Crystalline products of tolbutamide decomposition in water after microwave treatment
Drebushchak, Tatiana N.; Pankrushina, Natalia A.; Mikheev, Aleksandr N.; Thumm, Manfred K. A.; CrystEngComm 15 (2013) 3582–; doi:10.1039/c3ce40145f

data_7209772
_publ_section_title
;
 Crystalline products of tolbutamide decomposition in water after
 microwave treatment
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3582
_journal_paper_doi               10.1039/c3ce40145f
_journal_volume                  15
_journal_year                    2013
_chemical_compound_source
;
Starting reagent was purchased from SIGMA
;
_chemical_formula_moiety         'C4 H12 N +, C12 H17 N2 O3 S -'
_chemical_formula_sum            'C16 H29 N3 O3 S'
_chemical_formula_weight         343.48
_chemical_name_common            'n-butylammoniun salt of tolbutamide'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.694(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5031(6)
_cell_length_b                   11.2985(5)
_cell_length_c                   25.4543(12)
_cell_measurement_reflns_used    4754
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2275
_cell_measurement_theta_min      3.0187
_cell_volume                     3838.8(3)
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18001
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_preparation
;
Microwave treatment of hot water-tolbutamide suspension
;
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7821
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0476P)^2^+4.1860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                5534
_reflns_number_total             7821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40145f.txt
_cod_data_source_block           TBAsalt
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7209772