Fabrication of egg shell-like nanovesicles from a thiocoumarin-based ε-amino ester: a potential carrier
Debnath, Mintu; Sasmal, Supriya; Haldar, Debasish; Journal of Materials Chemistry B 5 (2017) 5450–; doi:10.1039/C7TB00025A

data_7236683
_publ_section_title
;
 Fabrication of egg shell-like nanovesicles from a thiocoumarin-based
 \e-amino ester: a potential carrier
;
_journal_issue                   27
_journal_name_full               'Journal of Materials Chemistry B'
_journal_page_first              5450
_journal_paper_doi               10.1039/C7TB00025A
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C11 H9 N O3 S'
_chemical_formula_sum            'C11 H9 N O3 S'
_chemical_formula_weight         235.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.448(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7463(4)
_cell_length_b                   21.3406(11)
_cell_length_c                   7.0237(5)
_cell_measurement_reflns_used    1414
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.8900
_cell_measurement_theta_min      3.1080
_cell_volume                     983.48(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & C4apuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'C98 plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.908
_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    -17.00  31.00   1.00   22.50    --  -25.61 -99.00 -60.00   48
  2  \w    -61.00 113.00   1.00   22.50    --   27.09 -19.00-120.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1052615000
_diffrn_orient_matrix_UB_12      -0.0033453000
_diffrn_orient_matrix_UB_13      -0.0440656000
_diffrn_orient_matrix_UB_21      0.0173357000
_diffrn_orient_matrix_UB_22      0.0107453000
_diffrn_orient_matrix_UB_23      -0.0902696000
_diffrn_orient_matrix_UB_31      0.0175559000
_diffrn_orient_matrix_UB_32      -0.0312664000
_diffrn_orient_matrix_UB_33      -0.0263371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3032
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.261
_diffrn_reflns_theta_min         3.105
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray SourC7'
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.25879
_exptl_crystal_size_mid          0.236554
_exptl_crystal_size_min          0.1258
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.7391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1722
_reflns_number_total             1993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tb00025a2.cif
_cod_data_source_block           tcnh2
_cod_original_cell_volume        983.47(11)
_cod_database_code               7236683
_chemical_oxdiff_formula         'C H N O S'
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H4), C3(H9), C4(H8)
2.b Idealised Me refined as rotating group:
 CA(H1c,H1d,H1e)
2.c Idealised tetrahedral OH refined as rotating group:
 N1(H1a)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-15
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.439
_oxdiff_exptl_absorpt_empirical_full_min 0.753