Reaction of pharmacological active tris-(2-hydroxyethyl)ammonium 4-chlorophenylsulfanylacetate with ZnCl2 or NiCl2: First conversion of a protic ionic liquid into metallated ionic liquid
Adamovich, S. N.; Mirskova, A. N.; Mirskov, R. G.; Schilde, Uwe; Chemistry Central Journal 7 (2013) 34–; doi:10.1186/1752-153X-7-34

data_1547206
_publ_section_title
;
 Reaction of pharmacological active tris-(2-hydroxyethyl)ammonium
 4-chlorophenylsulfanylacetate with ZnCl2 or NiCl2: First conversion of a
 protic ionic liquid into metallated ionic liquid
;
_journal_name_full               'Chemistry Central Journal'
_journal_page_first              34
_journal_paper_doi               10.1186/1752-153X-7-34
_journal_volume                  7
_journal_year                    2013
_chemical_formula_moiety         '(C12 H30 N2 Ni O6(2+), 2(C8 H6 Cl O2 S)(+)'
_chemical_formula_sum            'C28 H42 Cl2 N2 Ni O10 S2'
_chemical_formula_weight         760.37
_chemical_melting_point          449
_chemical_name_systematic
; 
 Bis[tris(2-hydroxyethyl)amine]-nickel(II)-
 bis-[(4-chlorophenylsulfanyl)acetate] 
;
_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
_cell_angle_alpha                81.034(8)
_cell_angle_beta                 77.830(8)
_cell_angle_gamma                73.120(8)
_cell_formula_units_Z            1
_cell_length_a                   8.0020(8)
_cell_length_b                   9.4980(10)
_cell_length_c                   11.6401(12)
_cell_measurement_reflns_used    7875
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      1.80
_cell_volume                     823.29(15)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_molecular_graphics
;
 DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
 180 frames, detector distance = 140 mm, t = 6 min
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, 1.0 \%'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5252
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0045(13)
_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   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                2201
_reflns_number_total             2714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            13065_2012_579_MOESM1_ESM.cif
_cod_data_source_block           mir2
_cod_database_code               1547206