4 N3 116.4(3) . .
C5 C4 N3 117.3(3) . .
O2 C6 N1 116.6(3) . .
O2 C6 C5 126.4(3) . .
N1 C6 C5 117.0(3) . .
C4 C5 C6 120.3(3) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
Ni1 O3 H3A 128(3) . .
Ni1 O3 H3B 121(3) . .
H3A O3 H3B 107(4) . .
H4A O4 H4B 103(5) . .
Ni1 O5 H5A 117(3) . .
Ni1 O5 H5B 119(3) . .
H5A O5 H5B 110(4) . .
Ni1 O6 H6A 113(3) . .
Ni1 O6 H6B 115(3) . .
H6A O6 H6B 117(4) . .
H7A O7 H7B 108(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 2.028(3) .
Ni1 O3 2.028(3) 2_655
Ni1 O5 2.032(3) .
Ni1 O5 2.032(3) 2_655
Ni1 O6 2.053(3) 2_655
Ni1 O6 2.053(3) .
S C2 1.680(3) .
O1 C4 1.268(4) .
O2 C6 1.272(4) .
N1 C2 1.351(4) .
N1 C6 1.387(4) .
N1 H1 0.8600 .
N3 C2 1.348(4) .
N3 C4 1.389(4) .
N3 H3 0.8600 .
C4 C5 1.389(5) .
C6 C5 1.391(4) .
C5 H5 0.9300 .
O3 H3A 0.88(3) .
O3 H3B 0.86(3) .
O4 H4A 0.86(3) .
O4 H4B 0.86(3) .
O5 H5A 0.86(3) .
O5 H5B 0.85(3) .
O6 H6A 0.86(3) .
O6 H6B 0.86(3) .
O7 H7A 0.88(3) .
O7 H7B 0.85(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O2 0.86 2.02 2.878(5) 176 2_566
N3 H3 O1 0.86 2.02 2.874(5) 173 2_656
O3 H3A O7 0.88(4) 1.89(4) 2.767(5) 172(4) 1_555
O3 H3B O7 0.86(4) 1.87(4) 2.709(5) 164(5) 2_665
O4 H4A O1 0.86(4) 1.89(4) 2.738(5) 165(4) 1_555
O4 H4B O2 0.86(5) 2.00(5) 2.837(5) 166(5) 1_655
O5 H5A O1 0.86(4) 2.03(4) 2.874(5) 168(4) 2_656
O5 H5B O2 0.85(4) 1.85(4) 2.692(5) 170(4) 2_666
O6 H6A S 0.86(3) 2.48(4) 3.294(4) 160(4) 2_555
O6 H6B S 0.86(4) 2.61(4) 3.458(4) 170(4) 1_555
O7 H7A O4 0.89(4) 2.03(4) 2.828(5) 150(4) 2_766
O7 H7B O4 0.85(4) 1.84(4) 2.681(5) 168(5) 1_554
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C4 N3 C2 N1 0.7(5) . . . .
C4 N3 C2 S -177.7(3) . . . .
C6 N1 C2 N3 0.9(5) . . . .
C6 N1 C2 S 179.3(3) . . . .
C2 N3 C4 O1 177.0(3) . . . .
C2 N3 C4 C5 -2.6(5) . . . .
C2 N1 C6 O2 -179.3(3) . . . .
C2 N1 C6 C5 -0.5(5) . . . .
O1 C4 C5 C6 -176.6(3) . . . .
N3 C4 C5 C6 2.9(5) . . . .
O2 C6 C5 C4 177.2(3) . . . .
N1 C6 C5 C4 -1.5(5) . . . .
