Synthesis, characterization, crystal structures and anti-diabetic activity of organotin (IV) complexes with 2-(4-hydroxynaphthylazo)-benzoic acid
Debnath, Paresh; Singh, Keisham Surjit; Devi, Thokchom Sonia; Singh, S.Sureshkumar; Butcher, Ray J.; Sieroń, Lesław; Maniukiewicz, Waldemar; Inorganica Chimica Acta 510 (2020) 119736–; doi:10.1016/j.ica.2020.119736

data_1564216
_publ_section_title
;
 Synthesis, characterization, crystal structures and anti-diabetic
 activity of organotin (IV) complexes with
 2-(4-hydroxynaphthylazo)-benzoic acid
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119736
_journal_paper_doi               10.1016/j.ica.2020.119736
_journal_volume                  510
_journal_year                    2020
_chemical_formula_moiety         'C17 H11 N2 O3, C6 H16 N, 2(H2 O)'
_chemical_formula_sum            'C23 H31 N3 O5'
_chemical_formula_weight         429.51
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.894(2)
_cell_angle_beta                 90.498(2)
_cell_angle_gamma                91.519(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7854(3)
_cell_length_b                   13.5964(3)
_cell_length_c                   15.4929(3)
_cell_measurement_reflns_used    20169
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.954
_cell_measurement_theta_min      5.654
_cell_volume                     2204.41(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -12.00  14.00   0.50   10.00    --   -1.56  56.00-130.90   52
  2  \w     25.00  60.00   0.50   10.00    --   -1.56  56.00-130.90   70
  3  \w     28.00  58.00   0.50   10.00    --   -1.56  82.00 -97.33   60
  4  \w    -12.00  55.00   0.50   10.00    --   -1.56  57.00-180.00  134
  5  \w    -22.00  50.00   0.50   10.00    --   -1.56  82.00 -42.72  144
  6  \w    -14.00  46.00   0.50   10.00    --   -1.56  62.00  18.66  120
  7  \w     32.00  64.00   0.50   10.00    --   -1.56  14.00 107.24   64
  8  \w     -1.00  28.00   0.50   10.00    --   -1.56  14.00 107.24   58
  9  \w    -12.00  36.00   0.50   10.00    --   -1.56  57.00 150.00   96
 10  \w    -20.00  30.00   0.50   10.00    --   -1.56  77.00  60.00  100
 11  \w    -27.00  23.00   0.50   10.00    --   -1.56  92.00  85.45  100
 12  \w    -70.00  -1.00   0.50   10.00    --   -1.56  -9.00  24.66  138
 13  \w    -62.00  -2.00   0.50   10.00    --   -1.56  -5.00 146.30  120
 14  \w    -69.00  -8.00   0.50   10.00    --   -1.56  -4.00  97.05  122
 15  \w    -70.00  -1.00   0.50   10.00    --   -1.56  -9.00 -21.49  138
 16  \w    -42.00  -4.00   0.50   10.00    --   -1.56  -1.00-122.95   76
 17  \w    -71.00  -2.00   0.50   10.00    --   -1.56  -8.00-141.59  138
 18  \w    -67.00  -2.00   0.50   10.00    --   -1.56  -8.00 -53.93  130
 19  \w    -23.00  21.00   0.50   10.00    --   -1.56  82.00 -97.33   88
 20  \w    -32.00  -3.00   0.50   10.00    --   -1.56 100.00-124.77   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15398
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         15398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+0.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                13149
_reflns_number_total             15398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-510-119736.cif
_cod_data_source_block           ksp12
_cod_database_code               1564216
_oxdiff_exptl_absorpt_empirical_full_min 0.549
_oxdiff_exptl_absorpt_empirical_full_max 1.689
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;