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_1564215
_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_absolute_configuration ad
_chemical_formula_moiety         'C29 H38 N2 O3 Sn [+ solvent]'
_chemical_formula_sum            'C29 H38 N2 O3 Sn'
_chemical_formula_weight         581.32
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   38.4630(3)
_cell_length_b                   38.4630(3)
_cell_length_c                   10.2363(1)
_cell_measurement_reflns_used    134965
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.995
_cell_measurement_theta_min      2.946
_cell_volume                     13114.75(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_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    -27.00  15.00   0.50    4.00    --   -1.56  92.00  75.00   84
  2  \w    -12.00  66.00   0.50    4.00    --   -1.56  57.00  60.00  156
  3  \w     44.00  69.00   0.50    4.00    --   -1.56  13.00 133.97   50
  4  \w     34.00  62.00   0.50    4.00    --   -1.56  15.00 179.47   56
  5  \w     -1.00  25.00   0.50    4.00    --   -1.56  13.00 133.97   52
  6  \w      0.00  51.00   0.50    4.00    --   -1.56  19.00 150.00  102
  7  \w     -1.00  30.00   0.50    4.00    --   -1.56  15.00 179.47   62
  8  \w    -22.00  28.00   0.50    4.00    --   -1.56 -99.00  60.00  100
  9  \w    -32.00  24.00   0.50    4.00    --   -1.56 -92.00 -37.00  112
 10  \w    -40.00  -1.00   0.50    4.00    --   -1.56 -11.00 -61.11   78
 11  \w      2.00  42.00   0.50    4.00    --   -1.56  11.00  -6.60   80
 12  \w     42.00  67.00   0.50    4.00    --   -1.56  57.00 -30.00   50
 13  \w     -3.00  70.00   0.50    4.00    --   -1.56  12.00  38.40  146
 14  \w     -4.00  57.00   0.50    4.00    --   -1.56  34.00 -75.47  122
 15  \w     17.00  43.00   0.50    4.00    --   -1.56  57.00-180.00   52
 16  \w    -12.00  14.00   0.50    4.00    --   -1.56  57.00-180.00   52
 17  \w    -11.00  42.00   0.50    4.00    --   -1.56  54.00-153.38  106
 18  \w    -12.00  19.00   0.50    4.00    --   -1.56  57.00 -30.00   62
 19  \w    -33.00  -8.00   0.50    4.00    --   -1.56 102.00-159.36   50
 20  \w    -63.00  -1.00   0.50    4.00    --   -1.56  -7.00-131.93  124
 21  \w    -63.00  -2.00   0.50    4.00    --   -1.56  -6.00 -14.56  122
 22  \w    -70.00  -1.00   0.50    4.00    --   -1.56 -10.00  68.86  138
 23  \w    -51.00  -1.00   0.50    4.00    --   -1.56 -10.00 118.77  100
;
_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_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            131510
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 2548 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+11.5274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0343
_reflns_number_gt                5141
_reflns_number_total             5150
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2020-510-119736.cif
_cod_data_source_block           ksp7_sq
_cod_original_cell_volume        13114.8(3)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               1564215
_exptl_absorpt_empirical_full_min 0.825
_exptl_absorpt_empirical_full_max 1.424
_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;