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)
Golovnev, Nikolay; Molokeev, Maxim; Vereshchagin, Sergey; Atuchin, Victor; Sidorenko, Maxim; Dmitrushkov, Michael; Polyhedron 70 (2014) 71–; doi:10.1016/j.poly.2013.12.021

data_1529226
_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       '\f and \w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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